book chapter

Chapter: 2D MXene—The New Frontier in

2D Materials
Abstract

MXenes are a class of two-dimensional transition metal carbides and nitrides that have been
experiencing a rise in popularity ever since the isolation of titanium carbide (Ti3C2Tx) in the year
2011. The unique combination of metallic conductivity (up to 24,000 S/cm) and natural
hydrophilicity that they possess is what separates them from other materials. As a matter of fact,
this chapter offers an in-depth review of the "post-graphene" era, with special emphasis on the ways
in which MXenes have the potential to overcome the ethanolic and volumetric limits of
conventional two-dimensional materials. This is achieved by permitting aqueous-based processing
and energy storage at high densities.

The paradigm shifts which took place between the years 2020 and 2025 are receiving a lot of
attention, particularly the substitution of the risky process of hydrofluoric acid (HF) etching with
fluoride-free synthesis methods that are more ecologically friendly. The following is a list of some
of the most important discoveries that have been made that are discussed in this paper:Use of
Protocols towards Green Synthesis: In the year 2024, an experiment of Lewis acidic molten salt
etching is expected to take place. This strategy has the dual advantage of removing risky HF and
enables for the precise design of surface terminations (for example, –Cl and –Br).

The use of Machine Learning (ML) approaches to predict with a high degree of confidence the
stability of ordered double transition-metal MXenes (for example, Mo₂TiC₂), which may
subsequently be tuned for hydrogen storage, is an example of AI-Accelerated
[Link]-Breaking Achievements: the launch of nitrogen-doped Mo₂CTₓ with metal-like
conductivities (>22,000 S/cm) and MXene aerogels that are accustomed to enduring a compressive
strain of 90%, making these flexible electronics extraordinarily [Link] in
biomedicine comprise the creation of mediator-free biosensors that have an extremely high level of
sensitivity. An instance of this is a clinical SARS-CoV-2 sensor that has exceeded a detection limit
of 0.4 aM.

This study discusses MXene as a material engineering structure for 6G wireless communication,
wearable engineered kidneys, and sustainable energy conversion. It also relates these breakthroughs
in synthesis to the achievement of excellent functional properties, such as shielding against
electromagnetic interference (EMI) with a strength of more than 90 decibels and volumetric
capacitances of more than 1,500 farads per cubic centimetre.
1. Introduction

1.1 The Rise of the "Flatland": A Brief History of 2D Materials

Transition​‍​‌ metals are known as very interesting materials, essentially because their open d-orbitals
make spin properties and various oxidation states quite unique and puzzling. Thus, they constitute a
very promising base for extremely thin nanomaterial research. In fact, the bulk transition metal
carbides (referring to metals from Groups 4–6) of the early 20th century were only noted for their
extreme hardness and chemical stability, among other things, which led them to be successfully used
in catalysis and energy storage . Everything was changed in 2011 with the finding of Ti3C2TX. This
was definitely the very first 2D transition metal carbide, and therefore its isolation triggered an
entirely new family of layered materials – nowadays called MXenes [1]. The serious interest in
two-dimensional (2D) materials—also known as the "single-layer revolution"—started to gain
momentum in 2004 when Andre Geim and Konstantin Novoselov from the University of Manchester
managed to extract graphene from bulk graphite by means of the so-called Scotch tape method. Apart
from receiving the Nobel Prize in Physics in 2010 for this discovery, the duo also revealed a material
that could be electrically, thermally, and mechanically extremely well-conducting and whose
existence only factually disproved the long-standing scientific conviction that purely 2D crystals are
thermodynamically unstable.
The so-called "Graphene Era" sparked a rush all around the world to discover additional materials
that are atomically thin. Following the discovery of graphene, scientists made the discovery of
hexagonal boron nitride (h-BN), which is commonly known as "white graphene" due to its insulating
qualities [2]. Subsequently were the Transition Metal Dichalcogenides (TMDs), e.g., Molybdenum
Disulfide (MoS2), which had the unique feature of a tunable bandgap offering more options than
graphene in this respect. Phosphorene, which is also known as black phosphorus, was the following
member of that family among those compounds. It possessed a high carrier mobility, but according to
the literature, its exposure to air might result in a quick loss of its properties.
Nevertheless, the problem of a suitable material that could at the same time provide metallic
conductivity (like graphene) and hydrophilicity (water solubility/processability) was still unsolved .
Surprisingly, this void was successfully bridged at Drexel University by the discovery of MXenes by
Yury Gogotsi and Michel Barsoum in 2011, having their contribution marking the opening of the
giant new field of 2D materials science ​‍‌.

1.2 Enter MXenes: The New Frontier

MXenes​‍​‌ (pronounced "max-enes") refer to one of the largest groups of 2D transition metal carbides,
nitrides, and carbonitrides to date [3]. They are obtained from their 3D precursors, the MAX
phases—ternary layered carbides and nitrides—by selective etching of the "A" layer (usually an
element from groups 13 or 14, such as aluminium) [3]. In most cases, the formula for MXenes is as
follows: Mn+1XnTx, M is an early transition metal, such as titanium, molybdenum, vanadium, or
niobium [4], ‘X’ is Carbon (C) and/or Nitrogen (N) [5] ‘n’ is an integer normally 1, 2, or 3 (which
corresponds to the M2X, M3X2, or M4X3 type structures) [6] ,Tx are the surface functional groups
(terminations) such as -OH, -O, -F, or -Cl, which are the natural surface groups of MXenes coming
from the synthesis process [7].
Mxene with the most titanium carbide (Ti3C2Tx) has been the first ever synthesized and is now the
most famous material of this type. Still, the family has developed quickly and includes dozens of
experimentally synthesized compositions and more than 100 theoretically predicted ​‍‌structures.

1.3 Why MXene is Superior: The Comparative Advantage

In spite of the fact that graphene is sometimes called out as the "wonder material" of the 21st century,
it is actually plagued by major drawbacks in the areas of volumetric performance and practical
processing [8]. MXenes have come out as an ideal option in some domains due to the offer an
innovative combination of traits that neither graphene nor transition metal dichalcogenides (TMDs)
can satisfy. Graphene independently fails to match with the properties of MXenes. This section
presents a synopsis of the specific advantages that MXenes possess in comparison to other 2D
families.

1.3.1 Metallic Conductivity Meets Hydrophilicity

The most important benefit of MXenes is their peculiar duality, which is that they exhibit the metallic
electrical conductivity of transition metals while at the same time the hydrophilicity of clays is
exhibited by them. The negative aspect of graphene is that it is naturally hydrophobic, which makes it
so it can be seriously complex to disperse it into aqueous solutions without the use of surfactants or
vigorous oxidation (as in graphene oxide), both of which greatly damage its conductive π-network.
Advantages of MXene: Because MXenes have a large number of surface terminations (-OH, -O, and
-F), they can be combined with water to produce a stable colloidal solution without the addition of
any additives. The most recent research indicates that even solution-processed Ti3C2T3 films are
capable of having conductivities that are greater than 20,000 S/cm. This is a value that is far higher
than that of solution-processed graphene or TMDs [9-10].
This makes it possible to generate inks for printable electronics in an environmentally benign manner,
that is, by utilising water as a solvent. This is something that is now difficult to do with graphene in
its purest form.
1.3.2 Superior Volumetric Capacitance

At the present time, energy storage systems in tiny devices, such as smartphones, wearable
electronics, implantable medical devices, and electric cars, have a very limited amount of space
available for energy storage. The volumetric capacitance, which is the amount of energy stored per
unit volume, is far more significant than the gravimetric capacitance, which is the amount of energy
stored per unit mass. This is because the volumetric capacitance is a measure of the amount of
energy that is stored per unit volume. In the case of real-world devices, for instance, a material may
be lightweight and have excellent gravimetric performance; yet, if it is unable to store sufficient
energy in a restricted amount of area, it may still fail to achieve the expectations that are typically
associated with such materials.

It is mostly due to the intrinsic density and packing efficiency of MXenes that they are able to
achieve such a high volumetric capacitance. This is the fundamental factor that determines the
magnitude of this capacitance. Graphene, carbon nanotubes (CNTs), and graphene aerogels are all
examples of nanomaterials that are based on carbon.. These nanomaterials are primarily dependent
on electric double-layer capacitance and have structures that are extremely porous and low density.
In spite of the fact that this porosity is advantageous for ion accessibility, it results in inferior
packing densities, which are typically lower than 1 g cm-3 in most cases. Consequently, there is a
significant limitation placed on the quantity of active material that may be packed into a particular
volume.

MXenes, on the other hand, are made up of layers of heavy transition-metal carbide or nitride,
which gives them a significantly greater intrinsic density of approximately 4 grammes per cubic
centimetre when they are operating at room temperature. This is because MXenes are formed of
layers of heavy transition-metal carbide or nitride. Due to the fact that MXene flakes have a
compact lamellar structure, it is much simpler for them to pack together in close proximity together.
In spite of this, the interlayer gap or surface terminations that are connected with the structure do
not impede the movement of ions inside the structure. Therefore, it is possible to contain an even
bigger quantity of electrochemically active material while yet maintaining the same volume of the
device. MXenes, in addition to their high density, possess the ability to store charge through a
combination of electric double-layer capacitance and quick surface redox processes. This
phenomenon, which is known as pseudocapacitance, is a result of the combination of these two
processes. The very high charge accumulation that is possible with this simultaneous
two-component charge-storage approach is achieved without compromising the rate capabilities.
The volumetric capacitances of MXene electrodes can be achieved within the range of 1,500–2,368
F cm-3, which is almost ten times larger than the ones of graphene aerogels, which are typically
limited to around 300 F cm-3. This is according to latest experimental data that has been presented.
There is a significant difference in performance between these two devices, which immediately
contributes to the energy storage devices being more compact, thinner, and more powerful.

Therefore, MXenes can be considered the most important material platform when it comes to
miniaturised supercapacitors. This is because It is vital to store the greatest amount of energy in the
smallest possible size, and ordinary carbon-based materials have already hit their fundamental
volumetric limitations. This is the reason why this is the case.

1.3.3 Unmatched Electromagnetic Interference (EMI) Shielding Effectiveness

A measurement of how well a material can filter or weaken electromagnetic radiation that is not
expressly wanted is referred to as electromagnetic interference shielding (EMI shielding). EMI
shielding is also known as electromagnetic interference shielding. This particular form of radiation
has the ability to interfere with the typical functioning of electrical devices if there is no effective
shielding in place protecting them. By and large, electromagnetic interference (EMI) shielding can
be accomplished in two distinct ways: either through reflection (as is the case with metals) or
through absorption (as is the case with carbon-based materials like carbon black or graphene
composites) [11].

Due to the fact that they contain both the mechanisms of reflection and absorption inside a single
material, MXenes are able to provide exceptional electromagnetic interference (EMI) shielding
capabilities. As is the case with conventional metals, the metallic conductivity of these materials
enables them to reflect electromagnetic waves that are incident upon them in an extremely effective
manner. Their layered structure of two-dimensional lamellae, on the other hand, ensures that they
are able to absorb electromagnetic radiation in a very efficient manner. The numerous internal
reflection mechanism that MXenes are capable of achieving is one of the most significant
advantages that they possess. It is possible to build various interfaces within the material by
stacking MXene nanosheets endpoint against one another. The electromagnetic waves that impact
the MXene film are reflected back and forth between these layers several times. This occurs when
the waves strike the film. As a result, the energy is continuously spread and weakened at the same
time. Not only does this "wave-trapping" effect result in a huge improvement in the shielding
performance, but it also makes it possible to use materials that are on the extremely thin side. To put
it another way, even films made of MXene that are only a few microns thick can have a shielding
efficiency that is greater than 90 decibels. The amount of electromagnetic radiation that is allowed
to pass through at this level of shielding is less than 0.0001% of the total electromagnetic radiation
that is incident. In the meantime, in order to achieve such shielding levels, the thickness of discs or
polymer–carbon composites would need to be measured in millimetres. This would result in these
materials being heavier, less flexible, and more difficult to incorporate into designs for compact
devices [12].

As a result, MXenes offer a distinct advantage for the next generation of electronic devices,
particularly for those products that require features that save space and are [Link]
technology, flexible electronics, aeronautical systems, and high-frequency 5G/6G communication
technologies are all examples of the types of equipment that fall into this category.
1.3.4 Compositional Tunability

Among the many benefits that MXenes possess in comparison to other two-dimensional materials,
one of the most important advantages is the amazing compositional tunability that they bring to the
table. MXenes have a structure that is chemically flexible and can be created atomically, essentially
layer by layer without changing their structure. On the other hand, graphene is constructed only of
carbon atoms arranged in a honeycomb lattice, and hexagonal boron nitride is characterised by a
rigid B–N framework. Both of these materials are in contrast to graphene.

The basic formula for MXenes is Mn+1XnTx, where M is an early transition metal (such as Ti, V, Nb,
or Mo), X is either carbon or nitrogen, n denotes the number of atomic layers, and TX represents the
surface terminations (–O, –OH, –F, –Cl). Examples of an early transition metal include Ti, V, Nb,
and Mo. Researchers have the ability to fine-tune parts of the MXene that is formed by the process
of individually adjusting the M element, the X species, and the layer thickness. These aspects
include the band structure, the density of carriers, magnetic properties, and electrochemical
behaviour of the MXene. The type of transition metal is responsible for determining a major
amount of the d-orbital configuration. This, in turn, is responsible for determining the conductivity,
redox activity, and work function of the material. As an additional point of interest, switching
between C and N can change the bond strength and electron localisation, whereas changing n can
have an effect on quantum confinement and layer interaction. An accomplishment that is
fundamentally unattainable in binary two-dimensional materials such as graphene or boron nitride
is the ability of MXenes to have properties that range from those of metals to those of
semiconductors. This is because MXenes can be shaped in such a broad variety of ways.

During the year 2025, research was conducted to further refine this tunability by developing double
transition-metal MXenes. One example of such a material is Mo2TiC2TX, which is characterised by
the presence of distinct metal atoms that occupy various atomic layers in an ordered position. This
particular kind of out-of-plane ordering makes it possible to selectively regulate charge transfer, ion
intercalation routes, and areas of catalytic activity. At the same time, high-entropy MXenes have
been recognised as a novel form of material that demonstrates synergistic electronic effects,
increased structural stability, and customisable electrochemical responses. Different transition
metals are arranged in the same lattice to form these MXenes, which are made of these transition
metals. MXenes have achieved a level of atomic-scale design control that is comparable to that of
Lego as a result of the combination of all of these variables combined together. Researchers are able
to effectively create materials one layer at a time with features already built in because to this
capability. When compared to traditional 2D materials, MXenes are distinguished by an exceptional
degree of compositional freedom. This transforms MXenes into a highly versatile platform that may
be utilised for the development of revolutionary applications in the realms of energy storage,
sensing, and the production of electronic devices [13].

Table 1: Property-Based Comparison of Representative 2D Materials

Property Graphene TMDs (e.g., MoS2) MXene (Ti3C2Tx)

Conductivity High (in pristine Low High (Metallic)

form) (Semiconducting)

Water Dispersibility Poor (Hydrophobic) Poor Excellent (Hydrophilic)

Volumetric Low (~300 F/cm³) Medium Ultra-High (>1500

Capacitance F/cm³)

Processing Method Toxic organic CVD / Exfoliation Aqueous/Green solvents

solvents

EMI Shielding Moderate (~20-40 Low Superior (>90 dB)

dB)

2. Synthesis: From Hazardous to Sustainable

2.1 Synthesis of MXenes

When it comes to MXenes, the method of synthesis that is used is an essential factor in defining
elements such as their electrical conductivity, physicochemical behaviour, structural stability, and
ultimately their potential for [Link] etching-based methods, top-down approaches, and
bottom-up approaches are the three basic categories that may be used to classify the MXene synthesis
processes that are now in use. The top-down etching strategy is still the one that is utilised the most
frequently [1]. MXenes are often produced from their parent MAX phases, which have the chemical
formula Mn+1AXn (n = 1, 2, 3). In most cases, MXenes are produced from their matrix. In the MAX
phase family, MXenes are considered to be a member. Through the process of selectively removing
the "A" element from the layered MAX phase, it is feasible to build two-dimensional MXene
structures using the generic formula MnXn-1 (n = 2, 3, and 4). This element is commonly a group IIIA
or IVA element. During this process, M is a representation of an early transition metal, and X is a
representation of either carbon or nitrogen simultaneously. As a result of the selective extraction of
the A-layer, the three-dimensional bonding network is weakened, and stacked MX layers are exposed.
This leads to the creation of MXenes that have a preserved hexagonal lattice rather than a cubic
structure.
MAX phases are composed of M–X octahedra in terms of their structural composition. In these
phases, X atoms occupy the centres of octahedral cages that are created by M atoms, and they share
edges within the lattice. In the event that the A atoms are removed, the ensuing M X ₋₁ layers are
not altered in any way. They continue to display strong in-plane M–X bonds, despite the fact that
their interlayer interactions are less. By undergoing this structural transition, it is feasible to produce
MXene sheets that are thin and aligned horizontally. The structural stability and mechanical durability
of these sheets are a direct outcome of the fact that they inherit many of the robust mechanical
properties that were present in the MAX phases that inspired them.
The top-down technique, which frequently involves chemical etching of MAX phases, has been the
most thoroughly explored of the many different synthesis routes. This is due to the fact that it is
compatible with a wide variety of MAX precursors, is scalable, and is reliable. In spite of the fact that
it frequently calls for a somewhat significant quantity of precursor material, this technique makes it
possible to manufacture multilayer MXenes with thickness and surface chemistry that can be well
controlled.
The bottom-up synthesis method, on the other hand, is a technique which calls for the fabrication of
MXene structures right from individual atoms or small organic/inorganic molecule precursors by
using the help of controlled crystal growth mechanisms. This technique is distinct from top-down
synthesis. This method is based on the bottom-up synthesis strategy. Although bottom-up synthesis is
less well-established in comparison to top-down procedures, it offers higher control over size
distribution, morphology, crystallinity, and surface terminal functions. Bottom-up synthesis is better
than top-down approaches. It is possible to construct MXenes with surface chemistry and structural
order that are suited to your specifications by precisely adjusting the growing circumstances. Because
of this, it is possible to engineer MXenes with these characteristics, which is especially useful for
complicated applications in the fields of electrical and optoelectronics. It is an attractive method for
the development of MXene in the future since it requires fewer precursor elements and permits the
production of two-dimensional designs at the atomic level. This approach is an intriguing strategy for
the development of MXene.
Over the course of its development, the synthesis of MXenes has resulted in a significant expansion
of the structural and compositional variety of MXenes. The change from traditional top-down
strategies that are centred on etching to the development of bottom-up fabrication processes is the
cause of this phenomenon. It is absolutely necessary to continue optimising these synthesis
techniques in order to achieve higher functional features, precise structural control, and
manufacturing that can be taken to a larger scale. This will make it possible for MXenes to be
incorporated into next-generation technologies in a more widespread manner, particularly in the areas
of energy, electronics, and green technology.

2.1.1 Top-Down Synthesis Strategies for MXenes

After the initial successful conversion of Ti3AlC2 into Ti3C2Tx, the top-down synthesis method has
emerged as the most dependable and commonly utilised method for the production of MXenes. It is
possible to obtain two-dimensional MXene sheets by this method, which involves selectively etching
bulk layered precursors in order to remove the A-layer from Mn+1AXn phases. Mechanical exfoliation
is ineffective due to the increased strength of the M–A metallic connection in comparison to van der
Waals interactions. Instead, chemical or electrochemical etching is required to get the desired results.
All of the flake size, defect density, surface terminations, and finally the physicochemical features of
MXenes are directly governed by the etching approach, intercalation strategy, and delamination
conditions that are selected.
The use of top-down techniques, which are well-established in the field of nanomaterial synthesis,
has proven successful in the synthesis of a wide variety of bulk precursors. These bulk precursors
include graphite, MoS2, WS2, black phosphorus, and g-C3N4. Ball milling, ultrasonication, liquid
exfoliation, chemical and electrochemical etching, hydrothermal and solvothermal treatments,
microwave irradiation, and intercalation are some of the methodological approaches that are
frequently utilised. It is possible that these methods have low yields or require post-treatments, but
they are scalable, operate at temperatures that are relatively low, and allow for the utilisation of
plentiful raw materials. HF etching, in-situ HF-forming etchants, molten-salt etching, alkaline
etching, electrochemical etching, and hydrothermal/solvothermal techniques are the top-down ways
that are considered to be the most important etching methods for MXenes.

[Link] HF-Based Chemical Etching

Direct HF etching continues to be the approach that is utilised the most frequently for the synthesis of
carbide MXenes. This process involves the selective removal of aluminium from MAX phases while
ensuring that the M–X bonds are not affected in any way. Etching for Ti3AlC2 is commonly
performed in HF containing fifty percent by weight at room temperature for a duration of two hours.
This is followed by repeated washing until the pH reaches about six. The release of hydrogen gas is
the outcome of the simultaneous introduction of surface terminations such as –F, –OH, and –O. While
raising the concentration of HF makes the etching process go more quickly, it also makes the fault
density more difficult to detect. MAX phases that are thinner, such as M2AX, require shorter etching
periods compared to M3AX2 and M4AX3 phases, which are thicker. Alhabeb et al. revealed that
etching periods of 24 hours, 18 hours, and 5 hours, respectively, are sufficient to remove aluminium
at concentrations of 5, 10, and 30 weight percent of hydrogen peroxide. When the concentration of
HF is higher, accordion-like morphologies are produced as a result of strong H2 evolution. On the
other hand, when the concentration is lower, structures that are closer to the parent MAX phase are
preserved. Furthermore, using the techniques of HF etching has made it possible to create more
complicated MXenes, such Mo4VC4TX and (V1−xTiX)2C. Additionally, it has permitted the production
of MXenes that are made from non-Al MAX phases, such as Ti3SiC2 and Mo2GaC, by applying
oxidation-assisted or fluoride-containing methods. This is despite the fact that in spite of
morphological differences, all concentrations are effective in removing Al.
The following reactions are significant events that take place during the HF etching of Ti3AlC2:

Ti3AlC2 + 3HF → Ti3C2 + AlF3 + 3/2 H2​

Ti3C2 + 2HF → Ti3C2F2 + H2​
Ti3C2 + 2H2O → Ti3C2(OH)2 + H2
[Link] In-Situ HF-Forming Etchants
Through the reaction of fluoride salts with strong acids, it is possible to create HF in situ, which can
increase both the safety and the quality of the flake. While simultaneously intercalating cations across
MXene layers, systems such as LiF/HCl, NaF/HCl, NH4F/HCl, and FeF3/HCl each create HF in a
progressive manner. Lamination into large flakes with low defects is made easier as a result of this
reduction in interlayer coupling. An investigation conducted by Ghidiu and colleagues showed usage
of LiF/HCl etching leads to the synthesis of a clay-like Ti3C2Tx. The exfoliation process is simplified
by this material, which also demonstrates improved interlayer spacing. An increase in the ratio of
LiF:Ti3AlC2 to 7.5:1 (using the MILD technique) enables delamination through the utilisation of
simple hand shaking, which ultimately leads to the fabrication of nanosheets with conductivities that
can reach up to 4600 ± 1100 S cm-.

LiF + HCl → HF + LiCl​

NH4F + H2O → NH3·H2O + HF

Among the reactions that are representative are the following: Despite the fact that this technique
enhances flake quality and safety, residual intercalated cations may have an effect on the behaviour of
chemicals and electronics.

[Link] Molten-Salt and Lewis-Acidic Etching

Molten salt etching makes it possible to produce MXenes that are difficult or even impossible to get
by aqueous high-frequency (HF) techniques. This is especially true for nitride MXenes at this point.
Following a thirty-minute period, the synthesis of Ti4N3Tx occurs as a result of the selective
elimination of Al from Ti4AlN3 by a mixture of LiF, NaF, and KF that is heated to 550 degrees
Celsius under Ar. Nevertheless, additional washing and delamination procedures are necessary, and
the MXenes that are produced as a result frequently exhibit reduced crystallinity and higher defect
densities of defects.
There is an alternate process that is based on redox-driven element replacement that is provided by
Lewis-acidic molten salts such as ZnCl2, for example. Zn momentarily occupies the A-site to create
Ti3ZnC2 when Ti3AlC2 is heated with ZnCl2 at 550 degrees Celsius for five hours. This causes Al to
be oxidised to volatile AlCl3, which has a boiling point of 178 degrees Celsius. A further reaction
with a surplus of ZnCl2 results in the synthesis of the Cl-terminated Ti3Cl2Cl2 MXene chemical
compound. Some of the more notable reactions are as follows:

Ti3AlC2 + 1.5ZnCl2 → Ti3C2 + 1.5Zn + AlCl3↑​

Ti3C2 + 2Cl- → Ti3C2Cl2 + 2e-
Through the utilisation of FeCl2, CoCl2, NiCl2, CuCl2, and various other salts that are connected to it,
this technology has been extended to cover other MAX phases. The redox-potential criteria of A-site
elements have been utilised to lead this technique.

[Link] Alkaline and Electrochemical Etching

A fluorine-free alternative can be accomplished by the use of alkaline etching, which can be carried
out with either sodium hydroxide or potassium hydroxide. By utilising this method, the aluminium
was dissolved as Al(OH)4-. In general, thorough etching necessitates the application of severe
conditions, such as a temperature of 270 degrees Celsius and a concentration of 27.5 M NaOH. This
procedure is modelled after the Bayer process. This leads to the formation of Ti3C2Tx that has a
significant number of –O and –OH terminations. It is necessary to exercise stringent control in order
to prevent oxidation or phase change, regardless the fact that it is environmentally friendly.
The electrochemical etching process completely avoids the use of hydrogen fluoride (HF) and instead
depends on the anodic dissolution of aluminium in electrolytes that contain chloride or hydroxide.
Later tactics that used NH4Cl/TMAOH electrolytes at +5 V were able to achieve etching in less than
five hours and produce huge MXene sheets. Earlier attempts had produced modest MXene fractions.
The following is an example of a reaction:
Ti3AlC2 − 3e- + 3Cl- → Ti3C2 + AlCl3
Although electrochemical methods are safer, they typically require complicated setups and variable
yields than other approaches.

[Link] Hydrothermal and Solvothermal Routes

Increased temperature and pressure (usually between 100 and 180 degrees Celsius, pH 6 and 9) are
utilised in hydrothermal synthesis in order to customise the size, thickness, and surface chemistry of
MXene. When the temperature of Ti3C2 is raised from 100 to 150 degrees Celsius, the average
particle diameter increases from 2.9 to 6.2 nanometres, while the monolayer thickness remains the
same (about 0.9 to 1.0 nanometres). Amorphous structures are formed as a result of over-etching
when temperatures are elevated to an extreme degree. It is possible to exert a greater degree of control
over the crystallinity and particle size of the final product by the utilisation of organic solvents in
place of water in solvothermal procedures. At a temperature of 150 degrees Celsius for a period of
eight hours, quantum dots that are composed of Ti3C2 filled with nitrogen have been produced. About
6.2 nanometres is the average diameter of these quantum dots, and about 1 nanometre is the average
thickness of these quantum dots. On the other hand, carbon quantum dot byproducts can be produced
from organic solvent chemicals.

Table: Comparison of Top-Down MXene Fabrication Strategies

Method Typical Key Reactions / Advantages Limitations

Conditions Features
 HF etching 5–50 wt% HF, Al → AlF3, High yield, Hazardous
RT–40°C, H₂ evolution universal HF, defects
2–90 h

In-situ HF LiF:HCl, HF generated in Safer, large Residual

(LiF/HCl) RT–40 °C situ,Li⁺ flakes cations
intercalation

Molten 550°C, Ar, 30 Al removal from Enables High energy,

fluoride salts min nitrides nitride defects
MXenes

Lewis-acidic ZnCl2 at 550 Al → AlCl3↑, HF-free, High

salts °C, 5 h Cl terminations tunable temperature
terminations

Alkaline 27.5M NaOH, Al → Al(OH)4- Fluorine-free Harsh

etching 270 °C conditions

Electrochemic +0.6 to +5 V, Anodic Al Safer, F-free Variable

al 5 h–5 d dissolution yield

Hydrothermal 100–180°C, Size-controlled Tunable Limited

pH 6–9 MXenes/QDs morphology scalability

Solvothermal 150°C, Doped MXene Precise control CQD

organic QDs byproducts
solvents

2.1.2 Bottom-Up Approaches for MXene and MXene-Like Materials

Bottom-up synthesis relies on assembling two-dimensional transition-metal carbides and nitrides
directly from molecular or atomic precursors rather than exfoliating bulk solids. Compared with
top-down etching, these approaches generally deliver materials with higher crystalline quality, fewer
structural defects, and better control over thickness, lateral size, and composition. Techniques such as
chemical vapor deposition (CVD), template-assisted synthesis, plasma-enhanced pulsed laser
deposition (PEPLD), molten-salt synthesis, and pyrolysis have therefore emerged as powerful routes
for preparing MXene-like materials and MXene quantum dots (MQDs), although their scalability and
cost remain key challenges.
[Link] Chemical Vapor Deposition (CVD)

CVD has been widely adopted for the large-area growth of graphene and transition-metal
dichalcogenides and has proven equally effective for producing ultrathin transition-metal carbides
and nitrides with superior crystallinity. In a pioneering study, ultrathin 2D Mo₂C crystals were grown
by placing an ultrathin Cu foil on a Mo foil and heating the system to 1085 °C under H₂. At this
temperature, Cu melts and serves simultaneously as a catalyst for CH₄ decomposition, a diffusion
medium for Mo atoms, and a sacrificial transfer layer. Carbon supplied from CH₄ reacts with Mo at
the Cu surface to form Mo₂C, and the large reactivity contrast between Cu and Mo₂C enables facile
transfer by Cu etching. Growth time and temperature directly control Mo₂C thickness, nucleation
density, and lateral size.
Methane concentration plays a decisive role in crystal morphology. At a low CH₄ flow rate of 0.1
sccm, fractal Mo₂C crystals form, whereas higher CH₄ flows of 0.3, 0.4, and 0.6 sccm yield
rectangular, pentagonal, and hexagonal crystals, respectively, due to increasing carbon
supersaturation. Notably, hexagonal Mo₂C exhibits a hexagonal structure rather than the
orthorhombic phase previously reported. The crystal thickness can also be tuned by adjusting the Cu
foil thickness.
CVD has also enabled nitride and boride growth. TaN thin films were synthesized at 1077 °C using
NH₃ as the nitrogen source on Ti/Cu foils, while replacing NH₃ with boron powder produced TaB
under similar conditions. Monoatomic ReC crystals were grown on Re(0001) substrates using C₂H₄ as
the carbon source. Graphene initially formed at 903 K, then decomposed into carbon atoms upon
annealing between 953 K and 1130 K, which dissolved into Re to form ReC. Vertical heterostructures
such as graphene/α-Mo₂C were fabricated by sequential growth at 1070 °C and 1090 °C, followed by
transfer onto Si/SiO₂ substrates. In another example, pristine Mo₂C formed at a CH₄:H₂ ratio of 1:600,
whereas increasing the ratio to 1:1000 induced graphene growth on Mo₂C. A one-step CVD process
using Ga droplets instead of Cu enabled the growth of in-plane WC/graphene heterostructures at
980–1020 °C.
Representative CVD reaction (Mo₂C growth):​
2Mo (diffused in Cu) + CH₄ → Mo₂C + 2H₂

[Link] Template-Assisted Synthesis

Template methods provide significantly higher yields than CVD by using pre-formed
two-dimensional transition-metal oxide nanosheets as structural scaffolds. These oxides are converted
into carbides or nitrides through controlled carbonization or ammoniation. For example, MoO₃-coated
NaCl crystals were prepared at 280 °C under Ar, then ammoniated at 650 °C to yield MoN@NaCl.
Dissolving NaCl in water produced free-standing 2D MoN nanosheets with excellent water
dispersibility, confirmed by a strong Tyndall effect. The nanosheets were uniform with a thickness of
~0.71 nm.
Similarly, layered δ-MoN nanosheets were obtained by first growing MoO₃ nanosheets via
hot-filament CVD, followed by ammoniation at 700 °C for 8 h in NH₃/Ar. Nitrogen-doped Mo₂C
nanosheets were produced through a two-step route involving MoO₂ nanosheets formed at 900 °C for
60 min under Ar/H₂, then calcined with C₂H₄N₄ at 450 °C for 2 h. These examples demonstrate that
template chemistry enables precise thickness and phase control, albeit through multistep and
time-consuming processes.
Representative template reaction (MoO₃ to MoN):​
MoO₃ + NH₃ → MoN + H₂O + N₂ (simplified)

[Link] Plasma-Enhanced Pulsed Laser Deposition (PEPLD)

PEPLD enables the growth of uniform 2D carbide films with controllable thickness. In this method,
CH₄ plasma is generated using a high-voltage electrode, while a KrF laser (248 nm) ablates a Mo
target. Using sapphire substrates, face-centered cubic (FCC) Mo₂C films with exceptionally smooth
surfaces were obtained. Film thickness could be precisely tuned from 2 to 25 nm by adjusting the
laser pulse rate. Although the films were uniform, they showed lower crystalline quality than
CVD-grown counterparts, with noticeable stacking faults. The FCC structure was attributed to the
favorable orientation relationship and minimal lattice mismatch between Mo₂C (111) planes and
sapphire (0003) planes.

[Link] Molten-Salt Bottom-Up Synthesis

Molten-salt synthesis offers a rapid and facile bottom-up route. Mo₂C quantum dots supported on
carbon nanosheets were synthesized by calcining molybdenum acetylacetonate, NaCl, and sucrose at
800 °C for 2 h. The resulting Mo₂C/C nanosheets were ultrathin (3.5 nm thick), with Mo₂C particles
of 23 nm diameter and a d-spacing of 0.237 nm corresponding to the (002) plane.

[Link] Pyrolysis-Based Routes

Pyrolysis is a simple, time-efficient, and environmentally benign approach. Mo₂C quantum
dot–carbon polyhedron composites were prepared by pyrolyzing Mo/ZIF-8 at 700 °C for 2 h under
Ar, followed by acid etching. Uniformly dispersed Mo₂C quantum dots exhibited a lattice spacing of
0.24 nm, indexed to the (111) plane of cubic Mo₂C. While promising, further optimization is required
to translate such routes into scalable MXene production.
Representative pyrolysis reaction (simplified):​
Mo-organic framework → Mo₂C + C (700 °C, Ar)

Comparative Summary of Bottom-Up MXene-Related Synthesis Methods

 Method Key Conditions Typical Thickness / Main Key Limitation
Products Size Advantage

CVD 980–1090 °C Mo₂C, WC Atomic to Highest High cost, low

CH₄/H₂, meta ReC, TaN few-nm crystallinity yield
substrates

Template 280–900 °C + NH MoN, Mo₂C ~0.71 nm High yield Multistep,

method or C source (MoN) uniformity time-consuming

PEPLD CH₄ plasma + 248 FCC-Mo₂C 2–25 nm Precise Lower

nm laser films thickness crystallinity
control

Molten salt 800 °C, NaC Mo₂C QDs/C 23 nm QDs Fast, simple Limited materia
matrix scope

Pyrolysis 700 °C, Ar Mo₂C QDs Few-nm Eco-friendly, Limited MXene

simple examples

3. Extraordinary Properties

3.1 Electronic and Transport Characteristics of MXenes

●​ Composition- and Termination-Dependent Electronic Behavior

MXenes are characterised by their electronic characteristics being highly influenced by the transition
metal (M), the X-site atom (C or N), and the surface termination groups [125,126]. A metallic
behaviour, like to that of graphene, is exhibited by the majority of MXenes in their purest form. In
their study on Tin+1Cn and Tin+1Nn (n = 1–9), Xie and colleagues used Density Functional Theory
(DFT) to determine that unmodified carbide and nitride MXenes are metallic. This is because the
Fermi level is situated within the transition-metal d bands, which is the reason for this phenomenon.
It is possible for MXenes to undergo a transition from metal to semiconductor after their surface is
functionalised with OH, OH, or OH. In addition, the hybridisation of metal d orbitals and O/F p
orbitals results in the introduction of new electronic bands that are located below the Fermi level.
This modification is the result of hybridisation. Since this is the case, a number of O-terminated
MXenes exhibit finite bandgaps that correspond to optical wavelengths, which makes them
appropriate for use in photodetectors. Sc2CT2 has been reported to have bandgaps of 1.03 eV (T = F),
0.45 eV (T = OH), and 1.8 eV (T = O), as well as bandgaps of 0.24 eV for Ti2CO2, 0.88 eV for
Zr2CO2, and 1.0 eV for Hf2CO2 [9].
●​ Carbide vs Nitride MXenes

It is generally accepted that nitride MXenes have a tendency to display a higher degree of metallicity
compared to carbide MXenes. Specifically, this is because nitrogen contributes one more valence
electron to the valence electrons. Ti3N2(OH)2, for example, is a more metallic compound than
Ti3C2(OH)2 [127]. Both the electrical conductivity and the charge transport capacity are improved as a
consequence of the an increase in the electron density.

●​ Double Transition-Metal and Topological MXenes

According to theoretical predictions [125,128], the majority of double transition-metal MXenes, such
as Mo2ZrC2O2, Mo2HfC2O2, and W2TiC2O2, it is hypothesised that they exhibit semiconducting
[Link] phenomenon known as spin–orbit coupling (SOC) is liable for lifting band
degeneracy at the Γ point in systems such as M2CO2 (where M represents Mo and W) and M′2M″C2O2
(where M′ represents Mo and W and M″ represents Ti, Zr, and Hf) [129,130]. Application of the Z₂
topological invariant, parity analysis shows that M2CO2 and M′2M″C2O2 are topological
non-conductor. However, M′2M″2C3O2 displays characteristics that are characteristic of topological
semimetals [129–132]. Furthermore to being shielded against non-magnetic disorder, these materials
have powerful conducting edge states. When compared to traditional topological insulators, which are
characterised by s–p band inversion, MXenes display d-orbital band inversion, in the form of dxy and
dxy/dₓ²₋ᵧ², which defines their topological behaviour from that of other insulators [133–136]. Some
examples of MXenes that exhibit SOC effects include W2C2O2, Mo2C2O2, and Cr2C2O2. Among these
MXenes, W2C2O2 demonstrates the highest SOC and is projected to have the capability of a
room-temperature photodetector [129].

●​ Electrical Conductivity and Carrier Transport

MXenes exhibit high electrical conductivity and carrier mobility [126], making them attractive for
electronics, supercapacitors, energy storage, and EMI shielding [44]. Among them, Ti₃C₂Tₓ is the
most extensively studied, with a conductivity of ~2400 S cm⁻¹ [48]. V₂C MXene shows an even
higher conductivity of ~3300 S cm⁻¹, highlighting its potential for wearable electronics [37,48].
Carrier mobility in MXenes can be exceptionally high. For example, Ti₂COₘ MXenes exhibit a
mobility of 1.03 × 10⁴ cm² V⁻¹ s⁻¹, surpassing graphene (0.3–1.2 × 10³ cm² V⁻¹ s⁻¹). Although CNTs
and rGO possess high conductivities (~15,100 S cm⁻¹), MXenes often outperform them in
electrocatalytic and electrochemical applications due to their surface chemistry and layered structure
[3,49].
When it comes to electronics, supercapacitors, energy storage, and electromagnetic interference
shielding [44], MXenes are appealing because of their high electrical conductivity and carrier
mobility [126]. With a conductivity of around 2400 S cm-1, Ti3C2Tx has been the subject of the most
thorough research among these materials [48]. It should be brought to your attention that V2C MXene
demonstrates an even higher conductivity of roughly 3300 S cm-1, which shows its potential for usage
in wearable electronics [37,48].There is the potential for MXenes to have extraordinarily high carrier
mobility. An example of this would be the mobility of Ti2COm MXenes, which is 1.03 × 104 cm2 V-1
s-1, surpassing the mobility of graphene, which ranges from 0.3 to 1.2 × 10³ cm2 V-1 s-1. Despite the
fact that carbon nanotubes (CNTs) and reduced graphene oxide (rGO) have high conductivities (about
15,100 S cm-1), Due to the surface chemistry and layered structure of MXenes, they have a tendency
to offer greater performance in electrocatalytic and electrochemical applications [3,49].

Table 1. Comparative overview of key physicochemical properties of MXenes and

representative conductive materials

Material Representative Electrical Typical Surface Specific Key Limitations

Class Materials Conductivity Chemistry / Surface
(S m⁻¹) Terminations Area

MXenes Ti₃C₂Tₓ (typical) 10⁵–10⁶ –F, –OH, –O High Restacking of

–Cl layers; oxidation
sensitivity

Carbon-base Carbon ≈10⁶ –COOH High Low volumetric

d materials nanotubes density
(CNTs)

Graphene ≈10⁶ Mostly iner High Limited

(pristine) pseudocapacitance

Reduced 1.6 × 10⁵ –O–, residua High Defect-induced

graphene oxide oxygen groups conductivity loss
(rGO)

Metallic Silver (Ag) 6.3 × 10⁷ None Low High weight; poor
conductors flexibility

Copper (Cu) 5.96 × 10⁷ None Low Low porosity

corrosion issues

Conducting Polyaniline ≈10⁵ Polymer Moderate Poor

polymers functional electrochemical and
groups long-term stability

●​ Tunability via Surface and Structural Engineering

The MXenes are materials that are extremely adjustable. It is possible to significantly increase
conductivity by substituting -F or –Cl with -OH in surface terminations [55]. Surface terminations are
of great significance. Intercalation of carbon or nitrogen, the production of surface vacancies, the
introduction of dislocations, and doping are some other tuning tactics that can be utilised. Doping is
particularly useful in multilayer MXenes, as it frequently results in higher performance [37]. As a
result of these changes, MXenes are able of exhibiting metallic (Ti2C, Ti3C2), semiconducting
(Ti3C2(OH)2, Ti3C2F2), or even insulating regimes [38,44]. There are other environmental elements
that have an effect on characteristics; for example, it has been demonstrated that exposure to moisture
can improve electrical conductivity, which enables sensing applications [37]. MXenes are
extraordinarily promising materials for the creation of electrical and optoelectronic devices that are
capable of the next generation because of their high conductivity, tunable band structure, and
surface-engineered charge transport in combination with one another.

3.2 Optical and Optoelectronic Characteristics of MXenes

In addition to their outstanding electronic conductivity, MXenes exhibit rich and highly tunable
optical properties, making them promising materials for transparent conductive electrodes,
optoelectronic devices, sensors, photodetectors, and nonlinear optical systems. MXenes possess a
broad spectral response, spanning ultraviolet (UV), visible, and near-infrared (NIR) regions, and
display linear and nonlinear light absorption, scattering, emission, photoluminescence (PL),
plasmonic behavior, and strong photothermal effects [126, 37].

Transparency, Absorption, and Thickness Dependence

The optical absorbance of MXene films scales linearly with thickness, independent of incident
wavelength. For example, Ti₃C₂Tₓ films etched using aqueous HF or NH₄HF₂ with thicknesses of 15,
28, 43, and 60 nm were examined at 240 nm and 800 nm. Thinner films showed higher transmittance
at longer wavelengths (800 nm), and absorbance exhibited a linear relationship with film thickness.
Notably, Ti₃C₂Tₓ films achieved ~90% transmittance, exceeding that of Ti₃AlC₂ thin films [74].
Spray coating provides a scalable alternative to magnetron sputtering for MXene thin-film
fabrication. Spray-coated Ti₃C₂Tₓ films with thicknesses ranging from 5–70 nm exhibited absorbance
in the 300–500 nm region. A 5 nm film showed 91.2% transparency, while transparency decreased to
43.8% at 70 nm, enabling tunable optical properties for different optoelectronic applications [74,
138]. Similarly, ultrathin delaminated MXene films achieved up to 97% transmittance, comparable to
graphene, which absorbs ~2.3% light per layer, whereas MXenes show ~3% loss per layer despite
being thicker (~1.5 nm vs 0.34 nm for graphene) [139, 140].

Optoelectronic Performance and Figure of Merit

The figure of merit (FOM) is commonly used to evaluate optoelectronic performance, defined by the
ratio of direct current conductivity (σDC) to optical conductivity (σOC), and depends on
transmittance (T) and sheet resistance (Rsh). Higher σOC/σDC ratios correspond to better
optoelectronic behavior. Compared with MoS₂, VS₂, reduced graphene oxide, and other 2D materials,
MXene thin films demonstrate superior FOM values, highlighting their advantage for transparent
electronics [137].

Effect of Surface Chemistry and Solvent Environment

MXene optical properties are strongly influenced by surface terminations and intercalation chemistry.
Films intercalated with DMSO or urea show modified interlayer spacing and transmittance [126].
MXenes terminated with –F and –OH groups exhibit reduced visible-light absorption and reflectivity,
while UV reflectivity increases [144]. Chemical intercalation alters the c-lattice parameter, further
tuning optical transparency [145].
The storage solvent also affects optoelectronic behavior. Ti₃C₂Tₓ films prepared from ethanol
dispersions become more resistive than those prepared from water while maintaining similar
transmittance. This arises from reactions between surface –O/–OH groups and ethanol, forming
alkoxide species that modify the electronic band structure [143].

Spectral Response and Photoluminescence

MXenes absorb light from UV to near-visible/NIR, with a broad absorption peak around ~800 nm
attributed to interband transitions [140]. While bulk MXenes show weak PL, MXene quantum dots
(MQDs) exhibit strong photoluminescence due to quantum confinement and edge effects. MQDs
derived from Ti₃C₂ and V₂C display quantum yields up to 10%, synthesized via hydrothermal cutting,
with morphology tunable by reaction temperature [150, 151].

Nonlinear Optical Behavior

MXenes show pronounced nonlinear optical (NLO) properties, particularly saturable absorption (SA),
where transmittance increases nonlinearly with light intensity. Ti₃C₂Tₓ exhibits strong SA across
800–1800 nm, studied using the Z-scan technique. At low pulse energies, one-photon SA dominates,
while at higher energies, multi-photon absorption becomes significant. The nonlinear absorption
coefficient is approximately −10⁻²¹ m² V⁻², indicating strong potential for optical switching and
ultrafast photonics [154]. Ti₃C₂Tₓ also operates effectively in the telecommunication C-band
(1550–1620 nm) [155]. Z-scan studies further show that Ti₃C₂Tₓ possesses a negative nonlinear
refractive index and outperforms graphene, TMDs, and black phosphorus in NLO response [38].

Plasmonic Properties
MXenes exhibit both bulk plasmons (BP) and surface plasmons (SP). For bare MXenes (Ti₂C, Ti₂N,
Ti₃C₂, Ti₃N₂), calculated plasmon energies are 10.00, 11.62, 10.81, and 11.38 eV, respectively [148].
Below 1 eV, reflectivity can reach ~100% when the electric field is parallel to the surface, but drops
below 50% when perpendicular [148]. As Ti₃C₂ thickness decreases, SP intensity increases while BP
intensity decreases, due to dominant surface effects. Surface terminations (–OH, –F) further modulate
plasmon behavior by altering electronic structure [158]. Strong photon–electron coupling arising
from metallic conductivity enhances plasmon excitation, benefiting sensing and imaging.

Photodetection and Photothermal Performance

MXenes such as Mo₂CTₓ demonstrate excellent photodetection capabilities with responsivity up to 9
A W⁻¹, detectivity ~5 × 10¹¹ Jones, and stable photoswitching over 400–800 nm, assisted by
plasmon-induced hot carriers [159]. Computational studies predict Ti₂C, Zr₂C, and Hf₂C to possess
band gaps suitable for visible-light optoelectronics [160].
MXenes also exhibit near-100% light-to-heat conversion efficiency, enabling applications in
photothermal therapy and solar-driven water evaporation [45]. Temperature-dependent studies reveal
that Nb-based MXenes show reduced optical performance at elevated temperatures, whereas Ti-based
MXenes remain optically stable at ambient conditions [37].

3.3 Chemical Structure, Surface Chemistry, and Stability of MXenes

Before 2014, MAX phases were reported mainly as random solid solutions, such as the 211 phases
(TixNb2–x)2AlC and (TixCr1–x)2AlC, the 312 phase (Ti0.5V0.5)3AlC2, and the 413 phase
(Cr0.626Ti0.375)4AlC3 [161]. A major breakthrough occurred when it was discovered that
combining heavy and light transition metals in M3AX2 and M4AX3 systems could lead to
chemically ordered structures, particularly exhibiting out-of-plane ordering [8].
In 2014, Liu et al. synthesized the first chemically ordered MAX phase, (Cr2/3Ti1/3)3AlC2,
belonging to the M3AX2 family [162]. This structure is characterized by a 2:1 ratio of M elements,
producing alternating atomic layers composed of a single transition metal. Selective etching of this
ordered MAX phase enabled the first synthesis of out-of-plane ordered MXenes (o-MXenes),
including Mo2TiC2, Mo2Ti2C3, and Cr2TiC2 [8].
Subsequently, in-plane ordered MXenes (i-MXenes) were developed using i-MAX precursors, such
as (Mo2/3Sc1/3)2AlC [15]. Etching this precursor in HF or LiF/HCl selectively removed both the
A-layer (Al) and the Sc atoms, yielding Mo1.33C MXene with well-ordered divacancies. These 2D
Mo1.33C nanosheets demonstrated enhanced electrical conductivity and very high volumetric
capacitance compared with conventional MXenes, highlighting the chemical and electrochemical
advantages of vacancy-engineered structures [8, 15].

Surface Terminations and Electronic Modulation

MXenes are intrinsically terminated with surface functional groups such as –O, –OH, –F, and –Cl,
introduced during etching or post-treatment processes. These terminations stabilize the surface by
satisfying metal coordination and lowering surface Gibbs free energy. The type, density, and
distribution of terminations depend on the etching chemistry, M/X composition, flake thickness, and
post-processing steps. Both theoretical and experimental studies confirm that electronic structure,
stability, and physicochemical properties of MXenes can be systematically tuned by controlling
surface terminations [3, 125, 163].
Surface chemistry strongly influences band structure and work function. Studies by Naguib et al.
showed that band gaps can be tuned by adjusting the nature and orientation of surface terminations
[3]. Liu et al. further demonstrated that –O terminations increase the work function, whereas –OH
terminations decrease it, due to shifts in the Fermi level [164]. This tunability is critical for
applications in electronics, sensing, and energy storage.
Interlayer Interactions and Exfoliation Behavior
Compared to their parent MAX phases, MXenes possess weak interlayer interactions, facilitating
exfoliation. In Ti3C2Tx, interlayer forces arise mainly from van der Waals interactions between O
and F atoms and hydrogen bonding between –O/–F and –OH groups on adjacent layers [165]. These
weak interactions enable efficient delamination into few-layer or single-layer nanosheets.
The etching route directly affects surface termination chemistry. For example, low HF concentrations
favor a higher proportion of –O terminations relative to –F in Ti3C2Tx, whereas LiF/HCl etching
results in water molecules coordinated to –O/–OH groups [118]. The delamination process further
influences flake thickness and dispersion behavior [165]. Simple sonication in water is generally
insufficient; therefore, intercalants such as dimethyl sulfoxide (DMSO), urea, and isopropylamine are
commonly employed to separate layers effectively [166].

Dispersibility and Solvent Compatibility

Due to abundant –O and –OH terminations, delaminated Ti3C2Tx nanosheets are highly hydrophilic
and disperse readily in polar solvents, including water, ethanol, propylene carbonate, and
N-methyl-2-pyrrolidone [167, 168]. In contrast, stable dispersions are not achievable in non-polar
solvents such as hexane or 1,2-dichlorobenzene. However, chemical modification with long-chain
molecules such as DHT enables Ti3C2Tx multilayers to become stable in non-polar media, as the
alkyl chains improve chemical compatibility [169].

Oxidation Behavior and Environmental Stability

The oxidation state of MXenes is generally lower than that of corresponding metal oxides and is
strongly influenced by surface terminations and environmental conditions [6]. Ti3C2Tx colloidal
solutions stored under ambient conditions oxidize to TiO2 within ~15 days, with oxygen identified as
the dominant degradation factor [40, 41].
Water also accelerates degradation. Ti2CTx and Ti3C2Tx degrade within 41 days in a water/argon
environment, whereas in an IPA/oxygen atmosphere, oxidation is dramatically slowed, requiring
approximately 5.5 years to reach similar degradation levels [42]. Oxidation can be suppressed using
antioxidants such as sodium L-ascorbate and by controlling temperature and atmosphere. For
example, V2CTx remains stable below 375 °C in argon, while Ti3C2Tx maintains stability up to 800
°C in argon [40, 41].

Hydrophilicity and Processability

MXenes exhibit strong hydrophilicity due to surface –O and –OH groups, enabling robust
interactions with water and uniform wetting behavior. Importantly, the ratio of surface terminations
can be precisely controlled during synthesis, allowing optimization of dispersion and interfacial
properties. This characteristic is particularly valuable for ink formulation and 3D printing of
composite electrodes, where stable, homogeneous dispersions are essential for scalable processing
and device fabrication [44].
4. Global Applications: The Multi-Field Impact

4.1 Energy Storage (Batteries & Supercapacitors)

●​ The rapid depletion of fossil fuels and escalating environmental pollution have intensified the
need for clean and renewable energy sources [160,161]. However, the intermittency of
renewable energy necessitates efficient electricity storage systems [162]. Electrochemical
energy storage devices have therefore gained significant attention due to their fast response,
versatility, and flexibility [163]. Among them, lithium-ion batteries (LIBs) dominate the
market, while sodium-ion batteries (SIBs), zinc-ion batteries (ZIBs), lithium–sulfur (Li–S)
batteries, and supercapacitors (SCs) are rapidly developing [164]. SIBs are particularly
promising for large-scale storage owing to abundant sodium resources and low cost [165].
●​ Improving battery energy density requires advanced cathode and anode materials with higher
capacity or voltage; however, challenges such as large volume changes, poor conductivity, and
unstable solid electrolyte interphase (SEI) layers limit practical application. MXenes address
these issues by acting as both electrochemically active materials and highly conductive 2D
substrates, enabling hybrid electrode architectures with improved performance [170]. Their
layered structure allows efficient Li⁺ intercalation, making them superior to graphene-based
electrodes [5].
●​ In 2012, Ti₂C MXene was first demonstrated as a LIB anode, delivering 225 mAh g⁻¹ at C/25
and 110 mAh g⁻¹ at 1C after 80 cycles [168]. Nb₂CTₓ and V₂CTₓ MXenes showed reversible
capacities of 170 mAh g⁻¹ and 260 mAh g⁻¹ at 1C, respectively, with stability up to 10C [61].
Ti₃C₂Tₓ delivered 123.6 mAh g⁻¹ at 1C with 47% coulombic efficiency, outperforming Ti₂C
[171]. A Ti₃C₂/CNT hybrid film achieved 428.1 mAh g⁻¹ at 0.5C after 300 cycles [172].
Laser-induced Mo₂CTₓ/Mo₂C anodes exhibited 340 mAh g⁻¹ capacity with 106.2% retention
over 1000 cycles [173]. Nb₂CTₓ/CNT paper electrodes exceeded 400 mAh g⁻¹ at 0.5C [174],
while V₂C delivered 250 mAh g⁻¹ at 50 mA g⁻¹ [72].
●​ Porous MXene engineering significantly enhances ion transport. Vertically aligned MXene
films with 200 μm thickness (vs. standard 100 μm) maintained fast ion/electron transport
[175,176]. Porous Ti₃C₂Tₓ exhibited 1250 mAh g⁻¹ at 0.1C and 330 mAh g⁻¹ at 10C [177].
●​ For SIBs, sodium (−2.71 V vs SHE) closely matches lithium (−3.04 V vs SHE) [178,179].
MXene anodes operate between 0.5–1.3 V vs Na/Na⁺ [180], enabling full-cell voltages of
2–2.8 V when paired with Na₃V₂(PO₄)₃ (~3.3 V) [181]. Despite larger Na⁺ radius (1.06 Å vs
0.76 Å for Li⁺), MXenes provide high conductivity and low diffusion barriers [182].
Ti₂C//Na₂Fe₂(SO₄)₃ cells delivered 90 mAh g⁻¹ at 1 A g⁻¹ and 40 mAh g⁻¹ at 5 A g⁻¹ at 2.4 V
[183]. Ti₃C₂/CNT anodes showed 421 mAh cm⁻³ at 20 mA g⁻¹ [184]. PDDA-BP/Ti₃C₂
exhibited 1112 mAh g⁻¹, stable over 500 cycles at 0.1 A g⁻¹ [185]. f-Ti₃C₂TₓDMSO delivered
196 mAh g⁻¹ after 500 cycles at 100 mA g⁻¹ [186]. 3D MXene architectures yielded 370
(Mo₂CTₓ), 330 (Ti₃C₂Tₓ), and 340 mAh g⁻¹ (V₂CTₓ) at 0.25C [187]. Sb₂O₃/Ti₃C₂Tₓ reached 295
mAh g⁻¹ at 2 A g⁻¹ [188]. SnO₂/MXene (ALD) anodes delivered 843 mAh g⁻¹ [189].
 VS₂/Ti₃C₂Tₓ hybrids achieved 522 mAh g⁻¹, 116% retention after 3000 cycles, and stability
from −40 to 70 °C [190].
●​ In Li–S batteries, MXenes suppress polysulfide (LiPS) shuttling via strong surface
interactions. S/Ti₂C (70 wt% S) delivered 1200 mAh g⁻¹ at C/5 and retained 80% capacity
after 400 cycles at C/2 [192]. Ti₃C₂ hosts showed 1290 mAh g⁻¹ initially and 970 mAh g⁻¹
after 100 cycles [193]. CNT–MXene hybrids achieved 1240 mAh g⁻¹ at 1.5 mg cm⁻² S
loading, retaining 450 mAh g⁻¹ after 1200 cycles, and 910 mAh g⁻¹ at 5.5 mg cm⁻² [195].
Ti₃C₂@Meso-C/S (73 wt% S) retained 705 mAh g⁻¹ after 300 cycles at C/2 [196].
HE-MXene/graphene systems sustained performance over 1200 cycles and 6000 h [198].
Ti₃C₂Tₓ/rGO/S delivered 1144.2 mAh g⁻¹ initially and 878.4 mAh g⁻¹ after 300 cycles [199].
Ti₃C₂-coated separators (520 nm thickness, 0.1 mg cm⁻³ loading) enabled 1050 mAh g⁻¹ at
0.2C and 745 mAh g⁻¹ at 1C [201]. MXene-Li composite anodes achieved 950 mAh g⁻¹,
retaining 840 mAh g⁻¹ after 100 cycles [202].
Table: MXene-Based Energy Storage Applications and Performance Metrics

Battery MXene / Composite Role Key Electrochemica Reference

Type Performance

LIB Ti₂C MXene Anode 225 mAh g⁻¹ at C/25; 110 mAh [168]
g⁻¹ at 1C after 80 cycles

LIB Nb₂CTₓ Anode 170 mAh g⁻¹; stable up to 10C [61]

LIB V₂CTₓ Anode 260 mAh g⁻¹ at 1C; stable up to [61]

10C

LIB Ti₃C₂Tₓ Anode 123.6 mAh g⁻¹ at 1C; 47% [171]

coulombic efficiency

LIB Ti₃C₂/CNT Anode 428.1 mAh g⁻¹ at 0.5C after 300 [172]
cycles

LIB Mo₂CTₓ/Mo₂C Anode 340 mAh g⁻¹; 106.2% capacity [173]

(LS-Mo₂CTₓ) retention over 1000 cycles

LIB Nb₂CTₓ/CNT paper Anode >400 mAh g⁻¹ at 0.5C [174]

LIB V₂C Anode 250 mAh g⁻¹ at 50 mA g⁻¹ [72]

LIB Porous Ti₃C₂Tₓ Anode 1250 mAh g⁻¹ at 0.1C; 330 mAh [177]
g⁻¹ at 10C

LIB Vertically aligned Anode Thickness 200 µm (vs 100 µm [175,176]

MXene film standard); fast ion/electron
transport
SIB Ti₂C // Na₂Fe₂(SO₄)₃ Full cell 2.4 V; 90 mAh g⁻¹ at 1 A g⁻¹; 40 [183]
mAh g⁻¹ at 5 A g⁻¹ 4.2

SIB Ti₃C₂/CNT Anode 421 mAh cm⁻³ at 20 mA g⁻¹ [184]

SIB PDDA-BP/Ti₃C₂ Anode 1112 mAh g⁻¹; stable after 500 [185]
cycles at 0.1 A g⁻¹

SIB f-Ti₃C₂TₓDMSO Anode 196 mAh g⁻¹ after 500 cycles a [186]
100 mA g⁻¹

SIB 3D MXene (Mo₂CTₓ / Anode 370 / 330 / 340 mAh g⁻¹ at 0.25C [187]
Ti₃C₂Tₓ / V₂CTₓ)

SIB Sb₂O₃/Ti₃C₂Tₓ Anode 295 mAh g⁻¹ at 2 A g⁻¹ [188]

SIB VS₂/Ti₃C₂Tₓ Anode 522 mAh g⁻¹; 116% retention [190]

after 3000 cycles; −40 to 70 °C

LIB SnO₂/MXene (ALD) Anode 843 mAh g⁻¹ [189]

Li–S S/Ti₂C (70 wt% S) Cathode 1200 mAh g⁻¹ at C/5; 80% [192]
retained after 400 cycles at C/2

Li–S Ti₃C₂ MXene Sulfur host 1290 mAh g⁻¹ initial; 970 mAh [193]
g⁻¹ after 100 cycles

Li–S MXene–CNT hybrid Cathode 1240 mAh g⁻¹ (1.5 mg cm⁻²) [195]
910 mAh g⁻¹ (5.5 mg cm⁻²)

Li–S Ti₃C₂@Meso-C/S (73 Cathode 1225 mAh g⁻¹ initial; 705 mAh [196]
wt% S) g⁻¹ after 300 cycles

Li–S HE-MXene/Graphene Separator Stable over 1200 cycles and [198]

modifier 6000 h

Li–S Ti₃C₂Tₓ/rGO/S Cathode 1144.2 mAh g⁻¹ at 0.5C; 878.4 [199]

mAh g⁻¹ after 300 cycles

Li–S Ti₃C₂-coated separator Separator Thickness 520 nm; 1050 mAh [201]
g⁻¹ at 0.2C; 745 mAh g⁻¹ at 1C

Li–S Ti₃C₂–Li composite Anode 950 mAh g⁻¹; 840 mAh g⁻¹ after [202]
100 cycles

MXenes as Emerging Platforms for Sustainable Energy Conversion

The transition toward renewable energy is critical for sustainable development, driving intensive
research into advanced energy conversion technologies such as photovoltaics, catalysis, and fuel cells
[223]. While silicon solar cells dominate the Chinese market, perovskite solar cells (PSCs) have
emerged as strong contenders due to their low cost and high efficiency. In parallel, key catalytic
reactions including hydrogen evolution (HER), oxygen evolution (OER), carbon dioxide reduction
(CO₂RR), and nitrogen reduction (NRR) have been widely explored [224].
4.2.1 MXenes as Interface Modifiers in Perovskite Solar Cells
PSCs offer advantages over silicon-based devices, including high absorption coefficients, simple
fabrication, and a high theoretical efficiency. Recent PSCs have achieved a power conversion
efficiency (PCE) of 25.7% [225]. However, interfacial defects and grain boundaries limit
performance [226]. MXenes have therefore been introduced as additives or transport layers due to
their high conductivity, tunable work function, and surface functionality [227].
In 2021, Ti₃C₂Clₓ MXene synthesized via CdCl₂ etching was incorporated into CsPbBr₃ films,
forming Pb–Cl interfacial bonds that reduced lattice strain and interfacial defects [159]. As a result,
all-inorganic CsPbBr₃ PSCs achieved a PCE of 11.08% and an open-circuit voltage of 1.702 V, along
with 100-day stability at 80% RH and 25 °C. Subsequently, Ti₃C₂Clₓ quantum dots (~8 nm) enabled
grain size enlargement from 273 to 453 nm, improving charge transport. The modified device
delivered a PCE of 21.31%, an open-circuit voltage of 1.19 V, and retained 84% efficiency after 1000
h at 40% RH [228]. These results highlight the effectiveness of Cl-terminated MXenes in enhancing
PSC efficiency and stability.

4.2 MXenes as Conductive Supports for Hydrogen Evolution

Hydrogen production via HER is a clean alternative to fossil fuels [229], but noble metal catalysts
(Au, Pt, Pd) remain costly and scarce [230]. MXenes have gained attention as HER catalysts due to
their layered structure, tunable surface chemistry, and high conductivity [231,232]. Ti₃CNCl₂ MXene
prepared by NiCl₂ molten salt etching was combined with CoS₂ to form a Ti₃CNCl₂@CoS₂ core–shell
catalyst [233]. Strong interfacial electron transfer and near-zero Gibbs free energy for H₂ adsorption
resulted in a Tafel slope of 89 mV dec⁻¹ and stable operation for 10 h in 0.5 M H₂SO₄ without current
decay.
4.2.3 MXene-Enabled Overall Water Electrolysis
Electrochemical water splitting requires a theoretical voltage of 1.23 V but is limited by sluggish
kinetics [235,236]. Cl-terminated Ti₃C₂Cl₂ MXene synthesized via CuCl₂ etching exhibited enhanced
interlayer spacing and active sites [237]. In 1 M KOH, Ti₃C₂Cl₂ showed an OER overpotential of 330
mV at 30 mA cm⁻², compared with 390 mV for HF-etched Ti₃C₂Tₓ. For HER, Ti₃C₂Cl₂ required 259
mV at 10 mA cm⁻², significantly lower than 444 mV for HF-Ti₃C₂Tₓ. Corresponding Tafel slopes
were 48 mV dec⁻¹ (OER) and 92 mV dec⁻¹ (HER), indicating superior bifunctional catalytic activity.
4.2.4 MXene-Supported Catalysts for CO₂ Electroreduction
The accumulation of CO₂ has intensified environmental concerns [238], motivating research into
CO₂RR for value-added fuel production [239]. Single-atom Cu-anchored Ti₃C₂Clₓ MXene
synthesized via ZnCl₂ molten salt etching exhibited a Cu loading of approximately 1.0 wt% [158].
The catalyst achieved a maximum Faradaic efficiency of 59.1% at −1.4 V for methanol production
and maintained >58% efficiency over 30 h, demonstrating excellent activity and durability.
4.2.5Electrocatalytic Nitrogen Fixation Using MXenes
Conventional ammonia synthesis via the Haber–Bosch process operates at 300–500 °C and 150–200
atm, consuming large amounts of energy [241]. Electrocatalytic NRR offers a sustainable alternative
[242], though it is limited by the strong N≡N bond [243]. Fe-anchored fluorine-free Ti₃C₂Tₓ MXene
containing 3.12 wt% Fe was prepared via FeCl₂ etching [244]. In 0.1 M Na₂SO₄, the catalyst achieved
an NH₃ yield of 18.25 µg h⁻¹ mg⁻¹ with a Faradaic efficiency of 21.8%, while maintaining stable
current density for 24 h.
Table 4. Energy Conversion Applications of MXenes
Energy MXene Material Role of MXene Key Performance Key Findings Ref.
Conversion Composite Metrics
System

Perovskite Ti₃C₂Clₓ MXene Additive in bulk PCE: 11.08%; Voc Pb–Cl bonding [159]
Solar Cells (CdCl₂ etched) & surface o 1.702 V; Stability reduces lattice
(PSCs) perovskite 100 days at 80% strain and
RH, 25 °C interfacial
defects,
improving
efficiency and
stability

Perovskite Ti₃C₂Clₓ quantum Additive in Grain size: 273 → Enhanced [228]

Solar Cells dots (~8 nm) perovskite 453 nm; PCE crystallinity,
(PSCs) precursor 21.31%; Voc: 1.19 reduced grain
V; Stability: 84% boundaries,
PCE retention after improved charge
1000 h at 40% RH transport

Hydrogen Ti₃CNCl₂@CoS₂ Electrocatalyst Tafel slope: 89 mV Strong [233]

Evolution dec⁻¹; Stability: 10 h MXene–CoS₂
Reaction (no current decay) interaction,
(HER) in 0.5 M H₂SO₄ ΔG(H*) ≈ 0, fas
charge transfer

Overall Water Ti₃C₂Cl₂ MXene Bifunctional OER overpotential Enlarged [237]

Splitting catalyst (HER & 330 mV at 30 mA interlayer
OER) cm⁻²; HER spacing and
overpotential: 259 active sites
mV at 10 mA cm⁻² outperform
Tafel slopes: 48 mV HF-Ti₃C₂Tₓ
dec⁻¹ (OER), 92 mV
dec⁻¹ (HER)
 CO₂ Single-atom Electrocatalyst Faradaic efficiency Cu–O [158]
Reduction Cu-Ti₃C₂Clₓ (Cu ≈ 59.1% at −1.4 V coordination
Reaction 1.0 wt%) Stability: >58% FE lowers energy
(CO₂RR) after 30 h barrier for CO
→ CH₃OH

Nitrogen Fe-Ti₃C₂Tₓ (Fe ≈ Electrocatalyst NH₃ yield: 18.25 µg Enhanced N [244]

Reduction 3.12 wt%) h⁻¹ mg⁻¹; Faradaic adsorption and
Reaction efficiency: 21.8% activation via
(NRR) Stability: 24 h Fe–O sites

4.3 MXene-Based Sensors

MXenes have emerged as advanced sensing materials due to their layered structure, which, together
with their moderate specific surface area, plentiful active sites, high electrical conductivity, efficient
ion transport, biocompatibility, and simplicity of functionalisation, has contributed to their emergence
as technologies [44]. In the context of environmental monitoring, industrial safety, and biological
diagnostics, they are the subject of substantial research for the purpose of their application in gas
sensors, chemical sensors, and biosensors [245].
It has been established that Ti3C2Cl2 MXene, which was synthesised using ZnCl2 etching, possesses
gas-sensing capabilities, with an NH3 response of 13.2% [246]. In hybrids composed of
Au/Pt/Ti3C2Cl2, a further boost is realised through the reduction of Au3+ and Pt4+ to metallic
nanoparticles by low-valence Ti species. The hybrids have the ability to perform colorimetric H2O2
sensing from HeLa cells, with a detection range of 50–10,000 μM and a limit of detection (LOD) of
10.24 μM. This demonstrates the capability of intracellular biosensing [247].
As a result of its non-toxicity, biocompatibility, metallic conductivity, and wide surface area, MXenes
are particularly appealing for use in implanted biosensors in the field of biomedical sensing (Xu et al.,
2020). Electrochemical etching was used to manufacture fluoride-free Nb2CTx nanosheets, which
allowed Nb2CTx/acetylcholinesterase biosensors for phosmet detection with a limit of detection
(LOD) of 0.046 ng mL-1 (Song et al., 2020). Similarly, acetylcholinesterase/chitosan–Ti3C2Tx/GCE
biosensors demonstrated the ability to detect malathion in a manner that was stable, reproducible, and
devoid of interference (Zhou et al., 2017).
MXenes also perform better than ordinary semiconductors when it comes to the detection of volatile
organic compound gases. Ti3C2Tx sensors have the capability to detect volatile organic compounds
(VOCs) at room temperature with limit of detection (LOD) values that range from fifty to one
hundred parts per billion (ppb). This allows them to achieve a signal-to-noise ratio that is two orders
of magnitude higher than that of other 2D materials (Kim et al., 2018a). At this time, target analytes
consist of NH3, NOx, SO2, CO, H2, and volatile organic compounds (VOCs) (Xin et al., 2020;
Bhardwaj et al., 2021). OH- and O-terminated MXenes display considerable VOC binding by
hydrogen bonding, in addition to heterostructures, Schottky junctions, and surface/structural
engineering (Mehdi Aghaei et al., 2021). This is also the case for heterostructures. The selectivity and
sensitivity of the system are both further improved by these additions.
Green synthesis routes have a significant impact on the behaviour of sensing. Using molten salts of
NaF/HCl, LiF/HCl, or ZnCl2, Ti3C2Tx and V2CTx exhibit gas-specific selectivity when they are
etched. Notably, ZnCl2 etched Ti3C2Tx shows superior responses to toluene, triethylamine, and NH3,
however, mesoporous MXene/ZnO nanorod composites demonstrate a response of 346% to NOx at a
concentration of 200 ppb, with a response time of 17 seconds and a recovery time of 24 seconds at a
concentration of 50 ppb of NOx . It is important to note that green-synthesized MXenes maintain or
improve sensing capability, which enables selective and environmentally friendly sensor systems.

Table: MXene-Based Sensors – Materials, Targets, and Performance

Sensor Type MXene / Composite Target Key Key Features Ref.
Analyte Performance
Metrics

Gas sensor Ti₃C₂Cl₂ (ZnCl₂ etched) NH₃ Response: High [246]

13.2% conductivity,
layered
structure

Biosensor Au/Pt/Ti₃C₂Cl₂ H₂O₂ Range: In-situ [247]

(colorimetric) (HeLa 50–10,000 μM intracellular
cells) LOD: 10.24 detection
μM

Biosensor Nb₂CTₓ/acetylcholinesterase Phosmet LOD: 0.046 ng Fluoride-free, Song e

mL⁻¹ biocompatible al.,
2020

Biosensor AChE/chitosan–Ti₃C₂Tₓ/GC Malathion Stable, Non-toxic, high Zhou e

E reproducible, conductivity al.,
interference-fre 2017
e

Gas sensor Ti₃C₂Tₓ VOCs LOD: 50–100 Low noise Kim e

ppb; S/N ambient al.,
~100× higher operation 2018a

Gas sensor MXene/ZnO nanorods NOₓ Response: Mesoporous, Wang

346% at 200 fast kinetics et al.
ppb; Response 2022
time: 17 s
Recovery: 24 s
 Gas sensor Ti₃C₂Tₓ, V₂CTₓ (NaF/HCl NH₃, NOₓ Gas-dependent Green Wang
(green LiF/HCl, ZnCl₂) VOCs selectivity synthesis, et al.
MXenes) tunable surface 2021f
chemistry

4.4 MXenes for Environmental Remediation and Water Purification

MXenes are increasingly applied in environmental remediation, particularly water purification, owing
to their hydrophilicity, layered architecture, large surface area, mechanical flexibility, stability, and
antifouling resistance. Ti₃C₂Tₓ MXenes have been fabricated as freestanding or supported membranes
with thicknesses ranging from nanometers to micrometers, offering high mechanical strength and
electrical conductivity. Notably, MXene membranes exhibit ultrafast water fluxes of 37.4 L (bar h
m²)⁻¹ [221].
For heavy-metal removal, delaminated Ti₃C₂Tₓ shows strong affinity toward Cu²⁺, achieving an
adsorption capacity of 78.45 mg g⁻¹, aided by oxygenated surface groups that suppress Cu₂O/CuO
formation [222]. MXenes have also been integrated into polymer composite membranes; horizontally
aligned Ti₃C₂Tₓ–OH nanosheets within PEI/PDMS blends enhance alcohol transport via –OH
adsorption sites [223].
Advanced MXene-based nanofiltration (NF) membranes demonstrate excellent dye and salt rejection.
HPEI-AgNP@Ti₃C₂Tₓ membranes deliver water permeability of 24.64–30.73 L m⁻² h⁻¹ bar⁻¹, with
~100% rejection of Congo red, methyl orange, and Rhodamine B, alongside salt rejection of 84.15%
(MgSO₄) and 56.58% (NaCl) [224]. A SLS-CNT/alk-MXene membrane shows >99% dye retention,
51.6 L m⁻² h⁻¹ bar⁻¹ flux, 813 Ω resistance, and 80% recovery, while degrading dyes within 1 h [225].
Photocatalytic self-cleaning membranes further enhance remediation. ZnO@Ti₃C₂Tₓ NF membranes
achieve 95.44% Congo red rejection, 138.81 L m⁻² h⁻¹ bar⁻¹ permeability, and maintain >88.48% RhB
rejection over six cycles, with efficient degradation of 10 ppm methylene blue [226]. BiOCl/Ti₃C₂Tₓ
heterostructures photodegrade 90% ciprofloxacin in 30 min under solar light via h⁺ and O₂⁻ radicals
[227].
MXenes also significantly enhance TiO₂-based photocatalysts. TiO₂/MXene (4:1) composites
improve methylene blue degradation to 96.44% (UV) and 40.19% (visible), 8.26× higher than pure
TiO₂ [228]. Ag@ZnO@Ti₃C₂ MXene heterojunctions achieve 90.54% MB and 86.76% levofloxacin
degradation under visible light, remaining stable over five cycles [229].
In desalination, ultrathin Ti₃C₂Tₓ membranes deliver 85.4 L m⁻² h⁻¹ flux with ~99.5% salt rejection for
3.5 wt% NaCl at 65 °C [230]. For oil–water separation, TA-APTES@MXene membranes show an
exceptional water flux of ~5990 L m⁻² h⁻¹ at 0.1 MPa [232].
MXenes further provide antibacterial activity, with Ti₃C₂Tₓ membranes exhibiting >73% inhibition
against B. subtilis, 67% against E. coli, and ~99% inhibition upon aging [233]. As adsorbents,
MXenes selectively remove ions such as Pb²⁺ even in the presence of Ca²⁺/Mg²⁺ [234], and enable
Cr(VI) reduction to Cr(III) with simultaneous adsorption [53]. Their tunable surface terminations
allow photocatalytic degradation efficiencies up to 81% MB within 5 h under UV, compared with
18% in the dark [235], while engineered TiO₂/Ti₃C₂ interfaces yield 2.3-fold higher dye degradation
than particulate TiO₂/Ti₃C₂ due to efficient charge separation [237].
As a result of its hydrophilicity, layered architecture, wide surface area, mechanical flexibility,
stability, and antifouling resistance, MXenes are increasingly being utilised in environmental
remediation, particularly in the purification of water. MXenes made of titanium dioxide and titanium
dioxide have been manufactured as freestanding or supported membranes with thicknesses ranging
from nanometres to micrometres. These membranes have been found to possess great mechanical
strength and electrical conductivity. Particularly noteworthy is the fact that MXene membranes
demonstrate ultrafast water flows of 37.4 L (bar h m2)3.
When it comes to the removal of heavy metals, delaminated Ti₃C₂Tₛ exhibits a strong affinity
towards Cu²⁺, obtaining an adsorption capacity of 78.45 mg g⁻¹. This accomplishment is made
possible by oxygenated surface groups that inhibit the formation of Cu₂O/CuO [222]. In addition,
MXenes have been included into polymer composite membranes. For example, horizontally aligned
Ti₃C₂Tₓ–OH nanosheets embedded inside PEI/PDMS blends have been shown to improve alcohol
transport by the use of –OH adsorption sites [223."
It has been demonstrated that nanofiltration (NF) membranes based on advanced MXene exhibit good
dye and salt rejection. In addition to exhibiting a water permeability of 24.64–30.73 L m⁻² h⁻¹ bar⁻¹,
HPEI-AgNP@Ti₃C₂Tₛ membranes have a rejection rate of around 100 percent for Congo red, methyl
orange, and Rhodamine B. Furthermore, these membranes exhibit a rejection rate of 84.15% (MgSO₄)
and 56.58% (NaCl) [224]. While degrading dyes in a span of just one hour, the SLS-CNT/alk-MXene
membrane demonstrates an impressive 99% dye retention, a flow of 51.6 L m⁻² h⁻¹ bar⁻¹, a resistance
of 813 Ω, and an 80% recovery rate [225]. All of these outstanding characteristics are achieved by the
membrane. Photocatalytic membranes that clean themselves are an additional improvement that can
be made to the cleaning process. Over the course of six cycles, ZnO@TiC2T2 NF membranes are
able to obtain a rejection rate of 95.44% for Congo red, a permeability of 138.81 L m⁻² h⁻¹ bar⁻¹, and a
rejection rate of more than 88.48% for RhB. Furthermore, they are able to efficiently degrade 10 ppm
methylene blue [226]. By using h⁺ and O₂⁻ radicals, BiOCl/Ti₃C₂Tₓ heterostructures are able to
photodegrade 90% of ciprofloxacin in a span of thirty minutes when exposed to sun light [227].
In addition, MXenes exert a significant improvement on photocatalysts based on TiO2. Methylene
blue degradation is improved by TiO2/MXene (4:1) composites to 96.44% (UV) and 40.19%
(visible), which is 8.26 times higher than the degradation produced by pure TiO2 [228]. In the
presence of visible light, Ag@ZnO@TiC2 MXene heterojunctions exhibit a degradation rate of
90.54% for MB and 86.76% for levofloxacin, while maintaining their stability over a period of five
cycles [229].
Ultrathin Ti₃C₂Tₛ membranes are capable of delivering a flow of 85.4 L m⁻² h⁻¹ in desalination, while
rejecting around 99.5% of salt for 3.5 wt% NaCl at a temperature of 65 °C [230]. At a pressure of 0.1
MPa, TA-APTES@MXene membranes exhibit an outstanding water flux of around 5990 L m⁻² h⁻¹,
which is useful for oil–water separation [232].
In addition, MXenes contain antibacterial properties, as evidenced by the fact that Ti₃C₂Tₛ
membranes demonstrate an inhibition rate of over 73% against B. subtilis, 67% against E. coli, and
over 99% inhibition after ageing [233]. The use of MXenes as adsorbents allows for the selective
removal of ions like lead ions, even when Ca2+/Mg2+ is present [234]. Additionally, MXenes enable
the reduction of Cr(VI) to Cr(III) while simultaneously adsorbing substances [53]. For example, their
tunable surface terminations provide photocatalytic degradation efficiencies of up to 81% MB within
5 hours under UV, which is compared to 18% in the dark [235]. Additionally, tailored TiO2/TiC2
interfaces result in 2.3-fold greater dye degradation than particle TiO2/TiC2 due to effective charge
separation [237].

Table: MXene-Based Systems for Environmental Remediation

Application MXene System Key Performance Metrics Ref.

Water filtration Ti₃C₂Tₓ membrane Water flux 37.4 L (bar h m²)⁻¹ [221]

Cu²⁺ adsorption DL-Ti₃C₂Tₓ Capacity 78.45 mg g⁻¹ [222]

NF membrane HPEI-AgNP@Ti₃C₂Tₓ 24.64–30.73 L m⁻² h⁻¹ bar⁻¹, ~100% dye [224]

rejection

Dye filtration SLS-CNT/alk-MXene >99% retention, 51.6 L m⁻² h⁻¹ bar⁻¹, 80% [225]
recovery

Photocatalytic NF ZnO@Ti₃C₂Tₓ 95.44% Congo red, 138.81 L m⁻² h⁻¹ bar⁻¹ [226]

Antibiotic BiOCl/Ti₃C₂Tₓ 90% ciprofloxacin in 30 min [227]

degradation

Desalination Ti₃C₂Tₓ membrane 85.4 L m⁻² h⁻¹, ~99.5% NaCl rejection [230]

Oil–water separation TA-APTES@MXene ~5990 L m⁻² h⁻¹ at 0.1 MPa [232]

Antibacterial Ti₃C₂Tₓ membrane >73% (B. subtilis), 67% (E. coli), ~99% [233]
aged

4.5 MXenes in Biomedical Applications: Biosensing, Therapy,

Imaging, and Drug Delivery
MXenes, as 2D nanomaterials, combine extreme thinness and a high surface-to-volume ratio with
rich surface chemistry and water solubility, making them strong candidates for biomedical
applications. Their abundant reactive sites enable enzyme and drug functionalization, while
hydrophilicity avoids toxic organic solvents. These features support applications in biosensing,
diagnostics, photothermal therapy (PTT), imaging, and drug delivery.
Biosensing.​
Mediator-free biosensors benefit from MXenes’ high conductivity and biocompatibility. An
organ-like Ti₃C₂ MXene biosensor enabled efficient hemoglobin immobilization and showed a linear
H₂O₂ detection range of 0.1–260 μM [238]. A PGOx@MXene/CS glucose sensor exhibited a linear
range of 0.03–16.5 mM, sensitivity of 48.98 μA mM⁻¹ cm⁻², LOD of 3.1 μM, and retained 85.83%
performance after 200 cycles [239]. Au/Ti₃C₂–GOx biosensors detected glucose from 0.1–18 mM
with 4.2 μA mM⁻¹ cm⁻² sensitivity and retained >93% response after 2 months [240]. A Ti₃C₂-based
FET detected dopamine with LOD of 100 nM and linear response from 100 nM to 50 μM [241]. A
Ti₃C₂Tₓ/Pt-C electrochemical biosensor for SARS-CoV-2 detected 1 aM–100 nM, with LOD 0.4 aM,
LOQ 60 copies mL⁻¹, 100% accuracy/sensitivity, and 97.87% specificity, effective for saliva, swabs,
and serum [242].
Photothermal therapy (PTT) and imaging.​
Ti₃C₂ nanosheets heated aqueous dispersions by >20 °C under 808 nm, 1.0 W cm⁻² irradiation (5 min
on–off cycles). In vivo, Ti₃C₂-SP raised tumor temperature from 30 °C to 58 °C under 808 nm for 10
min, achieving complete tumor ablation [243]. MnOₓ@Ti₃C₂-SP platforms enabled combined
MRI/PAI/PTT [244]; Ta₄C₃/MnOₓ and Ta₄C₃-IONP MXenes provided MRI contrast (IONP for
T₂-weighted MRI) [245,246]. Ti₃C₁.₁₅N₀.₈₅F₀.₈₈(OH)₀.₅₆ showed strong NIR absorption of 36.6 L g⁻¹
cm⁻¹ (808 nm) and 43.5 L g⁻¹ cm⁻¹ (1064 nm) [247].
Drug delivery.​
Ti₃C₂ MXenes exhibit drug-loading up to 211.8% and pH/NIR-triggered release. Ti₃C₂-SP-DOX
enabled endogenous (H⁺) and exogenous (NIR) release [248]. MXene/Ag NP SERS-traceable carriers
achieved LOD 10⁻⁸ M (4-MBA) and glutathione-triggered DOX release [249]. MXene@Gellan gum
hydrogels enabled NIR-responsive release with good biocompatibility [250]. Ultrathin Ti₃C₂Tₓ
showed 47.1% photothermal conversion efficiency and 72.8% DOX loading; a targeted
Ti₃C₂Tₓ-DOX-PMAsh-Tf platform inhibited tumors in vitro/in vivo [251].
Nanozymes and antibacterial activity.​
MXene-based nanozymes enhanced ROS generation and tumor regression; an Nb₂C-based plasmonic
assembly reduced HeLa cell viability by 38.67% versus pristine nanozymes [Hao et al., 2021]. V₂C
MXenzymes mimicked multiple antioxidant enzymes and restored redox homeostasis in vivo (Feng
et al., 2021). MXenes also show antibacterial effects: fresh Ti₃C₂Tₓ membranes inhibited >73% B.
subtilis and 67% E. coli, increasing to >99% upon aging, with >70% cell death after 24 h (Rasool et
al., 2017).

4.6 MXene-Enabled Field-Effect Transistors: Sensing and Electronic

Applications
Heavy-Metal Ion Detection Using MXene FETs
MXene-based field-effect transistors (FETs) have demonstrated exceptional capability for detecting
toxic heavy-metal ions, particularly Hg²⁺ and Ag⁺, owing to the high surface activity and
environmental sensitivity of two-dimensional MXenes. According to Liu et al., Ti₃C₂Tₓ-based MXene
FETs enable rapid Hg²⁺ detection within 10 s, with a detectable concentration as low as 5 ppm. The
Hg²⁺ adsorption energy on MXenes is calculated to be −1.298 eV, indicating strong binding affinity.
Importantly, these MXene-FET sensors retain functionality in high-salinity environments, exhibiting
a strong response even in 1 M NaCl, which confirms their suitability for real water sample analysis,
including tap water.
Upon adsorption, Hg²⁺ is reduced to Hg⁺ and interacts with surface terminal groups such as –Cl.
Structural and electrical stability of Ti₃C₂Tₓ MXenes was verified by SEM imaging and output
characteristics after 4 days of air storage, while transfer curves confirmed their n-type semiconducting
behavior.​
Similarly, Ti₃C₂Tₓ MXene FETs for Ag⁺ detection showed response times of only a few seconds,
combined with high sensitivity, selectivity, and ease of operation.

MXenes as Contacts and Electrodes in High-Performance FETs

MXenes are increasingly used as electrodes and contact layers in high-performance FET
architectures. Jiao Xu et al. employed stacked Ti₂C(OH)ₓFᵧ MXene flakes as source electrodes to
fabricate WSe₂ p-FETs and MoS₂ n-FETs. Electrical transport measurements at room temperature
confirmed efficient carrier injection, attributed to favorable band alignment between MXenes and
semiconductor channels.
Further improvements were achieved by intercalating Ti₃C₂Tₓ with didecyldimethyl ammonium
bromide (DDAB), which significantly enhanced charge-carrier mobility in ambipolar polymer-based
OFETs. MXenes have also been demonstrated as source electrodes in metal-halide perovskite FETs,
using (PEA)₂SnI₄ as the semiconducting layer. Additionally, an ultrathin Ti₂CO₂ semiconductor FET
seamlessly integrated with Ti₂CF₂ metallic electrodes has been theoretically proposed, highlighting
MXenes’ versatility across metallic and semiconducting roles.

Flexible and Organic FET Architectures

For flexible electronics, uniform MXene electrode arrays have been fabricated on plastic substrates
for high-performance organic FETs (OFETs). Using asymmetric source–drain MXene electrodes,
pentacene-based p-type OFETs showed efficient hole injection under negative drain voltage (Vᴅ).
Energy band analysis confirmed reduced carrier-injection barriers at the MXene/organic interface,
enabling stable transistor operation.

Virus and Biomolecule Detection via MXene-FET Platforms

MXene-FETs have been extended to ultrasensitive biosensing, including virus detection. During the
COVID-19 pandemic—when over 46.6 million infections and 1.2 million deaths were reported
worldwide—MXene–graphene hybrid FETs were developed for 2019-nCoV and influenza virus
detection. These sensors exhibited an average response time of 50 ms and a limit of detection (LOD)
of 125 copies mL⁻¹, with a ~10% change in source–drain current and gate voltage.
Additionally, graphene-based FET biosensors functionalized with antibodies against the
SARS-CoV-2 spike protein successfully detected virus antigens in nasopharyngeal swab samples,
cultured virus, and protein solutions, confirming clinical applicability.

Salinity and Chemical Sensing

Ti₃C₂Tₓ MXene FETs exhibit a strong response toward high-salinity alkaline environments, enabling
applications in seawater and wastewater monitoring. Upon NaOH treatment, XPS analysis revealed
increased Ti–OH and O–Ti–O bond intensities and a corresponding decrease in Ti–X bonds,
providing a clear electronic signature for alkali detection.
For gas sensing, single-atom Pt-implanted Ti₃C₂Tₓ MXene FETs significantly outperformed pristine
MXenes. These sensors detected triethylamine (TEA) at concentrations as low as 14 ppb, with
excellent multicycle stability. Density functional theory (DFT) simulations confirmed enhanced
adsorption and charge-transfer mechanisms due to Pt single atoms.

Neurotransmitter, Exosome, and Biomarker Detection

Highly conductive Ti₃C₂Tₓ MXene micropattern FETs have been used for label-free dopamine
sensing and real-time monitoring of hippocampal neuron spiking activity. Structural characterization
confirmed the removal of Al from Ti₃AlC₂, with (002) XRD peaks shifting from 9.5° to 8.8° and
(004) peaks from 19.4° to 18.5°, indicating successful MXene formation and interlayer expansion.
MXene-based extended-gate FET (EGFET) biosensors enabled exosome detection in human serum,
targeting the CD9 biomarker with a LOD of 10.64 pM. For inflammatory marker sensing, spiral
interdigitated MXene-assisted FETs (SiMFETs) achieved an IL-6 detection range of 10 fg mL⁻¹ to
100 ng mL⁻¹, maintaining stable performance for 2 months with high selectivity and repeatability.

MXenes as Gate Electrodes

MXenes can also function as van der Waals (vdW) gate electrodes. In GaN high-electron-mobility
transistors (HEMTs), Ti₃C₂Tₓ MXene gates with a thickness of ~100 nm were spray-coated onto
AlGaN/GaN wafers. The vdW gap between the MXene gate and AlGaN layer resulted in reduced
hysteresis during up-sweep and down-sweep measurements, outperforming conventional Ni/Au gate
electrodes and demonstrating superior interface quality.

5. Environmental Impact and Circular Economy of

MXenes

5.1 Environmental Cost of MXene Synthesis and the Transition

toward Greener Routes

The classic top-down synthesis techniques are mostly responsible for the environmental pressure that
is associated with the manufacturing of [Link] acid (HF) or in-situ prepared HF
solutions (such LiF/HCl, for example) are commonly utilised in the way of traditional etching of
MAX phases rather than different techniques. Etching is a process that involves getting rid of the
A-layer, which is usually made up of aluminium components. This removal is done in a careful
manner. The use of HF in chemical processes is beneficial; however, it is extremely corrosive and
dangerous, and it results in the production of waste streams that are abundant in fluoride. On top of
that, it raises significant issues for both the environment and organisations that employ people. Due to
the fact that these negative consequences are occurring, the scalability of MXene synthesis within
frameworks of sustainable manufacturing is significantly restricted.
As a means of responding to the problem, the field has gradually begun to implement green synthesis
[Link] of all of them, the Lewis acidic molten salt etching technique is a revolutionary
step forward that marks a step forward in the progression of things. Molten salts that are heated to
high temperatures, such as ZnCl2, FeCl2, or CuCl2, are utilised in redox-driven replacement chemical
reactions in order to eliminate the A-site element. These processes are carried out at elevated
temperatures. Fluoride complexation is not utilised in this process. Through this method, aqueous
hydrogen fluoride is completely removed, which results in a large reduction in harmful effluents and
deterioration caused by oxidation.
One more advantage that comes with sustainability is the integration of processes. Using Lewis acidic
etching, it is possible to simultaneously produce MXenes and metallic nanoparticles, facilitating the
direct formation of MXene/metal nanocomposites without the necessity for additional steps to
incorporate them afterward. In addition to reducing the length of synthesis routes, this also reduces
the total amount of energy consumed and the amount of chemicals used, bringing the production of
MXene into alignment with the concepts of green chemistry.

5.2 MXenes as Functional Materials for Environmental Remediation

From a circular economy perspective, materials must actively contribute to restoring environmental
quality and enabling resource recovery. MXenes excel in this role due to their layered structure, high
density of active sites, and tunable surface terminations.
Water Purification and Resource Recovery
MXene nanosheets are intrinsically hydrophilic, allowing rapid water transport while simultaneously
interacting strongly with dissolved ions and organic molecules. Delaminated Ti₃C₂Tₓ nanosheets
exhibit a copper adsorption capacity of 78.45 mg g⁻¹, demonstrating their ability to recover valuable
metals from wastewater rather than merely immobilizing them.
In membrane-based filtration, the lamellar architecture of MXenes forms sub-nanometer transport
channels that facilitate high flux without sacrificing selectivity. Pure MXene membranes achieve
water permeabilities as high as 37.4 L bar⁻¹ h⁻¹ m⁻², exceeding many polymeric and ceramic
membranes.
Performance is further enhanced through composite design. Sodium lignosulfonate–CNT/alkalized
MXene membranes achieve over 99% retention of hazardous dyes such as Methyl Blue and Congo
Red while sustaining a flux of 51.6 L m⁻² h⁻¹ bar⁻¹. Similarly, HPEI-AgNP@Ti₃C₂Tₓ membranes
exhibit near 100% rejection of organic dyes and meaningful salt rejection (e.g., for MgSO₄ and
NaCl), enabling water reuse and industrial loop closure.
Catalytic Degradation of Pollutants
Beyond physical separation, MXenes actively participate in chemical degradation pathways. Their
metallic conductivity promotes charge separation, while surface terminations facilitate redox
reactions. For example, BiOCl/Ti₃C₂Tₓ heterostructures photodegrade 90% of ciprofloxacin within 30
min under solar irradiation, addressing the growing threat of antibiotic residues. Likewise,
TiO₂/MXene composites demonstrate methylene blue degradation rates 8.26 times higher than pure
TiO₂, illustrating the synergistic role of MXenes in photocatalysis.
In order for materials to be regarded a part of a circular economy approach, they must actively
contribute to the reconstruction of environmental quality and the facilitation of resource recovery. In
this particular function, MXenes are able to perform extraordinarily well due to their layered
structure, high density of active sites, and surface terminations that may be customised ,the
reclamation of resources and the purification of water. Despite the fact that they have a significant
interaction with dissolved ions and organic molecules, MXene ,Ti₃C₂Tₓ nanosheets are inherently
hydrophilic, which enables them to easily transport water. Through an example of a copper
adsorption capacity of 78.45 mg g⁻¹, the nanosheets of delaminated titanium carbide demonstrate their
capability to recover important metals from wastewater. The standard plan of action, which consists
of only immobilising the metals, stands in contrast to this novel way.
The lamellar architecture of MXenes that is used in membrane-based filtering creates transport
channels that are sub-nanometer in size. Over the course of the process, it is possible to attain high
flow through these channels with no loss of selectivity. When compared to the water permeability of
other polymeric and ceramic membranes, the water permeability of pure MXene membranes can
reach as high as 37.4 L bar⁻¹ h⁻¹ m⁻². This is a substantial level of enhancement.
In order to get even greater performance enhancements, designing with composite materials is
possible. In the presence of a flux of 51.6 L m⁻² h⁻¹ bar⁻¹, sodium lignosulfonate–CNT/alkalized
MXene membranes are able to obtain a retention rate of over 99% for hazardous dyes including
Methyl Blue and Congo Red. Furthermore, regarding organic dyes, HPEI-AgNP@Ti₃C₂Tₓ
membranes show an impressive rejection rate of around 100 %. The fact that these membranes have a
high rejection rate for salts, such as sodium chloride and magnesium sulphate, makes it possible to
reuse water and to close industrial loops of production. An approach that is catalytic in nature to the
degradation of pollutants .Besides their role in the process of physical separation, MXenes are also
actively involved in a wide variety of chemical breakdown pathways. This is in addition to their
function in the process of physical separation. It is easier for redox reactions to take place when
surface terminations are present, and the metallic conductivity of surface terminations aids to help
separate charges. For example, heterostructures made up of BiOCl/Ti₃C₂Tₓ are able to photodegrade
ninety percent of ciprofloxacin in just thirty minutes when they are subjected to the photodegradation
process of the sun. This novel approach effectively handles the matter of antibiotic residues, which is
becoming an increasingly serious issue. An additional example of the synergistic effect that MXenes
play in photocatalysis is demonstrated by the fact that TiO₂/MXene composites exhibit methylene
blue degradation rates that are 8.26 times higher than those of pure TiO₂.
5.3 Energy Efficiency and Carbon Neutrality Contributions
Circular economies depend on low-carbon energy systems and efficient material utilization. MXenes
contribute meaningfully to both through electrocatalysis and energy storage.
Carbon Capture and Utilization (CCU)
The electrochemical reduction of CO₂ into fuels and chemicals offers a pathway to close the carbon
loop. Single-atom Cu anchored on Ti₃C₂Tₓ MXene achieves a Faradaic efficiency of 59.1% for
methanol formation at −1.4 V, demonstrating selective CO₂ conversion. The high density of electronic
states near the Fermi level and strong metal–support interactions stabilize reaction intermediates,
improving efficiency and selectivity.
Green Ammonia Synthesis
MXenes also show promise in the nitrogen reduction reaction (NRR), offering an alternative to the
energy-intensive Haber–Bosch process. Fe-functionalized MXene catalysts deliver a Faradaic
efficiency of 21.8% with an ammonia yield of 18.25 µg h⁻¹ mg⁻¹ at ambient conditions. This
low-temperature, electrochemical route supports decentralized and sustainable fertilizer production.

5.4 Material Lifespan, Reusability, and Recyclability

Longevity and reuse are central to material circularity. MXene-based systems demonstrate
encouraging durability across applications.
In energy storage, high-entropy MXene composites in Li–S batteries maintain stable electrochemical
performance over 1,200 cycles, minimizing replacement frequency. In environmental remediation,
ZnO@Ti₃C₂Tₓ membranes retain separation efficiency over six regeneration cycles, with dye
rejection remaining above 88.48%.
Recoverability is equally important. Sodium lignosulfonate–CNT/alkalized MXene membranes
exhibit an 80% recovery rate after fouling, highlighting their potential for repeated industrial
deployment without significant performance loss.

6. Why Some MXene Applications Will Succeed—and

Others Will Not: A Critical Analysis

6.1 The Winners: High-Value, Space-Constrained Applications

6.1.1 electromagnetic interference (EMI)

The biggest likelihood of commercial success is associated with applications that make use of the
unique duality that MXene possesses, which is the combination of hydrophilic processing and
metallic conductivity. As a result of its superior performance metrics in these areas, MXene is able
to justify a higher price point than other materials that are currently in use.
Protection against electromagnetic interference (EMI): The proliferation of 5G and 6G
telecommunications calls for the utilisation of shielding materials that are not only incredibly thin
but also perform exceptionally well. Carbon composites frequently demand thicknesses that are not
possible in order to achieve significant attenuation. This is sometimes the case. On the other hand,
conventional metal shields are nothing more than an additional burden and added mass to the
system. The "multiple internal reflection" mechanism that MXenes possess allows electromagnetic
waves to be trapped and dispersed between the conductive layers, which is the reason why they are
successful in this circumstance.
Justifications for its success: In place of millimetres of polymer composites, a few microns of
MXene were used. The manufacturing benefit that results from the ability to print these shields
directly onto circuit boards using aqueous inks (because to the hydrophilicity of the material)
justifies the expense of the material.

6.1.2 Microsupercapacitors and Wearable Energy:

In the competition for miniaturisation, volumetric capacitance, which refers to the amount of energy
per unit volume, is more important than gravimetric capacitance, which refers to the amount of
energy per unit weight. In the industry, porous carbon is considered the norm since it is too "fluffy"
(low density <1 gcm-3) to store adequate energy in small places.
Because MXenes are dense (about 4 grammes per cubic centimetre) and store energy through rapid
surface redox reactions (pseudocapacitance), this endeavour is expected to be successful. The
volumetric capacitances of MXene hydrogels have been measured to be 1500 F cm-3, which is nearly
three times higher than the capacitances of carbon electrodes using experimental data. It is more
likely that this performance disparity will be accepted when it comes to wearable devices, which are
characterised by a limited amount of space.

6.1.3 Mediator-Free Biosensors:

​
At this time, commercial glucose sensors are dependent on enzymatic mediators, which wear down
over time and reduce their shelf life. For "mediator-free" sensing, the metallic conductivity of MXene
makes it possible for direct electron transfer to take place.
Why it will be successful: Through clinical trials, it has been established that sensors based on
MXene are capable of detecting viral markers (such as SARS-CoV-2 RNA) with a detection limit of
0.4 aM (attomolar) and a hundred percent accuracy, which is a major improvement over the optical
approaches that are currently in use. That this application is able to combine high sensitivity with
extended stability is what makes it a successful proposition.
6.2 The At-Risk Applications: Commodity and Bulk Markets
Conversely, applications that attempt to force MXene into "commodity" roles where cheap,
established alternatives exist face a high risk of commercial failure.
●​ Bulk Water Treatment (Adsorption):​
While MXenes are excellent adsorbents for heavy metals and dyes—with adsorption
capacities for copper reaching 78.45 mg g-1—they compete against activated carbon, which
costs pennies per kilogram.
○​ Why it will likely fail: Unless the target pollutant is extremely high-value or toxic
(requiring specificity that carbon lacks), the cost of synthesizing MAX phase
precursors and the etching process makes MXene economically unviable for municipal
water treatment.
●​ Standard Lithium-Ion Battery Anodes:​
Research shows MXene anodes achieve capacities (~400 mAhg-1) comparable to or slightly
better than graphite (~372 mAhg-1).
○​ Why it will likely fail: Graphite is dirt cheap and boasts a massive, mature supply
chain. A marginal improvement in capacity does not justify the massive cost
differential. MXene will likely only succeed here as a conductive additive (in small
quantities) rather than as the primary active material.

6.3 The Critical Filter: The Stability and Scalability Bottleneck

The dividing line between success and failure is also drawn by the synthesis method. The traditional
Hydrofluoric Acid (HF) etching route is a barrier to success due to safety hazards and the resulting
lower quality (fluorine-terminated) material.
●​ The "Killer" Flaw: Oxidation. Ti3C2Tx tends to degrade into titanium dioxide (TiO2) and
carbon when exposed to water or air, destroying its conductivity. Applications requiring
long-term environmental stability (e.g., outdoor solar cells) will fail unless this is solved.
●​ The Path to Success: The shift toward Lewis acidic molten salt etching (e.g., using CuCl2) is a
critical enabler. This method produces Fluorine-free MXenes with better electrochemical
performance (e.g., higher capacity in Li-ion batteries due to -O and -Cl terminations) and
improved safety. Applications utilizing this synthesis route have a much higher chance of
survival than those relying on HF-etched material.

Table : The Commercial Deployment of MXenes: Perspectives on Opportunities and Limitations

Commerc
Application Market Benchmark MXene Performa Limiting ial
Area Class Materials Advantage nce Factor Outlook
Metrics
Electromagne High-value Metals (Cu, Combined Shielding Material High
tic , Al), carbon reflection + effectivene cost probability
Interference space-con composites absorption ss > 90 dB of success
(EMI) strained via lamellar with due to
Shielding electronics multiple-refl micron-thic ultrathin
(5G/6G, ection k films form factor
aerospace mechanism (≈99.9999 and
, % printable
wearables) attenuation aqueous
) inks

Microsuperca Miniaturize Activated Extremely Density ≈ 4 Oxidation Strong

pacitors & d carbon, high g cm⁻³; stability success
Wearable electronics graphene volumetric volumetric potential
Energy , aerogels capacitance capacitanc where
Storage implantabl from dense e up to volume,
es, IoT pseudocapa 1500 F not weight,
citive cm⁻³ (vs. is the key
structure ~300 F constraint
cm⁻³ for
carbon)

Mediator-Fre Clinical Enzyme-bas Direct Detection Surface High

e Biosensors diagnostic ed electron limit 0.4 oxidation, likelihood
s, electrochemi transfer aM, 100% biofouling of
point-of-ca cal sensors enabled by clinical adoption
re testing metallic accuracy; due to
conductivity stability > superior
60 days sensitivity
and shelf
life

Bulk Water Municipal Activated High Cu²⁺ High Low

Treatment and carbon, adsorption adsorption synthesis likelihood
(Adsorption) industrial zeolites capacity capacity cost, of success
wastewate and surface 78.45 mg scalability except for
r functionality g⁻¹ niche,
high-toxicit
y
pollutants

Lithium-Ion Mass-mar Graphite Slightly MXene ≈ Cost, Unlikely to

Battery ket energy higher 400 mAh oxidation, replace
Anodes storage theoretical g⁻¹ vs. immature graphite;
(Primary capacity graphite ≈ supply viable only
Material) 372 mAh chain as
g⁻¹ conductive
additive
 Outdoor or Solar cells, Metals, High Conductivit Severe Commerci
Long-Term sensors, stable conductivity y rapidly oxidation ally
Environmenta infrastruct oxides and degrades in unviable
l Devices ure processabili upon air/water without
ty oxidation stabilizatio
to TiO₂ n
strategies

EMI + Energy Defense, Multilayer Simultaneo High SE + Manufactu Strategic

Hybrid aerospace composites us shielding fast charge ring scale niche
Applications , drones and energy capability success
storage likely

Printable/Flex Smart ITO, polymer Clay-like Stable Cost vs. Moderate–

ible textiles, conductors rheology conductivit ITO high
Electronics foldable and y under success in
devices mechanical thousands premium
durability of bending devices
cycles

HF-Etched General — Established Fluorine-te Safety, Low

MXene research synthesis rminated poor commerci
Applications prototypes route surfaces stability al viability

Lewis-Acid Advanced — F-free Higher Process Highest

Etched energy & terminations electroche optimizati chance of
MXene electronics (–O, –Cl), mical on long-term
Applications improved performan survival
stability ce and
safety

7. Evolution of MXenes: From Fundamental Studies to

Practical Challenges:
Following the discovery of graphene, there has been a significant increase in the amount of research
interest given to two-dimensional (2D) materials. MXenes, which are exfoliated from stacked MAX
phases, have quickly evolved as a desirable material family due to their superior electrical
conductivity, varied surface chemistry, layered structure, and compositional diversity. In particular,
among them, MXenes have emerged as a family of materials that have been beneficial. Although
MXenes have features that are equivalent to those of graphene, research on MXenes is still in its early
stages, particularly with regard to the control of synthesis and the scalability of the phenomenon.
It is through the process of chemical etching of MAX phases that include Al or Si that the vast
majority of MXenes are formed. Because of this process, surface terminations such –F, –OH, and –O
are introduced into the system. The bare MXenes that do not have surface groups are still not well
investigated, despite the fact that these terminations are frequently advantageous. Bottom-up
approaches such as chemical vapour deposition (CVD), template-assisted synthesis, and
plasma-enhanced pulsed laser deposition (PEPLD) have been developed in order to overcome this
issue. However, at the present time, CVD has only been successful in synthesising a limited number
of MXenes, such as Mo₂C. The difficulty of applying these methodologies to different types of
compositions continues to be a significant one.
MXenes have developed beyond its traditional forms in terms of their structure and composition,
resulting in the creation of i-MXenes, o-MXenes, double transition-metal MXenes, and high-entropy
MXenes. This has resulted in a significant expansion of the design space. MXenes have shown that
they have a great amount of potential in the field of energy storage, despite the fact that inadequate
electrochemical stability continues to be a barrier. In addition to having excellent conductivity,
non-delaminated MXenes provide substantial quantities of interlayer space for the storage of charged
particles. There are a great number of semiconducting MXenes with direct and indirect bandgaps that
have been predicted by theoretical research; nevertheless, no practical realisation has yet been
accomplished. It is possible to produce semiconducting behaviour through quantum confinement
using MXene quantum dots (QDs). The shift from Ti3C2 to TiO2 quantum dots is an example of an
oxidation process that requires careful management.
In the realm of environmental remediation, MXenes, and more specifically Ti3C2Tx, are employed
extensively for the aim of water treatment, adsorption, and membrane separation by means of a wide
range of applications. This is in contrast to the fact that virgin MXenes have low photocatalytic
activity due to their restricted light absorption and quick charge recombination. Surface chemistry
tailoring makes it possible for efficient photocatalysis and pollutant adsorption to take place. On the
other hand, the fabrication of MXene membranes that are not only stable but also exceptionally
hydrophilic remains a difficult task.
The use of MXenes in biological applications is now being researched at a quick pace due to the fact
that they possess a large surface area, conductivity, and photothermal efficiency. Biosensors,
photothermal cancer therapy, and drug administration are some examples of these uses among others.
The clinical translation of promising treatments is hampered by the fact that there is a dearth of data
about biosafety, toxicity, and long-term biocompatibility at the present time.
The conventional method of producing MXene is not only costly but also dangerous, and it requires a
lot of energy. It relies on high-temperature MAX synthesis and toxic HF etching, which are both
practices that are not environmentally friendly. Molten salt protected synthesis, alkali etching, ionic
liquids, electrochemical etching and Lewis acidic molten salt etching are some examples of green
synthesis techniques that are just starting to develop. These strategies offer enhancements in security,
termination control and scalability. Particularly noteworthy is the fact that Lewis acidic etching makes
it possible to achieve uniform halogen terminations (–Cl, –Br, and –I), programmable termination
exchange, in-situ metal nanoparticle creation, and the ability to apply to non-Al MAX phases and
nitride MAXs. There are still challenges to be conquered, however, in terms of the efficiency of
delamination, the stability of termination in air, the aggregation of metal nanoparticles, and the
optimisation of parameters.
It is essential that future research on MXene take the following into consideration:
 a)​ An technique to synthesis that is not only safe but also favourable to the environment and
scalable
b)​ Reasonable precursors for MAX, including those obtained from recycled and bio-sourced
sources, are included in this category.
c)​ Engineering enhancements and controlled terminations for use in the event of faults
d)​ Within the context of Lewis-etched MXenes, delamination is a phenomenon.
e)​ Toxicological and life-cycle impact assessments that are exhaustive in nature
f)​ Growth in the areas of semiconducting MXenes, catalysis, innovative biomedical systems,
and environmentally friendly energy technologies
In general, MXenes are a class of two-dimensional materials that are undergoing rapid development
and demonstrate outstanding potential in the fields of energy, environment, electronics, and
biomedicine. However, before extensive practical deployment can take place, there are fundamental
difficulties that need to be cleared up in the areas of synthesis, stability, and safety.

References

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synthesis, properties, and applications of MXenes. Oxford Open Materials Science, 5(1),

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14.​
synthesis
Synthesis of MXene

The development of MXene synthesis pathways had a significant impact on their

electrical characteristics, physicochemical features, and a wide range of
applications. In general, there are three types of MXene synthesis techniques:
Etching, top-down, and bottom-up. In the etching method, the “A” elements from
the MAX phases of the parent three-dimensional (3D) layer result in the MXenes
layered structures. Until now, the most prevalent approach for synthesizing
MXenes has been recognized as the top-down strategy (see Figure 2). Unlike the
top-down fabrication approach, which usually requires a large number of precursor
materials, the bottom-up synthesis fabrication route requires few organic or
inorganic molecules/atoms when carefully constructing the structure. Using a
crystal growth method, the precursors can be assembled into a definite 2D order
constituting the MXene structures. The advantages of the bottom-up approach
allow for exquisite control of the size distribution, shape, and surface terminal
functionalities of MXenes in an appropriate way [31].
Normally, MXenes refers to M
n
X
n–1
(n = 2, 3, and 4) layers formed by removing interlayer “A” atoms from the
metal-ceramic MAX phase (where M stands for the transition metals, A is the
group IIIA or IVA elements, and X represents the C and N elements). The M and X
atoms stack to form a hexagonal lattice in the MAX phase, with the atoms of X
occupying the M octahedral cage center shared by its edges. When the atoms of A
are removed from the layer of M
n
X
n–1
, the hexagonal-lattice of MX, rather than the cubic lattice, is preserved. Hence, the
layer of M
n
X
n–1
 can be produced by removing the A-atoms. As with its predecessor MAX,
MXenes thin sheets are frequently oriented horizontally. The bulk of MXenes have
good mechanical features and are likely to be quite durable [32].

2.2. Top-Down Approaches

Top-down synthesis refers to a process where large bulk structures

are broken down into smaller particles. Following the successful
synthesis of Ti3C2Tx MXene from Ti3AlC2, top-down
synthesis has become the primary approach for preparing MXene
materials. This involves removing the A layer from the precursor
Mn þ1AXn phase through a process called etching, converting it
into MXene. The M-A bond in the precursor is too strong to be
broken through mechanical exfoliation, so chemical etching
methods are used instead. MXenes, however, can be produced
from non-MAX phases that contain both MX layers and A-containing
compound layers. The bond between these compound
layers and MX layers is weaker compared to the single elemental
A layers found in conventional MAX phases [49]. The choice of
synthesis methods has a significant impact on the quality, size,
and properties of the resulting MXene flakes. Some of the etching
techniques, the role of intercalation of ions between the MXene
flakes and delamination are discussed below.

For a long time, the top-down strategy has been well-established, especially in the
synthesis and design of nanomaterials. These methods often involve the cleavage
of 2D or 3D bulky precursor material into essential minute quantum particles
[48,49,50]. Graphite, carbon nanotubes, graphene, MoS2 crystals, WS2 powder,
black phosphorus, g-C3N4, and other three-dimensional and two-dimensional bulk
precursors have been effectively transformed into quantum dots utilizing the
top-down technique. Ball-milling [51], liquid exfoliation, chemical etching,
electrochemical [52], intercalation, hydrothermal/solvothermal treatment,
ultra-sonication, microwave irradiation, and other procedures are among them. The
majority of the top-down approaches establish the initial O2-containing
functionalities on the surface of catalysts, which facilitate the creation of defects in
the catalysts [53]. The surface defects serve as reactive sites and allow the bulk
molecules to split into tiny quantum particles [54]. This technique is of great
significance because it can be operated at low temperatures. Further, copious raw
materials can be used in this technique, and large-scale production can be achieved.
The low yield and the need for particular treatments are, however, drawbacks. The
most extensively utilized top-down approaches for the fabrication of MXene
include ultrasonication, ball-milling, intercalation, hydrothermal, solvothermal,
micro-explosion, and acid reflux. In this section, the details of top-down
approaches for the synthesis of MXenes are discussed.
HF etching
Etching of most of the carbide containing MAX phase is done by
treating the material in an aqueous solution of hydrofluoric acid
(HF). With the right HF concentration and etching temperature,
high quality MXene flakes can be produced. The MXene produced
have a functional group -OH, -F, or -O attached to its surface. The
first MXene to be produced through selective etching is Ti3C2. It is
produced by the selective etching of Al from Ti3AlC2 using hydrofluoric
acid (HF) [50]. During the etching process, Ti3AlC2 powders
are placed in a solution of 50 wt% Hydrofluoric Acid (HF) for 2 h
at room temperature. Afterward, centrifugation is performed,
and the powders are cleaned with deionized water until the pH
level is close to 6. This process selectively etches the Al layer
while preserving the Ti-C bonds, as the Ti-A bonds are stronger
in comparison as shown in Fig. 3. As a result, surface groups such
as F, OH, or a combination of both are formed and attached to
the MXene surface [7]. The reaction also produces H2 gas. The
formation of these surface groups is facilitated by the electrophilic
nature of the outer transition metal in conjunction with
the surface groups. Increasing the concentration of HF increases the no. of
defects. Thinner MAX phases such as M2AX require less exposure
time to HF in comparison to thicker MAX phases such as M3AX2
and M4AX3 [51]. Alhebeb et al. observed that lower concentration
of HF is sufficient to etch the Al layer. The HF concentrations of
5, 10, and 30 wt % are compared, with 5 wt % proving sufficient
for Al removal, though higher concentrations (≥30 wt %) require
shorter etching times (5 h for 30 wt %, 18 h for 10 wt %, and 24 h
for 5 wt %). The synthesis process includes gradually adding
Ti3AlC2 to HF, followed by washing and centrifugation cycles until
the supernatant reaches a neutral pH (�6). The resulting
MXenes, labeled as 30F-, 10F-, and 5F-Ti3C2Tx, exhibit different
morphologies. Higher HF concentrations (30 wt %) results in an
accordion-like structure, due to gas release (H2) during the exothermic
reaction. Lower HF concentrations (5 wt %) result in a
less altered structure, barely distinguishable from the original
MAX phase. Despite the morphological differences, all HF concentrations
effectively etch Al layer. [52]. In Fig. 4, the Scanning
Electron Microscope (SEM) images and the corresponding X-ray
diffraction (XRD) data reveals the possibility of MAX phase etching
at low HF concentrations. Ying et al. produced Ti3C2Tx nanosheets
by etching bulk Ti3AlC2 powders in HF aqueous solution
for 24 h. The interspace between the Ti and C layers is filled with
H2 gas and thus enlarged. The layers were later intercalated with
dimethyl sulfoxide (DMSO) and delaminated to 2-D Ti3C2Tx nanosheets
by sonication [53]. Zhou et al. proposed a technique that
involves alloying Ti into V2AlC, resulting in a weaker M-A bond.
This weaker bond facilitates the etching process of the (V1-
xTix)2AlC MAX phase using a 30 wt% HF solution, yielding (V1-
xTix)2C [54]. In another study, the Mo4VAlC4 MAX phase was
etched to produce Mo4VC4Tx. Interestingly, the central M layer in
this case exhibits twinning, a feature not observed in other MAX
phases or MXenes [55]. This study suggests the potential existence
of a subfamily of MXenes with twinned central metal
layers in the M'4M''X4Tx structural configuration. Furthermore,
non-Al-containing MAX phases have also been subjected to etching
to produce MXenes. Alhabed et al. achieved the etching of the
Si layer in Ti3SiC2 through oxidation-assisted HF-oxidant mixtures,
resulting in Ti3C2 [56]. Similarly, Mo2C can be obtained by
etching the Ga layer in Mn þ1GaXn precursor using an acidic solution
containing Fþ ions [57]. Some phases possess an Al-
containing compound layer with structures like (MC)n(Al, Si)4C3
and (MC)nAl3C2, rather than a single Al layer. These structures
can be etched using HF solutions to form Zr3C2Tx and Hf3C2Tx
[58, 59].Tao et al. used 40 wt% HF as an etchant to produce Ti3C2
MXene at room temperature. The Al layers were exfoliated by
stirring the sample for 24 h [60]. Naguib et al. synthesized Nb2C
and V2C MXene by HF etching for its use in Li-Ion batteries.
Nb2AlC and V2AlC were dipped in 50% HF solution for the exfoliation
of Al layers for 90 h at room temperature [61].
HF forming etchants
HF is dangerous and has the ability to enter the eyes, skin,
muscles, and bones, leading to lasting harm. A widely recognized
approach, suggested by Ghidiu et al., involves the creation of HF
acid on the spot by combining fluoride salts (such as LiF, NaF, KF,
NH4F, and FeF3) with HCl. In this process, fluorides release F-
,
while Hþis derived from HCl. The resulting hydrophilic MXenes
exhibited an increase in volume when hydrated, enabling them
to be molded similar to clays [62]. This modified approach offers
a relatively safer and simpler method, while also allowing for a
faster process of separating MXene flakes. This separation facilitates the insertion
of cations into the interlayer space,
thereby reducing the strength of interlayer interactions. This
technique enables the production of larger flakes with fewer
atomic defects compared to MXenes obtained through pure HF
etching. Nonetheless, this approach is unable to fully etch the
MAX phase, leading to significant challenges in achieving high
yields for mass production. This etching strategy introduces additional
chlorine (Cl) terminations, which can be problematic.
Different etching agents (e.g. HF, LiF/HCl, FeF3/HCl) significantly
influence the surface chemistry, structure, and properties
of MXenes [63, 64]. These agents determine the type of surface
terminations (–F, –OH, –O), oxidation sensitivity, delamination
ability, and defect concentration [65].
Hydrothermal etching with low-toxicity agents (e.g. NaBF4, HCl) results in
MXenes with larger
interlayer distances and higher BET surface areas than traditional
HF etching [66]. The particle size and morphology of the
MAX phase also play a critical role. Reducing the particle size
through methods like ball milling decreases the intensity and
time required for etching and affects the quality of the resulting
MXenes [67]. In 2014, Ghidiu synthesized Ti3C2Tx by etching
Ti3AlC2 using a LiF/HCl solution, which generates in situ HF to remove
the Al layer from the MAX phase [68]. Wang followed in
2016, using NH4F to achieve a similar outcome, with HF generated
during the etching process. These methods reduce interlayer
coupling and increase the spacing between MXene layers,
thus making delamination into monolayer or few-layer flakes
easier [69]. The pre-intercalation of NH4 or Li⁺ cations during
etching helps facilitate this process. Below are the reactions on
the etching of Ti3C2Tx by LiF/HCl and NH4F.
LiF +HCl !HF þLiCl (2.1)
NH4F þ H2O !NH3:H2O þHF (2.2)
Hand-shaking the Ti3AlC2/LiF mixture alone results in high-
quality MXene nanosheets with fewer defects and larger dimensions.
The shaking process can also yield single or few-layer
MXene sheets with improved structural integrity [70]. Kajiyama
et al. synthesized Ti2CTx MXene by stirring the Ti2AlC powders in
of 30 ml of 6 M HCl aqueous solution containing 0.9 M LiF for 15 h
at 40�C. The same group also synthesized Ti3C2 MXene by etching
Ti3AlC2 in a mixture of 30 ml of 10 M HCl aqueous solution containing
2.3 g LiF for 15 h at 40�C [71]. Wang et al. reported the formation
of Ti3C2Tx MXene by etching the Al layer from Ti3AlC2
MXene using FeF3/HCl solutions. 1.5 g of Ti3AlC2 powders were introduced
into the FeF3/HCl mixture (2 g of FeF3.3H2O added to
20 ml of 6 M HCl) and heated to 60�C for 50 h [62]. Liu et al.
reported the formation of V2C MXene from V2AlC MXene by immersing
it in a NaF/HCl solution. The solution contains 40 ml of
HCl and 2 g of NaF. 2 g of V2AlC powders were introduced to the
mixture and heated at 90�C for different times (48, 72, 128, and
168 h) [72]. An acid mixture containing a lower concentration of
HF in a mixture is also used in the process of etching. HF/HCl
mixture is used to etch the MXene Mo2Ti2C3 from Mo2Ti2AlC3
and Mo2TiC2 from Mo2TiAlC2 respectively. TBAOH is then used as
an intercalant which is followed by manual shaking and washing
[73]. Another efficient method involves the generation of HF
through the hydrolysis of ammonium hydrogen bifluoride
(NH4HF2). This is followed by the selective etching of MAX-phase
precursors over an extended etching period. Initially, this process
was successfully demonstrated on thin epitaxial Ti3AlC2 films
and later adapted for powders [74, 75]. Natu et al. have demonstrated
an alternative method for etching and delaminating MAX
phases into MXenes using organic polar solvents and NH4HF2,
without the need for water [76]. Lipatov et al. employed two different
methods to etch MXene from MAX phase. In the first
method, a ratio of 5 : 1 of LiF to Ti3AlC2 was utilized, requiring
sonication to exfoliate the Ti3C2Tx flakes. Conversely, in the second
method, using a ratio of 7.5 : 1 for the same components, sonication
was unnecessary as shown in Fig. 5 [77]. This discovery
expands the potential applications of MXenes to diverse environments
that are sensitive to water.
Salt etchants
A higher formation energy indicates stronger bonding of aluminum
(Al) atoms in N-based MAX phases, making their removal
more difficult. On the other hand, a lower cohesive energy suggests
that N-based MAX phases are less stable and potentially
prone to dissolution in HF solutions [78]. To overcome this challenge
and successfully obtain nitride MXenes, a recently introduced
approach involves the use of a ternary eutectic molten
fluoride salt mixture consisting of KF, LiF, and NaF as an etchant.
This method enables the selective etching of aluminum (Al) from
the MAX phases, leading to the synthesis of Ti4N3Tx MXenes [79].
The molten salt and MXenes mixture were subjected to heating
in an argon environment at a temperature of 550�C for a duration
of 30 min. This elevated temperature provided additional energy
for the reaction, enabling it to overcome the bonding differences
in the N-based MAX phase. Subsequently, in order to eliminate
any remaining and excess fluorides, extra washing steps involving
H2SO4 and deionized water were necessary. However, the
resulting Ti4N3Tx exhibited smaller flake size and lower crystallinity
compared to MXenes prepared using HF etchants [80]. The
A-site element in transition metals, such as Pt, Zn, Ni, and Fe, is
important in the synthesis of MXene-based composites, which
are synthesized through selective etching methods. This process,
involving fluoride ions from salts or mixtures like HCl/LiF and
HF, removes the A layer from the MAX phase, using Al due to its
high reactivity in fluoride solutions. However, challenges arise in
finding a sustainable, fluorine-free method for MXene synthesis,
and exploring the range of MAX phase precursors beyond the traditional
A-site elements in groups XIII–XVI. Li et al. achieved successful
synthesis of various MAX phases containing zinc (Zn) by
utilizing the elemental replacement method with molten zinc
chloride (ZnCl2). They also managed to convert Ti3ZnC2 and
Ti2ZnC MAX phases into Ti3C2Cl2 and Ti2CCl2 MXene, respectively,
by stripping the zinc component in a molten salt environment
consisting of ZnCl2 as shown in Fig. 6. The molten state of a
Lewis acid like ZnCl2 exhibited strong acidity, which facilitated
the displacement of aluminum (Al) from the MAX phase. ZnCl2
dissociates into ZnCl2
4 and Zn2þions. Zn2þ
, as a Lewis acid, plays
a crucial role by accepting electrons and coordinating with Cl-
ions. During this interaction, Al atoms in Ti3AlC2, which are
weakly bonded, undergo oxidation and are converted to Al3þ in
an acidic medium through a redox reaction. After the Al layer is
removed, Zn atoms are intercalated into the Ti3C2 layers, forming
Ti3ZnC2. The Zn atoms in Ti3ZnC2, being weakly bonded, are easily
removed, and Cl− ions take their place, forming Ti3C2Cl2. This
reaction is similar to HF etching, where Zn2+replaces H+and Cl-
replaces F-
. The volatility of AlCl3 served as the driving force for
the outward diffusion of aluminum. Furthermore, the presence
of a liquid environment promoted diffusion and facilitated the
complete progress of the replacement reaction. The process involved
placing the Zn-containing MAX phase mixed with mortar
into an alumina crucible, followed by subjecting it to a tube furnace
at 550�C for 5h under an argon atmosphere. The resulting
product was then washed with deionized water and dried at
40�C. The main objective behind obtaining the Zn-containing
MAX phase was to extract the weak Zn-Ti bonds present in
Ti3ZnC2, as they readily dissolved in the molten ZnCl2 salt. At the
same time, chloride ions (Cl−) naturally incorporated themselves
into the MXene nanosheets due to their presence in the molten
salt, leading to the formation of a more stable phase, Ti3C2Cl2
[81]. The synthesis of Ti2ZnCl2 occurs in two steps. First, Ti3ZnC2
is produced, which involves the incorporation of zinc into the
structure. In the second step, Ti3ZnC2 undergoes further etching
in molten ZnCl2. This two-step mechanism mirrors the traditional
chemical etching process used to synthesize MXenes.
Ti3AlC2 þ1:5 ZnCl2 !Ti3ZnC2 þ0:5 Zn þAlCl3 NH4F þ H2O !NH3:H2O þHF
(3.1)
(3.2)
Ti3C2Tx was synthesized by Arole et al. through the etching
process of Ti3AlC2 using SnF2. They combined Ti3AlC2 and SnF2
in a ratio of 1 : 6 and subjected the mixture to a temperature of
550�C for a duration of 6 h. Afterward, KOH was employed to
cleanse the resulting product and eliminate any surplus
salts [82].
Alkaline treatment
Alkaline etching is an alternative method for synthesizing
MXenes from MAX phases using strong bases like NaOH or KOH.
Alkaline etching dissolves the A-layer (mostly aluminum) using
hydroxide ions (OH−), resulting in a more environmentally
friendly and safer process. This method is advantageous due to
its reduced toxicity and potential to cause fewer defects in the
MXene structure, though it can be slower and less efficient.
Challenge lies in the delamination of MXene layers into monolayers
or few-layer structures. Ti3AlC2 powders after treatment
in low concentration (10–20 wt %) HF then immersed in tetramethylammonium
hydroxide (TMAOH) resulting in the formation of
Ti3C2 as shown in Fig. 7. In addition to the formation of Ti3C2, ammonium
oxide/hydroxide layers are also formed on the surface
and so cleaning the surface is required to remove these compounds
[83]. A combination of alkali and hydrothermal methods
is also used for etching. Al layers from Ti3AlC2 are etched using
sodium hydroxide (NaOH) followed by H2SO4 hydrothermal treatment.
However, this leads to incomplete etching as Al layers are
removed only from the outer surface of Ti3AlC2 [84]. Drawing inspiration
from the Bayers process employed in Bauxite refining,
Li and his colleagues developed a fluorine-free technique to
completely remove the aluminium layer from Ti3AlC2 through
the use of corrosive NaOH solutions. By subjecting the material
to high temperatures and concentrated NaOH solutions, they
were able to obtain high-purity Ti3C2Tx. The process involves the
oxidation of aluminium, resulting in the formation of aluminium
oxide hydroxides, followed by their dissolution in the alkali solution
[85]. Notably, when the ScAl3C3 compound was etched using
an organic base aqueous solution of tetramethylammonium
hydroxide (TMAOH), a new hydroxide-terminated carbide
called ScCxOH was formed, instead of the expected MAX phase.
ScCxOH exhibits a unique structure where the Sc layer is positioned
between the OH group at the top and the C layer below.
Unlike conventional metallic MXenes, ScCxOH demonstrates
semiconducting properties [86].Electrochemical etching
Electrochemical etching involves the transfer of charges between
targeted materials. Etching Ti3AlC2 through electrochemical
means using dilute solutions of NaCl, HCl, or HF is challenging
due to material corrosion. Electrochemical exfoliation is emerging
as a promising, safe, and cost-effective technique for synthesizing
MXene-based materials, offering a non-toxic alternative to
traditional fluoride-based etching, which poses health risks. Sun
et al. used this method involves the use of a three-electrode system
where Ti2AlC acts as the working electrode in a diluted HCl
solution. Applying a voltage of þ0.6 V over five days successfully
etched Ti2CTx. However, etching was limited to the surface due
to the formation of carbon-derived carbides (CDCs) [87]. Likewise,
low concentrations of these solutions hinder the etching process.
To address this, Yang et al. devised a method that relies on the
anodic corrosion of Ti3AlC2 in a dual-component aqueous
electrolyte composed of NH4Cl and TMAOH as shown in Fig. 8.
During this process, aluminum dissolves, and ammonium hydroxide
intercalates between the MXene flakes, facilitating the
separation of MXene sheets. In this etching procedure, the presence
of chloride ions (Cl-) is pivotal in the anodic etching of aluminum
layers, while ammonium hydroxide (NH4OH) aids in
exposing the edges of the etched anode, thereby promoting the
overall reaction. This method achieved higher yields and larger
MXene sheets in just 5 h under a slight voltage of þ5 V [88]. The
mechanism is as follows:
Ti3AlC2–3e– þ3Cl– ! Ti3C2 þ AlCl3 (4)
Pang et al. used a different approach involves utilizing thermally
assisted electrochemical etching, where a composite electrode
comprising MAX, carbon black (CB), and carbon fiber cloth
(CFC) is immersed in a diluted HCl etchant. By employing this
method, the resulting MXenes exhibit distinctive flower-shaped
structures and tunable characteristics, which are contingent
upon the specific etching conditions employed [89].
Among the top-down approaches, HF etching is the most used
technique, offering high yields. Despite its efficiency, this method
involves handling hazardous HF, raising oncerns about safety
and environmental impact [90]. Alkaline etching on the other
hand is a safer alternative but its yeild is quite lower thus limiting
its practicality for large-scale production [67].
Electrochemical etching is a advanced method which has variable
yields and a higher cost. Athough this method avoids the
need for hazardous chemicals, the complex setup and higher
cost limits its scalability for industrial applications [91]. Although
HF etching remains the most practical method for large-scale
MXene production, its environmental impact due to hazardous
waste necessitates the adoption of greener, more sustainable
alternatives. Emerging etching techniques, such as LiF-HCl systems
makes a balance between safety, cost, and efficiency which
provides us with a direct alternative to HF method.

2.2.1. Hydrothermal Approach

This is a heterogeneous reaction approach, which involves the heating of aqueous

solutions above the boiling point of water within a high-pressure autoclave
containing precursor materials. The synergetic effect of the elevated temperature
and pressure and the solution pH can be employed to alter the QD size, shape,
morphology, and properties [55]. In addition, the pH of the solution, reaction
temperature, and time period play a vital role in the production of MXene. To
synthesize MXene, a reaction temperature of 100 to 180 °C and pH of 6 to 9 are
kept standard [56], because the reaction duration is influenced by the pH and
temperature. Furthermore, by adjusting the conditions of the hydrothermal
reaction, the material size, properties, and thickness can be altered. Xue et al. [57]
employed a hydrothermal technique to create water-soluble Ti3C2 MXene and
observed that by altering the hydrothermal reaction temperature to 79 °C, the
properties, thickness, and size of MXene can be tailored. The MXenes obtained at
100, 120, and 150 °C resulted in particles with average diameters of 2.9, 3.7, and
6.2 nm, respectively, and average thickness of 0.99, 0.91, and 0.89 nm, showing
that the monolayers make up the bulk of particles. At the time of reaction, the Ti3C2
QDs exhibits the -NH surface functionalities, and at a lower temperature (i.e., 100
°C), a new MXene structure is formed in which the d-spacing value can be
confirmed. On the other hand, the MXENE formed at 120 °C exhibits a fusion
structure with CTi in the core and TiO2 on the surface. However, because most of
the Ti atoms were etched away at an elevated temperature (i.e., 150 °C), an
amorphous MXENE structure was formed. According to Xiao and et al. [58],
below 100 °C, the MXene structure cannot be produced. They made MXene
(Ti3C2Tx) by varying the reaction temperature from 60 to 80 and 100 °C. Instead of
MXene, abundant nanoribbons, including a few Ti3C2Tx nanoflakes, were formed
at a temperature of 60 °C. By increasing the temperature to 80 °C, the shrinkage of
the particles size occurred, and various-sized nanodots were formed. Ultrafine
nanodots are generated and uniformly spread on the nanosheets at 100 °C. More
MXenes have been synthesized by applying different hydrothermal conditions
[59,60]. By adapting alternative hydrothermal conditions, MXene with doped
heteroatoms have also been produced, utilizing the elements’ consequent
precursors. Using Nb2C nanosheets precursor material and L-cysteine as a source
of sulfur and nitrogen, Xu and his co-workers fabricated heteroatom-co-doped
Nb2C MXene (S, NMXene) via the hydrothermal method at 160 °C. The particles
size of MXene was between 2.6 and 4.7 nm. The fabricated S, N-MXene has a
lateral size of 3.56 nm, remarkably smaller than those of the MXene (i.e., 2.4 nm)
and N-MXene (i.e., 2.66 nm). The S, N-MXene had an average thickness of 1.74
nm, indicating that a monolayer was developed [61]. Recently, Peng et al. [62]
fabricated 2D MXene (i.e., h-Ti3C2) via the hydrothermal method using
low-toxicity etchants (i.e., NaBF4, HCl). The TEM micrograph of the resultant
h-Ti3C2 MXene (Figure 5a) revealed a layered structural morphology. As is clear
from Figure 5b, the 2D h-Ti3C2 nanoflakes are very thin and transparent. The
selected area HR-TEM micrograph of the h-Ti3C2 nanoflakes (Figure 5c) revealed
d-spacing of ~0.264 nm and ~0.155 nm, corresponding to the (0−110) and (0−210)
planes of the Ti3C2, respectively. The FFT pattern revealed hexagonal symmetry as
can be seen from the inset of Figure 5c. It is important to note that the
hydrothermal etching technique not only avoids the use of HF acid but is also an
efficient method for the preparation of Ti3C2 nanoflakes.

2.2.2. Solvothermal Approach

The solvothermal process is simple and more efficient than the hydrothermal
method and has been widely utilized to make MXene. It is similar to the
hydrothermal process with the mere distinction that, instead of water, a
non-aqueous organic solvent is used to make the precursor solution. Because the
size, distribution, and material crystallinity can be precisely regulated as needed,
the solvothermal method is regarded to be more successful and adaptable as
compared to the hydrothermal method [63]. Furthermore, adjusting experimental
parameters such as the reaction’s temperature, time duration, and solvent type, the
desired result can be fine-tuned. Feng et al. [64] used a solvothermal technique to
fabricate nitrogen-doped Ti3C2 MXene. In conclusion, the exfoliated MXene was
used to make three different forms of MXene QDs with varied amine doses. To
fabricate NTi3C2 QDs, di-ethylene-triamine, di-methyl-formamide (DMF), and the
exfoliated MXene were mixed in equal amounts at 150 °C for 8 h. NTi3C2 QDs
with an average particle size of 6.2 nm and a width of 1 nm were obtained,
indicating the monolayer formation. To synthesize the QDs, the solvothermal
reaction time was optimized. The particle size decreased with the increase in the
solvothermal reaction time. Recently, Feng et al. [64] demonstrated the fabrication
of in-situ N-doped Ti3C2 MXene QDs via the amine-assisted solvothermal method.
The SEM micrograph of pristine MXene (Figure 5d) confirmed multi-layers with a
thickness of approximately 5 μm. The TEM micrograph (Figure 5e) reveals a
remarkable reduction in the particle size of MXene (i.e., from 600 nm to 6 nm),
confirming the formation of N-MXene QDs. As is clear from the HR-TEM
micrograph (Figure 5f), the resultant QDs exhibit high crystallinity with a lattice
spacing of 0.193 nm (101 plane). The resultant QDs revealed diverse fluorescence
quenching responses toward the detection of various metal cations. Similarly, Niu
et al. [65] used the solvothermal approach to fabricate three types of Ti3C2Tx QDs
from the Ti3C2 MXene precursor, labelling them e-Ti3C2, f-Ti3C2, and s-Ti3C2 QDs.
Their particle size varied depending on the solvent, and the average particle sizes
for e-Ti3C2, f-Ti3C2, and s-Ti3C2 QDs were observed to be 2.5–0.2, 3.3–0.2, and
1.8–0.1 nm, respectively. The particles’ thickness was in the range of 1.0-2.5 nm.
The particles’ thickness and lateral sizes were influenced by the polarity of the
solvent, oxidation reaction, and boiling point. The disadvantage of this technique is
the generation of carbon quantum dots (CQDs) from organic precursors. The
undesirable CQDs have an impact on the product’s optical and catalytic
capabilities [66].

2.2.3. Ball-Milling Approach

Different QDs have been successfully fabricated via the ball-milling approach,
which is an extensively used top-down method for reducing the size of
nanoparticles. The physical and morphological features of the produced materials
are influenced by a variety of factors such as the milling type (wet or dry), speed of
the milling, the ratio of the ball to powder weight, and milling time duration.
Zhang et al. [67] used the ball-milling procedure to fabricate various-sized Ti3C2Tx
MXene nanodots (TNDs) by mixing Ti3C2Tx with diverse solid-state precursors
such as red P, S, C, and Si (see Figure 6a). Ball-milling of the mixture was
performed at 550 rpm for 48 h under an argon environment, while keeping the
powder-to-ball weight ratio at roughly 1:20. The of FE-TEM image of the Ti3C2Tx
(Figure 6b) showed a μm-long thin layered structure. The red-P-assisted
ball-milling of Ti3C2Tx results in QDs with a lateral diameter and thickness in the
range of 6–25 nm (Figure 6c). The HR-TEM micrograph of Ti3C2Tx (Figure 6d)
revealed an interlayer spacing of ~0.91 nm, corresponding to the (0002) planes,
which confirms the development of MXene nanodots. During this process, the
TiOX (X = C, P, S, Si) bond formation occurs, causing the delamination and
reduction in the particle size of Ti3C2Tx MXene, which is governed by the strength
of the OX link. The stronger the –OX interaction, the smaller the particle size will
be. Due to the strong TiOX connection, a solid-state element existed in the product.
This is an ideal method used to fabricate nanocomposites.

2.2.4. Ultrasonic Approach

The ultrasonic technique is an environmentally friendly and risk-free technique

used for the fabrication of MXene QDs. Due to the solvents’ acoustic, cavitation,
and reverberation, the ultrasonication process changes the layered, as well as
nonlayered, materials into QDs. In this technique, the inherent features of materials
are effectively retained. Solvents such as DMSO, DMF, N-methyl-2-pyrrolidone
(NMP), and tetra-butylammonium hydroxide (TBAOH), with their high boiling
points and surface energies, could overcome the binding force of bulk materials
and transform them into highly dispersed, small-sized QDs. To produce the
Ti3AlC2 MXene directly from the MAX phase, Yu et al. [68] used etching-assisted
exfoliation and mechanical-force–assisted liquid exfoliation approaches with the
solvent TBAOH. The bulk particles of Ti3AlC2 break down into smaller particles
with new edges and surface sites during ultrasonic treatment. By treating the OH
group with a solvent, these sites were removed as Al(OH)4. Meanwhile, the
formation of isolated MXene sheets took place [68]. These sheets were then
transformed into MXene via the bath sonication. The thickness and average lateral
size of the obtained MQDs were 0.6 and 4.9 nm, respectively. Before being utilized
in aqueous media via the ultrasonication technique, the organic solvents with high
boiling points require extensive post-treatment. High-temperature rotary
evaporation as post-treatment affects the quantum dots’ optical and catalytic
capabilities. As a result, methods for synthesizing MXene in an aquatic
environment gained a great deal of attention. Furthermore, widespread utilization is
challenging due to the lengthy sonication method and low output yield. As a result,
combining the ultrasonication technique with hydrothermal and solvothermal ones
is highly effective to shorten the reaction time and increase the yield. To fabricate
V2C MXene, Huang et al. [69] used an ultrasonication-hydrothermal method.
Throughout the synthesis procedure, the V2C sheets were ultrasonically treated for
1 h in an Ar environment, and the suspension was treated hydrothermally at 120 °C
for 6 h. The SEM micrograph of V2C MXene (Figure 6e) revealed a layered
structure. The average size of the generated V2C MXene was 4.13 nm, and it was
2.33 nm thick (see Figure 6f). The lattice fringes with d-spacing of 0.247 nm
(Figure 6g) were accredited to the (01¯10) plane of the V2C MXene. Another way
to fabricate MXene is through intercalation ultrasonication. To synthesize Ti3C2
QDs, Wang et al. [70] used the ultrasonic intercalation technique. The Ti3C2
nanosheets were treated for 24 h with 25% aqueous TMAOH to produce guest
intercalation and the host-layer fragment. After that, the resultant intercalated Ti3C2
nanosheets were sonicated in an Ar atmosphere for 10 h.
Lewis Acidic Etching
Method
In 2019, Huang’s group proposed a brand-new, safe and green
method, namely Lewis acidic molten salts etching, to prepare
Cl-terminated MXene [66]. Owing to a series of advantages,
Lewis acidic etching has attracted intensive attention since it
was presented, greatly promoting the development of MXenes
in the past three years. The introduction of Lewis acidic molten
salts etching approach is mainly classified into following four
aspects: etching mechanism, terminations regulation, in-situ
formed metals and delamination of multi-layered MXenes.
3.1 Etching Mechanism
The mechanism of Lewis acidic molten salts etching method
is based on the replacement reaction between Lewis acidic
molten salts and A-site atoms in MAX precursor. Taking the
etching of ­Ti3AlC2 MAX precursor by the firstly used Lewis
acidic salt ­ZnCl2 as an example, Huang et al. thoroughly mixed
the ­Ti3AlC2 and ­ZnCl2 with a molar ratio of 1:1.5 in a glovebox
and the mixture was placed in alumina crucible, which is then
heated at 550 °C for 5 h in a tube furnace under Ar atmosphere
(Fig. 6a) [66]. It can be observed that main peaks of final
product shift to lower angles relative to those of ­Ti3AlC2 MAX
in the X-ray diffraction (XRD) patterns (Fig. 6b), revealing an
enlarged lattice parameter. Additionally, the densely-packed
structure can still be kept, and high-angle annular dark-field
scanning transmission electron microscopy (HAADF-STEM)
image in Fig. 6c suggests that interlayer element is brighter
compared with other elements, thus proving that ­Ti3ZnC2
MAX has been successfully prepared. The specific formation
mechanism can be described by Eqs. (15–16):
Ti3AlC2 + 1.5ZnCl2 = Ti3C2 + 1.5Zn + AlCl3 ↑
(15)
Ti3C2 + Zn = Ti3ZnC2
(16)
It is well-known that ­ZnCl2 will exist in the form of molten
state at 550 °C and is ionized into ­Zn2+ cations. Then, the
­Zn2+ with strong electron obtaining ability will react with
Al atoms in ­Ti3AlC2 to generate ­Al3+ cations and Zn atoms.
­Al3+ cations are prone to combine with ­Cl− anions to form
­AlCl3, which will evaporate at 178 °C. At the same time, Zn
atoms can diffuse into the interlayer of ­Ti3C2 and occupy the
position originally belonging to Al atoms, thereby leading
to the generation of new MAX phase ­Ti3ZnC2. It is worth
mentioning that the removal of ­AlCl3 from the system con-
siderably accelerates the element replacement reaction.
When the molar ratio of ­Ti3AlC2 and ­ZnCl2 further
increases to 1:6, ­Ti3C2 MXene with -Cl termination
instead of ­Ti3ZnC2 MAX can be successfully obtained.
Firstly, the classical multi-layered structure is observed
for ­Ti3C2Cl2 MXene (Fig. 6d). Then, the XRD pattern
of as reacted product indicates that the strongest (104)
peak at around 39° of ­Ti3AlC2 MAX almost vanishes and
the (002) peak moves to a lower angle of 7.94° (Fig. 6e),
suggesting an expanded interlayer spacing. Additionally,
the characteristic XRD peaks of Zn metal can also be
observed. Further, Ti-Cl chemical bond in ­Ti3C2Cl2
MXene can be confirmed by Cl 2p X-ray photoelectron
spectroscopy (XPS) spectra (Fig. 6f) [66]. Above
discussions effectively confirm the formation of ­Ti3C2Cl2
MXene and the reaction process can be described by
following equations:
Ti3ZnC2 + Zn2+ = Ti3C2 + Zn2+
2
(17)
Ti3C2 + 2Cl−
= Ti3C2Cl2 + 2e−
(18)
Zn2+
2 + 2e−
= 2Zn
(19)
As exhibited in Fig. 6a, the formation of ­Ti3C2Cl2
MXene can be divided into two stages including the initial
formation of ­Ti3ZnC2 MAX shown in Eqs. (15–16) and
the subsequent reaction of ­Ti3ZnC2 MAX with excessive
­ZnCl2 to obtain ­Ti3C2Cl2 exhibited in Eqs. (17–19). Spe-
cifically, the Zn atoms in ­Ti3ZnC2 MAX can be separated
from interlayer and react with excessive ­Zn2+ to generate
­Zn2
2+ cations, and the ­Cl− anions can easily intercalate
into the interlayer of ­Ti3C2, forming Ti–Cl chemical bond
(Fig. 6g). Meanwhile, the ­Zn2
2+ cations gain electron to
form Zn metal. In general, ­Zn2+ cations and ­Cl− anions in
­ZnCl2 act as ­H+ and ­F− in HF etchant, respectively.
Later in 2020, Prof. Huang and coworkers generalized
the previously proposed Lewis acidic etching method,
which greatly expands the family of Lewis acidic molten
salts ­(FeCl2, ­CoCl2, ­NiCl2, ­CuCl2, ­CdCl2, CuI, ­CuBr2, etc.)
and can prepare various MXenes from Al, Si and Ga-based
MAX precursors [67]. They immersed ­Ti3SiC2 MAX in
­CuCl2/NaCl/KCl mixed molten salts at 750 °C (Fig. 6h),
and NaCl and KCl play a role in providing molten salts
environment. The etching process is illustrated as follows:
Ti3SiC2 + 2CuCl2 = Ti3C2 + SiCl4 ↑ + 2Cu
(20)
Ti3C2 + CuCl2 = Ti3C2Cl2 + Cu
(21)
Specifically, the zero-valence Si atoms in the interlayer
lose electrons to become ­Si4+ cations and then combine with
­Cl− anions to form ­SiCl4, which can readily escape as gas at
around 57 °C. Subsequently, the ­Cu2+ cations can obtain elec-
trons to transform into Cu metal. Finally, excessive ­Cl− anions
can be grafted onto exposed Ti atoms, resulting in the forma-
tion of ­Ti3C2Cl2 MXene. It is worth mentioning that individual
HF is difficult to etch ­Ti3SiC2 [85], while Lewis acidic salts can
readily complete the above etching process, which reflects the
superiority of Lewis acidic etching. After the etching process,
NaCl, KCl and excessive ­CuCl2 can be eliminated by washing
the etching products with deionized water.
Further, Huang et al. proposed an effective criterion to
determine whether the A-site atoms in MAX can react with
metal ions in the Lewis acidic salts. They found that the metal
ions in the Lewis acidic salts with high electrochemical redox
potential can etch the MAX precursor with low redox poten-
tial A-site atoms. The relationship between redox potential
of A-site elements, redox potential of Lewis acidic salts and
Gibbs free energy is illustrated in Fig. 6i. For example, ­CuCl2
molten salt can easily remove the Si atoms from ­Ti3SiC2 MAX
as mentioned above, which is ascribed to the higher redox
potential of ­Cu2+/Cu pair (−0.43 V versus ­Cl2/Cl−) compared
with that of ­Si4+/Si pair (−1.38 V versus ­Cl2/Cl−). The gen-
eral etching reaction between A-site elements in MAX phase
and Lewis acidic molten salts ­MQy (Q
=
Cl, Br or I) can be
described as follows:
A + z∕yMQy
= AQz + z∕yM
(22)
It can be inferred that the difficulty degree of etching
­Mn+1AXn precursors by Lewis acidic molten salts is independ-
ent of M, X and n values, and only depends on the redox poten-
tial of A-site element. Therefore, based on Lewis acidic etching
criterion, a large number of MAX phases ­(Ti3AlC2, ­Ti3ZnC2,
­Ti3SiC2, ­Ti3AlCN, ­Ti2GaC, ­Ti2AlC, ­Ta2AlC, ­Nb2AlC, etc.) can
be etched by using different Lewis acidic salts ­(FeCl2, ­CoCl2,
­NiCl2, ­CuCl2, ­CdCl2, AgCl, CuI, ­CuBr2, etc.).
The reaction mechanism of Lewis acidic etching method
is basically clear now, but the understanding of Lewis acidic
etching method can still be further deepened by optimizing
etching parameters such as reaction atmosphere and etchant
compositions. For example, in order to prevent the oxidation
of the prepared MXenes, the inert gas such as Ar is gener-
ally used for protection in the process of Lewis acidic etch-
ing. However, Lin et al. proposed a simple one-pot synthesis
method, containing molten salts shielded strategy for MAX
preparation and subsequent in-situ Lewis acidic etching, to
achieve the preparation of MXenes under air atmosphere
(Fig. 6j) [112]. Specifically, they thoroughly mixed Ti, Al
and C powders with NaCl and KCl salts, and the mixture
was then pressed into a pellet. Subsequently, the pellet was
further placed in a salt bed composed of NaCl and KCl
which can melt at around 650 °C to insulate the air, and the
­Ti3AlC2 MAX can be obtained by heating at 1300 °C for
1 h in muffle furnace without Ar protection. Finally, ­CuCl2
was introduced to the reaction system at 700 °C to achieve
the in-situ etching of ­Ti3AlC2 MAX for 10 min, thus leading
to the quick formation of Cl-terminated ­Ti3C2Tx MXene.
Therefore, with the assistance of the molten salts shielding
strategy, Lewis acidic molten salts can directly etch MAX
precursor in air atmosphere, which greatly promotes the
development of Lewis acidic etching method. In addition,
Zhang et al. demonstrated one-step eutectic etching strategy
for the synthesis of in-plane porous ­Ti3C2Cl2 MXene by reg-
ulating the etchant composition from ­ZnCl2 to NaCl/ZnCl2
mixture [113]. When ­ZnCl2 is used to etch the MAX phase,
the volatilization of generated ­AlCl3 at high temperature will
cause structural/crystal defects in the precursor, which will
then evolve into void space. However, the generated pores
will gradually collapse owing to the absence of temporary
physical support during cooling process. Further, they found
that when the etchant is changed into a mixture of ­ZnCl2
and NaCl in a molar ratio of 4:6, the NaCl mole percent will
gradually increase to 72% with the progress of etching pro-
cess, which makes the salt melt shift across the phase bound-
ary and leads to the precipitation of NaCl particles at 550 °C
based on the phase diagram (Fig. 6k). The formation of NaCl
particles can occupy void space to prevent the shrinkage
and collapse of pores, finally resulting in a large increase
in mesoporous volume and specific surface area. Therefore,
the pore structure of the prepared MXenes can be greatly
adjusted by the manipulation of etchant composition. The
above-mentioned two works indicate that the Lewis acidic
etching method still possesses broad development space and
can be further improved from different aspects in the future.

2.1. Etching Method

MXenes can be prepared in a number of different ways. Due to changes in their

etching methods, various terminal functionalities can be attached to the M atoms to
complete their coordination spheres, so as to lower their surface Gibbs free energy.
As a result, the MXenes surface features have a great influence on their fabrication.
Herein, different types of the preparation methods are discussed.

2.1.1. Etching with Hydrofluoric Acid (HF)

Due to the in-depth research on MXenes, etching procedures have been widely
employed, especially the HF acid etching method, which is still the most
commonly used procedure. Naguib et al. [33] proposed the fabrication of the
Ti3AlC2 MAX phase via HF acid etching in 2011. Using a simple displacement
process, the HF acid removes Al layers from the Ti3AlC2 MAX phase with H2
production. In addition, the reaction of deionized water with the HF acid solution
produces Ti3C2Tx (where T represents the -O, -F, and -OH) as well as H2. The HF
acid etching was used to successfully strip the Ti2AlC, (Ti0.5Nb0.5) 2AlC, Ti3AlCN,
Ta4AlC3, (V0.5Cr0.5) 3AlC2, Nb2AlC, and a series of the MAX complexes of
Zr3Al3C5, Ti3SiC2, and Mo2Ga2C, into Mxenes [34]. The HF acid etching has
continuously been the most useful synthesis process for MXenes materials from
2011 to date. In the HF acid etching process, the time period, temperature, and F
ions density play an important role in the design of high-quality MXenes layers.
Alhabeb et al. [35] confirmed that Ti3C2TX, with high concentration HF acid,
produces an excellent layered structure, which is difficult to achieve with other
acid solutions. MXenes obtained via the HF acid etching approach retained their
unique surface characteristics, along with the –O, –OH, and –F functionalities.
Recently, Kim et al. [36] studied the etching behavior of MAX-phase Ti3AlC2 in
various etching agents at the atomic scale employing ion-beam and electron
microscopy. They investigated the change in the structure of the Ti3AlC2 phase as a
function of the etching agents and etching time, revealing that the edge Al atoms at
the mid layers of MAX-phase Ti3AlC2 are not etched, despite the interaction with
the HF etchant. Further, etching of the grain boundary occurred in the HF etchant.
As revealed in the STEM micrograph (Figure 3a), employing the bulk etching
technique, the etching of Ti3AlC2 for 3 h displayed numerous etched regions.
Further, the SAED pattern (inset Figure 3a) reveals the expansion of d-spacing of
the MAX-phase Ti3AlC2 (i.e., 0.97 nm) to 1.02 nm, confirming the successful
conversion to Ti3C2Tx MXene at the etching boundary.

2.1.2. Modified Acid Etching Approach

Acid fluoride solutions have corrosive and poisonous properties, and due to these
reasons, researchers are finding techniques to prevent HF acid from being used
directly to extract the Al layers from MAX phases. The foremost approach, known
as original-location HF acid etching, replaces the HF acid with fluoride salts (i.e.,
LiF, NH4HF2, FeF3, KF, and NaF) and HCl [37]. Usually, during the synthesis of
MXenes via the etching of Al or Ga layers of the MAX phase by HF acid, an
undesired byproduct (i.e., AlF3·3H2O) is formed. To synthesize MXenes free of
this impurity, it is necessary to illuminate the factors that initiate its formation.
Thus, modified etching approaches are widely employed. For instance, Cockreham
et al. [38] deduced the conditions that led to the formation of the byproduct
AlF3·3H2O, while proceeding the etching process with cobalt fluorides (i.e.,
CoF2/CoF3). The SEM micrograph of the CoF3/MAX sample (Figure 3b) do not
show any AlF3·3H2O impurity. The MXenes interlayer distance formed via the
modified acid-etching approach is improved because of the cation’s intercalation,
which minimizes the inner force between layers, and potentially delaminates the
material layers during ultrasonication. As a result, this approach shortens the
previously noted time-consuming multi-step synthesis process, enabling the
synthesis of few-layer MXene in a single step [39].

2.1.3. Modified Fluoride-Based Acid Etching

Researchers have worked hard to find better means to remove the atom layers from
MAX in order to prevent the significant toxicity that HF etching causes. Apart
from HF, etching MAX precursors can also be performed with a mix of fluoride
salts (i.e., KF, NaF, LiF, and NH4F) and strong acids. Fluoride salts and strong
acids have been discovered to selectively etch atoms and led to the cation’s
intercalation (i.e., K+, Na+, Li+, and NH4+) in situ. The introduction of water
between MXene layers increases the interlayer space while lowering MXene layer
contact. It is worth noting that the amount of fluoride salt and strong acid in the
final MXene fragments can affect their quality and size. For example, the
multilayered Ti3C2 generated by the clay approach (5M LiF/6M HCl) requires a
subsequent sonication step for delamination into single flakes, which frequently
results in tiny defective MXene flakes [40].

2.1.4. Molten Salts Etching

MXene can also be produced by heating the MAX phases, such as Ti4AlN3, in a
molten fluoride salt mixture (i.e., LiF, NaF, KF (29:12:59 weight ratio %)) at 550
°C under argon shielding to make Ti4N3. The etching procedure can be completed
in 30 min. Because the TinNn–1 has a lower stability than TinCn–1, it can be dissolved
in HF or other fluoride-based acids used as the etching agent. As a result, the
molten-salts etching method has the benefit of a relatively quick processing time.
Additional cleaning (washing with DI H2O and H2SO4) and delamination (in
TBAOH solution) are compulsory. The crystallinity of delaminated Ti4N3 is lower
than that of the MXene obtained via the HF etching, as indicated by the XRD
patterns of the resultant Ti4N3. The TiO2 phase is also visible in the obtained
product. In comparison to the HF and fluoride-based acids etching, the molten salts
etching process has the benefit of producing MXenes with limited stability in the
HF or fluoride-based acids solution. This technique, on the other hand, has the
following disadvantages: (a) The etching process consumes a significant amount of
heat and energy; (b) the resultant MXenes reveal low purity and crystallinity; (c)
the resultant MXenes have abundant surface defects and vacancies [41]. Very
recently, Liu et al. [42] reported the synthesis of MS-Ti3C2Tx via the intercalation
of the tetrabutylammonium hydroxide (TBAOH), followed by layer separation via
sonication. The as-obtained Cl-terminated MS-Ti3C2Tx was utilized as an anode in
a Li-ion battery, which achieved a high specific capacity and exceptional rate
capability. The TEM micrograph (Figure 3c) reveals clear Ti3C2Tx nanosheets with
distinct edges, with a lateral size of ~600 nm.

The SAED pattern (Figure 3d) reveals sharp reflections corresponding to the
hexagonal crystal symmetry, suggesting that the TBAOH treatment did not altered
the crystallinity of Ti3C2Tx. The HR-TEM micrograph (Figure 3e) confirmed a 2.05
nm thickness, equivalent to two layers, considering the monolayer thickness of
∼1.03 nm. Besides TBAOH, some other organic molecules such as isopropyl amine
and dimethyl sulfoxide (DMSO) have also been found to be effective intercalants
for the delamination of HF-MXenes.

2.1.5. Etching without Fluoride

Although several etching conditions for synthesizing MXenes have been

confirmed, most synthesis techniques need HF or fluoride-based chemicals, which
may result in the creation of -O and -F terminations on the interface of MXene. In
particular, -F terminations decrease the electrochemical performance of
MXenes-based supercapacitors [43]. Thus, fluoride-free fabrication techniques are
necessary to provide acceptable electrochemical performances. Li et al. [44]
developed an alkali-assisted hydrothermal etching technique for the fabrication of
Ti3C2 MXene using a NaOH solution as the etching agent. Because of the strong
interaction between Al and alkali, alkali might be used as an etchant for Ti3AlC2
MAX phase. Obtaining high-purity multi-layered MXenes is still a big challenge.
In this case, the Bayer procedure was used to etch Al layers while avoiding damage
to the Ti3C2 MXene skeleton by using a high alkali concentration (i.e., 27.5 M) and
a high temperature (i.e., 270 °C). Very recently, Chen et al. [45] reported the
fabrication of a fluoride-free and chloride-containing Ti3C2Tx MXene via
electrochemical etching as revealed in Figure 4a. In the synthesis process, Ti3C2Tx
was delaminated via sonication in the absence of any toxic organic intercalant. The
thickness of the resultant Ti3C2Tx nanoflakes was ∼3.9 nm (see Figure 4b), and
their dispersion in an aqueous medium was very highly stable. The SAED pattern
of the Ti3C2Tx (inset Figure 4b) displays hexagonal symmetry as a result of the
hexagonal arrangement of the Ti-atoms at the 002 surface of Ti3C2Tx MXene. The
lattice fringe, with d-spacing of 0.27 nm, can be accredited to 100 planes of the
Ti3C2Tx MXene as is clear from the HR-TEM micrograph (Figure 4c). Based on the
theoretical predictions and experimental results, the surface-attached −F
remarkably hinder the electrolyte ions’ transportation and sacrifices the
electrochemically active sites, which results in low performance of MXenes for
applications in Li-ion batteries and supercapacitors [46,47]. Thus, the fabrication
of MXenes using F-free methods is highly desirable.
Non‑Lewis Acidic
Etching Methods
2.1 HF Etching
It is well known that graphene can be obtained by mechani-
cal exfoliation of graphite because there is only weak van der
Waals interaction between the layers [68, 69]. However, the
metallic bond between M and A atoms in MAX precursors is
stronger than van der Waals force, which makes it impossible
to obtain MXenes via mechanical stripping of MAX precur-
sors [21, 26]. Therefore, researchers have to explore other
methods to prepare MXenes. In 2011, Gogotsi and Naguib
et al. immersed ­Ti3AlC2 MAX precursor in HF aqueous solu-
tion at room temperature and the Al layers can be selectively
removed owing to the large difference between Ti-C and Ti–Al
bond strength, thus leading to the successful preparation of
multi-layered ­Ti3C2Tx MXene with obvious accordion-like
morphology (Fig. 5a–b) [11, 70–72]. For the HF etchant, ­H+
cations serve as oxidant and ­F− anions act as ligand to com-
bine with by-product of the reaction. The etching process is
presented as follows:
Ti3AlC2 + 3HF= Ti3C2 + AlF3 + 3∕2H2
Ti3C2 + 2H2O= Ti3C2(OH)2 + H2
(2)
Ti3C2 + 2HF= Ti3C2F2 + H2
(3)
Ti3C2 + 2H2O= Ti3C2O2 + 2H2
(4)
Specifically, the almost zero-valence Al atoms in
­Ti3AlC2 precursor lose electrons to become ­Al3+ cations
and then combine with ­F− anions ligand to form soluble
­AlF3 [70, 71]. Simultaneously, the multi-layered ­Ti3C2
MXene is generally modified with –O, –OH and –F groups
based on Eqs. (2–4). The introduction of surface functional
groups results in the shift of (002) peak to lower angle,
which can effectively confirm the successful preparation
of MXenes [70, 73]. Since then, a series of MXenes such
as ­Ti2CTx, ­Nb2CTx, ­V2CTx, ­Ti3CNTx and ­Nb4C3Tx have
been successfully prepared by HF etching [13, 74–77].
Additionally, the obtained multi-layered MXenes can be
intercalated by large organic molecules such as dimethyl
sulfoxide (DMSO), urea, tetramethylammonium hydroxide
(TMAOH), isopropanol (IPA), isopropyl amine (i-PrA),
tetrabutylammonium hydroxide (TBAOH), which further
expands the gallery spacing and weakens the interlayer
interaction [78–81], finally enabling the multi-layered
MXenes to be delaminated into few-layered or single-
layered MXenes (Fig. 5c) [82].
MAX precursors with different M-site atoms, A-site
atoms, X-site atoms and n values usually require different
HF concentration, etching time and reaction temperature.
Generally, Mo-based and Nb-based MAX require higher
HF concentration than Ti-based MAX to prepare corre-
sponding MXenes [83, 84]. In addition, the etching of Si-
based MAX including ­Ti3SiC2 requires HF and other strong
oxidants ­(H2O2, ­KMnO4, etc.) to complete together [85].
Besides, compared with carbide MXenes, nitride MXenes
require more precise adjustment of etching parameters dur-
ing the preparation process, because the M–N bond may
be broken under the attack of HF etchant [57]. However,
harsh reaction environment could result in the formation
of defects, such as Ti vacancy, which can adversely affect
the electronic conductivity of MXenes [86]. Furthermore,
some non-MAX precursors such as ­Zr3Al3C5, ­Hf3Al4C6
and ­Mo2Ga2C can also be etched by HF to obtain ­Zr3C2Tx,
­Hf3C2Tx and ­Mo2CTx MXene, respectively, which greatly
expands the scope of precursors and is of great significance
to the development of MXenes [18–20]. In general, HF etch-
ing method with excellent universality plays a crucial role
in the rapid development of MXenes and some researchers
still adopt this approach to prepare MXenes until now. Nev-
ertheless, the strong corrosiveness of HF greatly increases
the experimental risk and deteriorates its industrialization
prospect. The development of a greener, safer and milder
etchant is still the focus in the field of MXenes.
2.2 In‑Situ HF Etching
In 2014, a relatively safe etching route by mixing HCl
and LiF was proposed by Ghidiu et al. to prepare ­Ti3C2Tx
MXene [65]. In this approach, HF can be in-situ generated to
initiate the etching process based on Eq. (5) and ­Li+ cations
spontaneously intercalate into the interlayer of ­Ti3C2Tx
MXene.
HCl + LiF= HF + LiCl
(5)
The c-lattice parameter of MXenes obtained by LiF/HCl
etching is greatly larger than that of MXenes prepared by HF
etching, which is mainly owing to the intercalation of ­Li+
cations and water molecules. Benefiting from the hydrophilic
nature, the prepared ­Ti3C2Tx MXene demonstrates clay-
like behavior and can be processed into different desired
shapes such as rolled film. Additionally, clay-like ­Ti3C2Tx
MXene can be shaped into the letter “M” and exhibit a high
electrical conductivity of 1500 S ­cm−1. More importantly,
thanks to the insertion of ­Li+ ions and water, the van der
Waals forces between the layers are weakened and multi-
layered MXenes can be directly centrifuged after sonication
to obtain few-layered MXenes. It is worth mentioning
that the molar ratio of LiF and ­Ti3AlC2 MAX has a great
influence on the lateral size of the final ­Ti3C2Tx MXene,
and higher LiF concentration favors the complete etching of
­Ti3AlC2 MAX and intercalation of more ­Li+ ions into the
MXene interlayers.
Therefore, in-situ HF etching is further upgraded to the
“minimally intensive layer delamination” (MILD) method in
2017 by increasing the molar ratio of LiF and ­Ti3AlC2 MAX
to 7.5:1.0, which can achieve the delamination of multi-layered
MXenes via simple hand-shaking process rather than ultra-
sonication [87]. The obtained ­Ti3C2Tx MXene nanosheets
demonstrate large lateral size and high quality, resulting in a
high electronic conductivity of 4600 ± 1100 S ­cm−1. So far,
other fluoride salts including NaF, KF, ­FeF3, etc., and acids
such as ­H2SO4 have also been used by researchers [88–91]. For
example, Soundiraraju et al. reported the successful prepara-
tion of ­Ti2NTx MXene by immersing ­Ti2AlN MAX in a mix-
ture of KF and HCl [89]. Generally, the in-situ HF etching
method based on LiF/HCl etchant has appeared the most in
the recently published articles on MXenes. The biggest advan-
tage of in-situ HF etching route is the improvement of experi-
mental safety and the ability to prepare MXenes nanosheets
with larger lateral sizes and fewer defects. However, cations
­(Li+
, ­Na+
, ­K+, etc.) will intercalate into MXenes interlayers
during the preparation process and it is difficult to eliminate
them from MXenes, which may have an adverse impact on
the further application of MXenes in some fields. The rela-
tionship between structure and properties should be further
investigated.
2.3 Bifluoride Salts Etching
In 2014, bifluoride ­NH4HF2 was used to etch the ­Ti3AlC2
MAX precursor to obtain ­Ti3C2Tx MXene [92]. The
reaction mechanism is summarized as follows:
Ti3AlC2 + 3NH4HF2 = (NH4)3AlF6 + Ti3C2 + 1.5 H2
(6)
Ti3C2 + aNH4HF2 + bH2O= Ti3C2(OH)xFy(NH3)c(NH4)d
(7)
In this method, the selective etching of Al layers from
­Ti3AlC2 MAX and the intercalation of ­NH3 and ­NH4
+ into
the interlayer of ­Ti3C2Tx MXene occur simultaneously. The
intercalation of ammonium species effectively increases
the interlayer spacing. Further, ­NaHF2 and ­KHF2 were also
utilized as etchants to prepare ­Ti3C2Tx MXene by Feng et al.
in 2017 and the etching mechanisms are similar to that of
­NH4HF2 [93] (Fig. 5d). In 2020, Natu et al. used ­NH4HF2
to etch ­Ti3AlC2 MAX with polar organic solvents as the
reaction medium instead of water, successfully realizing the
water-free synthesis of ­Ti3C2Tx MXene [94]. The ­NH4HF2
can be decomposed into HF and ­NH4F, and HF plays the
role of etching the Al atomic layers. It is noteworthy that
the as-prepared ­Ti3C2Tx MXene is highly fluorinated and the
ammonium cations surrounded by organic solvent molecules
can intercalate into the layers, which endows MXene with
the largest interlayer spacing of 5.07 nm up to now. Overall,
the bifluoride salts etching is safer relative to HF etching.
However, bifluoride salts are currently only used to etch
­Ti3AlC2 MAX and the universality of the method requires
to be further improved.
2.4 Electrochemical Etching
During the etching process of MAX precursors by using
the three methods mentioned above, the researchers may
be directly or indirectly exposed to hazardous HF, which
reduces the safety of the experimental process. Moreover,
high content of -F surface group may reduce the electronic
conductivity of obtained MXenes and block ion transport,
which is not conducive to their application in metal-ion
batteries [59]. Therefore, it is urgent to explore fluorine-
free etching method. In 2014, Gogotsi et al. removed
M-atom and A-atom layers from ­Ti3AlC2, ­Ti2AlC and
­Ti3SiC2 MAX precursors to prepare carbide-derived
carbons via electrochemical etching approach [95]. In
2015, Zhao et al. selectively extracted Ti atom layers
from ­Ti2SC MAX to obtain carbon/sulfur nanolaminates
through electrochemical etching [96]. It can be observed
that the above two works failed to obtain MXenes by
electrochemical etching method. In 2017, Sun et al. firstly
synthesized ­Ti2CTx MXene without -F termination in
diluted HCl aqueous electrolyte at 0.6 V for 5 days via
electrochemical etching [97], and the mechanism can be
exhibited as follows:
Ti2AlC + yCl−
+ (2x + z)H2O
→ Ti2C(OH)2xClyOz + Al3+ + (x + z)H2 + (y + 3)e−
(8)
Al3+ + 3e−
→ Al
(9)
At first, only the surface of ­Ti2AlC MAX that is in contact
with the electrolyte can be etched and the generated ­Ti2CTx
MXene is coated on the surface of MAX, which prevents
electrolyte from entering the interior and makes it difficult
for the inner MAX to be further etched. Subsequently, the
­Ti2CTx MXene on the surface will be transformed into a
carbon layer. Finally, a three-layered structure including
carbide-derived carbon, ­Ti2CTx MXene and unetched ­Ti2AlC
MAX are obtained, thus leading to a low yield of MXenes.
Some key parameters such as electrolyte concentration,
etching potential and time have been proven to have a direct
impact on the final etching products.
In 2018, Feng et al. prepared ­Ti3C2Tx MXene with a large
lateral size of 18.6 μm in a binary aqueous electrolyte con-
taining ­NH4Cl and TMAOH (Fig. 5e) [98]. In this method,
the weak Ti–Al bond is broken and then ­Al3+ cations com-
bine with ­Cl− anions to form ­AlCl3. The obtained ­Ti3C2
can be terminated by –OH group and the etching process is
illustrated as follows:
Ti3AlC2−3e−
+ 3Cl−
= Ti3C2 + AlCl3
(10)
Ti3C2 + 2OH−
−2e−
= Ti3C2(OH)2
(11)
Ti3C2 + 2H2O= Ti3C2(OH)2 + H2
(12)
It is noteworthy that the intercalation of ammonium species
and TMAOH can expand the interlayer spacing of ­Ti3C2Tx
MXene and expose more active sites, greatly promoting the
etching of inner MAX phase and thus resulting in a relatively
high etching yield of at least 60%. Later, a general strategy
based on thermal-assisted electrochemical etching route
was proposed by Hao’s group to synthesize various MXene
­(Ti2CTx, ­Cr2CTx and ­V2CTx) [99]. In this approach, 1 M HCl
solution is chosen as electrolyte and the heating facilitates
the etching of MAX precursor. Specifically, when the
etching time and temperature is increased to 9 h and 50 °C,
respectively, the obvious accordion-like morphology can be
observed for ­Ti2CTx MXene. In general, the electrochemical
etching enables the preparation of fluorine-free MXenes for
the first time and is safer and milder than conventional HF
etching method. However, over-etching and low etching
yield are unavoidable issues, which greatly hinders the large-
scale utilization of electrochemical etching method.
2.5 Alkali Etching
In addition to acids, alkalis can also be utilized to selectively
etch MAX precursors. The earliest attempt to prepare
MXenes via alkali etching was to immerse ­Ti3AlC2 MAX
in dilute aqueous NaOH solution at 80 °C by Xie et al. in
2014 [100]. However, only the outermost MAX can be
etched owing to the low NaOH concentration. Further,
Zhang et al. proposed a NaOH-assisted hydrothermal
process in 2018 to prepare ­Ti3C2Tx MXene with a high
yield of 92% (Fig. 5f) [101]. In this method, the ­OH− anions
attack Al-atom layers in ­Ti3AlC2 MAX to form Al (oxide)
hydroxides, which can further dissolve in alkali solution as
soluble Al(OH)4
− anions. It is noteworthy that high reaction
temperature (270 °C) and NaOH concentration (27.5 M) can
greatly speed up the whole process and promote complete
etching of ­Ti3AlC2 MAX. The etching process can be
described as follows:
Ti3AlC2 + OH−
+ 5H2O= Ti3C2(OH)2 + Al(OH)−
4 + 2.5H2
(13)
Ti3AlC2 + OH−
+ 5H2O= Ti3C2O2 + Al(OH)−
4 + 3.5H2
(14)
It is worth mentioning that special attention should be paid
to controlling reaction condition when MXene is prepared
by alkali etching method. A recent work by our group
found that ­Ti3C2Tx MXene can be completely converted to
­K2Ti8O17 nanowires after immersed in 5 M KOH solution
at 50 °C for 10 days [102]. The reaction mechanism can be
described as follows: The Ti-C bond in ­Ti3C2Tx MXene is
easily destroyed in the concentrated alkali environment and
MXene is oxidized into titanium oxide nanoparticles, and
the titanium oxide nanoparticles can then react with KOH
to generate the final ­K2Ti8O17 nanowires. Accordingly, the
stability of various MXenes in concentrated alkali solution
deserves further investigation. In general, although MXenes
with abundant –O and –OH functional groups can be
prepared via alkali etching route, harsh reaction condition
Page 9 of 49 68
greatly increases the experimental risk, which makes alkali
etching unsuitable for large-scale preparation of MXenes.
2.6 Common Molten Salts Etching
The above-mentioned methods for preparing MXenes are all
based on the wet chemical etching route. However, Gogotsi
et al. reported molten salts etching method to prepare ­Ti4N3Tx
MXene in 2016, which opens the door to the preparation of
MXenes via dry chemical etching techniques [103]. In this
method, a mixture of LiF, NaF and KF is used to selectively
etch Al-atom layers from ­Ti4AlN3 MAX precursor at 550 °C
under Ar atmosphere to synthesize ­Ti4N3Tx MXene, and the
few-layered nanoflakes can be obtained by TBAOH interca-
lation and subsequent ultrasonication. It is worth mention-
ing that since the discovery of MXenes, ­Ti4N3Tx is the first
nitride MXene that has been experimentally synthesized. In
2021, Zong et al. reported the synthesis of ­Ti2NTx MXene
by etching ­Ti2AlN MAX precursor with the mixture of fluo-
ride salt (KF, LiF, and NaF) in a molar ratio of 1:3 at 550 °C
[104]. Up to now, the family of nitride MXenes only con-
tains ­Ti2N, ­Mo2N, ­V2N and ­Ti4N3 [89, 103, 105], which is
mainly due to the difficulty in preparation. Firstly, the num-
ber of nitride MAX precursor is relatively limited due to the
high formation energy. Then, M-A bond in nitride MAX
exhibits high strength compared with that of carbide MAX,
indicating that larger exfoliation energy is needed for nitride
MAX. Finally, nitride MXene is prone to dissolve in HF solu-
tion and exhibits poor structural stability owing to the low
cohesive energy [38, 71]. Therefore, great efforts should be
made to explore the suitable etching route for nitride MAX.
In general, molten salts etching, as the first method to pre-
pare nitride MXenes, is of great significance. However, this
method is only applicable to the preparation of ­Ti4N3Tx and
­Ti2NTx MXene at present, and the obtained MXene exhibits
high content of -F surface group. The above two key points
greatly limit the development of common molten salts etch-
ing method.
2.7 Other Etching Methods
In addition to the etching methods described above, there are
other methods that can also be used to prepare MXenes. In
2017, Gogotsi’s group presented an ammoniation strategy
to transform ­Mo2C and ­V2C MXene to corresponding ­Mo2N
and ­V2N at 600 °C by using ­NH3 as nitrogen source (Fig. 5g)
[105], which further enriches the family of nitride MXenes.
It is worth mentioning that the obtained ­Mo2N and ­V2N
MXene demonstrate higher room temperature electronic
conductivity than their carbide counterparts. In 2020, Sun
et al. successfully prepared mesoporous ­Mo2C MXene via
ultraviolet-driven etching of ­Mo2Ga2C precursor, which
avoids the utilization of hazardous HF and greatly improves
the experimental safety [106]. They also presented thermal
reduction strategy to synthesize ­Ti2C MXene from ­Ti2SC
MAX. In this method, reductive gas such as ­H2 can react
with weakly-bonded S atoms, continuously accelerating the
etching process [107]. In 2021, iodine-assisted etching route
was developed by Feng et al. to synthesize ­Ti3C2Tx MXene
rich in -O terminations in anhydrous acetonitrile at 100 °C
(Fig. 5h) [108]. Owing to the water-free etching process,
­Ti3C2Tx MXene with an average lateral size of 1.8 µm
exhibits superior structural integrity and can be stored
stably in water for more than 2 weeks. Further, Jawaid et al.
successfully prepared halogenated ­Ti3C2Tx MXene under
anhydrous environment by using halogens ­(Br2, ­I2, ICl,
IBr) as etchants, and the halogen terminations may endow
MXenes with some new properties [109]. Besides, ionic
liquids such as 1-butyl-3-methylimidazolium hexafluoro-
phosphate ­(BMIMPF6) was utilized as etchant to prepare
­Ti2CTx MXene at 80 °C for 20 h [110]. The ionic liquids can
intercalate into interlayers, leading to expanded interlayer
spacing and the separation of layers.
Compared with above-mentioned top-down methods, the
bottom-up approaches are usually able to synthesize defect-
free 2D materials, which can also be utilized to obtain high-
quality MXenes. In 2015, Ren et al. developed chemical
vapor deposition method to fabricate large-area high-quality
ultrathin α-Mo2C nanosheets, which possess a thickness of
few nanometers and a lateral size of around 100 µm [111].
Moreover, the prepared α-Mo2C MXene exhibits superior
stability under various environments including water, HCl
or annealing at 200 °C in air. More importantly, this method
reveals excellent generality and can also be used to construct
WC and TaC crystals. In conclusion, many various methods
have been proposed to prepare MXenes until now. However,
each etching route has its own shortcomings and is unlikely
for large-scale utilization in the future. As we all know,
exploring a safe, green, non-hazardous, low-cost and easily
scalable preparation method is the biggest challenge for the

2.3. Bottom-Up Approaches

Bottom-up synthesis
Bottom-up synthesis methods like chemical vapor deposition
(CVD), template methods, and plasma-enhanced pulsed laser deposition
(PEPLD) have emerged as promising techniques for producing
high-quality 2D transition metal carbides (TMCs) and
nitrides. Compared to selective etching methods, CVD offers
higher crystalline quality.
Chemical vapor deposition
In recent years, CVD has become an important technique for producing
graphene and transition metal dichalcogenide (TMDs)
allowing for consistent, large-area growth on metal substrates
like copper, silicon and nickel [92, 93]. This method has been crucial
for the synthesis of thin 2D MXene films. Xiu and colleagues
were the first to create ultrathin 2D Mo2C crystals using a specific
method. They placed an ultrathin Cu foil on a Mo foil, which
served as the growth substrate. This setup was heated to a temperature
of 1085�C in the presence of H2 gas. The high temperature
caused the Cu to melt, allowing Mo atoms to diffuse onto
the liquid copper surface. During the growth process, the top liquid
Cu layer plays several important roles. It acts as a catalyst to
decompose methane into carbon atom while also acting as a medium
to regulate the diffusion of Mo into Cu substrate. The Cu
layer serves as a sacrificial layer, facilitating the easy transfer of
the Mo2C crystals to a different substrate by etching, due to the
large difference in chemical reactivity between Cu and Mo2C.
CH4 was introduced to provide carbon, acting as a precursor. The
properties of the Mo2C crystals, such as thickness, nucleation
density, and lateral size, were influenced by factors like growth
time and operating temperature [94]. Geng et al. demonstrated
that the morphology of Mo2C crystals can be controlled by varying
the concentration of methane (CH4) during the CVD process.
At low CH4 flow rates (0.1 sccm), fractal Mo2C crystals formed,
while higher CH4 concentrations led to different polygonal
shapes due to increased carbon supersaturation. Specifically, at
flow rates of 0.3, 0.4, and 0.6 sccm, the predominant crystal
shapes were rectangles, pentagons, and hexagons, respectively.
It was found that the hexagonal Mo2C crystals have a hexagonal
structure, differing from the orthorhombic structure reported by
Xu et al. The thickness of the Mo2C crystals was found to be tunable
by adjusting the thickness of the copper foil [95]. In a different
study by Wang et al., a TaN thin film was synthesized using
NH3 as a nitrogen source. A Ti/Cu foil was used as the growth
surface, and the growth temperature was set at 1077�C, which is
lower than the melting point of Cu. The copper foil remains solid
throughout the growth at temperatures near its melting point
(1077�C). The team also synthesized TaB crystals by using boron
powder instead of NH3 [96]. Qi and colleagues synthesized a
monoatomic ReC crystal on Re (0001) substrates through the
Synthesis, properties, and applications of Mxenes | 9
CVD method. They used C2H4 as the carbon source and achieved
graphene growth on the Re (0001) substrate at 903 K. By raising
the temperature and annealing between 953 K and 113 K, the graphene
decomposed into carbon atoms that dissolved into Re [97].
Furthermore, the CVD method was employed by Deng et al. to
create a graphene/α-Mo2C vertical heterostructure. Graphene
was grown on a Cu/Mo substrate at 1070�C and then heated to
1090�C to generate 2D α-Mo2C. This structure was later transferred
to a Si/SiO2 substrate [98]. Kang and colleagues conducted
a study to fabricate ultrathin Mo2C crystals both with and without
graphene as shown in Fig. 9. When employing a ratio of
1 : 600 for methane to hydrogen flow, pristine Mo2C was successfully
formed. When the same ratio adjusted to 1 : 000, graphene
formation occurred on the surface. Zeng et al. reported the
growth of a 2D in-plane WC/graphene heterostructure using a
one-step CVD process. They replaced the Cu foil with a Ga droplet
and utilized a growth temperature ranging from 980�C to
1020�C [99].
Template method
Apart from chemical vapor deposition (CVD) method, template-
based approaches have been developed for synthesizing two-
dimensional (2D) transition metal carbides (TMCs) and nitrides
(TMNs), offering much higher yields compared to CVD. These
template methods use two-dimensional transition metal oxides
(TMOs) nanosheets as templates. This involves processes like
carbonization or ammoniation of the initial sample. Xiao et al.
synthesized 2D MoN using this template approach. They first created
MoO3-coated NaCl by annealing a Mo precursor on NaCl
crystals in an Ar atmosphere at 280�C. Subsequently,
MoO3@NaCl crystals were ammoniated using NH3 at 650�C to
yield MoN@NaCl powders as shown in Fig. 10. By removing NaCl
with deionized water, they obtained 2D nanosheets of [101]. The
2D MoN nanosheets are highly dispersible in water, as evidenced
by the Tyndall effect. The nanosheets were found to be highly
uniform with a thickness of approximately 0.71. In another study
by Joshi et al., they produced 2D layered δ-MoN nanosheets using
a template method. Initially, they synthesized 2D layered MoO3
nanosheets through hot-filament chemical vapor deposition
(HFCVD). This involved heating a Mo wire in the presence of O2 at
a temperature near the melting point of Mo. The resulting MoO3
nanosheets were then deposited onto a cooler substrate.
Subsequently, these MoO3 nanosheets were ammoniated at
700�C for 8 h in an NH3/Ar gas environment, leading to the formation
of 2D δ-MoN nanosheets [102]. In a similar study, Jia et al.
produced N-doped Mo2C nanosheets through a two-step process
involving template synthesis. They started by creating MoO2
nanosheets as templates using a chemical vapor reduction technique.
MoO3 powders were subjected to this technique in the
presence of Ar/H2 gas at 900�C for 60 min, resulting in MoO2
nanosheets. These MoO2 nanosheets were then subjected to calcination
with C2H4N4 at 450�C for 2 h, followed by another round
Plasma enhanced pulsed layer deposition
Zhang et al. developed extensive 2D face-centered cubic (FCC)-
structured Mo2C crystals on a sapphire substrate using plasma-
enhanced pulsed layer deposition (PEPLD). In this method, as
shown in Fig. 11, a high-voltage electrode is employed to generate
CH4 plasma at the entrance of the chamber for CH4.
Simultaneously, a KrF laser operating at a wavelength of 248 nm
is focused onto a Mo metal target. The 2D structures exhibit an
exceptionally even surface. By adjusting the parameters, the
thickness of the sample can be modulated within the range of 2
to 25 nm The FCC Mo2C films were uniform, smooth, and tunable
in thickness from 2 to 25 nm by adjusting the laser pulse rate.
However, these films exhibited lower crystalline quality than
those synthesized by CVD, with significant stacking faults observed.
Zhang et al. proposed that the unique FCC structure arose
from the orientation relationship and minimal lattice mismatch
between the (111) planes of Mo2C and the (0003) planes of the
sapphire substrate which helped in its growth [104].
Bottom-up approaches for MXene synthesis, such as CVD,
PVD, and the Template Method, offer distinct advantages and
challenges. Both CVD and PVD are sophisticated techniques that
involve the deposition of MXene layers onto a substrate under
controlled conditions [105]. However, their yield can be limited
by factors such as the substrate used, temperature, and deposition
time. The cost of these methods is relatively high which
makes them less suitable for large-scale production, despite their
precision in producing high-quality, uniform films. On the other
hand, the Template Method is more cost-effective which makes
it a better option for producing MXene in certain applications
where high-scale production and lower costs are critical, though
the process is more time-consuming and less scalable compared
to more industrial methods like HF etching [106]. However,
bottom-up method involve the direct assembly of MXene layers
from precursor gases or vapors, the resultant films tend to have
fewer defects and contaminants compared to top-down
approaches that rely on chemical etching or exfoliation [107].

In contrast to the top-down procedures, which employ bulk material as precursors,

the bottom-up approaches use molecular material as precursors. Bottom-up
approaches could also be used to make MQDs from tiny precursors of organic and
inorganic molecules. Bottom-up approaches have a number of advantages,
including greater atomic usage, structural and morphological control, and faster
functionalization, among others, which give QDs better structures and properties
[71,72,73]. The previous investigations provide an excellent foundation for
bottom-up MXene preparation. However, for large-scale fabrication, simple, highly
efficient precursors with low toxicity, gentle reaction conditions, excellent
crystallinity, monodispersity, and high yields must be addressed. Meanwhile,
because of their relatively simple operating conditions compared to the top-down
methods, one-pot bottom-up methodologies will likely be employed to prepare
MXene in the future to fulfil the incremental application requirements. As there is
a little research on the bottom-up methodologies for MQD fabrication, the study is
promising, and great stress should be given to these strategies [56].

2.3.1. Molten Salt Synthesis

Due to its ease of use and short reaction time, the molten salt synthesis process has
lately gained favor. Using molybdenum acetylacetonate as a precursor, Cheng et al.
[74] synthesized a Mo2C QDs/carbon nanosheet (Mo2C/C) composite. In a typical
synthesis, the molybdenum acetyl-acetonate precursor, NaCl, and a sucrose
mixture were calcined for 2 h at 800 °C under an air environment as depicted in
Figure 7a. The SEM scan corroborated the nanosheet structure (Figure 7b),
demonstrating the importance of the method. The TEM micrograph further
confirmed the uniform and ultrathin structural morphology of the Mo2C/C
nanosheets (Figure 7c). According to the HR-TEM image (Figure 7d), the particle
diameter implanted on the carbon sheets was 23 nm with a d-spacing value of 2.37,
corresponding to the (002) plane of Mo2C. The nanosheet had a thickness of 3.5
nm, according to the AFM analysis.
2.3.2. Pyrolysis Approach

Pyrolysis is a well-known bottom-up methodology for MXene since it is a

time-saving, easy, and ecologically benign procedure. Wang et al. [75] fabricated
the Mo2C QDs-carbon polyhedron composites via a simple pyrolysis technique
(see Figure 8a). In summary, the Mo/ZIF-8 was synthesized via the solvothermal
method and then pyrolyzed at 700 °C for 2 h in an Ar environment before being
acid etched. The SEM micrograph (Figure 8b) clearly indicated the carbonization
of organic frameworks and the development of Mo2C as an individual polyhedron.
The TEM micrograph (Figure 8c) revealed uniformly dispersed ultra-small black
dots in the carbon matrix. The lattice fringe (i.e., 0.24 nm) of cubic-Mo2C was
aligned with the (111) direction plane, as revealed in the HR-TEM image (inset
Figure 8c). Despite the fact that significant works have been reported on the
synthesis of MQDs using diverse synthetic techniques, further research is needed
to make these bottom-up synthesis routes easy, efficient, and commercial. As a
result, in bottom-up approaches, the molecular precursors with the choice of
elements sources, as well as parameters of the reaction such as reaction time,
temperature, and precursor concentration, are crucial in the QDs synthesis. This
approach is efficient, simple, and monodisperse in comparison to the top-down
ones, with high yield, improved crystallinity, and normal conditions required for
the reactions. Still, very little research has been conducted on the synthesis of
MXene. These approaches will receive more attention in the near future in order to
address the needs of incremental applications. Carbon nanotubes have a
conductivity of 15 100 S cm−1, whereas reduced graphene oxide has a conductivity
of 15 100 S cm−1 [76]. As a result, the strong metallic and electrical conductivity of
Ti3C2Tx allowed it to work better as an electrocatalyst. In the case of surface
functionalization and composition, Ti2COm (1.03 × 104 cm2 V–1 s–1) has a better
carrier mobility than pure graphene (0.3–1.2 × 103 cm2 V–1 s–1) [43]. In addition,
the surface functional group of Ti3C2Tx (x = –O, –OH, –F) provides a large number
of sites and influences electrocatalytic efficiency. Owing to the substantial density
of state (DOS) around the Fermi level, they show strong electrocatalytic activity
[43].
prompt
Phase 1: The Structure (The Blueprint)
Use this prompt first to establish a logical flow.

Prompt:

"Act as a senior researcher in Materials Science. I am writing a comprehensive

review paper titled '2D MXene: The New Frontier of 2D Materials'.

Please provide a detailed outline for this paper. The outline should include:

1.​ Abstract: Key themes to cover.

2.​ Introduction: Evolution from Graphene to MXenes, and the MAX phase
precursors.
3.​ Synthesis Strategies: Top-down (HF etching, Fluoride-free) vs. Bottom-up
approaches.
4.​ Unique Properties: Electrical, mechanical, surface termination effects (-F,
-OH, -O).
5.​ Emerging Applications: Energy storage (Supercapacitors/Batteries), EMI
shielding, Biomedical, and Environmental remediation.
6.​ Challenges & Future Outlook: Stability issues and oxidation.

Please organize this logically with main headings and sub-headings."

Phase 2: Drafting the Content (Section by Section)

Once you have the outline, generate the text in chunks to ensure depth and technical accuracy.
Do not ask for the whole paper at once.

1. For the Introduction & Background

Prompt:

"Using the outline we created, write the Introduction section. Start with the
limitations of Graphene and the discovery of Ti3C2Tx in 2011 at Drexel University.
Explain the general formula M{n+1}Xn Tx clearly. Use academic, formal language
suitable for a high-impact journal."

2. For Synthesis Methods (Crucial Technical Detail)

Prompt:

"Write the section on Synthesis Strategies. Compare and contrast Hydrofluoric

Acid (HF) etching versus In-situ HF formation (MILD method). Discuss the
mechanism of selective etching of the 'A' layer from the MAX phase. Include the
chemical equations for the etching process using LaTeX formatting."

3. For Properties & Characterization

Prompt:

"Write the section on Physicochemical Properties. Focus on how surface

terminations (Tx) affect the electronic band structure (metallic vs. semiconducting
behavior). Discuss the role of hydrophilicity in processing. Also, describe key
characterization techniques like XRD patterns (shifting of the (002) peak) and XPS
analysis."

4. For Applications (The "New Frontier" aspect)

Prompt:

"Write the section on Applications. Focus on why MXene is considered the 'New
Frontier.' specifically detail:

1.​ Energy Storage: Why the volumetric capacitance is superior to

carbon-based materials.
2.​ EMI Shielding: The mechanism of absorption vs. reflection.
3.​ Environmental: Adsorption of heavy metals and dyes.​
Provide specific examples or theoretical performance metrics where
possible."

Phase 3: The "Polishing" Prompts

Use these to refine the output.

●​ To Check for Gaps: "Review the text generated so far. Are there any critical recent
developments (post-2023) in MXene research that we missed, such as non-MAX phase
precursors or i-MXenes?"
●​ To Add Visual Descriptions: "Describe 3 scientific figures/diagrams that would be
essential for this review paper (e.g., a schematic of the etching process). provide the
captions for them."

💡 Pro-Tips for Best Results

1.​ Request LaTeX: For chemical formulas (like Ti3C2Tx) and equations, explicitly tell
Gemini: "Use LaTeX formatting for all chemical formulas and equations."
2.​ Ask for Comparisons: MXenes are often compared to Graphene or transition metal
dichalcogenides (TMDs). Asking Gemini to "Provide a comparison table of MXene vs.
Graphene properties" adds immense value to a review paper.
3.​ Tone Check: If the output feels too casual, tell Gemini: "Rewrite this paragraph to be
more formal and objective, avoiding passive voice."
outline
Review Paper Outline
Title: 2D MXene: The New Frontier of 2D Materials

Target Audience: Researchers in Materials Science, Nanotechnology, and Electrochemistry.

1. Abstract
●​ Hook: Brief introduction to the post-graphene era and the rise of transition metal
carbides/nitrides (MXenes).
●​ Scope: Summarize the review's coverage—from the MAX phase precursors and diverse
etching strategies to unique physicochemical properties.
●​ Key Focus: Highlight why MXenes are the "New Frontier" (tunable surface chemistry,
metallic conductivity, hydrophilicity).
●​ Applications & Outlook: Briefly mention breakthrough applications (Energy storage,
EMI shielding, Environmental) and current bottlenecks (oxidation stability).

2. Introduction
●​ 2.1 The Rise of 2D Materials: Brief history from Graphene to TMDs (Transition Metal
Dichalcogenides) and the need for materials combining metallic conductivity with
hydrophilicity.
●​ 2.2 Discovery of MXenes: The 2011 breakthrough at Drexel University (Ti3C2Tx).
●​ 2.3 Structural Classification:
○​ Explanation of the general formula M{n+1}Xn Tx (where M = transition metal, X =
C/N, T = surface termination).
○​ Distinction between 211, 312, 413, and 514 phases.

3. Synthesis Strategies: From MAX to MXene

●​ 3.1 Top-Down Approaches (Etching):
○​ HF Etching: The traditional method (advantages vs. safety hazards).
○​ In-situ HF Formation (MILD method): Using LiF/HCl (mechanism of cation
intercalation and clay-like properties).
○​ Fluoride-Free Etching: Electrochemical etching, alkali treatment, and Lewis
acidic molten salts (essential for bio-applications).
●​ 3.2 Delamination: How to convert multi-layered MXene (ML-MXene) into few-layered or
single-layered flakes using intercalants (DMSO, TBAOH).
●​ 3.3 Bottom-Up Approaches: Chemical Vapor Deposition (CVD) for high-quality,
large-area films (briefly, as top-down is more common).
4. Unique Physicochemical Properties
●​ 4.1 Surface Chemistry & Terminations: The critical role of -F, -O, and -OH groups in
defining behavior.
●​ 4.2 Electronic Properties: Metallic conductivity (rare for solution-processable 2D
materials) and the semi-metal to semiconductor transition based on surface groups.
●​ 4.3 Mechanical Properties: Flexibility and strength for wearable electronics.
●​ 4.4 Optical & Magnetic Properties: Plasmonic behavior and potential in spintronics.

5. The "New Frontier": Emerging Applications

●​ 5.1 Electrochemical Energy Storage:
○​ Supercapacitors: Pseudocapacitance mechanisms and volumetric capacitance.
○​ Batteries: Use as electrode materials in Li-ion and Na-ion batteries (handling
volume expansion).
●​ 5.2 Environmental Remediation:
○​ Adsorption of heavy metals and toxic dyes (Malachite Green, Methylene Blue).
○​ Membrane technology for desalination.
●​ 5.3 Electromagnetic Interference (EMI) Shielding: High absorption effectiveness due
to internal reflections in the layered structure.
●​ 5.4 Biomedical Applications: Photothermal therapy (PTT), drug delivery, and
biosensors (focus on biocompatibility of Fluoride-free MXenes).

6. Critical Challenges & Limitations

●​ 6.1 Oxidation Stability: The tendency of MXenes to degrade into TiO2 in water/air and
strategies to prevent it (storage in argon, composites).
●​ 6.2 Scalability: The difficulty of producing kg-scale quantities with uniform quality.
●​ 6.3 Cost: The high cost of MAX phase precursors.

7. Future Outlook & Conclusion

●​ Next Gen MXenes: Double transition metal MXenes and i-MXenes.
●​ Machine Learning: Using AI to predict stable MXene structures.
●​ Concluding thought: Summarize why MXene is not just a "graphene alternative" but a
superior material for specific, high-performance applications.

Next Step
Now that we have the structure, would you like to generate the text for the Introduction section
first? (I can make sure to include the general formulas and the comparison to Graphene).
application
4.1 Energy Storage
Due to the rapid consumption of fossil fuels and gradually
serious environmental pollution, the development of clean
renewable energy has become more and more important
[160, 161]. However, the intermittency and instability of
renewable energy makes it necessary to store the generated
electricity [162]. In recent years, electrochemical energy
storage devices have received increasing research interests

because of their fast response speed, versatility and applica-

tion flexibility [163]. Among the various electrochemical

energy storage devices, LIBs currently occupy an absolute

dominant position. Other technologies such as SIBs, ZIBs,
Li–S batteries and SCs are in a rapid development period
[164]. In particular, SIBs are promising for large-scale
energy storage in the following few years owing to the low
price and abundant sodium resources [165].
4.1.1 Lithium‐Ion Batteries
In the past three decades, significant progress has been made
in the development of LIBs technology. Derived from the
high power and energy density, long cycle life, high energy
conversion efficiency and low discharge rate, LIBs system
has now been widely used in consumer devices, electric

vehicles and large-scale energy storage [166, 167]. Lay-

ered materials have been intensively studied as electrode

materials for LIBs due to their unique structural stability.

As early as 2012, Tang et al. confirmed that Ti3C2 MXene

possesses low Li+ diffusion barrier, superior electronic con-

ductivity, low discharge voltage and high lithium storage

capacity via theoretical computation, making it a promis-

ing LIBs anode [59]. Since then, a large number of works

have experimentally proved that MXene-based anodes can

deliver relatively high discharge capacity, stable long-term
cyclic performance and outstanding rate performance [72,
168–171]. The theoretical capacities of MXene electrodes
depends on formula weight, interlayer spacing as well as
the type of transition metals and surface groups. MXenes

with low formula weights such as V2C and Ti2C can afford
large gravimetric capacities [88, 172, 173]. In addition, large
interlayer spacing can allow more Li+ ions to intercalate into

the MXenes, accordingly leading to higher specific capaci-

ties [30, 174]. Surface functional groups such as –F and –OH

has been proved to impede Li+ transportation via theoretical

calculations, which is unfavorable for realization of theoreti-

cal specific capacity [59, 172]. However, O-terminated Ti3C2

MXene can absorb two Li layers, confirming the lithium

affinity of –O functional groups and thus contributing to the
enhanced lithium storage capacity (Fig. 10a) [120].
It is worth mentioning MXenes obtained by Lewis acidic

etching method may exhibit better electrochemical perfor-

mance due to the absence of –F and –OH surface groups

and the introduction of –O termination. In 2020, Li et al.

prepared multi-layered Ti3C2Tx MXene (T=–O and –Cl)
via CuCl2 etching of Ti3SiC2 precursor [67]. When used
as anode for LIBs, the obtained Ti3C2Tx MXene exhibit a
distinct pseudocapacitive-shaped cyclic voltammetry (CV)

curves without redox peaks in organic electrolyte. In com-

parison, MXene anodes synthesized by HF etching gener-
ally show obvious redox peaks in CV profiles [168, 171]. In

addition, Ti3C2Tx MXene delivers a discharge capacity of

205 mAh g−1 at 0.6C rate, corresponding to the fact that per
Ti atom can transfer around 0.4 electrons. Further, superior
long-term cyclic stability up to 2400 cycles can be obtained
for multi-layered Ti3C2Tx MXene electrode. The superior
lithium storage performance can be attributed to the strong
adsorption ability of -O surface group on Li+ cations [120].

Moreover, the Li+ insertion/deinsertion storage mecha-

nism can be confirmed by the enlarged/decreased interlayer

spacing through in-situ XRD measurement. In 2021, the

Nb2CTx MXene (T=–O and –Cl) with obvious accordion-

like morphology was prepared by CuCl2 molten salt etch-
ing of Nb2AlC precursor [119]. The theoretical calculations

indicate that –O surface groups can obtain more electrons

from Nb atoms than –Cl termination for Nb2CTx MXene,
thus resulting in the substitution of –O for –Cl functional

groups during ammonium persulfate solution washing pro-

cess, which is conducive to its lithium storage performance.

Nb2CTx MXene anode delivers a high discharge capacity of

330 mAh g−1 at 50 mA g−1 (Fig. 10b), which is larger than
the theoretical specific capacities of Nb2C (305 mAh g−1)
and Nb2CO2 (292 mAh g−1). Additionally, capacity rising
phenomenon can be clearly observed for Nb2CTx MXene

68 Page 22 of 49 Nano-Micro Lett. (2023) 15:68

© The authors [Link]

at 1000 mA g−1 (Fig. 10c), which can be attributed to the
electrochemical activation and common pillaring effect.
In 2022, Lin et al. prepared Ti2CTx and Ti3C2Tx MXene
by one-pot method in an air atmosphere with Ti, C, and Al

powders as precursor, simultaneously achieving the synthe-

sis of MAX and in-situ CuCl2 etching in molten salts system

[112]. When served as anodes for LIBs, Ti2CTx and Ti3C2Tx

electrode both exhibit rectangular and symmetric CV curves
in a voltage range of 0.1–2 V (Fig. 10d), which is similar to
those of previously reported MXene electrodes prepared by
Lewis acidic etching [67]. Furthermore, Ti2CTx anode shows
discharge capacities of 256 and 164 mAh g−1 at 0.5 and
10 mV s
−1, respectively. In comparison, specific capacities

of 164 and 113 mAh g−1 can be obtained for Ti3C2Tx elec-
trode at the same scan rate. The superior rate performance of

these two MXene electrodes is mainly due to the pseudoca-

pacitive-controlled charge storage mechanism. Later, Chen

et al. reported the synthesis of Ti3C2Tx, Ti2CTx, Ti3CNTx

and Ti4N3Tx MXene via molten salts-shielded synthesis
strategy in air atmosphere with MAX phases as precursor
and CuCl2 molten salt as etchant [175]. The low-melting

eutectic salt reaction medium can effectively restrain the oxi-

dation of MXenes at high temperature. More importantly,

the proposed method can be used to prepare Ti3C2Tx MXene

on a relatively large scale. The distinct accordion-like struc-

ture can still be obtained for Ti3C2Tx MXene prepared from

Fig. 10 a Valence electron localization function of Ti3C2O2Li2 with or without an extra Li layer.
Reproduced with permission from [120] Copy-
right 2014, American Chemical Society. b Rate performance of Nb2CTx MXene. c Long-term
cyclic performance of Nb2CTx MXene. Repro-
duced with permission from [119] Copyright 2021, Wiley–VCH. d CV curves of Ti2CTx and
Ti3C2Tx MXene. Reproduced with permission from

[112] Copyright 2021, The Authors, published by Springer Nature. e SEM image of Ti3C2Tx
MXene prepared from 60 batch of Ti3AlC2 MAX. f

Specific capacities of Ti3C2Tx, Ti2CTx and Ti3CNTx MXene at various C-rates. Reproduced
with permission from [175] Copyright 2022, Zheng-
zhou University. g Elemental composition comparison of Ti3C2Fx, Ti3C2Clx and Ti3C2Brx
MXenes. h Long-term cyclic performance of Ti3C2Fx,

Ti3C2Clx and Ti3C2Brx MXenes at 1 A g−1. Reproduced with permission from [178] Copyright
2022, Elsevier. i TEM image of Ti3C2Tx/Sn
anode after 2200 cycles. Reproduced with permission from [145] Copyright 2022, Elsevier

Nano-Micro Lett. (2023) 15:68 Page 23 of 49 68

13

60 g batch of Ti3AlC2 MAX (Fig. 10e), demonstrating supe-

rior scalability. Among the Ti3C2Tx, Ti2CTx and Ti3CNTx

MXene electrodes, Ti2CTx anode delivers the largest dis-

charge capacity, and the three electrodes all exhibit excellent

rate performance (Fig. 10f).

Recently, Cao et al. demonstrated the successful prepara-

tion of multi-layered Ti2NTx MXene (T=–O and vCl) via

CuCl2 etching at 450 °C for 1 h [176]. The existence of

Ti-Cl and Ti–O bonds can be confirmed by XPS and XAS
measurement. Theoretical calculations indicate that the
Gibbs energy change of –O substituting –Cl termination is
−2.3 eV, while the value of –O replacing –F surface group
is 0.07 eV, demonstrating that –Cl can be readily substituted

by –O. The obtained Ti2NTx MXene can deliver high dis-

charge capacities of 303.4 and 158.4 mAh g−1 at 0.1 and 5

A g−1, respectively. More importantly, a large capacity of

350 mAh g−1 after 1,200 cycles at 1 A g−1 can be obtained

for Ti2NTx electrode, revealing outstanding cycling stabil-

ity. A hybrid capacitor by pairing Ti2NTx anode and super

activated carbon cathode can demonstrate an energy density

of 45.36 Wh kg−1 at 123.32 W kg−1. It is noteworthy that

the MXene electrodes mentioned above are all at multi-

layered state, and few-layered MXene electrodes may show

better electrochemical performance. Liu et al. reported the

synthesis of exfoliated Ti3C2Tx MXene (termed as e-MS-
Ti3C2Tx) via CuCl2 molten salts etching and subsequent

TBAOH intercalation [153]. The e-MS-Ti3C2Tx electrode

delivers discharge capacities of 225 and 95 mAh g−1 at 0.2

and 16 A g−1, respectively, which is higher than that of unex-

foliated Ti3C2Tx anode. The boosted rate performance of

e-MS-Ti3C2Tx electrode is mainly assigned to the enhanced

contact area between electrode and electrolyte after exfolia-

tion. Additionally, the increased content of -O termination

after TBAOH treatment will also benefit the lithium storage

performance [177].
The type of halogen terminations may have an influence
on the electrochemical performance of MXene. Liu et al.
synthesized Ti3C2Tx MXene with –F, –Cl or –Br functional
groups via HF, NiCl2 or NiBr2 etching, respectively [178].
The typical accordion morphology can be afforded for three
halogenated MXenes. The element composition analysis
shows that Ti3C2Brx MXene possesses the highest content
of –O surface group among the Ti3C2Fx, Ti3C2Clx and
Ti3C2Brx MXene (Fig. 10g). This phenomenon is mainly
assigned to the fact that the formation energy of Ti–Br bond
is the lowest compared with that of Ti–Cl and Ti–F bonds

according to theoretical calculations. Consequently, –O

can easily replace the -Br surface group when the prepared
Ti3C2Brx MXene is exposed to air, and the highest content
of -O functional group contributes to the largest discharge
capacity of 189 mAh g−1 for Ti3C2Brx anode. Finally, the
Ti3C2Brx electrode exhibits the best rate performance and
cyclic performance relative to Ti3C2Fx and Ti3C2Clx anode
(Fig. 10h). The electrode materials mentioned above are
all individual MXenes, while the MXene/active metal
composites can also be utilized as anodes for LIBs. Wu et al.
reported the preparation of Sn-nanoconfined Ti3C2Tx MXene
hybrids via SnCl2 molten salt etching of Ti3AlC2 [145]. The
Sn nanoparticles are in-situ grown and confined between the
Ti3C2Tx MXene during the etching process. It is noteworthy
that the confined effect of MXene can effectively prevent
the aggregation of Sn nanoparticles at high temperature and
accommodate its large volume variation upon cycling. As
a result, Ti3C2Tx/Sn anode remains a reversible capacity
of 226.2 mAh g−1 after 1000 cycles at 0.2 A g−1, which
is higher than that of pure Ti3C2Tx and Sn electrode. The
volume expansion of Sn nanoparticles can gradually enlarge
the interlayer spacing of MXene from 1.17 to 1.34 nm after
2200 cycles (Fig. 10i), which greatly exposes more active
sites upon cycling and contributes to the obvious capacity
rising phenomenon.

4.1.2 Sodium‐Ion Batteries

SIBs possess a similar working mechanism to LIBs. It is well
known that the working voltage of SIBs is lower than that
of LIBs, thus resulting in a relatively low energy density of
SIBs [179, 180]. However, due to the abundance of sodium
resources and attractive cost-effectiveness [181], SIBs are
promising to be utilized in some fields that do not require
high energy density, such as large-scale energy storage [182,
183]. As a type of negative electrode for SIBs, transition
metal sulfides exhibit high theoretical specific capacities
and safe discharge voltage [184]. Nevertheless, large volume
expansion and inferior charge transfer kinetics of transition

metal sulfides greatly deteriorate their sodium storage perfor-

mance [185]. Our group has been working on improving the

electrochemical performance of transition metal compounds

in the past few years [73, 117]. Recently, we proposed a gen-

eral strategy for constructing Ti3C2Tx MXene/transition metal

sulfides (Ti3C2Tx/MSy, T=–O and –Cl, M=Fe, Co and Ni)

68 Page 24 of 49 Nano-Micro Lett. (2023) 15:68

© The authors [Link]
heterostructures as SIBs anodes through directly sulfurizing
Lewis acidic etching products (MXenes/metal composites)
(Fig. 11a–b) [147]. Different from the traditional construction
process of preparing MXene first, then adsorbing transition
metal ions and finally vulcanizing, this strategy simplifies
the preparation procedure of MXene/transition metal sulfides
hybrids via rationally utilizing Lewis acidic etching products.
Additionally, this fabrication process avoids the use of HF
as etchant and water as reaction medium, which effectively

improves the experimental safety and alleviates the oxida-

tion of MXene, respectively. For the fabricated Ti3C2Tx/FeS2

heterostructures, FeS2 nanoparticles are in-situ grown and

tightly fixed on the Ti3C2Tx MXene substrate (Fig. 11c–d),

demonstrating a stable framework for continuous Na+ inser-

tion/extraction. Furthermore, O 1 s XPS spectrum and theo-
retical calculations confirm that Ti3C2Tx MXene and FeS2

nanoparticles demonstrate interfacial electronic coupling

effect via Ti–O–Fe bonds (Fig. 11e–f), facilitating the rapid

interfacial electron transfer from MXene to FeS2. Addition-

ally, Ti3C2Tx/FeS2 hybrids also exhibit rapid Na+ diffusion

kinetics and mechanical strain release channels. Conse-

quently, derived from the above advantages, the Ti3C2Tx/FeS2

anode delivers a reversible capacity of 474.9 mAh g−1 after

600 cycles at 5 A g−1 (Fig. 11g), and reveals a high capac-

ity of 456.6 mAh g−1 at 10 A g−1, suggesting outstanding

long-term cyclic performance and rate capability. In addition,

the full-cell device assembled with Ti3C2Tx/FeS2 anode and
Na3V2(PO4)3 cathode can demonstrate a discharge capacity
of 431.6 mAh g−1 after 1000 cycles at 3 A g−1 and an energy
density of around 130 Wh kg−1 at a power density of 415
W kg−1, indicating superior application prospect of Ti3C2Tx/
FeS2 heterostructures.
Copper sulfide (CuS), as another common transition metal
sulfide, also possesses high theoretical capacity and low

Fig. 11 a Schematic of the fabrication process of Ti3C2Tx/MSy hybrids. b XRD pattern of

Ti3C2Tx/FeS2 composites. c SEM image of Ti3C2Tx/
FeS2 hybrids. d HRTEM image of Ti3C2Tx/FeS2. e O 1 s XPS spectra of Ti3C2Tx/FeS2. f
Charge density difference of Ti3C2Tx/FeS2 composites.

g Cyclic performance of Ti3C2Tx MXene and Ti3C2Tx/FeS2 hybrids at various current

densities. Reproduced with permission from [147] Copy-
right 2022, Wiley–VCH

Nano-Micro Lett. (2023) 15:68 Page 25 of 49 68

13

price, and has been widely studied as anode for SIBs. How-
ever, electrode pulverization and inferior electrochemical

reaction kinetics have an adverse effect on its performance

[186]. In order to improve the sodium storage performance
of CuS, our group readily fabricated Ti3C2Tx/CuS hybrids
(T=–O and –Cl) via CuCl2·2H2O etching and following

in-situ sulfurization treatment [148]. The construction pro-

cess also achieves the effective application of Lewis acidic

molten salts etching products. Plenty of CuS nanoparticles

are distributed among the Ti3C2Tx MXene substrate, and

they are connected by Ti–O–Cu covalent bonds. Benefit-

ing from the extremely boosted electron transfer and Na+

migration, enhanced sodium adsorption and structural

integrity, the obtained Ti3C2Tx/CuS anode delivers stable
long-term cyclic performance with a discharge capacity of
347 mAh g−1 after 800 cycles at 3 A g−1 and wonderful
rate performance with a high capacity of 346.3 mAh g−1 at
8 A g−1. More importantly, the constructed SIBs full cell
with Na3V2(PO4)3 cathode and Ti3C2Tx/CuS anode reveals a
capacity of 189.6 mAh g−1 after 800 cycles at 2 A g−1. In the
above-mentioned two works, MXene/transition metal sulfide
heterostructures are efficiently constructed by rationally
utilizing Lewis acidic etching products, namely MXenes/
metal composites, which fully reflects the great advantages
of Lewis acidic etching relative to other etching methods.

4.1.3 Zinc‐Ion Batteries

Due to the flammability of organic electrolyte, LIBs and
SIBs systems possess inevitable potential safety hazards,

resulting in the combustion of electric vehicles and large-

scale energy storage devices from time to time in the past

few years [187]. Therefore, ZIBs system has recently

attracted considerable attention owing to the use of aqueous
electrolyte, which possesses high safety and low price [188,
189]. Additionally, ZIBs also demonstrate other important
merits, such as high eco-efficiency and ionic conductivity
of approximately 1 S cm−1 [190]. The halogen electrodes
including Br2 and I2 exhibit conversion reaction mechanism
and high theoretical specific capacities, and have been
widely investigated as cathode materials for ZIBs [191–193].
Fortunately, the MXenes obtained by Lewis acidic etching
can be endowed with –Br or –I functional groups, so it is
necessary to investigate their zinc storage performance
(Fig. 12a). In 2021, Li et al. prepared Ti3C2 MXene with

–Cl, –Br and –I functional groups through CuCl2, CuBr2 and

CuI etching, respectively [123]. When applied as cathodes
for ZIBs, the Ti3C2Br2 and Ti3C2I2 MXenes exhibit obvious
redox peaks in CV profiles and flat discharge–charge
plateaus in galvanostatic charge–discharge curves, while
Ti3C2Cl2 MXene shows no redox peaks and oblique
charge–discharge curves. The conversion reaction process
of Ti3C2Br2 and Ti3C2I2 MXene is illustrated as follows:
In contrast, the Cl− anions in Ti3C2Cl2 MXene will loss
electrons and turn into Cl2 gas, which may escape from
the MXene interlayer, making this conversion reaction
irreversible. Consequently, Ti3C2Br2 and Ti3C2I2 MXene
demonstrate energy densities of 129 and 135.6 Wh kg−1,
respectively, which is significantly higher than that of
Ti3C2Cl2 MXene. This work realizes the application of
halogen terminations for the first time, and also suggests that
the electrochemical performance of MXenes can be greatly
improved by regulating the surface groups.
It is worth mentioning that the reaction mechanism of

above-mentioned Ti3C2I2 MXene is still stopping at indi-

vidual I

−/I0
redox pair, thus resulting in a low discharge
voltage of around 1.3 V when used as ZIBs cathode. If the
I
0
/I+ redox pair can be activated, the discharge voltage can
be further increased. However, I

+ cations are unstable in

common electrolytes such as ZnSO4 solution. In order to
solve this issue, Li et al. first synthesized Ti3C2I2 MXene

via CuI etching and then chose electrolyte system that con-
tains electronegative F− or Cl− anions, which can consid-
erably stabilize the I

+ cations during the cycling process

[194]. Specifically, once I

+ cations are generated, F− or

Cl− anions can combine with them, making I

+ cations exist
stably, which can be effectively confirmed by the peak
at 200 cm−1 in the in-situ Raman spectra of the Ti3C2I2
MXene (Fig. 12b). Therefore, the I
0

/I+ redox pair are suc-

cessfully activated in ZnCl2+ KCl electrolyte and a higher

reduction peak at 1.66 V can be observed (Fig. 12c). As

expected, Ti3C2I2 MXene in ZnCl2 + KCl electrolyte
affords a large discharge capacity of 207 and 126 mAh g−1

at a current density of 0.5 and 5 A g−1, respectively, show-

ing superior rate performance. Additionally, outstanding

cyclic stability can be delivered for Ti3C2I2 MXene with

2Br (27) − − 2e− → 2Br0
2I (28) − − 2e− → 2I0

68 Page 26 of 49 Nano-Micro Lett. (2023) 15:68

© The authors [Link]

approximately 80% capacity retention after 2800 cycles.
The excellent zinc storage performance is attributed to

the rapid electron/Zn2+ transfer kinetics and strong con-

finement effect of MXene that prevents interlayer iodine

active species from escaping to the outside. In short, the

additional high discharge plateau at 1.65 V endows Ti3C2I2
MXene with a large energy density of 280 Wh kg−1. The
above two works indicate that MXenes prepared by Lewis
acidic molten salts etching has broad development space
in aqueous ZIBs.

4.1.4 Lithium‐Sulfur Batteries

Li–S batteries have received extensive attention since its
birth in 1962. Compared with LIBs, SIBs and ZIBs systems,
Li–S batteries demonstrate a very high theoretical energy
density of 2600 Wh kg−1 and have been regarded as one of
the most promising energy storage devices in the future [195,
196]. However, ultralow electronic conductivity of sulfur
(10–30 S cm−1) and Li2S, sluggish reaction kinetics, severe
shuttle effect of LiPSs and low utilization rate of sulfur

Fig. 12 a Schematic diagram of the working mechanism of Zn/halogenated Ti3C2 MXene cells.
Reproduced with permission from [123] Copy-
right 2021, American Chemical Society. b In-situ Raman spectra of the Ti3C2I2 cathode around
200 cm−1. c CV curves of Ti3C2I2 cathode in

ZnCl2+KCl electrolyte or conventional ZnSO4 electrolyte. Reproduced with permission from

[194] Copyright 2021, Royal Society of Chem-
istry. d HAADF-STEM image of SA-Zn-MXene. e Charge density difference for Li2S4
polysulfides adsorbed on SA-Zn-MXene and MXene. f

Rate capabilities of S, S@MXene and S@SA-Zn-MXene. Reproduced with permission from

[157] Copyright 2020, Wiley–VCH. g Schematic
of the preparation process of N-MX-CoS2 hybrids. h Adsorption test of MX-Co, MX-CoS2 and
N-MX-CoS2. i Galvanostatic charge–discharge

curves of Li–S batteries with various materials-modified separator at 0.2C. j Long-term cyclic
stability of Li–S batteries with various materials-
treated separators at 1 C. Reproduced with permission from [146] Copyright 2021, Elsevier

Nano-Micro Lett. (2023) 15:68 Page 27 of 49 68

13

result in inferior rate performance and cyclic durability

[197]. Luckily, MXenes are expected to improve the
electrochemical performance of Li–S batteries owing to their
metallic conductivity, chemical adsorption ability, catalytic
effect and structural diversity [198, 199]. In 2020, single
atom zinc implanted Ti3C2Tx MXene (SA-Zn-MXene) as
sulfur host was successfully fabricated via ZnCl2 etching of
Ti3AlC2 MAX [157]. They found that Zn2+ cations in ZnCl2
molten salt can not only react with the interlayer Al atoms,
but also replace a few Ti species in MXene lattice during
the etching process, which can be further confirmed by the
bright dots corresponding to Zn atoms in HAADF-STEM
image (Fig. 12d). On one hand, the SA-Zn-MXene exhibits
strong interaction with Li2S4 polysulfides (Fig. 12e), and can
catalyze the polysulfides transformation by decreasing the
reaction barriers. On the other hand, the nucleation of Li2S2/

Li2S can be significantly boosted by Zn atoms in MXene lat-

tice. Additionally, the large volume variation of sulfur upon

cycling can be accommodated by flexible Ti3C2Tx MXene.

Consequently, the S@SA-Zn-MXene electrode exhibits the
lowest overpotential of 23 mV and superior rate performance
with a high capacity of 517 mAh g−1 at 6C (Fig. 12f). More
importantly, the enhanced cyclic stability can be obtained
for S@SA-Zn-MXene, which delivers a discharge capacity
of 706 mAh g−1 after 400 cycles at 1C.
Polar metal compounds including metal oxides, metal
sulfides, metal selenides, metal nitrides, metal borides and

metal phosphides have been considered as effective electro-

catalysts to accelerate reaction kinetics of LiPSs [200–202].

In 2022, Yang et al. obtained N-doped Ti3C2Tx MXene-CoS2

heterostructure (N-MX-CoS2) via CoCl2 etching and sub-

sequent in-situ sulfidation treatment with thiourea as sul-
fur source (Fig. 12g), and then utilized N-MX-CoS2 as a

bifunctional catalyst to modify the commercial separator

[146]. The N element can be doped into the hybrids during
the process of thiourea pyrolysis, which can be proved by
the existence of N–C and Ti–N peaks in XPS spectra. This
strategy enables CoS2 nanoparticles to be tightly anchored
among the MXene substrate. In the N-MX-CoS2 hybrids,
the N atoms and polar CoS2 nanoparticles can form strong
chemical interaction with LiPSs and provide rich catalytic
sites to facilitate LiPSs conversion reaction. The Ti3C2Tx
MXene with metallic-level conductivity can further promote

sulfur redox reaction kinetics. Since N-MX-CoS2 hetero-

structure possesses dual functions of adsorption and cataly-
sis, the shuttle effect of LiPSs can be effectively inhibited

and polarization can be greatly decreased (Fig. 12h–i).

Finally, the batteries with modified separator deliver supe-

rior rate performance (775 mAh g−1 at 4C) and excellent

long-term cycling stability with a low decay rate of 0.052%

per cycle (651 mAh g−1 after 700 cycles at 1C and 721.6
mAh g−1 after 400 cycles at 2C) (Fig. 12j). To our relief, a
series of MXenes/metal compound composites with strong
binding energy can also be synthesized via Lewis acidic
etching route, which is worthy of in-depth exploration and
may provide new inspiration to the further development of
Li–S batteries.

4.1.5 Metal Anodes‐Based Batteries

Metal anodes including Li, Na, K, Al, Mg and Zn have been
intensively investigated in high-performance secondary
metal batteries in the past few decades owing to their low
plating/stripping potentials and high theoretical specific
capacities, thus leading to high energy densities [203–206].
Nevertheless, there are some key factors that deteriorate
the electrochemical performance of metal anodes. First, the
uneven deposition of metals during the discharge process
will contribute to the uncontrolled growth of dendrites,

which can pierce the separator and result in the short-

circuit of cells. Then, the nearly infinite volume expansion

leads to the rupture of solid electrolyte interphase (SEI)

layer. In addition, the side reactions and the formation of
“dead metal” will continuously consume the electrolyte
and metal sources. Consequently, metal anodes generally
demonstrate low coulombic efficiency, short cycle life and
serious safety hazards [207, 208]. Some common strategies
such as optimizing electrolyte composition, building
artificial SEI film and fabricating three-dimensional robust
frameworks have been utilized to enhance the performance
of metal anodes [209]. Fortunately, MXenes with high
electronic conductivity, low ion migration barrier, unique
layered structure and sufficient functional groups can greatly
facilitate the plating/stripping kinetics, effectively preventing
the dendrite growth [15, 210].
For example, single zinc atoms immobilized Ti3C2Clx
MXene (Zn-MXene) as a host for lithium metal was reported
through ZnCl2 molten salts etching (Fig. 13a–b), and the
content of Zn monoatoms is around 0.87 at% [156]. It is

worth mentioning that sufficient reaction time is condu-

cive to the substitution of Zn for Ti. Due to the lithiophilic

68 Page 28 of 49 Nano-Micro Lett. (2023) 15:68

© The authors [Link]

nature of Zn, the lithium metal can preferentially nucleate
around the single atom Zn sites on the surface of Ti3C2Clx
MXene. When the plating level increases to 5 μAh cm−2,
a flat and smooth morphology can be obtained (Fig. 13c).

Furthermore, Li metal grows vertically along the nuclea-

tion site to form a bowl-shaped lithium at higher deposition

amounts (Fig. 13d–e), finally achieving dendrite-free Li

metal anode. Therefore, Zn-MXene films can exhibit a low
nucleation overpotential of 11.3 mV for half battery and a
long cycle life of 1200 h for symmetric cells at 1 mA cm−2

with a fixed capacity of 1 mAh cm−2. In addition, the Zn-

MXene//LiFePO4 full cell delivers a high capacity of 150

mAh g−1 at 0.5C and superior cyclic stability with a capacity

of about 100 mAh g−1 after 500 cycles at 10C.
In recent years, MXenes have attracted extensive attention

in inhibiting the growth of Zn dendrites due to their supe-

rior lattice matching [211]. More importantly, the surface

groups of MXenes are considered to affect the adsorption

energy and migration kinetics of Zn2+ ions. Based on this
point, Li et al. reported the synthesis of various halogenated
MXenes including Ti3C2Cl2, Ti3C2Br2 and Ti3C2I2 MXene
as interface layers via corresponding Lewis acidic molten
salts etching to regulate the Zn deposition [212]. They
found that above-mentioned halogenated MXenes possess

Fig. 13 a Schematic showing the preparation of Zn-MXene for Li nucleation and growth. b
HAADF-STEM image of Zn-MXene nanosheets.
c-e SEM images of Zn-MXene nanosheets after Li plating with capacities of 5, 20 and 60 μAh
cm−2, respectively. Reproduced with permission
from [156] Copyright 2020, American Chemical Society. f Calculated atomic distance between
Zn atom and neighboring halogen termination as

well as Zn adsorption energies of different MXene surfaces. g SEM image and EDS mapping of
the Ti3C2Cl2-Zn electrode after cycling. h Long-
term cyclic performance of various symmetric cells. i Schematic diagram of the Zn deposition
process on the MXene substrate. Reproduced with

permission from [212] Copyright 2021, American Chemical Society

Nano-Micro Lett. (2023) 15:68 Page 29 of 49 68

13

metallic-level conductivities and good affinity to Zn metal

via theoretical simulation (Fig. 13f), which is conducive to
the deposition of Zn2+ ions. Consequently, Zn2+ ions tend

to grow horizontally rather than vertically under the regula-

tion of outermost halogen surface groups, which effectively

inhibits the disordered growth of Zn metal at the beginning.

Subsequently, the constructed coherent heterogeneous inter-

face induces the uniform deposition of Zn metal (Fig. 13i).

As expected, the obtained halogenated MXene-Zn anode

exhibits better electrochemical performance than bare Zn

metal anode. Among the MXenes with –Cl, –Br or –I ter-

minations, the –Cl functionalized Ti3C2 MXene-Zn anode

possesses the strongest ability to inhibit the growth of Zn

dendrites derived from its medium adsorption and diffusion
for Zn2+. Consequently, Ti3C2Cl2-Zn electrode exhibits a flat
and smooth surface after cycling, and a cycle life of 840 h

at 2 mA cm−2 with a fixed capacity of 1 mAh cm−2 for sym-

metric cells (Fig. 13g–h). Finally, the Ti3C2Cl2-Zn//Ti3C2I2

full cell demonstrates superior long-term cyclic stability up

to 9,000 cycles, which is better than that of Zn//Ti3C2I2 bat-

tery. The above two works indicate that MXenes obtained

by Lewis acidic etching have a good induction effect on the

uniform growth of metal anodes.
4.1.6 Dual‐Ion Batteries
As a novel battery concept, the dual-ion batteries (DIBs)

demonstrate a brand-new working mechanism, which is real-

ized by intercalating the anions and cations of electrolyte

into respective electrodes. In general, DIBs possess some

advantages such as high theoretical energy density, low cost
and long cycle life [213]. Nevertheless, low anode specific
capacity of DIBs still remains a big problem. MXenes, as
a type of 2D layered material, have abundant nano-level
channels to allow the insertion and de-insertion of ions and
can be regarded as electrodes for DIBs. In 2022, Ti3C2Cl2
MXene with adjustable in-plane porosity was obtained by
eutectic molten salts (NaCl/ZnCl2) etching (Fig. 14a) [113].

The formation mechanism of in-plane pore has been dis-

cussed previously in detail. Specifically, the surface area

and mesoporous volume of Ti3C2Cl2 MXene increase gradu-

ally with the rise of NaCl content in ZnCl2/NaCl mixture

(Fig. 14b–e), which can create more active sites and ben-
efit the Li+ migration. For example, when the mole per-
cent of NaCl in ZnCl2/NaCl mixture is 60%, the obtained

Ti3C2Cl2-60 MXene delivers a specific surface area of 85

m2 g−1 and pore size concentrates on 3–4 nm. Additionally,
Ti3C2Cl2-60 demonstrates superior TiC6 octahedral core
symmetry and low Li+ migration kinetics. Consequently,
the Ti3C2Cl2-60 MXene as LIBs anode delivers a discharge
capacity of 382 mAh g−1 at 0.1 A g−1. Further, when paired
with graphite cathode, Ti3C2Cl2-60/graphite DIBs afford
a high discharge capacity of 242 mAh g−1 at 0.1 A g−1

(Fig. 14f), and the superior cyclic stability with 83% capac-
ity retention can also be obtained (141 mAh g−1 after 1000

cycles at 1 A g−1), demonstrating excellent electrochemi-

cal performance. The in-plane porous MXene produced by

Lewis acidic molten salts etching can also be utilized in

other fields such as catalysis.
4.1.7 Supercapacitors
SCs store and release energy through the physical adsorption
and desorption of electrolyte ions on the electrode surface,
and show higher energy density compared with common
capacitors [214]. Up to now, SCs have been regarded as a
reliable and promising energy storage device due to high
power density, environmental friendliness and high safety
[215]. MXenes become one of the best electrodes for SCs

owing to the moderate specific area, high electronic con-

ductivity, rich ion diffusion channels and large faradaic

pseudocapacitance [28, 216]. MXene was first used as elec-

trode material for SCs in 2013 [217]. Yury et al. reported

the synthesis of a series of cations (Li+, Na+, K+, NH4

+
and Mg2+)-intercalated Ti3C2Tx MXene, and a volumetric

capacitance of 350 F cm−3 can be obtained in KOH electro-

lyte, which is better than that of traditional porous carbon.

Later, freestanding Ti3C2Tx films prepared by LiF/HCl etch-

ing exhibit a high volumetric capacitance of 900 F cm−3

at 2 mV s−1 in H2SO4 electrolyte [65]. Recently, MXenes

synthesized by Lewis acidic etching have also been investi-

gated as electrode materials for SCs. For example, Ti3C2–Cu

composites was prepared by CuCl2·2H2O Lewis acidic

salts etching in 2021, and the Cu nanoparticles are tightly
anchored on the Ti3C2Tx MXene via Ti–O–Cu interfacial
bond [122]. Previous studies have shown that O-terminated
MXenes exhibit high capacitance due to the easy absorption
of H+ by –O functional group. The Ti3C2–Cu electrode is
able to deliver a capacitance of 885 F g−1 at 0.5 A g−1 in
H2SO4 electrolyte. Additionally, the symmetric SCs based

68 Page 30 of 49 Nano-Micro Lett. (2023) 15:68

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on Ti3C2–Cu achieve a high areal energy density of 103.3
μWh cm−2 at 0.8 mW cm−2. The superior electrochemical
performance of Ti3C2–Cu electrode is mainly attributed to

high content of –O termination, high pseudocapacitive con-

tribution of Cu nanoparticles, boosted charge/mass transfer

kinetics and strong interaction between MXene and Cu.

Later, Khan et al. synthesized Ti3C2Cl2, Ti3C2Br2 and

Ti3C2I2 MXene via CuCl2, CuBr2 and CuI molten salts etch-
ing, respectively [218]. When used as electrode materials

for SCs in 3 M H2SO4 electrolyte, typical pseudocapacitive-

shaped CV curves can be obtained and a specific capacity of

92, 29 and 63C g−1 can be afforded for Ti3C2Cl2, Ti3C2Br2

and Ti3C2I2 MXene at 5 mV s
−1. Further, the capacity reten-
tion ratio can reach as high as 85.22% after 10,000 cycles

at 1.4 A g−1 for Ti3C2I2 electrode, suggesting outstanding

long-term cyclic stability. The excellent electrochemical
performance of –F, –Br or –I functionalized MXene mainly

benefits from the high electrochemical activity of corre-

sponding halogen surface groups. In order to further improve

the performance of MXenes produced by Lewis acidic etch-

ing, several common and effective strategies such as tuning

the interlayer spacing and compositing MXene with other

Fig. 14 a Schematic showing the preparation of in-plane porous Ti3C2Cl2 MXene via eutectic
etching. b N2 adsorption–desorption isotherms
of various MXenes. TEM images of Ti3C2Cl2 MXene obtained by eutectic etching with c 0%, d
33% and e 60% NaCl mole percent in the NaCl/
ZnCl2 mixture. f Rate performance of Ti3C2Cl2-60/graphite DIBs. Reproduced with permission
from [113] Copyright 2021, Wiley–VCH. g
Schematic demonstrating the preparation of MXene-NaCl and MXene-CTAB. h XRD patterns of
MXene, MXene-NaCl and MXene-CTAB.
Reproduced with permission from [219] Copyright 2021, Elsevier. i HRTEM image of
QD-Ti3C2Cl2@NiAl-LDHs composites. j The free energy

diagram of pseudocapacitive process on the QD-Ti3C2Cl2@NiAl-LDHs. k Specific capacities of

the various electrodes at different current densi-
ties. Reproduced with permission from [222] Copyright 2021, Elsevier

Nano-Micro Lett. (2023) 15:68 Page 31 of 49 68

13

electroactive materials have been proposed by researchers.

For example, Zhang et al. reported the synthesis of Ti3C2Cl2
MXene via CdCl2 etching in 2022 and then increased the
interlayer spacing of MXene by the intercalation of NaCl
and cetyltrimethylammonium bromide (CTAB), respectively
(Fig. 14g) [219]. As expected, large organic cation CTA+
can greatly enlarge the interlayer spacing to 1.16 nm, while
the small Na+ cation-intercalated MXene shows a value of

1.14 nm (Fig. 14h). The large interlayer spacing of MXene-

CTAB can increase the contact area between MXene and

electrolyte, boost the ion diffusion kinetics and decrease the

charge transfer resistance. Additionally, the CTA+ cations

can react with the ions between MXene layers, and effec-
tively adsorb counter ions in the electrolyte to deliver addi-
tional specific capacitance. Consequently, the Ti3C2Cl2

MXene-CTAB electrode can provide a higher capacitance

of 258.28 F g−1 in (NH4)2SO4 electrolyte than MXene-NaCl.
The highest energy density of MXene-CTAB electrode can
reach 11.48 Wh kg−1 at a power density of 200 W kg−1.
More importantly, Ti3C2Cl2 MXene-CTAB exhibits superior
cyclic durability with only 7% capacitance loss after 3000
cycles at 1.0 A g−1, which is superior to that of Ti3C2Cl2
MXene and Ti3C2Cl2 MXene-NaCl.

LDHs have been regarded as promising electrode mate-

rials for SCs owing to their high specific capacitance and

energy density [220]. However, low electronic conductivity

of LDHs results in inferior rate capability and cyclic per-

formance [221]. Hybridizing LDHs with highly conduc-
tive MXenes may lead to great improvement in electrode

performance. In 2022, Zhao et al. firstly prepared Ti3C2Cl2

MXene nanodots (QD-Ti3C2Cl2) via CdCl2 etching and sub-

sequent hydrothermal reaction, and the nanodots are dis-
tributed on the surface of MXene nanosheets [222]. Then,

the negatively-charged QD-Ti3C2Cl2 can integrate with posi-

tively-charged NiAl-LDHs to electrostatically fabricate QD-
Ti3C2Cl2@NiAl-LDHs composites, where the NiAl-LDHs
nanosheets are dispersed on MXene nanosheets (Fig. 14i).

Derived from the superior charge transfer kinetics of QD-

Ti3C2Cl2, a small band gap of 0.52 eV can be obtained for

QD-Ti3C2Cl2@NiAl-LDHs, which is lower than that of

NiAl-LDHs (1.51 eV), demonstrating enhanced electronic

conductivity. Additionally, compared with NiAl-LDHs, QD-

Ti3C2Cl2@NiAl-LDHs hybrids possess a higher specific

area of 658.74 m2 g−1 and lower Gibbs free energy of redox

reaction (−0.355 eV) (Fig. 14j), greatly accelerating the
mass transport and adsorption of active species. Therefore,

the obtained QD-Ti3C2Cl2@NiAl-LDHs electrode achieves

a pretty high capacitance of 2010.8 F g−1 at 1.0 A g−1
(Fig. 14k), and excellent long-term cyclic performance with
94.1% capacitance retention after 10,000 cycles, which is
better than those of NiAl-LDHs electrode. Additionally, a
large energy density of 100.5 Wh kg−1 can be delivered for
QD-Ti3C2Cl2@NiAl-LDHs at a power density of 299.8 W
kg−1. The above examples reveal that MXenes prepared by

Lewis acidic etching are promising anodes for electrochemi-

cal energy storage systems.

4.2 Energy Conversion

Exploring renewable energy is one of the greatest challenges
for the sustainable development of contemporary society.
Advanced energy conversion systems such as photovoltaic
electrodes, catalysis, and fuel cell, will play a crucial role
in the future [223]. For example, photovoltaic devices such
as silicon solar cells have been commercialized on a large
scale and dominate the market in China, and perovskite solar
cells (PSCs) are attracting increasing attention. Additionally,
several common and classical catalysis reactions including
hydrogen evolution reaction (HER), oxygen evolution
reaction (OER), carbon dioxide reduction reaction (CO2RR)
and nitrogen reduction reaction (NRR) have also been
widely investigated in the past decades [224].
4.2.1 Perovskite Solar Cells

Compared with silicon solar cells, PSCs possess the advan-

tages of low cost, high absorption coefficient, easy prepara-
tion and high theoretical photoelectric conversion efficiency

(PCE). In recent years, a high PCE value of 25.7% can be

obtained for PSCs, which makes PSCs become one of the
most promising photovoltaic devices in the near future [225].
However, defective interfaces and grain boundaries of PSCs
greatly deteriorate device performance [226]. Recently,

MXenes have been intensively researched in PSCs as addi-

tive, electrode or hole/electron transport layer owing to their

high electrical conductivity and carrier mobility, adjustable

work function, abundant surface functional groups and
excellent mechanical property [227]. In 2021, Zhou et al.
synthesized Ti3C2Clx MXene suspension via CdCl2 etching
and following IPA intercalation, and the Ti3C2Clx MXene
as addictive is then incorporated into the bulk and surface

68 Page 32 of 49 Nano-Micro Lett. (2023) 15:68

© The authors [Link]

of perovskite film (Fig. 15a–b) [159]. The peak shift in Pb
4f XPS spectrum indicates that the -Cl surface group with
strong electron-withdrawing ability in Ti3C2Clx MXene and
the unsaturated Pb2+ in CsPbBr3 can form Pb-Cl bond along
the interface (Fig. 15c). The strong interaction between

Ti3C2Clx MXene and CsPbBr3 can effectively relieve the lat-

tice strain of perovskite (Fig. 15d), and the defects situated at

the interface and grain boundaries can be healed. Therefore,

a high PCE of 11.08% and open-circuit voltage of 1.702 V
can be obtained for the fabricated all-inorganic CsPbBr3
PSCs. More importantly, the Ti3C2Clx-functionalized
CsPbBr3 devices exhibit outstanding long-term stability of

100 days under 80% relative humidity and 25 °C (Fig. 15e),

demonstrating the high-quality of perovskite films.
Later, Ti3C2Clx quantum dots (Ti3C2Clx QDs) with
an average size of around 8 nm were prepared through
CuCl2 etching, subsequent hydrothermal reaction and
ultrasonication treatment (Fig. 15f) [228]. As followed,

the Ti3C2Clx QDs is introduced into the precursor solu-

tion to fabricate perovskite layer via one-step process-
ing. Similarly, the -Cl functional groups in Ti3C2Clx

QDs can generate chemical bond with Pb2+ cations in

Rb0.05Cs0.05(FA0.83MA0.17)0.90Pb(I0.83Br0.17)3 perovskite
compound, which can also be confirmed by the peaks move

Fig. 15 a Schematic showing the preparation of Ti3C2Clx MXene. b Cross-sectional SEM image
of all-inorganic PSCs. c Pb 4f XPS spectra
of CsPbBr3 perovskite film. d Schematic of released strain in the CsPbBr3 grains with Ti3C2Clx
MXene. e Long-term stability of the devices in
air under 80% relative humidity and 25 °C. Reproduced with permission from [159] Copyright
2021, The Authors, published by Wiley–VCH.

f Schematic demonstrating the preparation of Ti3C2Clx QDs. g SEM images of pristine and
Ti3C2Clx QDs-modified perovskite films. h Sche-
matic illustration of the perovskite-Ti3C2Clx QDs-SnO2 heterojunction. i Reverse and forward
scans for the pristine and Ti3C2Clx QDs-modified

devices. j Normalized PCEs against storage time for the pristine and Ti3C2Clx QDs-treated
devices. Reproduced with permission from [228]
Copyright 2021, Elsevier

Nano-Micro Lett. (2023) 15:68 Page 33 of 49 68

13

in Pb 4f and Cl 2p XPS spectra. Additionally, scanning

electron microscopy (SEM) images demonstrate that the
perovskite grain size can be enlarged from 273 to 453 nm
after the addition of Ti3C2Clx QDs (Fig. 15g), reducing the
number of grain boundary. The introduction of Ti3C2Clx
QDs acting as nucleation sites can effectively slow down
the growth of perovskite crystal and the film crystallinity
can be greatly enhanced with an optimized orientation, thus
leading to fewer crystal distortion. Moreover, the interfacial
charge transfer resistance between perovskite layer and SnO2
electron transport layer can be greatly reduced owing to the

highly conductive Ti3C2Clx, and the energy level align-

ment can be further improved (Fig. 15h). Consequently, the

Ti3C2Clx QDs-modified device can deliver a high PCE value

of 21.31% and an open-circuit voltage of 1.19 V (Fig. 15i).
Furthermore, the extraordinary long-term stability with 84%
PCE retention after 1000 h storage time under 40% relative
humidity can be afforded for Ti3C2Clx QDs-modified device
(Fig. 15j). The two works indicate that the Cl-terminated
MXenes prepared by Lewis acidic etching has great potential
to enhance the performance of PSCs devices.
4.2.2 Hydrogen Evolution Reaction
H2 is regarded as a clean and renewable energy source that
can replace fossil fuels in the future owing to its high heat
value and pollution-free combustion product. The HER is
an effective method to produce high-purity H2 via water
splitting [229]. Some noble catalysts such as Au, Pt and
Pd have been widely used to accelerate the H2 evolution
kinetics and decrease overpotentials because of their high
activities [230]. Nevertheless, high price and low reserve
greatly impede the large-scale application of noble catalysts.
In recent years, MXenes have been considerably researched

as catalyst derived from their 2D layered structure, tailor-

able surface chemistry, diverse composition, high electri-
cal conductivity and superior mechanical stability [231,

232]. Particularly, the polar terminations of MXenes can

strongly interact with other materials to form high-perfor-

mance catalysts. For example, Jiang et al. firstly synthesized
Ti3CNCl2 MXene via NiCl2 molten salt etching of Ti3AlCN
MAX. Then, Ti3CNCl2@CoS2 core–shell architecture as
efficient HER catalyst can be obtained by hydrothermal

reaction [233]. Theoretical calculations reveal that electron

can transfer from Ti3CNCl2 MXene to CoS2 through -Cl
functional group, demonstrating strong interaction between
them. Additionally, the Gibbs free energy of H2 adsorption
of Ti3CNCl2@CoS2 hybrids is close to zero, indicating a
strong catalytic activity. It is noteworthy that the electrons

of Ti3CNCl2@CoS2 become more delocalized, which sug-

gests that H+ cations are easy to combine with electrons. As

a result, benefiting from the synergistic effect of CoS2 and

highly-conductive Ti3CNCl2, the constructed Ti3CNCl2@
CoS2 hybrids deliver a low Tafel slope of 89 mV dec−1 and
small charge transfer resistance in 0.5 M H2SO4 electrolyte.
Moreover, boosted long-term stability can be obtained for
Ti3CNCl2@CoS2, which can sustain catalytic activity for
10 h and the current density shows almost no attenuation.
4.2.3 Overall Water Splitting
Water splitting provides a simple, effective and promising
method for H2 and O2 production, which can effectively solve
the energy crisis [234]. In general, electrolysis of water is
composed of HER at the cathode and the OER at the anode

and requires a theoretical voltage of 1.23 V [235]. Neverthe-

less, the multi-electron reaction results in sluggish kinetics,

which greatly limits the H2 and O2 production and increases

the drive voltage [236]. Exploring high-performance electro-

catalysts can effectively solve the above-mentioned issues.

For example, Sarfraz et al. reported the synthesis of Cl-

terminated Ti3C2Cl2 MXene via CuCl2 etching of Ti3AlC2

precursor in 2022, and Ti3C2Cl2 MXene with obvious lamel-

lar structure is then used as catalyst for water splitting in

1 M KOH solution [237]. Compared with Ti3C2Tx MXene

obtained by HF etching (HF-Ti3C2Tx MXene), Ti3C2Cl2
MXene possesses an enlarged interlayer spacing, more active
sites and stable architecture. Therefore, Ti3C2Cl2 electrode
shows a smaller overpotential of 330 mV than HF-Ti3C2Tx
MXene (390 mV) at 30 mA cm−2 for OER. Similarly, a lower
HER overpotential of 259 mV can be obtained for Ti3C2Cl2
at 10 mA cm−2, while HF-Ti3C2Tx MXene demonstrates a
large overpotential of 444 mV at the same current density.
Notably, Ti3C2Cl2 electrode exhibits a low Tafel slope of 48
and 92 mV dec−1 for OER and HER, respectively, indicating
excellent catalytic activity for water splitting.

68 Page 34 of 49 Nano-Micro Lett. (2023) 15:68

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4.2.4 Carbon Dioxide Reduction Reaction
In recent years, the depletion of fossil fuels has produced
a large amount of CO2, leading to a huge impact on the

environment, such as greenhouse effect and the extinc-

tion of some species [238]. Therefore, it is necessary to

reduce CO2 emission or find effective ways to use it. The

CO2RR is an effective and green method to convert CO2
into high-value chemicals or fuels [239]. However, CO2RR
suffers from sluggish kinetics owing to the good stability
of CO2, and efficient catalysts are therefore required [240].

In 2021, Zhao et al. synthesized single atom Cu immobi-

lized Ti3C2Clx MXene (SA-Cu-MXene) as CO2RR electro-
catalyst via ZnCl2 molten salt etching of Ti3(Al1−xCux)C2

MAX (Fig. 16a) [158]. It is worth mentioning that the Cu

atoms can be well preserved during the selective etching
process. The content of Cu single atoms is approximately
to be 1.0 wt% and many bright dots representing Cu atoms
can be observed in HAADF-STEM image (Fig. 16b).
Additionally, XAS measurement indicates that Cu atoms
are coordinated by –O surface groups of Ti3C2Clx MXene
via Cu–O bond (Fig. 16c). Owing to the superior charge
transfer kinetics of MXene and unsaturated electronic
structure of Cu atoms, the obtained catalyst can greatly
reduce the energy barrier from CO2 to CH3OH and deliver
a maximum Faradaic efficiency value of 59.1% at −1.4 V

(Fig. 16d–e), demonstrating outstanding catalytic capa-

bility. More importantly, a high Faradaic efficiency of

over 58% can still be obtained after 30 h, which indicates

enhanced stability.
4.2.5 Nitrogen Reduction Reaction
NH3, as a particularly important chemical material, has
played a key role in industry and agriculture. At present,
large-scale NH3 synthesis mainly relies on the traditional

Fig. 16 a Schematic of the synthesis of SA-Cu-MXene. b HAADF-STEM image of

SA-Cu-MXene. c XAS spectra of SA-Cu-MXene. d Free

energy diagram of CO2 to CH3OH. e Faradaic efficiency of SA-Cu-MXene at various potentials.

Reproduced with permission from [158] Copy-
right 2021, American Chemical Society. f Schematic of the preparation of HD-Fe-MXene. g
Faradaic efficiency of different materials at various

potentials. Reproduced with permission from [244] Copyright 2022, The Authors, published by
Wiley–VCH

Nano-Micro Lett. (2023) 15:68 Page 35 of 49 68

13

Haber–Bosch process, which requires to be carried out

under high temperature and pressure (300–500 °C and
150–200 atm) [241]. In short, Haber–Bosch process not only

consumes huge energy but also releases plenty of green-

house gases into the atmosphere. The electrocatalytic NRR
has attracted intensive attention as a green method to pro-
duce NH3 at room temperature and atmospheric pressure

[242]. Nevertheless, promising electrocatalysts with supe-

rior stability and high activity are also required to promote

the NRR process, which suffers from a large overpotential

and low yield of NH3 owing to the strong N≡N bond in N2
[243]. For example, Wang et al. prepared highly dispersed

Fe immobilized in fluorine-free Ti3C2Tx MXene (HD-Fe-

MXene) as NRR electrocatalyst in 0.1 M Na2SO4 electrolyte

through FeCl2 etching and HCl washing (Fig. 16f) [244]. The
XRD pattern indicates that the formed Fe nanoparticles can
be eliminated by HCl, and energy-dispersive spectroscopy
and XPS analysis demonstrate that the remaining Fe atoms

with a content of 3.12 wt% are highly anchored on the sur-

face of Ti3C2Tx MXene via Fe–O bond. Benefiting from the

rich active sites and outstanding electrical conductivity of

Fe atoms and fluorine-free Ti3C2Tx MXene, the adsorption
and activation of N2 as well as charge transfer kinetics can

be considerably improved. Consequently, the obtained elec-

trocatalyst can afford a high NH3 yield of 18.25 μg h−1 mg−1

and a Faradaic efficiency of 21.8% (Fig. 16g). Additionally,

boosted stability with almost unchanged current density after
24 h testing can be obtained for HD-Fe-MXene electrode.
4.3 Sensors
In modern society, sensors play an increasingly significant
role in environmental protection, disease detection and
industrial production, etc. Currently, there are different
types of sensors, such as gas sensors, biosensors and sound
sensors [245]. Owing to the medium specific surface area,
layered structure, rich active sites and superior electronic
conductivity, MXenes have been regarded as promising sen-
sitive materials in recent years [44]. For example, Wu et al.

synthesized Ti3C2Cl2 MXene via ZnCl2 etching in 2021 and

investigated its gas-sensing performance [246]. They found
that Ti3C2Cl2 MXene exhibits a response value of 13.2%
to NH3, indicating the potential of Ti3C2Cl2 MXene in gas
sensors. In addition, Au/Pt/Ti3C2Cl2 hybrids as sensors were
fabricated by ZnCl2 etching and subsequent self-reduction

process (Fig. 17a) [247]. The Ti species with low-valence

can effectively reduce Au3+ and Pt4+ cations to Au and Pt
nanoparticles, respectively, which are then distributed on
the surface of Ti3C2Cl2 nanosheets (Fig. 17b). By virtue of
the superior catalytic activity of obtained Au/Pt/Ti3C2Cl2
composites, a colorimetric sensing platform is constructed
to in-situ detect the H2O2 from HeLa cells. The fabricated
sensor possesses a wide detection range of 50–10,000 μM
and detection limit of 10.24 μM (Fig. 17c), demonstrating
promising application in intracellular biosensing.
4.4 Microwave Absorption
With the rapid development of information technology in
recent years, smart devices based on electromagnetic wave

have been utilized more and more frequently, thus result-

ing in increasingly serious electromagnetic pollution [248,

249]. Therefore, exploring advanced microwave absorption

materials is becoming increasingly important. MXenes dem-

onstrate great potential in the fields of microwave absorption

based on the following aspects: (1) The layered architecture

can realize multiple reflection and scattering of electromag-

netic wave; (2) The high electronic conductivity endows

MXenes with high dielectric loss; (3) The surface groups of

MXenes will produce dipole under electromagnetic field,
which further strengthens the dielectric loss [52]. It is note-
worthy that MXenes/metal hybrids obtained by one-step

Lewis acidic etching can exhibit good microwave absorption

performance due to the addition of ferromagnetic metals. For
example, Wang et al. firstly prepared Ti3CNCl2(Co) hybrids
via CoCl2 etching, and Ti3CNCl2(Co) composites were then
distributed on the surface of reduced graphene oxide (RGO)
nanosheets to form Ti3CNCl2-decorated RGO aerogel via
the crosslinking effect of dopamine hydrochloride (Fig. 17d)

[250]. Benefiting from the conductivity loss of 3D intercon-

necting conductive network, improved polarization loss of

abundant heterogeneous interfaces and surface functional

groups as well as magnetic loss of Co nanoparticles, the
Ti3CNCl2/RGO aerogel can deliver a minimum reflection
loss intensity of -62.62 dB at 17.2 GHz with a thickness of

2.5 mm (Fig. 17e), indicating its boosted microwave absorb-

ing ability.

Applications of MXene
MXene in energy storage
It is crucial to develop advanced cathode and anode materials
that can increase the capacity or voltage of batteries, leading to
higher energy density. However, there are significant challenges
in achieving this, such as large volume changes, poor electrode
conductivity, and unstable solid electrolyte interphase (SEI)
films, which greatly impede their practical applications.
Thankfully, the utilization of MXenes has provided a promising
solution to these issues. MXenes, with their distinctive structures

and physicochemical properties, can act as both electrochemi-

cally active materials and 2D conductive substrates. This allows

for the construction of advanced hybrid electrodes, effectively

addressing the aforementioned challenges and paving the way

for improved battery performance [170]. MXenes have demon-

strated their utility in energy storage systems as a result of their

exceptional electrochemical properties and remarkable conduc-

tivity. They are extensively employed as electrodes in Lithium

Ion (Li-ion) batteries. The layered structure of MXenes enables

the intercalation of Liþ ions, making them more favorable as
electrode materials when compared to other two-dimensional

carbon nanomaterials like graphene [5]. In 2012, Naguib et al. pio-

neered the utilization of MXene, specifically Ti2C-based MXene,

as a negative electrode in Li-ion batteries. They reported a

steady-state capacity of 225 mAhg−1 at a C/25 rate, and after 80

cycles, the capacity at 1C rate was 110 mAhg−1 [168]. The afore-
mentioned research group also developed Nb2CTx and V2CTx as

electrode materials for Li-ion batteries. Nb2CTx exhibited a re-

versible capacity of 170mAhg−1 at a lithiation voltage lower than

the previous MXene, while V2CTx demonstrated a capacity of

260mAhg−1 at 1C rate. Importantly, both of these MXenes dem-

onstrated excellent cycling stability, with the ability to withstand

high cycling rates of up to 10C [61]. In a study by Sun et al.,

Ti3C2Tx MXene was investigated as an anode material for Li-ion

batteries. The research revealed that the Ti3C2Tx MXene exhib-

ited a capacity of 123.6 mAhg−1 at a 1C rate, with a coulombic ef-
ficiency of 47%. Notably, the performance of Ti3C2Tx MXene

surpassed that of 2D Ti2C, demonstrating its superior capabilities

as an anode material [171]. When considering the orientation of
these 1D nanostructures in relation to MXenes, MXene/1D
hybrids can be categorized as vertically or horizontally loaded

models. These hybrid structures are anticipated to exhibit syner-

gistic effects, leveraging the structural benefits of both 2D
MXenes and 1D nanostructures, thereby enhancing the perfor-
mance of lithium-ion batteries (LIBs) [170]. In a study conducted

by Liu et al., a hybrid thin film composed of 2-D Ti3C2 and carbon

nanotubes (CNTs) was fabricated and employed as an anode ma-

terial for lithium-ion batteries. The research revealed that this

hybrid film exhibited a notable reversible capacity of

428.1 mAhg−1 at a 0.5 C rate, even after undergoing 300 cycles.

The presence of CNTs in the film contributed to its high conduc-

tivity, facilitating rapid charge transfer during the electrochemi-
cal reaction [172]. Mo2CTx, show great potential for energy

storage but suffer from slow kinetics and poor cycling stability

due to partial oxidation into MoOx, leading to structural degrada-

tion. To address this, Bayhan et al. developed a laser-induced

Mo2CTx/Mo2C (LS-Mo2CTx) hybrid anode. Mo2C nanodots en-

hance redox kinetics, while laser reduction minimizes oxidation-
related degradation. The hybrid's strong connections improve

conductivity and structural stability during cycling. This LS-

Mo2CTx anode demonstrated a significantly improved capacity

(340mAh g−1
) and excellent cycling stability (106.2% retention)

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over 1000 cycles [173]. A composite “paper” electrode comprising

of Nb2CTx and carbon nanotubes (CNT) was developed by
Mashtalir et al. and utilized as an anode material. This electrode
demonstrated a capacity exceeding 400 mAh g−1 at a rate of 0.5C
[174]. In a separate study by Liu et al., V2C MXene was synthe-
sized and employed as an anode material, exhibiting a specific

capacity of 250 mAh g−1 at a current density of 50 mA g−1 [72].

In addition to the chemical composition of MXenes, the ma-

nipulation of porous structures is crucial for enhancing ion diffu-
sion within electrodes. Various strategies have been proposed to

construct porous nanoarchitectures for MXene-based electrodes.

One notable approach involves vertically aligning MXene flakes
into thick films, with a thickness of 200 μm, which is double the
standard thickness for practical applications (100 μm).
Remarkably, even with this increased thickness, the electrodes

still achieved fast ion and electron transport, resulting in excel-

lent electrochemical performance [175, 176]. Another effective

technique involves introducing in-plane holes in the 2D MXene

nanosheets, which effectively reduces the ion transfer pathways.
For instance, mesoporous MXene flakes were obtained through a
chemical acid etching process applied to partially oxidized
MXene. The enhanced accessibility of the electrolyte to ions in
the mesoporous MXene led to a significant improvement in its

performance. These findings highlight the importance of pore en-

gineering in MXene-based lithium-ion battery (LIB) electrodes. E.

Ren et al. successfully created porous Ti3C2Tx MXene flakes that

possess a significant specific area and open structures. These

flakes can be transformed into films without relying on the sup-

port of carbon nanotubes (CNTs). The porous MXene exhibited

an impressive capacity of 1250 mAh g−1 at a 0.1C rate. Even when

subjected to a high cycling rate of 10C, the porous MXene still
maintained a capacity of 330mAh g−1
. [177].
Sodium-ion batteries (SIBs) are being explored as a promising
alternative to lithium-ion batteries (LIBs) for large-scale energy
storage, thanks to the similarity in the low potential of sodium

(−2.71 V versus SHE) to lithium (−3.04 V versus SHE) and the cost-
effectiveness of abundant sodium resources [178, 179]. The po-
tential windows of MXene anodes in SIBs mosrange from 0.5 to

1.3 V versus Na/Naþ [180]. When combined with a sodium-ion

cathode like Na3V2(PO4)3, which exhibits stable voltage plateaus
at around 3.3 V versus Na/Naþ, the resulting SIBs can achieve an
overall voltage range of 2–2.8 V [181]. However, the larger size of
sodium ions (1.06 Å) compared to lithium ions (0.76 Å) leads to
slower kinetics of sodium ion insertion/extraction and significant
volume expansion. In this context, the emergence of MXenes
with high electrical conductivity, wide interlayer spacing, and
low diffusion barriers for sodium ions presents new opportunities

for the design of high-performance electrodes specifically tai-

lored for SIBs [182]. In a study conducted by Wang et al.,

Na2Fe2(SO4)3 was employed as the positive electrode, while Ti2C

MXene served as the negative electrode in a Na-ion battery. The

battery operated at a high voltage of 2.4 V, demonstrating a spe-

cific capacity of 90 mAh g−1 at a current density of 1 Ag−1

, and a
capacity of 40 mAh g−1 at a higher current density of 5 Ag−1 [183].
Xie et al., developed a prototype Na-ion cell, utilizing a Ti3C2Tx/
CNTs electrode. The incorporation of CNTs served two purposes:
preventing the restacking of MXene nanosheets and creating a
well-defined porous structure to facilitate smooth transport of
the electrolyte. The presence of functional groups on the surface

of Ti3C2 MXene played a crucial role in enabling sodium-ion stor-

age, resulting in excellent electrode properties. The Na-ion bat-
tery constructed with a Ti3C2/CNTs anode demonstrated a

volumetric capacity of 421 mAhcm−3 at a current density of

20 mA g−1 [184]. In a study by Zhao et al., a PDDA-BP/Ti3C2 hetero-
structure was synthesized and employed as an electrode mate-
rial in Na-ion batteries as shown in Fig. 13b. The device exhibited

an impressive reversible capacity of 1112mAg−1

. This high ca-

pacity was maintained even after 500 cycles at a low current den-
sity of 0.1 Ag−1 [185]. Wu et al., designed a heterostructure based

on the Ti3C2Tx electrode. This heterostructure, known as f-

Ti3C2TxDMSO electrode, exhibited a favorable capacity of 196

mAhg−1 at a current density of 100mAg−1 after undergoing 500

cycles [186]. Zhao and colleagues conducted a study where they
transformed 2D MXene flakes into hollow spheres and a 3D
structure using a template method. These structures were
intended for application in sodium-ion batteries. In the original

2D form, the MXene flakes tended to stack together, thereby lim-

iting their electrochemical performance. However, the research-
ers found that the 3D microporous MXene architecture offered a

more favorable alternative. When tested in sodium-ion batteries,

the MXene materials, specifically Mo2CTx, Ti3C2Tx, and V2CTx,
demonstrated a reversible capacity of 370, 330, and 340mAhg−1
,

respectively, at a rate of 0.25C [187]. Guo et al. used a facile-

solution method to fabricate Sb2O3/Ti3C2Tx composite for use in

Na-ion batteries which shows a high performance of 295 mAhg−1

at 2 Ag−1 [188]. Ahmed et al. developed a SnO2/MXene hetero-

structure for utilization as an anode material in lithium-ion bat-
teries. To create this structure, SnO2 was deposited within the

MXene layer through the use of Atomic Layer Deposition (ALD)as

shown in Fig. 13c. To enhance its performance, a thin layer of
HfO2 was deposited onto the surface. The fabricated device
exhibited a favorable specific capacity of 843 mAhg−1
, indicating
promising energy storage capabilities [189]. Layered transition
metal dichalcogenides hold promise as anodes for sodium-ion
batteries (SIBs) but suffer from restacking, which limits capacity
and stability. Zhao et al. designed a 2D VS2/Ti3C2Tx MXene hybrid,
fabricated using a simple liquid-mixing method. The hybrid uses
fast, reversible sodium intercalation in VS2, while the Ti3C2Tx
matrix enhances charge transfer and reduces volume expansion.
This design delivers outstanding performance, including high
specific capacity (522mAh g−1

), long cycle life (116% retention af-

ter 3000 cycles), and reliable performance across extreme tem-
peratures (−40�C to 70�C) [190]. Other than Lithium and sodium

batteries, aluminum-ion batteries (RAIBs) offer advantages like

cost-effectiveness, safety, and high energy density, but face chal-

lenges such as low capacity and poor cycling stability. However,

Yuan et al. investigated AlCl4− ion intercalation in transition

metal cathodes to enhance their energy storage potential and
Coulombic efficiency. It was found that the lattice distortion in
CoSe2, caused by AlCl4− ions, affects battery stability. MXene as

a support material reduces CoSe2 size, minimizing lattice distor-

tion and improving reversibility and cycle stability [191].

Lithium-sulfur (Li-S) batteries have gained considerable popu-

larity alongside lithium-ion (Li-ion) and sodium-ion (Na-ion) bat-
teries in recent years. In the field of Li-S batteries, MXenes have

made significant contributions. One of the primary challenges

faced by modern Li-S batteries is the formation of lithium poly-

sulfides (LiPSs) in the electrolyte. These soluble polysulfides can

lead to reduced sulfur utilization and lower coulombic efficiency

of the battery cell. MXenes, due to their abundant surface chem-
istry, exhibit a strong chemical interaction with lithium polysul-
fides, effectively inhibiting their diffusion. This characteristic of

MXenes helps extend the lifetime of the Li-S battery cell by miti-
gating the negative effects of LiPSs. Liang and colleagues were

the first to utilize Ti2C MXene nanosheets as cathode material in

Li-S batteries. The hydroxyl terminated groups present on the
Synthesis, properties, and applications of Mxenes | 15

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surface of Ti2C undergo a redox reaction with lithium polysul-

fides (LiPSs), resulting in the formation of thiosulfate as depicted

in Fig. 13a. This reaction is followed by a metal-sulfur reaction,

which exposes the Ti atoms capable of bonding with additional
LiPSs through Ti-S Lewis-acid-base interactions. The composite

containing 70% sulfur by weight (S/Ti2C) exhibited impressive cy-

clic performance, reaching a capacity of 1200 mAh/g at a C/5 cur-
rent rate. Moreover, it maintained 80% of its capacity over 400

cycles when tested at a C/2 current rate [192]. Zhao and col-
leagues employed exfoliated Ti3C2 MXene as a host for sulfur in

their study. This MXene exhibited an initial discharge capacity of

1290 mAh g−1

, and after 100 cycles, it retained a capacity of

970mAh g−1 [193]. Li et al. fabricated MOF-derived CoSe2 nano-

particles in N-doped carbon-layered MXene hollow spheres to

create MXene@CoSe2/NC heterostructures. Density functional

theory (DFT) calculations showed that this composite enhances
polysulfide affinity and lowers the energy barrier for Li2S decom-
position. The resulting electrodes delivered excellent perfor-
mance, with a large areal capacity and stability over 200 cycles

[194]. To further enhance the performance of Li-S batteries,

Carbon Nanotubes (CNTs) were integrated with MXene, forming
an interwoven structure of MXene nanosheets and CNTs. The

MXenes used in this study were Ti2C, Ti3C2, and Ti3CN. The inclu-
sion of CNTs served two purposes: anchoring polysulfides to the

MXene surface and facilitating electron transport between the

nanosheets. At a sulfur loading of 1.5 mg cm−2

, the initial dis-

charge capacity was measured at 1240 mAh g−1

, which decreased
to 450mAh g−1 after 1200 cycles. However, at a higher sulfur
loading of 5.5 mg cm−2

, a stable capacity of 910 mAh g−1 was

achieved [195]. The combination of mesoporous carbon and
MXene in a heterostructure plays a beneficial role in sulfur

loading and effectively mitigates the volumetric expansion of sul-

fur electrodes. In the case of Ti3C2@Meso-C/S cathodes with a

sulfur content of 73% by weight, they demonstrated an initial ca-

pacity of 1225 mAh g−1

. After 300 cycles at a C/2 cycle rate, the re-

versible capacity remained at 705mAh g−1 [196]. Lithium–sulfur

(Li–S) batteries face challenges such as the shuttle effect, slow

sulfur conversion, and lithium-dendrite growth, limiting their
practical use. Li Chen et al. developed a novel multiscale V2C
MXene (VC) with a spherical confinement structure. VC acts as a
bifunctional promoter, enhancing lithium polysulfide scavenging
and improving Li2S nucleation/decomposition kinetics [197].
Liang et al. designed a novel high-entropy MXene doped graphene

composite (HE-MXene/G@PP) as a bifunctional mediator for sepa-

rator modification in Li-S batteries. This composite enhanced

electrical conductivity, accelerates lithium polysulfide (LiPS) re-

dox conversion, and ensures uniform lithium deposition. The

battery demonstrated exceptional long-term cycling stability,

maintaining performance over 1200 cycles and 6000h [198].
Another study by Bao et al. focused on the synthesis of a Ti3C2Tx/
rGO/S hybrid structure, where Ti3C2Tx/rGO/S nanosheets were

utilized as the cathode host material for Li-S batteries. This hy-
brid structure exhibited a high initial capacity of 1144.2 mAh g−1

at 0.5 C. After 300 cycles, the capacity was measured at

878.4 mAh g−1 [199]. The inclusion of a conductive layer between

the cathode and separator in Li-S batteries enables improved uti-

lization of sulfur. This conductive layer serves multiple purposes

by preventing the formation of lithium polysulfide and acting as

a secondary current collector. Lin et al. conducted a study where
they synthesized a composite material consisting of Ti3C2
nanosheet-covered glass fibers, while commercially available
bulk sulfur was used as the cathode material. The Li-S battery
Figure 13. Schematic of MXene for use in Lithium-Sulfur batteries (a) Ti2C acts as a host for
sulfur deposition in Li-S batteries. LiPSs bond with Ti2C

MXene via a Ti-S Lewis acid-base interaction thus preventing the formation of LiPSs.
Reproduced with permission from ref [192] Copyright 2015, Wiley-
VCH. (b) The Fig. shows the charge transfer mechanism of Na-ion battery electrode made using
PDDA-BP/Ti3C2 heterostructure. Reproduced with

permission from ref [185] Copyright 2019, Elsevier. (c) Shows the different fabrication
techniques involved in the deposition of SnO2 on Ti3C2 MXene to
form a heterostructure which is used as an electrode for Li-ion batteries. Reproduced with
permission from ref [189] Copyright 2017, Elsevier.
16 | Borah et al.
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January 2026

incorporating this composite demonstrated an initial discharge

capacity of 820 mAh g−1

. After 100 cycles, the discharge capacity

was measured at 721 mAh g−1

, indicating good cycling stability

[200]. In the work conducted by Song et al., Ti3C2Tx nanosheets

were synthesized and applied as a coating on a “Celgard” mem-

brane. The resulting film had a thickness of 520 nm, and the

loading mass of Ti3C2Tx was 0.1 mg cm−3

. The performance of the

device using this configuration exhibited a high initial capacity of
1050 mAh g−1 at a rate of 0.2C and a capacity of 745mAh g−1 at a
rate of 1 C [201]. MXenes have demonstrated utility in preventing

the formation of lithium dendrites on the negative lithium elec-

trode surface. These dendrites can lead to short circuits and ac-
celerate reactions between the electrolyte and lithium

polysulfide (LiPS) species. Li et al. developed a flexible anode com-

posed of a lamellar structured Ti3C2 MXene-lithium film. This de-
sign effectively controls the nucleation and growth of lithium

dendrites. When coupled with a sulfur/carbon cathode, the Li-S

cell exhibited a reversible capacity of 950 mAh g−1 and retained a
capacity of 840 mAh g−1 after 100 cycles, indicating promising
stability and performance [202].
MXene in optoelectronics
MXenes have demonstrated promising optoelectronic properties,
making them valuable in the field of solar cells. Their tunable
bandgaps and good conductivity make them attractive for vari-
ous applications. MXenes have been utilized as electrodes and as

electron/hole transport layers in perovskite solar cells and quan-

tum dot sensitized solar cells. In a study by Miyasaka and col-
leagues, UV-ozone treated Ti3C2Tx MXenes were employed as

electron transport layers in perovskite solar cells as depicted in

Fig. 14a. The presence of Ti3C2Tx nanosheets facilitated electron

transport by modifying the band diagram. Remarkably, the

power conversion efficiency (PCE) of the solar cells increased
from 5% to 17% after 30 min of UV treatment, highlighting the
significant impact of MXenes on device performance as shown in
[203]. Fu et al. explored the utilization of MXene as an electrode in

silicon solar cells. They fabricated a heterostructure by drop-

casting delaminated Ti3C2Tx onto the nþ-Si surface. This

approach resulted in a significant improvement in power conver-

sion efficiency (PCE), reaching 11.5% [204]. Chen and co-workers,

a CuSe/Ti3C2 heterostructure was screen-printed onto a graphite

sheet. This heterostructure served as a counter-electrode in

quantum dot-sensitized solar cells. The device exhibited an effi-

ciency of 5.1% [205]. Karimipour et al. studied the stability of pe-
rovskite solar cells (PSCs) with functionalized 2D titanium

carbide (Ti3C2) MXene at the interface between the halide perov-

skite and the hole transport layer. The MXene was functionalized

using an organic additive, enhancing the link between the layers.

MXene-based PSCs showed improved efficiency (�22%) com-

pared to control devices (20.56%). Stability tests, including real

outdoor conditions (ISOS-O), showed that MXene-modified devi-

ces retain nearly 100% efficiency under continuous light and last
over 600 h, while control devices degraded completely. This is the
first stability assessment of MXene-based PSCs under outdoor

conditions [206]. Nirmal et al. reported the development of a flexi-

ble, transparent, and conductive electrode based on a MXene/Ag/

MXene hybrid structure for inverted organic solar cells (OSCs)

with memory and learning capabilities. The optimized FTCE
exhibits 84% transmittance, low resistance (9.7 Ω sq−1

), and dura-
bility after 2000 bending cycles. The OSC using this electrode

achieves a power conversion efficiency of 13.86% and reliable

performance over hundreds of cycles. The memristive OSC

Figure 14. Schematic of the use of MXene in optoelectronics. (a) Shows the structure
ITO/ETL/CH3NH3PbI3/Spiro-OMeTAD/Ag combined with Ti3C2Tx
MXene used in perovskite solar cells. Ti3C2Tx MXene is used here as an electron transport layer
(ETL). Reproduced with permission from ref [203]
Copyright 2019, Wiley-VCH. (b) Single element photodetector device made from a hydroxyl
functionalized semiconducting ScCxOH fabricated via a
laser photolithographic technique. A Ti layer with an Au protection cap is used as an electrode
on a Si/SiO2 substrate. Reproduced with permission
from ref [86]. Copyright 2019 American Chemical Society. (c) Ti2CTx MXene used as electrode
in an InSe-based photodetector. EBL patterning and
Plasma etching is performed on a vertically stacked InSe/Ti2CTx Field-effect Transistor (FET)
to obtain the InSe/Ti2CTx photodetector. Reproduced with
permission from ref [213]. Copyright 2019, American Chemical Society.

Synthesis, properties, and applications of Mxenes | 17

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shows excellent switching behavior, endurance, and memory re-

tention, mimicking biological synapses [207]. Deng et al. studied a

novel poly(3,4-ethylenedioxythiophene): poly(styrenesulfonate)

(PEDOT: PSS) hybrid hole transport layer (HTL) to improve or-
ganic solar cell (OSC) performance. By optimizing the Nb2C

MXene doping ratio, a record power conversion efficiency (PCE)

of 19.33% was achieved in single-junction OSCs with the ternary
active layer. Nb2C MXene enhances the phase separation of
PEDOT and PSS, boosting conductivity, hole mobility, and charge
extraction, while reducing recombination [208]. Kai et al. explores
the use of tetrabutylammonium bromide-functionalized Ti3C2Tx

(TBAB-Ti3C2Tx) as a cathode buffer layer (CBL) to enhance perov-

skite solar cells (PVSCs). The TBAB-Ti3C2Tx improves charge

transfer, reduces work function, and optimizes energy level

alignment for efficient charge extraction. It also prevents iodine
ion migration, reducing defect states and charge recombination.
The resulting device, based on MAPbI3 perovskite, achieves
a high power conversion efficiency of 21.65% with enhanced
stability [209].
MXenes possess excellent electrical and optical properties,

making them promising candidates for photodetector applica-

tions. Although the utilization of MXenes in this area is still rela-
tively limited, there is significant potential for further growth.

Zhou and colleagues developed a photodetector using 2D

ScCzOH MXene shown in Fig. 14b, which exhibited a direct band

gap of 2.5 eV [86]. Velusamy et al. fabricated nanosheets of vari-

ous MXenes, including Mo2CTx, Ti3C2Tx, Nb2CTx, Ti2CTx, and

V2CTx, derived from different MAX phases. Photodetectors were

then fabricated on paper substrates using these MXenes. Among

the different MXenes, the Mo2CTx-based photodetector demon-

strated the best photoelectric performance. The Mo2CTx devices

exhibited relative stability under ambient conditions and me-

chanical stresses, making them suitable for durable photodetec-
tion in the visible range. The photodetector achieved a
photosensitivity of 9 mAW−1

, a light-dark current switching ratio

of 250, and a detectivity of 5x1011 [159]. Kang et al. developed a

photodetector that utilizes a vertical van der Waals heterostruc-

ture composed of Ti3CTx and n-Si. This design takes advantage of

Ti3CTx's adjustable work function, allowing for the formation of

a favorable Schottky junction with Si through van der Waals

forces. The vertical heterostructure facilitates the efficient sepa-

ration and transmission of photonic-induced carriers. The photo-
detector exhibited a high switching ratio of 105 and a significant

photosensitivity of 26.95 mAW−1 [210]. In a subsequent study,

Kang and colleagues developed a vertical heterojunction photo-

detector consisting of Mo2C-graphene (Gr)/Sb2S0.42Se2.58/TiO2/

fluorine-doped tin oxide (FTO) layers. Sb2S0.42Se2.58 was used as a

light-absorbing material, suitable for photovoltaic devices. The
device demonstrated simultaneous light response on both the
FTO side and the Mo2C-Gr side. At a wavelength of 650 nm and a
light density of 2.5 mWcm−2

, the device exhibited a switching ra-

tio of 70 and a photoresponsivity of 35.91 mAW−1 at zero bias

voltage [100]. Li and colleagues developed a Ti3C2/Cu2O hetero-

junction photochemical photodetector using a sample heating

process. This photodetector was specifically designed for glucose

concentration detection. Under visible light irradiation for
400 seconds, the photocurrent remained stable and reproducible
in a glucose solution with a concentration of 1 μM, demonstrating
good stability [211]. In a study by Deng et al. in 2019, a fully
sprayed, large-area flexible photodetector was synthesized using
CsPbBr3/Mxene, with Ti3C2Tx utilized as an electrode. The device
demonstrated a high light-dark current switching ratio of ap-
proximately 2.3 × 103 [212]. Yang et al. employed Ti2CTx to

fabricate an InSe-based photodetector shown in Fig. 14c. The de-

vice exhibited a low dark current of 5 nA, a fast photoresponse

time of 0.8 ms, and a high photoresponsivity of 1.1x104 A/W

[213]. Montazeri et al. fabricated a metal-semiconductor-metal

semiconductor (MSM) photodetector where they deposited trans-

parent Ti3C2Tx-based metal contacts on GaAs substrate. When

they compared the MXene-GaAs-MXene(MX-S-MX) photodetec-

tor with that of the Ti/Au-GaAs-Ti/Au(MSM) photodetector, they

found that MX-S-MX photodetectors were better than MSM pho-

todetector in terms of photoresponsivity, EE, and specific detec-
tivity [214]. Gurbuz et al. focuses on improving Schottky-type

photodiodes by addressing the restacking issues of 2D materials

like MXenes, which limits their efficiency. The team synthesized
3D V2C MXene nanoflowers using ultrasonic treatment and
freeze-drying to solve this problem. These 3D nanoflowers were
applied as interlayers on p-type and n-type Si wafers. The V2C
MXenes/p-Si device showed an excellent rectification ratio [215].

Thota et al. demonstrates the use of 2D MXene nanosheets spin-

coated onto 1D GaN nanorods to form a van der Waals Schottky

junction for efficient UV detection (λ 1⁄4 382 nm) without an exter-

nal power supply. The built-in electric field in the junction

enhances electron-hole pair separation, improving the UV detec-

tion performance compared to pristine GaN nanorods. The self-
powered MXene/GaN device exhibited high photoresponsivity

(48.6 mAW−1

), detectivity (5.9 × 1012 Jones), and quantum effi-

ciency (543%) [216]. Di et al. introduces Ti3C2Tx MXene film as an

efficient transparent conducting electrode for lead sulfide (PbS)

colloidal quantum dots photodiodes with controllable near-

infrared transmittance. By using solution-processed interface en-
gineering, the defects between the MXene and PbS layers are

minimized, improving carrier concentration. The resulting

Ti3C2Tx/PbS CQDs photodiodes exhibit high detectivity
(5.51 × 1012 cm W−1 Hz1/2), a wide dynamic response range

(140 dB), and large bandwidth (0.76 MHz) at 940 nm in a self-

powered state [217]. Zheng et al. presents a hybrid MXene/ZnO

nanorods Schottky junction UV photodetector with significantly

enhanced performance compared to pure ZnO nanorods photo-

detectors. By spin-coating 2D Ti3C2-MXene onto a 1D ZnO nano-
rod array, the device achieves higher optical absorption in the UV

range. At 368 nm and 5 V bias, the MXene/ZnO PD exhibits an on/

off ratio of 806, responsivity of 142.2 mA W−1

, and specific detec-

tivity of 2.03 × 1010 jones [218].

In recent times, MXenes have also found applications in light-

emitting diodes (LEDs). Ahn et al. utilized Ti3C2 as an electrode in

an organic light-emitting diode (OLED), achieving a current effi-

ciency of 102 cd A−1 and a quantum efficiency of 28.5% ph/el

[219]. Lu et al. tested an LED device using polyethyleneimine (PEI)

modified ZnO as the active layer and Ti3C2Tx as the electron
transport layer (ETL). This LED exhibited a luminance of 3260
cdm−2 and a quantum efficiency of approximately 17% [220].
MXene in environmental remediation

MXenes are increasingly employed in water purification applica-

tions due to their desirable properties, including high water flow

rates, stability, and resistance to fouling. Their layered structure

provides hydrophilicity, flexibility, and a large surface area, mak-

ing them excellent materials for water treatment. Researchers

have used Ti3C2Tx MXenes in various forms for ion and molecule
rejection, such as freestanding or supported membranes with

thickness ranging from nanometers to micrometers. These mem-

branes exhibit flexibility, mechanical strength, and electrical

conductivity. For instance, MXene membranes have demon-

strated exceptionally fast water flow rates of 37.4 l/(Bar.h.m2

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[221]. Shahzad et al. synthesized 2D Ti3C2Tx MXene nanosheets to

extract copper from water. They observed that delaminated (DL)-
Ti3C2Tx exhibited remarkable copper removal capabilities due to
its substantial surface area and hydrophilic nature. The presence

of oxygenated groups within the MXene layers reduced the for-

mation of Cu2O and CuO. The adsorption capacity is found to be

at 78.45mg g−1 [222]. Wu et al. designed Ti3C2Tx with -OH func-

tional groups as nanofillers for creating two polymer blends: hy-
drophilic polyethyleneimine (PEI) and polydimethylsiloxane

(PDMS) to fabricate solvent-resistant nanofillers (SNRF)

composite membranes. These horizontally oriented Ti3C2Tx
nanosheets, utilizing -OH groups as adsorption sites, facilitated
the transport of alcohol molecules [223]. Li et al. introduces a
novel MXene-based nanofiltration (NF) membrane enhanced
with Ag nanoparticles (AgNPs) and crosslinked with hyper-
branched polyethyleneimine (HPEI) for improved water perme-
ability and stability. The HPEI-AgNP@Ti3C2Tx MXene membrane

demonstrated excellent water permeability (24.64–30.73

Lm − 2h−1bar − 1

) and near 100% rejection of dyes like Congo red,

methyl orange, and Rhodamine B during long-term use. It also
showed high rejection rates for salts such as MgSO4 (84.15%) and

NaCl (56.58%) [224]. Zhang et al. fabricated a sodium lignosulfo-

nate carbon nanotube/alkalized MXene (SLS-CNT/alk-MXene)

composite membrane, designed for efficient wastewater treat-

ment. The membrane, fabricated using a polyethersulfone sub-
strate and a layer-by-layer self-assembly technique,

demonstrated over 99% retention of Methyl Blue and Congo Red

dyes and a permeation flux of 51.6 Lm−2 h−1bar−1

. It also effec-
tively degraded organic dyes like Methyl Orange and Rhodamine

B within 1 h. The membrane exhibited low resistance (813 Ω), ex-

cellent stability, and 80% recovery [225]. Li et al. introduces

ZnO@Ti3C2Tx MXene nanofiltration (NF) membranes, incorporat-

ing ZnO nanoflowers with Ti3C2Tx MXene for water purification.

The membrane exhibited photocatalytic self-cleaning properties

under visible light, achieving 95.44% Congo red rejection and an
excellent water permeability of 138.81 Lm−1 2h−1bar − 1
. Compared
to Ti3C2Tx MXene or ZnO alone, the ZnO@Ti3C2Tx membrane
demonstrated superior photodegradation of 10 ppm methylene
blue and maintained high separation performance over six cycles
with > 88.48% RhB rejection [226]. Chen et al. developed a 2D-2D
BiOCl/Ti3C2Tx MXene (BM) heterostructures, developed via elec-
trostatic self-assembly, that can photodegrade the antibiotic cip-
rofloxacin by 90% within 30 min under solar irradiation. The

combination of BiOCl and MXene enhances light absorption and

accelerates electron-hole separation, improving photocatalytic
efficiency. Reactive oxygen species, primarily hþ and O2−, play a
key role in the degradation process. These BM nanohybrids offer

a promising and eco-friendly approach for the removal of emerg-

ing contaminants from water, showcasing potential for environ-
mental applications in green water purification [227]. Zhang et al.

studied on enhancing the photocatalytic degradation efficiency

of TiO2, particularly under visible light, for dye wastewater treat-

ment. By synthesizing TiO2/MXene composites via a low-
temperature hydrothermal reaction, the researchers achieved

significant improvements in methylene blue (MB) dye removal.

The optimal TiO2 to MXene mass ratio (4 : 1) boosted MB degrada-

tion to 96.44% under UV light and 40.19% under visible light

which is 8.26 times higher than pure TiO2 [228]. Liu et al. synthe-
sizerd a ternary Ag@ZnO@Ti3C2 MXene heterojunction using hy-
drothermal and chemical deposition methods, enhancing the

photocatalytic performance of MXene. By integrating ZnO and Ag

nanoparticles, the heterojunction improves visible light

absorption and charge separation. The optimized photocatalyst

achieved high degradation rates for methylene blue (90.54%) and
levofloxacin (86.76%) under visible light, with strong stability
over five cycles. The primary active species driving degradation

were identified as hydroxyl radicals (-OH) and superoxide radi-

cals (O2-) [229]. Liu et al. fabricated ultrathin Ti3C2Tx MXene

membrane via facile filtration method and was tested for perva-
poration desalination. They showed excellent results in salt re-
jection having high hydrophilicity and 2D interlayer transport

channels. The membrane shows a water flux of 85.4 Lm2

h−1 with
a salt rejection of 99.5% (approx.) for 3.5 wt% NaCl solution at a
temperature of 65�C [230]. Berdiyorov et al. conducted the first
principle density functional theory to determine the possibility of
a charge selective ion transport through the Ti3C2(OH)2 MXene
[231]. Lin et al. designed a composite of plant derived polyphenol

tannic acid (TA) and 3-aminopropyltriethoxysilane (APTES) nano-

particles with MXene. The TA-APTES@MXene membrane as

depicted in Fig. 15a was used for oil/water separation and it was
found that the water flux is approx. 5990 l.m−2 h−1 at 0.1 MPa,
thus showing its hydrophilic behaviour [232].
Rasool et al. tested the antibacterial properties of Ti3C2Tx

MXene for antibacterial properties. Ti3C2Tx membranes were pre-

pared by filtration on a polyvinylidene (PVDF) support. These

were tested against Escherichia coli (E. coli) and Bacillus subtilis

(B. subtilis) by the growth of bacteria on the surface of the mem-

brane shown in Fig. 15b. Also, these membranes were exposed to

bacterial suspensions. The antibacterial fresh rate, when com-

pared to that of control PVDF [233], reaches more than 73%

against B. subtilis and 67% against E. coli. As the age of the mem-
brane progresses it shows bacterial growth inhibition of 99%

[233]. Several ions such as Liþ, Kþ, NHþ

4 , Mg2þ can be intercalated

in between MXene sheets and thus MXene nanosheets can be
used as adsorbents. Peng et al. designed a 2D alk-MXene
Ti3C2(OH/ONa)xF2-x which exhibited selective sorption of Pb2þ in
presence of other competing ions like Ca2þ and Mg2þ [234]. Ying
et al. similarly designed 2D Ti3C2Tx MXene for the removal of
toxic Cr (VI) from water. This is done by reducing Cr(VI) to Cr(III)
and then absorbing Cr(III) simultaneously [53]. MXenes have
strong absorption in both visible and UV wavelength and they
have remarkable anisotropic carrier mobility. Even though

MXene show narrow band-gap, by tuning their surface termina-

tion groups, they can be used for photocatalysis applications.

Mashtalir et al. tried to use ML Ti3C2Tx MXene as a photocatalyst

for the degradation of MB and acid blue. Degradation of ML was
upto 81% within 5h under the exposure of UV light. On the other
hand, 18% degradation occurred in the dark. The formation of

TiO2 on the MXene surface further contributed to the photocata-

lytic activity under UV light [235]. Gao et al. designed TiO2/Ti3C2

nanocomposites via hydrothermal process. The photocatalytic

activity was monitored by photodegradation of methyl orange
(MO) and it was found that the photocatalytic activity is much
better than pure TiO2 nanomaterials under UV light [236]. Chao
et al. fabricated a composite of (001) facets of TiO2 nanosheets

and layered Ti3C2. (001) facets of TiO2 are highly active and there-
fore can afford high-efficiency photogeneration of electron-hole

pairs and the carrier separation is promoted by hole trapping ef-

fect by interfacial Scottky Junction with Ti3C2. Ti3C2 acts as a res-
ervoir for holes. Interface formation originates because of the

overlapping of Ti d orbital and O p orbital as shown in Fig. 15c.

The photocatalytic activity of the composite towards the degra-

dation of methyl orange die was monitored under UV and it is

Synthesis, properties, and applications of Mxenes | 19

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found that the degradation 2.3-fold higher than particulate TiO2/
Ti3C2 [237].
MXene in biomedical applications
2D nanomaterials are used in biomedical applications for their
extreme thinness, and high surface-to-volume ratio. MXenes
have all these properties in addition to properties such as rich
surface chemistry, solubility in aqueous solutions which makes
them a potential candidate for its use in biomedicine. MXenes

provide abundant reactive sites for enzyme and drug functionali-

zation due to their rich surface chemistry while its hydrophilic

nature avoids the need for potentially toxic organic solvents.

Mediator-free biosensors operate by the electron transfer be-

tween immobilized electroactive enzymes and the electrode sur-
face. The enzymes perform redox reaction with the analyte of

interest. However, the electroactive centres of these enzymes are

situated deep inside the protein structure, and so the enzymes

often denature when immobilized on electrode. Wang et al. pre-

pared an organ-like Ti3C2 structure to fabricate a mediator-free

biosensor which exhibited excellent Haemoglobin (Hb) immobili-

zation, with good biocompatibility for redox reaction, displaying

good protein bioactivity and stability The biosensor displayed

good performance with a linear range of 0.1–260 μM for H2O2
[238]. Tong et al. presents the development of a highly sensitive

and stable enzyme electrochemical biosensor using a nanocom-

posite (PGOx@MXene/CS), created by assembling GOx polynano-
gel (PGOx) onto MXene nanosheets. The large surface area of

MXene enabled efficient enzyme loading, while also catalyzing

the decomposition of toxic H2O2, enhancing enzyme stability.
The glucose sensor exhibited a linear detection range of

0.03–16.5 mM, sensitivity of 48.98 μA mM−1

cm−2
, and a detection
limit of 3.1 μM. Even after 200 cycles, the sensor retained 85.83%
of its initial performance, making it ideal for continuous blood
glucose monitoring [239]. Rakhi et al. reported the fabrication of a
glucose biosensor by the immobilization of glucose oxidaze (GOx)
on Au/Ti3C2 composite. The biosensor displayed response in the

glucose concentration range from 0.1 to 18 mM with a high sensi-

tivity of 4.2 μAmM−1

cm−2

. The sensor also showed excellent sta-

bility, reproducibility and repeatability. It retains over 93% of its

initial response after 2 months of storage [240]. Xu et al. reported

a Ti3C2 based Field-effect Transistor (FET) device produced using
the microcontact printing technique as shown in Fig. 16c used to

measure dopamine concentration and record the electrical activ-

ity of neurons cultured on FET. The interactions between the do-
pamine molecules and free electrons in the surface groups of

MXenes increases the number of electron holes which results in

the increased conductance of FET. The detection limits are as
low as 100 nM and it shows high linear conductance modulation
for concentration in the range from 100 nM to 50 μm [241]. M
Bolourinez had developed a rapid, accurate, and cost-effective
electrochemical biosensor for detecting SARS-CoV-2. Using

MXene nanosheets (Ti3C2Tx) and carbon platinum (Pt/C) to am-

plify the signal, the biosensor targets the RdRp gene region of the

virus. Differential pulse voltammetry (DPV) detected concentra-

tions ranging from 1 aM to 100 nM, with a detection limit of 0.4

aM. Clinical tests showed 100% accuracy and sensitivity, 97.87%

specificity, and a limit of quantification (LOQ) of 60 copies/mL.
This biosensor was effective in detecting COVID-19 from saliva,
swabs, and serum, proving its potential for rapid diagnostics
[242]. Cancer is one of the leading causes of death worldwide in
Figure 15. Schematic of the use of MXene in environmental remediation. (a) TA-APTES
nanoparticles and MXene composite were used for the
separation of oil/water separation. Reproduced with permission from ref [232] Copyright 2022
Elsevier. (b) Multi-layered ML-Ti3C2Tx and delaminated
Ti3C2Tx nanosheets were used for the growth inhibition of [Link]. Reproduced with
permission from ref [233] Copyright 2016, American Chemical
Society. (c) DFT optimized Ti3C2/TiO2 heterostructure used for photocatalytic application. The
Ti-O-Ti bonds are labeled as Ti1-O1-Ti2 and Ti3-O2-Ti4
respectively. C, O, Ti, and H elements are represented by black, red, cyan, and green balls
respectively. Reproduced with permission from ref [237]
Copyright 2016, American Chemical Society.
20 | Borah et al.

Downloaded from [Link] by guest on 16

January 2026

recent years. Photothermal therapy (PTT) with near infrared radi-

ation is promising alternative to traditional methods such as che-
motherapy and radiotherapy as it has high site specificity and

does minimal damage to normal tissue. Lin et al. first mentioned

the use of Ti3C2 MXene in PTT. Ti3C2 nanosheets were prepared
by prolonged exfoliation of the MAX phase in 40% wt. HF for

3 days followed by intercalation with tetrapropylammonium hy-

droxide (TPAOH). When Ti3C2 nanosheets were dispersed in

aqueous solutions at 38�C and a laser irradiation of 808 nm at

low power density (1.0W cm−2

) was allowed to fall in the solution

for 5 min on-off cycles, it is seen that the temperature is in-

creased by more than 20�C even at low concentration. The Ti3C2

MXene is functionalized with soybean polysulfide (SP) to improve

the colloidal stability while retaining its photothermal property.
4T1 tumor-bearing mouse were injected with Ti3C2-SP
Nanosheets with NIR laser irradiation at 808 nm focused on the
tumor site for 10 min. The temperature rose from 30�C to 58�C
resulting in complete ablation of cancer cells [243]. Dai et al.
reported a combined Magnetic Resonance Imaging (MRI),

Photoacoustic Imaging (PI) and PTT theragnostic platform by fab-

ricating MnOx nanosheets on Ti3C2 nanosheets via in situ redox

reaction from a KMnO4 precursor. It is then followed by Soybean

Polysulfide (SP) functionalization. Ti3C2 in the composite offers
high photothermal conversion efficiency while MnOx realizes the

unique tumor microenvironment-responsive T1-weighted MR im-

aging of tumors [244]. The same group reported the use of Ta4C3/

MnOx MXene in diagnostic imaging and photothermal therapy

[245] and later on a Ta4C3 MXene functionalized with supermag-

netic iron-oxide nanoparticles (IONP) was used for the same pur-
pose. IONP act as excellent contrast agents for T2-weighted MRI

[246]. Zhu et al. used metal carbonitride Ti3C1.15N0.85F0.88(OH)0.56

for photothermal Therapy shown in Fig. 16b which showed a
strong NIR absorption of 36.6 Lg−1 cm−1 at 808 nm and 43.5
Lg−1 cm−1 at 1064nm [247].
Han et al. reported the use of MXenes in drug delivery systems.
Ti3C2 possess high drug-loading capacity as high as 211.8%. The
Ti3C2 MXenes functionalized with Soybean Polysulfide (SP) can
electrostatically absorb molecules such as doxorubicin (Dox).
Dox is a chemotherapeutic drug used to treat cancer. After the

Ti3C2-SP-Dox nanosheets reaches the cell, the drug can be trig-

gered endogenously through the interference of the Hþ ions with

the electrostatic interaction between Dox and Ti3C2-SP as

depicted in Fig. 16a. It can also be triggered exogenously via NIR
irradiation [248]. Y chen et al. developed a novel MXene/Ag NPs
film for surface-enhanced Raman scattering (SERS)-traceable
drug delivery. The film, prepared via a two-step self-assembly
process, demonstrated high SERS sensitivity with a detection
limit of 10−8 M using 4-mercaptobenzoic acid (4-MBA) as a probe.
It exhibited excellent uniformity, stability, and repeatability. The

film was used as a nanocarrier to load the anticancer drug doxo-

rubicin (DOX), with SERS tracking. Glutathione (GSH) triggered 4-

MBA release, facilitating efficient DOX delivery [249]. J Hi et al.

designed a MXene/Gellan gum (MXene@GG) hydrogel with en-

hanced photothermal conversion efficiency and stability for

near-infrared (NIR) light-responsive drug delivery in cancer treat-

ment. By physically mixing MXene nanosheets, FeCl2, and Gellan

gum, the hydrogel demonstrates superior photothermal proper-

ties compared to MXene solutions, enabling precise control of

drug release. Cell experiments confirm good biocompatibility

and maintained anticancer activity of doxorubicin (DOX) after
Figure 16. Schematic of the use of MXenes in the different areas of biomedicine. (a)Ti3C2 is
surface modified by SP which further helps in drug loading
and is then released by inner or external irradiation. Reproduced with permission from [248]
Copyright 2018, Wiley-VCH. (b) Metallic Carbonitride
MXene is injected into tumor-bearing mice. In presence of NIR irradiation, the temperature
increases resulting in the ablation of cancer cells.
Reproduced with permission from ref [247] Copyright 2022 Wiley-VCH. (c) Ti3C2-based FET
device used as a biosensor for the detection of dopamine.
Reproduced with permission from ref [241] Copyright 2016 Wiley-VCH.

Synthesis, properties, and applications of Mxenes | 21

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NIR-triggered release. The MXene@GG hydrogel offers a promis-

ing approach for intelligent, localized cancer treatment through

controlled, NIR-responsive drug delivery [250]. M Wu et al. syn-

thesized an ultrathin Ti3C2Tx MXene nanosheets which demon-
strated excellent photothermal conversion efficiency (47.1%)
under 808 nm infrared laser irradiation and a high drug loading
efficiency (72.8%) with doxorubicin (DOX). A multifunctional
nanomedicine platform (Ti3C2Tx-DOX-PMAsh-Tf) was developed
by modifying the nanosheets with polymethacrylic acid and
transferrin for targeted cancer therapy. The platform exhibited

biocompatibility and responsiveness to glutathione (GSH), facili-

tating controlled drug release. In vitro and in vivo experiments

showed the effective inhibition of human hypopharyngeal squa-

mous cell carcinoma, combining photothermal therapy with

DOX for enhanced cancer treatment [251].

properties
2.2. Properties of MXene

2.2.1. Capacitive Properties

MXene has rich oxidation-reduction sites, which leads to high capacitance [33,34]. Taking Ti3C2Tx
MXene as an example, Ti’s oxidation state continuously changes owing to the hydration of the
oxygen-containing terminal groups, providing charge transfer capability for the valence transition metal
[35,36]. The end groups on the surface of MXene also play a key role in energy storage [37]. Generally
speaking, =O functional groups are more stable than -OH and -F because they share more electrons with
the M element in the MXene layer, and the conversion between the =O and -OH end groups during
charge and discharge processes provides a large number of active sites for redox reactions [38,39]. The
unique layered structure of 2D MXene means a larger surface area, and the multi-layered structure is
more conducive to ion intercalation and transmission [40]. Supercapacitors made from MXene have
excellent volumetric capacitance (about 1500 F cm−3) [34,41]. In addition, the layered structure of MXene
allows it to adapt to various intercalating agents, which helps to expand the electrochemical reaction
activity of MXene compared to the surface area, enhancing pseudocapacitance and cycling stability
[42,43]. The good energy storage capacity of MXene is reflected in the devices fabricated with it, which
have high energy and power densities.

2.2.2. Conductivity

MXenes have excellent conductivity, with a metallic conductivity of up to ~24,000 S cm−1. The
structure of MXene contains many transition metal elements, for example, titanium and molybdenum,
which usually have high conductivity, forming conductive channels in the MXene structure and promoting
electron transmission [44,45,46], thereby improving the overall conductivity of MXene [47,48,49]. MXene
is a 2D material with a large specific surface area, which means higher electron accessibility. Electrons
can freely transmit on the 2D plane, reducing electron scattering losses and improving conductivity
performance. The morphology of MXene also has a great impact on its conductivity; single-layer and
large-sized flakes have better interaction than multi-layered and small-sized flakes, usually improving
conductivity [14,50,51]. In addition, compared with other 2D materials such as metal sulfides/hydroxides
or graphene, MXene has plenty of chemical functional groups, for example, hydroxyl and fluorine atoms,
and by changing these functional groups, the electronic structure and charge transfer properties of
MXene can be controlled, affecting its conductivity performance [52]. Overall, the improvement of MXene
conductivity is mainly due to its unique structure, containing transition metal elements and abundant
chemical functional groups, which together make MXene an excellent conductive material with a multitude
of potential applications. The MXene’s excellent conductivity ensures rapid electron transmission, making
it possible to achieve high-power density supercapacitors. In the manufacturing process of electrodes,
conductive agents and current collectors are not even necessary, which helps to improve the energy
density of the entire device [53,54].

2.2.3. Hydrophilicity

MXene has good hydrophilicity mainly due to the abundant oxygen, hydrogen, and other functional
groups in its layered structure, including -OH, -F, etc., making the MXene surface highly polar [55,56,57].
In water, these polar functional groups can form hydrogen bonds and other interaction forces with water
molecules, causing attractive forces between MXene particles and water molecules, showing excellent
hydrophilicity [58]. What’s more, the interlayer structure of MXene contains lots of hydrogen bond
acceptors, contributing to forming hydrogen bonds with water molecules, which also increases its
compatibility with water [59]. Furthermore, the hydrophilicity of MXene can be improved due to its
characteristics such as the porous structure and high specific surface area, because these characteristics
can help to expand the contact surface area between MXene and water, and the mutual interaction with
water can also be improved as well [60]. To summarize, the superior hydrophilicity of MXene is gained
due to its features, including the abundant polar functional groups, hydrogen bond sites, porous structure,
high specific surface area, and the layered structure of MXene. This property equips MXene with
excellent dispersion, stability, as well as application potential in water-based systems, preparing for its
widely used application in water-based supercapacitors and other fields [61,62].

2.2.4. Mechanical Flexibility

The layered structure of MXene is critical to its flexibility in the sphere of mechanics. MXene consists
of numerous layers of 2D nanosheets, which are put on top of each other via relaxed bonding. The
function of the 2D nanosheets is that they allow MXene to slide and shear under forces that are produced
by external objects, which also gives MXene great deformability and ability to bend [63]. Meanwhile,
through the method of intercalating other materials (like polymers or liquids), the MXene’s layered
structure can be greatly improved to form composite materials, as well as enhance its flexibility [64,65].
Chu et al. synthesized two-dimensional transition metal carbide/polyimide (Ti3C2Tx MXene/PI) films
through in situ polymerization and a simple scratch method, which showed enhanced flexibility. It can
better adapt to the deformation of the capacitor, which is conducive to improving the contact efficiency
between the electrode and the electrolyte of the capacitor, thus improving the performance [66]. M-Xenes’
mechanical characteristics are decided by their structural combination, size, defects, density, incomplete
nanosheet edges, surface end groups, and M–X elements. Like other 2D materials, each thin sheet
determines its inner mechanical properties [67]. The surface end groups are essential for improving the
mechanical characteristics of M-Xenes. For instance, =O end groups can strengthen the M-Xenes’s
interlayer attraction. And it can also improve the M-Xenes’ resistance to shear and strain. The
high-specific surface area and mesoporous structures can also enhance the flexibility of M-Xenes
materials. Through applied high-specific area and mesoporous structures, the contract surface and
external environment can be increased, and the stress concentration can be reduced, which can provide
more and more displacement and deformation space and enhance M-Xene’s flexibility and durability,
which reduce the influence of external vibration on the internal structure of the capacitor. Furthermore,
according to a study by Guo et al., under uniaxial and biaxial conditions, respectively, upon the addition of
=O end groups, the results have shown that the tensile range of Ti2C was increased to 28%and 20%,
which indicates the inhibitory influence of surface terminal groups on Ti2C’s collapse [68]. Therefore, the
addition of =O end groups of Ti2C can prevent the capacitor from being easily damaged when bending or
stretching to maintain stable performance. In conclusion, the mechanical flexibility of M-Xenes material
originates from its high specific area, layer structure, mesoporous structure, and chemical composition.
Therefore, M-Xenes has a wide range of potential applications. It also is the source of inspiration for the
new materials to become reliable and flexible. Sun et al. modulated size refinement to decrease the grain
size, introducing more grain boundaries, which stopped dislocations and crack propagation under
deformation. This resulted in increased strength and toughness. The MXene with the size refinement
showed increased energy density and power density of the supercapacitors [69,70]. Mechanical
performance will affect the electrode’s electrochemical performance, especially in future applications,
where the electrode of flexible electronic devices will be subjected to stress, bending, and twisting. To this
end, we summarize the relative advantages of mechanical flexibility of MXene and other kinds of
two-dimensional materials at Table 1. MXene has excellent mechanical flexibility, which helps to maintain
good electrochemical performance and facilitates its application in flexible supercapacitors and
micro-supercapacitors [71].
Properties of MXenes

The layered structures and surface functional groups of MXenes endow them with exceptional
properties, paving the way for a wide range of applications for these promising materials. The 3D bulk
precursors of MXenes (MAX phases), along with delamination and synthesis methods, play a critical role
in determining their properties [3]. The most interesting features of MXenes are outlined in the next
sections.

3.1. Mechanical Properties

MXenes exhibit outstanding mechanical properties, including remarkable flexibility, high tensile
strength, and significant flexural rigidity. The Young’s modulus of a Ti3C2Tx monolayer has been
calculated to range between 0.33 TPa and 0.03 TPa, making it the highest among all 2D materials,
including graphene oxide (GO). Notably, the flexibility of Ti3C2Tx is impressive: it has been reported that
a Ti3C2Tx film can support up to 4000 times its weight without experiencing any shape distortion or
structural damage [6].

The elastic behavior of MXenes is strongly influenced by their surface terminal groups. Specifically,
the strength and length of surface bonds play a key role in determining their mechanical properties.
Experimental studies indicate that MXenes with O-terminal groups are the most suitable candidates for
applications such as supercapacitors and structural materials due to their exceptional flexibility [3]. The
Ti-O bond is notably stronger than the Ti-OH and Ti-F terminations [37]. Density Functional Theory (DFT)
simulations conducted on Ti3C2 and Ti2C with different surface terminations have demonstrated that
shorter bond lengths—such as those associated with oxygen groups—indicate stronger contacts,
whereas F and OH bonds, being longer, result in weaker interactions [38].

Regarding Ti-C bonds, previous studies have shown that Ti2C, Ti3C2, and Ti₄C3 MXenes exhibit
considerable rigidity. However, graphene remains a superior alternative due to its higher strength and
stiffness [37]. Additionally, M-N and M-C bonds contribute to the tensile strength of MXenes, reaching
1050 GPa [39] and opening significant opportunities for their use as reinforcing materials in composite
structures. While MXenes may demonstrate slightly lower performance compared to graphene, they offer
excellent compatibility with polymeric phase to produce composites.

The thickness and number of layers also significantly influence the Young’s modulus of MXenes.
When comparing carbide and nitride MXenes, the latter exhibit higher maximum values. In both cases, a
decrease in the number of layers correlates with an increase in the Young’s modulus [37].

3.2. Chemical Stability

The oxidation state of MXenes depends on their surface terminal groups and is generally lower than
that of the corresponding metal oxides. The stability of MXenes is heavily influenced by their surrounding
environment [6]. For example, the stability of Ti3C2Tx colloidal solutions was tested under ambient
conditions. It was observed that the solution degrades into TiO2 within 15 days, identifying air, specifically
oxygen, as the primary factor responsible for the oxidation of Ti3C2Tx [40,41].

Water also plays a significant role in the degradation of MXene solutions. Colloidal solutions of
Ti2CTx and Ti3C2Tx degrade within 41 days in a water/argon environment. In contrast, when exposed to
an IPA/oxygen environment, the degradation process is significantly slower, taking approximately 5.5
years to achieve similar results [42].

MXene oxidation can be mitigated through the use of antioxidants, such as sodium L-ascorbate, and
by maintaining specific environmental conditions, which vary depending on the MXene type. For instance,
V2Ctx remains stable in an argon atmosphere at temperatures below 375 °C, whereas Ti3C2Tx can
maintain its stability in argon up to 800 °C [40,41] (see Figure 6 [43]).

Figure 6. Ti3C2Tx dispersibility in different solvents and evolution over time (reprinted from [43] with CC
license).

MXenes exhibit a remarkable hydrophilic nature, due to the presence of O and OH surface groups,
which play a crucial role in enabling strong interactions with water. These groups enhance the ability of
MXenes to attract and spread water across their surface. The ratio of surface terminations can be
precisely controlled through synthesis methods, allowing for the optimization of their hydrophilic
properties. This characteristic is particularly valuable in the production of inks for 3D printing of composite
electrodes, where achieving a stable and uniform dispersion of materials in solvents is essential [44].

3.5. Surface Modification and Multifunctionalization

The most studied MXenes feature hydroxyl (-OH), oxygen (-O), or fluorine (-F) terminal groups,
which provide these materials with high stability, a significant surface charge, and a hydrophilic nature.
However, after delamination, MXenes often require enhancements to certain properties, making surface
engineering a critical factor [25].

Surface modification is typically achieved through two main approaches: polymer-based strategies
and inorganic particle surface chemistry. The former approach involves the immobilization of specific
molecules or polymers onto the MXene surface via non-covalent or covalent interactions. For example,
soybean phospholipids (SPs) have been utilized to modify the surface of Ta4C3Tx films, enhancing their
stability in physiological environments [24]. An example of inorganic particle-based surface chemistry [24]
is the preparation of AuNPs/Ti3C2Tx, achieved by immobilizing gold nanoparticles on the MXene surface
to improve electrical conductivity [56].

The layered structure of MXenes, characterized by a high surface area and significant interlayer
distances, facilitates ion intercalation, which can improve energy storage performance in applications
such as batteries and supercapacitors [37]. Figure 9 illustrates the structure of Ti3C2Tx and provides a
simplified scheme of the intercalation process, highlighting the increased interlayer spacing after ion
insertion. Electrochemical intercalation of Ti3C2Tx cations, such as Al3+, is one example, with other ions
like Li+, Na+, Mg2+, K+, and NH4+ also being widely studied [57].

Figure 9. (A) Ti3C2Tx microscopic layered structure; (B) cations intercalation process (reprinted from [57]
with CC license).

However, the structure of MXenes still carries important challenges. Their tendency to reassemble
and the lack of a controlled porosity are notable limitations [3]. In order to address these issues, a study
proposed a method involving sequential bridging using hydrogen and covalent bonding agents to achieve
optimal layer density and reduce vacancies in MXenes [24]. Table 3 lists additional approaches designed
to control porosity and voids [3].

Table 3. Various synthesis techniques to obtain porous MXenes.

Nevertheless, many of the multifunctionalization techniques discussed above still require further
research, especially considering that studies on graphene and graphene oxide (GO) are more advanced
at present [25].

. Applications

4.1. Biomedical Applications

Thanks to their interesting and highly tunable properties, such as hydrophilicity, large surface area,
and exceptional conductivity, MXenes became promising materials for a wide range of biomedical
applications (Figure 10 [24]) [25]. This section explores some of the most significant and recent studies in
this field.
 Figure 10. Illustration of the most attractive examples of using of MXenes in the biomedical field.
reprinted from [25] with CC license.

Inorganic MXene-based materials possess appealing properties, often surpassing those of organic
materials, which typically offer exceptional biocompatibility but are frequently prone to significant chemical
and thermal instability. MXenes are distinguished by their highly tunable structure and
multifunctionalization capabilities [25], chemical affinity [11], remarkable physiological stability, and
excellent biosafety [25]. For biomedical applications, toxicity and biocompatibility require careful
consideration. MXene biosafety can be compromised by factors such as exfoliation, nanotoxicity/cell
internalization [58], release of toxic ions, and generation of reactive oxygen species (ROS), which all carry
potential hazards to cells, organs, and tissues [11]. Numerous studies have been conducted to assess the
biosafety of MXenes, but further efforts are needed, particularly to certify their long-term stability [25].
Both in vivo (e.g., on mice [25]) and in vitro (e.g., using cell cultures [11]) studies have demonstrated low
toxicity levels for MXenes. For instance, in an in vitro experiment, Ti3C2-SP and Ta4C3-SP films showed
negligible effect on 4T1 cell viability. Similarly, in vivo tests on mice demonstrated normal behavior after
administration of Nb2C-PVP at a dosage of 20 mg/kg [25].

MXene can be incorporated in biomedical coatings to improve biocompatibility and make them
electrically conductive, as recently reviewed by Anvari Hohestani et al. [59]. In this regard, an interesting
example includes the study of Mayerberger et al. [60] who incorporated Ti3C2Tx MXene flakes into
chitosan nanofibers for use in passive antibacterial wound dressings. Antibacterial tests against E. coli
and S. aureus also showed a significant reduction in colony-forming units, with decreases of 95% and
62%, respectively [59].

Surface modification and the use of polymer composites are effective strategies to enhance biosafety
and prevent the degradation of MXenes [11]. For instance, the incorporation of OTES-functionalized
Ti3C2Tz MXene into poly(lactic acid) membranes has been shown to improve biocompatibility, promoting
cell adhesion, proliferation, and osteogenic differentiation, while also enhancing mechanical properties
[61].

4.1.1. Biosensing

MXene-based biosensors have been tested in the human body to detect and analyze biomolecules
and their effects. These biosensors consist of three main components: a sensing element to identify the
target, a transducer to convert biochemical signals into electrical signals, and a data interpreter for
analysis [11]. The exceptional properties of MXenes, such as their large surface area [25] and high
charge activity for efficient target capture [62], excellent photon absorption capability, rapid electron
transfer fluorescence quenching [25], and remarkable sensitivity and selectivity [58], make them highly
promising for a wide range of biosensing applications. Electrochemical biosensors, known for their rapid
response, simplicity, and cost-effectiveness, have also demonstrated significant potential in applications
such as pesticide detection and analysis in agriculture, specifically for paraoxon [62]. Furthermore,
MXene-based biosensors have shown optimal performance in detecting glucose, circulating tumor DNA
[11], dopamine [25], NADH, and uric acid [58]. For instance, an electrochemical biosensor using
antibody-functionalized Ti3C2Tx MXene nanosheets was developed for point-of-care detection of vitamin
D. The sensor achieved high sensitivity (LOD of 1 pg mL⁻1) and a wide dynamic range (0.1–500 ng
mL⁻1), suitable for clinical screening of deficiency and toxicity levels. This MXene-based platform is
low-cost, fast, and ideal for remote diagnostics [63].

4.1.2. Imaging

Quantum size effects, intrinsic photothermal properties, element-driven contrast enhancement, and
efficient loading of functional contrast agents (CAs) make MXenes highly suitable for imaging
applications. The most extensively studied imaging modalities include photoacoustic imaging (PAI),
magnetic resonance imaging (MRI), X-ray computed tomography (CT), and luminescent imaging [64]. PAI
is a non-invasive, non-ionizing technique that overcomes optical photon scattering to enable deep tissue
imaging. It generates photoacoustic signals from the light absorption of tissue molecules, which are then
converted into images via a transducer, effectively capturing biological information [24]. Among the
explored materials, Nb2C-MSNs-SNO composite nanosheets have exhibited exceptional performance as
PA contrast agents [64], while Nb2CTx-PVP stands out for its remarkable stability and photothermal
conversion efficiency [24]. Additionally, Ta4C3-SP nanosheets have shown promising
contrast-enhancement capabilities [25]. MRI offers excellent spatial resolution, superior soft tissue
contrast, and the advantage of avoiding ionizing radiation [64]. Ti3C2 MXenes have demonstrated
significant potential in MRI applications due to their enhanced contrast properties [65]. CT imaging
remains one of the most widely used methods due to its effectiveness, non-invasive nature, and ability to
achieve deep tissue penetration. It generates 3D scans by segmentally scanning a body section with
X-rays. Notably, MnOx/Ta4C3Tx-SP composite nanosheets have shown superior performance in CT
imaging compared to iodine-based iopromide [66], a commonly used clinical agent, owing to tantalum’s
high X-ray attenuation coefficient [24]. For luminescent imaging, the production of MXene quantum dots
(MQDs) significantly enhances luminescent properties [67]. MQDs exhibit small dimensions, strong
photoluminescence (PL) characteristics, remarkable stability, low toxicity, and tunable wavelengths [24].
Ti3C2 MQDs have demonstrated excitation-dependent photoluminescent spectra and impressive
quantum yields (up to 9.9% [25]) [64]. Similarly, Nb2CTx QDs [48] have shown outstanding
enzyme-responsive degradability, robust resistance to photobleaching, and remarkable stability [24].

4.1.3. Theranostic Applications

Theranostic applications combine therapeutic and diagnostic functions within a single platform [11].
Photothermal therapy (PTT) is a prominent approach in cancer and tumor treatment, leveraging the
exceptional properties of MXenes (Figure 11 [68]). PTT employs photothermal agents accumulated within
tumors to act as internal energy absorbers, converting NIR light energy into heat, leading to necrosis
and/or apoptosis of cancer cells [24]. High photothermal performance has been observed in various
studies, including in vivo and in vitro experiments, with materials such as Ti3C2, which is distinguished by
its rapid light-to-heat conversion, Ta4C3, known for its excellent biocompatibility, high conversion
efficiency (44.7%), and strong absorption band, and Nb2C, the latest addition, which shows high
performance in both NIR-I and NIR-II biowindows. Moreover, Ti3C2 has been utilized in a synergistic
therapy combining photothermal ablation with DOX-based chemotherapy, demonstrating outstanding
stability, complete eradication of 4T1 cells without recurrence, and a drug encapsulation capacity of
84.2% [25]. Immunotherapy works by enhancing or activating the immune system to prevent or eliminate
tumor cells. A 3D-printed Nb2CTx scaffold for breast cancer treatment showed promising results, but
immunotherapy still requires additional therapeutic strategies (e.g., PTT and PDT) to achieve optimal
outcomes [24].

Figure 11. Example of 3D-printed scaffold for bone tissue regeneration and tumor ablation (reprinted from
[68] with CC license).

4.1.4. Tissue Engineering

Tissue engineering aims to design and develop biological tissues to restore or regenerate functions
lost due to disease or injury [69]. MXenes have been explored in various tissue engineering fields,
including stem cell engineering [69], skin tissue engineering, nerve tissue engineering, and myocardial
tissue engineering [64]. Research has shown that Ti3C2Tx enhances cell proliferation and osteogenic
differentiation in PLA scaffolds and promotes the production of cell spheroids [70], with both in vitro and in
vivo tests highlighting their excellent biocompatibility [64]. Additionally, MXene/PLLA-PHA electrospun
nanofibers [71] were found to improve the activity, growth, and osteogenic differentiation of BMSCs [70].
Ti3C2Tx has shown great promise in tissue engineering, particularly due to its functionalized conductive
surface, which supports stem cell differentiation and enables precise photothermal stimulation of dorsal
root ganglion neurons, facilitating the development of advanced neural therapy models [72]. Furthermore,
Ti2C was used to develop bio-functional engineered cardiac patches (ECP) [73] that can repair
myocardial infarction (MI) when applied to the natural heart. These patches demonstrated remarkable
effectiveness in enhancing heart function, reducing infarct size, and alleviating inflammation [64].
Additionally, an MXene-reinforced PVA cryogel scaffold was developed for neural tissue engineering,
successfully promoting PC-12 cell proliferation, neurite outgrowth, and reducing oxidative stress, showing
strong potential for neural regeneration applications [74].

The suitability of MXenes for bone tissue engineering applications has also been investigated; a
comprehensive overview of this specific topic can be found elsewhere [75].

4.1.5. Drug Delivery

The distinct 2D architecture and tunable physicochemical features of MXenes make them attractive
candidates for targeted drug delivery. Among them, Ti3C2Tx stands out due to its ultrathin morphology,
strong near-infrared responsiveness, effective photothermal properties, and adaptable surface chemistry.
Despite these advantages, Ti3C2Tx-based carriers often exhibit limited drug-loading capacity and poor
retention at target sites, leading to premature clearance and potential tissue damage. Similarly to other
2D inorganic materials, MXene-based systems also face stability issues under physiological conditions,
complicating controlled drug release [70]. In order to overcome these challenges, integrating magnetic
nanoparticles into MXene structures has been proposed, enabling external magnetic fields to guide and
retain the drug carriers at the desired location, with drug release triggered by specific internal or external
stimuli [76].

Recent studies have demonstrated the use of MXene-based systems, particularly Ti3C2Tx, for
efficient drug delivery. For instance, a dual therapeutic agent (DOXjade), formed by linking DOX to a
deferasirox derivative, was successfully loaded onto Ti3C2-PVP MXene, achieving high loading capacity
of 210%, pH-triggered drug release of 5.3 with release time in a range from 0 to 72 h [77]. Other
strategies involved functionalizing Ti3C2Tx with polymers like PEG or chitosan, or forming composites
with Co nanowires (CoNWs) to enhance drug loading and ensure pH-responsive release, favoring drug
liberation in acidic tumor environments, such as breast cancer, reaching loading and release efficiencies,
respectively, up to 225% and 77%, with a release time of 24 h [78].

4.2. Electronic Applications

The remarkable and tunable electrical and electronic properties of MXenes position them as strong
candidates for a wide range of electronic applications. This section highlights the most extensively studied
and promising examples in this context.

4.2.1. Supercapacitors

Many features of MXenes make them promising candidates for the design of micro-supercapacitors
(MSCs) and for use in high-precision integrated circuits (Figure 12 [79]). The morphology of MXenes
plays a crucial role in determining their electrochemical performance. For instance, after etching the 3D
bulk precursor, the material capacitance can be enhanced by the intercalation of water molecules within
the layered structure, facilitated by the 2D slits. Additionally, water dielectric constant is key for shielding
external electric fields. The small thickness of MXenes contributes to superior ion diffusion and further
enhances capacitance. The functional groups of MXenes, along with their tunability, endow these
materials with excellent energy density, acting as active sites that promote ion insertion and removal. As a
result, MXene-based MSCs stand out for their excellent flexibility, high power density and voltage,
compact dimensions, and remarkable durability [10]. To further enhance the performance of
MXene-based supercapacitors, such as ion transfer and accessibility, composite materials have been
developed by combining MXenes with organic polymers (also called conductive polymers or ICPs), metal
oxides [43], metal hydroxides, and carbon materials [80]. The intercalation of these elements expands the
interlayer spacing and minimizes MXene rearrangements [43]. Ti3C2Tix/ZnMnNi LDH van der Waals
heterostructured electrodes [81] were produced through the combination of MXene and layered double
hydroxides that showed a great capacitance of 2065 F/g at 5 mV/s and a capacitance retention rate of
99.8% after 100,000 cycles at 1 A/g [81]. Another notable example is the combination of graphene and
MXene in a modified MXene/graphene oxide (MX-rHGO) film [79], which has demonstrated impressive
volumetric capacitance (1445 F/cm3) at a scan rate of 2 mV/s, excellent mass loading, and outstanding
durability, retaining 93% of its capacitance after 10,000 cycles at 5 A/g [81].
 Figure 12. (a) Production of the MXene/holey graphene film; (b) the impact of real mass loading on the
volumetric capacitance of MXene film and MX-rHGO3; (c) capacitance maintenance of MX-rHGO3 at 5
A/g for 10,000 cycles; (d) gravimetric and (e) volumetric energy and watt densities of MX-rHGO3-based
symmetric supercapacitors (reprinted from [79] with CC license).

4.2.2. Perovskite Solar Cells

Perovskite solar cells (PSCs) have shown great potential in the field of photovoltaic technology due
to their low production cost and high efficiency [82]. Since the first studies on the application of MXenes in
PSCs, dating back to 2018 [83], power conversion efficiencies (PCEs) of these devices have reached
values comparable to those of the most widely used silicon solar cells, up to 26%. Considering that this
performance has been achieved in silicon cells over 70 years of research, perovskite solar cells are
supposed to match and surpass them. PSCs are distinguished by their high-quality structure, which can
be further enhanced through MXene additives, offering improved conductivity, reduced diffusion
resistance, and tunable properties [82]. For example, the optoelectronic performance of
(BA)2(MA)4Pb5I16 films has been improved by adding Ti3C2Tx nanosheets, achieving a PCE of 15.71%
and a short-circuit current density of 20.87 mA/cm2 [84]. Other MXenes, such as Nb2CTx [85], V2CTx
[62], and Mo2CTx [86], have also been studied for PSC applications, and further research is needed to
identify additional effective additives [82]. Moreover, it is essential to optimize MXene production by
developing more sustainable methods than HF etching, aiming to support mass production. Another
aspect that warrants further investigation is the most efficient dosage of MXenes and the concentration of
functional groups to maximize PSC performance, particularly in terms of stability, chemical compatibility,
and durability [82].

4.2.3. Batteries

In the realm of energy storage, lithium–sulfur batteries (LSBs) stand out as highly effective devices,
thanks to their exceptional specific capacities, impressive energy densities [87], and superior safety
standards, surpassing even lithium-ion batteries (LIBs) [38]. MXene-based materials have proven to
significantly enhance LSB performance due to their remarkable electrochemical properties. MXenes are
extensively utilized in cathodes, interlayers, and separators, where they improve durability, enhance
catalytic processes, support lithium polysulfide and Li2S kinetics, increase sulfur loading, and facilitate
lithium anode hosting [87]. For example, Ti3C2Tx has been employed to coat separators, achieving an
impressive capacity of 850.9 mAh/g with a sulfur loading of 2.8 mg/cm2 and maintaining a capacity
retention of 89.66% [88].

Furthermore, Ti3C2Tx MXene has been applied in aqueous zinc metal batteries (ZMBs) as an
electrolyte additive [89], effectively inhibiting Zn dendrite nucleation and growth—common issues that
compromise battery efficiency or cause internal short circuits [38]. Additionally, high-purity V2CTx MXene,
used as an anode in LIBs [90], has exhibited outstanding electrochemical performance (Figure 13) [91].

Figure 13. Schematic illustration of a lithium-ion battery system (reprinted from [91] with CC license).

A hollow MoSe2@MXene composite was synthesized via a hydrothermal method by growing MoSe2
nanoflakes on hollow MXene spheres. This 3D structure, used as an anode in sodium-ion batteries,
demonstrated excellent cycling stability and rate performance, delivering 350.7 mAh g⁻1 after 1000 cycles
at 1 A g⁻1 with 93.7% retention. Its high performance is due to the synergistic effect between MoSe2 and
MXene, which prevents material aggregation and improves sodium-ion transport [92]. A Sn4P3@MXene
anode with a protective MXene shell enables inward expansion and stable cycling, delivering 302.1
mAh/g at 10 A/g and 94.9% retention over 1500 cycles. The full cell achieves 287.8 Wh/kg and 390.5
mAh/g after 500 cycles, highlighting its practical potential [93].

A PTCDA-based potassium-ion battery anode using MXene as an electrochemically active binder

achieved 462 mAh/g at 50 mA/g, 116.3 mAh/g at 2000 mA/g, and excellent stability over 3000 cycles with
only ~0.0033% capacity loss per cycle. The MXene/Super-P matrix improved conductivity suppressed
PTCDA solubility, and enhanced K⁺ adsorption. The full cell reached 179.5 Wh/kg energy density,
highlighting MXene’s role in enabling stable, high-performance organic PIBs [94]. The CNS@Ti3C2
composite, created by encapsulating Ti3C2 MXene with carbon nanospheres from carbon quantum dots,
enhances potassium storage in PIBs. It delivers 229 mAh/g at 100 mA/g after 200 cycles and 205 mAh/g
at 500 mA/g after 1000 cycles, with >99% coulombic efficiency, offering a promising approach for
high-performance potassium-ion batteries [95].

4.3. Separation and Filtration Applications

MXenes offer significant potential in the design of membranes for separation applications thanks to
their remarkable properties such as hydrophilicity, conductivity, and high flexibility (Figure 14) [96]. This
section discusses some of the most valuable examples and provides a future outlook in this field.
 Figure 14. A scheme of the benefits of MXene-based membranes for separation processes (reprinted
from [96] with CC license).

4.3.1. Water Treatment

Over the years, MXenes have been engineered as functional membranes for water treatment and ion
sieving due to their remarkable hydrophilicity and their overall negative charge. The surface
functionalization of MXenes enhances their layered structure, improving permeability, enabling the
separation of ions of different dimensions. The size-exclusion mechanism promotes the selection of ions
smaller than the channels, while the Donnan exclusion method sieves negative ions, allowing only
positive charges to permeate through electrochemical interactions with the net charge of MXenes [96]. An
optimal MXene-based membrane should exhibit high water flux, excellent selectivity, and remarkable
mechanical and chemical stability, particularly in resisting fouling [97]. In order to enhance fouling
resistance, Ag nanoparticle-modified Ti3C2Tx (Ag@MXene) membranes have been developed [98],
achieving impressive water flux (approximately 420 L m⁻2 h⁻1 bar⁻1), high rejection rates for bovine serum
albumin (100%), methyl green (92.3%), and rhodamine B (RhB, 79.9%) [96]. Additionally, the combination
of graphene oxide (GO) and Ti3C2Tx in a 90 nm thick membrane [99] has demonstrated significant
performance in rejecting positively charged dye molecules with radii greater than 5 Å [100]. MXenes have
gained attention as promising materials for seawater desalination and pollutant removal to address the
global demand for freshwater [101]. A Ti3C2Tx-based membrane has achieved nearly 100% efficiency in
NaCl separation, with water permeance reaching 85 L m⁻2 h⁻1 bar⁻1 at 65 °C [100]. Furthermore, Ti3C2
MXenes have been employed in photothermal water desalination under solar irradiation, leveraging their
high light-to-heat conversion efficiency [102]. Regarding the antibacterial properties of MXene-based
membranes, fresh Ti3C2Tx nanosheets [103] have shown a 73% antibacterial rate against Bacillus
subtilis and 67% against Escherichia coli through direct contact damage. Upon air oxidation, these
nanosheets can inhibit bacterial growth by up to 99% [96].

4.3.2. Gas Separation

Gas separation technologies are crucial for a wide range of industrial and environmental applications,
such as H2 purification and CO2 capture [104], and are known for their low energy consumption,
operational simplicity, and scalability [105]. Two-dimensional materials like MXenes are emerging as
excellent alternatives to traditional polymer-based membranes due to their superior mechanical strength,
layered structure, and tunable properties. The interlayer spacing and channel length of MXenes are key
factors in determining their selectivity and performance in gas separation applications. In general, wider
channels lead to improved permeability and selectivity [105]. Research has shown that Pd intercalation in
MXene-based membranes [106] can enhance H2 permeability and H2/CO2 selectivity [105]. Additionally,
an MXene/PEG mixed matrix membrane [107] was designed to enhance CO2 permeability for CO2/N2
and CO2/CH4 separation [105]. The presence of functional groups and surface reactivity also plays a
significant role in membrane performance: CO2, due to its quadrupole moment, can be easily absorbed
by MXene interlayers, which facilitates effective H2/CO2 separation [104]. A recent study tested the
permeability of He, H2, CO2, N2, and CH4 in C180 at room temperature and under different pressures,
revealing that larger molecules like N2 and CO2 exhibit lower permeability compared to smaller ones
such as He and H2, as illustrated in Figure 15 [104].
Figure 15. Single gas permeabilities, permeances, and H2/CO2 selectivity at different pressures in C180
(reprinted from [104] with CC license).

The effectiveness of gas separation can also be temperature-dependent. MXene-based membranes

were tested for H2 selectivity at high temperatures (320 °C) over 200 h of continuous testing, with no
significant changes in performance or structure. However, as the temperature increased, both
permeability and selectivity decreased significantly, highlighting an area that requires further investigation
[108].
picture promt
From Gemini
Based on the detailed content of your book chapter, here are 10 suggested images to visually enhance
the text. These are strategically placed to illustrate complex mechanisms (like synthesis and shielding)
and showcase applications.

I have provided a Description (for your caption) and a Generative AI Prompt (which you can
copy-paste into tools like Midjourney, DALL-E 3, or Adobe Firefly to generate the image).

1. The "MAX to MXene" Transformation

●​ Placement: Section 1.2. Enter MXenes: The New Frontier (near the general formula
description).
●​ Why: To visualize the fundamental concept of exfoliating a 3D block into 2D sheets by
removing the "A" layer.
●​ Prompt:​
A high-quality 3D scientific illustration showing the transformation of a MAX phase crystal
into MXene. On the left, a solid block of densely packed atomic layers with alternating red
(Metal), blue (Aluminum), and black (Carbon) layers. In the center, an ethereal 'etching' effect
where the blue Aluminum layers are dissolving away. On the right, the resulting 'MXene'
material: the remaining red and black layers fanned out like an open deck of cards, with small
glowing 'T' functional groups attached to the surfaces. Clean white background, textbook
diagram style.

2. Top-Down vs. Bottom-Up Synthesis Map

●​ Placement: Section 2. Synthesis: From Hazardous to Sustainable (Introductory paragraphs).
●​ Why: To contrast the two main fabrication routes discussed in the text.
●​ Prompt:​
A split-screen comparison infographic. Left side (Top-Down): A beaker containing a bubbling
green liquid (acid) with a bulk crystal turning into floating flakes. Label this 'Etching'. Right
side (Bottom-Up): A glowing vacuum chamber where gas molecules are settling onto a
substrate to form a perfect, single hexagonal sheet. Label this 'CVD Growth'. Use a clean, flat
vector art style with a blue and green color palette.

3. The Lewis Acidic Etching Mechanism (Green Route)

●​ Placement: Section "Molten-Salt and Lewis-Acidic Etching".
●​ Why: This is a key "Recent Breakthrough" (2024-2025) mentioned in the text and needs a
distinct visual from the traditional acid method.
●​ Prompt:​
A molecular schematic illustrating 'Lewis Acidic Molten Salt Etching'. Show a Ti3AlC2
atomic structure submerged in a bath of molten ZnCl2 (represented as a hot orange liquid).
Depict a 'Substitution Reaction': Zinc atoms swapping places with Aluminum atoms, followed
by the Aluminum evaporating away as AlCl3 gas bubbles. The final product shows MXene
sheets terminated with Chlorine atoms (green spheres). Detailed, realistic molecular rendering.
4. EMI Shielding: The "Internal Reflection" Trap
●​ Placement: Section 1.3.3 Unmatched EMI Shielding Effectiveness.
●​ Why: To explain the unique "absorption + reflection" mechanism that makes MXene superior
to metal or carbon.
●​ Prompt:​
A cross-section diagram of an MXene film blocking electromagnetic waves. Incoming red sine
waves (EMI Radiation) hit the layered MXene barrier. Show three distinct interactions: 1)
Some waves bouncing off the surface (Reflection), 2) Most waves entering the material and
bouncing frantically between the parallel MXene sheets (Multiple Internal Reflections), and 3)
The waves fading out into heat (Absorption). Dark background with glowing red waves for
contrast.

5. MXene vs. Graphene: The Volumetric Advantage

●​ Placement: Section 1.3.2 Superior Volumetric Capacitance or Table 1.
●​ Why: To visualize the "Density Factor" argument—why MXene packs more energy in less
space than porous graphene.
●​ Prompt:​
A comparative 3D illustration of two battery electrodes. Left (Graphene): A fluffy, porous
aerogel structure that looks like a sponge, with lots of empty space. Right (MXene): A dense,
brick-like stacking of aligned sheets. Show 'Energy Particles' (glowing dots) packed tightly
into the MXene structure, while the Graphene structure has them loosely scattered. Caption:
'Volumetric Capacitance: Density Matters'.

6. Battery Intercalation Mechanism

●​ Placement: Section 4.1. Energy Storage (Batteries & Supercapacitors).
●​ Why: To illustrate how ions (Li^+ or Na^+) move between layers and how the structure
expands.
●​ Prompt:​
A close-up molecular view of a Lithium-ion battery anode made of MXene. Show Lithium ions
(small glowing spheres) smoothly flowing into the gaps between stacked MXene sheets. The
sheets slightly expand to accommodate the ions ('Breathing' effect). Background suggests a
battery environment with electrolyte fluid. High-tech, blue and silver color scheme.

7. Perovskite Solar Cell Interface

●​ Placement: Section 4.2.1 MXenes as Interface Modifiers in Perovskite Solar Cells.
●​ Why: To show the specific location where MXene is applied (interface) to improve efficiency.
●​ Prompt:​
A layered diagram of a solar cell device. Layers from bottom to top: Glass, Electrode, Electron
Transport Layer, MXene Interface Layer (highlighted in gold), Perovskite Crystal Layer
(colorful, faceted grains), and Top Electrode. Zoom in on the MXene layer to show it bridging
the gaps between Perovskite grains, smoothing the flow of electrons.

8. Wearable "Electronic Skin" Biosensor

 ●​ Placement: Section 4.3 MXene-Based Sensors or 4.6 MXene-Enabled FETs.
●​ Why: To visualize the "Flexible" and "Transparent" industrial applications mentioned in Case
Study 1 & 3.
●​ Prompt:​
A photorealistic concept shot of a human wrist wearing a futuristic 'Electronic Skin' patch. The
patch is ultra-thin and transparent, with a visible hexagonal grid pattern made of gold-black
MXene ink. A holographic projection above the wrist displays 'Glucose Level' and 'Hydration'
data. Soft, medical-tech lighting.

9. Water Filtration Membrane Mechanism

●​ Placement: Section 4.4 MXenes for Environmental Remediation.
●​ Why: To illustrate how the "tortuous path" of the stacked layers blocks contaminants.
●​ Prompt:​
A 3D cutaway view of a water filtration membrane. Dirty water containing large dye molecules
(red blobs) and bacteria (green shapes) flows from the top. The membrane consists of tightly
stacked MXene flakes. The water molecules (small blue dots) weave through the complex,
winding path between the flakes and emerge clean at the bottom, while the red and green
contaminants are trapped on the top surface.

10. Photothermal Cancer Therapy

●​ Placement: Section 4.5 MXenes in Biomedical Applications.
●​ Why: To illustrate the "NIR-triggered" therapy concept.
●​ Prompt:​
A medical illustration inside the body. A cluster of cancer cells (irregular, dark shapes) is
targeted by MXene nanoparticles. A beam of Near-Infrared (NIR) red light penetrates from
outside, hitting the MXenes. The MXenes are glowing orange/red with heat, causing the
surrounding cancer cells to dissolve (ablation), while healthy cells nearby remain unaffected.

From ChatGpt
Figure 1. Evolution of 2D Materials Leading to MXenes

Placement: Section 1.1 The Rise of the “Flatland”​

Purpose: Contextualizes MXenes within the broader 2D materials timeline.

Image prompt:​
“Scientific timeline illustration showing the evolution of 2D materials: graphite → graphene (2004)
→ h-BN → MoS₂ → phosphorene → MXenes (2011). Include atomic-layer schematics, dates, and key
properties (conductivity, hydrophilicity). Clean academic infographic style.”

Figure 2. MAX Phase to MXene Transformation Mechanism

Placement: Section 1.2 Enter MXenes: The New Frontier​

Purpose: Visually explains selective A-layer etching.
Image prompt:​
“Step-by-step schematic showing conversion of Ti₃AlC₂ MAX phase to Ti₃C₂Tₓ MXene via selective
Al etching. Highlight M–X octahedra, removed Al layers, surface terminations (–O, –OH, –F).
High-resolution materials science diagram.”

Figure 3. Structural Comparison: Graphene vs TMDs vs MXenes

Placement: Section 1.3 Why MXene is Superior​

Purpose: Reinforces comparative advantage.

Image prompt:​
“Side-by-side atomic models of graphene, MoS₂, and Ti₃C₂Tₓ MXene showing layer thickness,
bonding, surface terminations, and water interaction. Annotated comparison for conductivity and
hydrophilicity.”

Figure 4. Hydrophilicity and Aqueous Ink Formation of MXenes

Placement: Section 1.3.1 Metallic Conductivity Meets Hydrophilicity​

Purpose: Demonstrates printable electronics advantage.

Image prompt:​
“Visual comparison of MXene flakes dispersing uniformly in water vs graphene aggregation. Include
contact angle illustration, aqueous ink bottle, and printed electronic circuit pattern.”

Figure 5. Volumetric Capacitance Comparison

Placement: Section 1.3.2 Superior Volumetric Capacitance​

Purpose: Emphasizes density-driven energy advantage.

Image prompt:​
“3D bar graph comparing volumetric capacitance: activated carbon (~300 F/cm³), graphene aerogel,
MXene (~1500–2300 F/cm³). Include electrode packing density visualization.”

Figure 6. EMI Shielding Mechanism in MXene Films

Placement: Section 1.3.3 Unmatched EMI Shielding Effectiveness​

Purpose: Explains multiple internal reflection mechanism.

Image prompt:​
“Cross-sectional schematic of layered MXene film showing incident electromagnetic waves
undergoing reflection, absorption, and multiple internal reflections between conductive layers.
Annotated with >90 dB shielding.”

Figure 7. Compositional Tunability of MXenes

Placement: Section 1.3.4 Compositional Tunability​

Purpose: Shows ‘materials-by-design’ capability.

Image prompt:​
“Crystal lattice diagram illustrating MXene compositional tunability by varying M (Ti, V, Mo), X
(C/N), and terminations (O, OH, Cl). Include high-entropy MXene concept visualization.”

Figure 8. Comparison of MXene Synthesis Pathways

Placement: Section 2 Synthesis: From Hazardous to Sustainable​

Purpose: Summarizes evolution of synthesis strategies.

Image prompt:​
“Flowchart comparing MXene synthesis routes: HF etching, in-situ HF (LiF/HCl), molten salt
etching, electrochemical etching, bottom-up CVD. Include safety, scalability, and termination
differences.”

Figure 9. Lewis Acid Molten Salt Etching Mechanism

Placement: Section Molten-Salt and Lewis-Acidic Etching​

Purpose: Highlights HF-free breakthrough.

Image prompt:​
“Reaction schematic showing ZnCl₂ molten salt etching of Ti₃AlC₂: Al → AlCl₃ evaporation,
temporary Ti₃ZnC₂ formation, final Ti₃C₂Cl₂ MXene. Include temperature (550 °C) and redox steps.”

Figure 10. Top-Down vs Bottom-Up MXene Synthesis

Placement: Transition between Top-Down and 2.3 Bottom-Up Approaches​

Purpose: Conceptual clarity.

Image prompt:​
“Conceptual illustration comparing top-down exfoliation of MAX phases vs bottom-up atomic
assembly using CVD and templates. Emphasize defect density, crystallinity, and size control.”
Figure 11. CVD Growth of 2D Mo₂C

Placement: Section 2.3.1 Chemical Vapor Deposition​

Purpose: Explains atomic-scale growth.

Image prompt:​
“CVD reactor schematic showing Mo foil, molten Cu catalyst, CH₄ decomposition, and formation of
ultrathin Mo₂C crystals at 1085 °C. Include diffusion arrows and crystal morphology evolution.”

Figure 12. Application Landscape of MXenes

Placement: Start of 4 Global Applications​

Purpose: High-impact overview figure.

Image prompt:​
“Application map of MXenes showing energy storage, EMI shielding, sensors, catalysis, solar cells,
and biomedical diagnostics. Use icons and performance highlights (conductivity, capacitance,
sensitivity).”