Ionics (2025) 31:7565–7593

[Link]

REVIEW

Recent advances in synthesis and fabrication of ­LiFePO4 cathode

materials: a comprehensive review
Anisa Surya Wijareni1 · Jotti Karunawan2 · Zela Tanlega Ichlas1 · Afriyanti Sumboja3 · Mohammad Zaki Mubarok1

Received: 9 May 2025 / Revised: 31 May 2025 / Accepted: 3 June 2025 / Published online: 13 June 2025
© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2025

Abstract
Lithium iron phosphate ­(LiFePO4/LFP) batteries have great potential to significantly impact the electric vehicle market. These
batteries are synthesized using lithium, iron, and phosphate as precursors. They offer several advantages, such as abundant
availability, low toxicity, high thermal stability, and cost-effectiveness, making them an attractive option for electric vehicle
applications. However, the widespread adoption of LFP batteries faces several challenges, including the limited availability
of suitable precursors and the need for a more optimized fabrication process to ensure consistent and efficient performance.
Therefore, a thorough understanding of the LFP battery fabrication process is essential. This paper aims to comprehensively
understand the synthesis routes and suitability of various iron sources for LFP battery production. These synthesis processes
include various synthesis methods such as hydrothermal, spray pyrolysis, sol-gel, solid-state, dry emulsion, microwave heat-
ing, carbothermal, mechanochemical activation, and coprecipitation. Each method offers specific advantages and disadvan-
tages regarding efficiency, quality of the resulting material, and compatibility with the available iron source. By exploring
and optimizing appropriate fabrication methods, we can overcome the key challenges hindering the development of LFP
batteries, increase their capacity and cycle life, and accelerate their adoption in the global electric vehicle market.

Keywords Cathode materials · Electric vehicles · Electrode · Energy storage · Li-ion battery

Introduction of the main contributors to greenhouse gas emissions. In

addition to efforts to overcome dependence on oil and reduce
In today’s world, the urgent need to address climate change greenhouse gas emissions, the concept of “sustainable trans-
has placed greenhouse gas emission reduction as a top prior- portation through the use of electric vehicles” has become
ity in global efforts, especially in the transportation sector. the focus of global attention today [4]. Electric vehicles are
With transportation being one of the most significant con- an effective solution to reduce greenhouse gas emissions
tributors to emissions, the shift to electric vehicles (EVs) because they do not produce carbon dioxide and carbon
has become a critical focus [1–3]. The transportation indus- monoxide emissions. The performance of electric vehicles is
try plays a significant role, consuming around 25% of total more efficient and has an efficiency three times higher than
energy consumption from fossil fuel combustion, and is one fossil fuel vehicles. In addition to environmental benefits,
electric vehicles also reduce noise [5–7]. Although fossil
fuels remain the dominant energy source in the global road
* Mohammad Zaki Mubarok transport sector, the transformation from fossil fuel vehicles
[Link]@[Link] to electric vehicles has been massive in recent years. In the
1
Department of Metallurgical Engineering, Faculty of Mining coming decade, society is expected to shift toward electric
and Petroleum Engineering, Institut Teknologi Bandung, Jl. vehicles as a more sustainable alternative [8].
Ganesha, 10, Bandung 40132, Indonesia An electric vehicle consists of four main components,
2
Research Centre of Advanced Materials, National Research namely an electric motor, a transmission, a power circuit,
and Innovation Agency, PUSPIPTEK Area, South and a battery [9]. Currently, the battery accounts for about
Tangerang, Banten 15314, Indonesia 40% of the total weight of an electric vehicle and con-
3
Material Science and Engineering Research Group, Faculty tributes to about 50% of its final price [10]. Lithium-ion
of Mechanical and Aerospace Engineering, Institut Teknologi batteries (LIBs) have been used as the power component
Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia

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7566 Ionics (2025) 31:7565–7593

in electric vehicles due to their high specific energy and

sound energy density. Lithium-ion batteries (LIBs) have
been used as the power component in electric vehicles
due to their high specific energy and sound energy den-
sity. The cathode is a critical component in LIBs that
determines electrochemical performance and commer-
cialization. ­L iCoO 2 was the first cathode material used
in 1991 by Sony, a Japan-based multinational company.
Over time, various new materials have emerged, includ-
ing ­LiFePO4 (LFP), which is known to be safe and widely
used since its introduction by Goodenough in 1996 [11].
In 2000, secondary lithium-ion batteries with the types of
­LiMnxNiyCo1-x-yO2 (NMC), LFP, and ­LiNixCoyAl1-x-yO2
(NCA) began to be commercialized [12, 13]. The NMC
and NCA batteries are classified as having a layered struc-
ture, where layers of transition metal oxides form a crys-
tal lattice that facilitates the movement of lithium ions Fig. 1  LFP-based LIB performance
between these layers. This layered structure enables high
energy storage capacity, although it is prone to degradation
if not properly maintained. In contrast, LFP batteries fea- interaction is critical to the performance of LFP as a cathode
ture an olivine crystal structure, which offers advantages in in rechargeable lithium-ion battery [17].
terms of enhanced thermal stability and improved safety. It is crucial to gain a deeper understanding of the over-
In the olivine structure, lithium ions travel through nar- all battery fabrication process to overcome the challenges
rower channels compared to those in the layered structure, faced by LFP batteries and improve their capacity value.
potentially impacting performance, particularly in terms of The fabrication process, which heavily depends on the
cycling stability [14]. Therefore, among the types of bat- source materials used (i.e., lithium, iron, and phosphate),
teries being developed, LIBs, especially those using LFP not only determines the final structure and morphology of
as the cathode material, have attracted significant attention the LFP cathode material but also significantly contributes
because of their potential to revolutionize the EV mar- to its electrochemical characteristics, including its capac-
ket. Currently, the largest producer of LFP batteries is in ity, cycle life, and efficiency. By understanding how each
China, which is 57% of global production, followed by material interacts during this process, we can identify steps
Australia at 17%, Chile at 5%, Brazil at 3%, and the USA to optimize LFP batteries, improve their performance, and
at 3% [15]. In June 2024, it was reported that LFP battery make them more competitive in electric vehicle and energy
installations increased by almost 35% [16]. storage applications.
Figure 1 illustrates the performance characteristics of This article explores the latest advances in LFP cathode
LFP-based LIBs, emphasizing several key aspects that con- materials synthesis, such as hydrothermal, spray pyrolysis,
tribute to their growing popularity in various applications, sol-gel, solid-state, dry emulsion, microwave heating, car-
particularly in electric vehicles (EVs) and energy storage bothermal, mechanochemical activation, and coprecipitation
systems (ESS). LFP offers several advantages over other methods, providing valuable insights into their applications
cathode materials, including lower cost, enhanced safety, across a range of iron sources. Through a comprehensive
excellent thermal stability, and environmental friendliness. review of these methods and recent research findings, this
These benefits have led to its widespread use in electric paper aims to provide insight into the current state of LFP
vehicles and energy storage systems. However, despite cathode materials synthesis and predict their future develop-
these advantages, LFP cathodes face challenges such as a ment directions.
low lithium-ion diffusion rate (approximately 10–14 c­ m2/s)
and low electrical conductivity (around 1­ 0−9 to 1­ 0−10 S/cm).
These limitations hinder performance at high charge and The role of LFP in sustainable energy storage
discharge rates, which ultimately affect the overall electro- systems
chemical efficiency of the battery. The LIBs operate through
intercalation and deintercalation processes, with the oxida- As shown in Fig. 2, in the 1970 s, the concept of lithium
tion reaction producing iron phosphate during charging. Iron batteries began to develop. The discovery of the LFP bat-
phosphate acts as an “anode” during discharge, undergoing tery occurred in 1996 by John B. Goodenough and his team
reduction to re-form lithium iron phosphate. This dynamic at the University of Texas, USA. They discovered that the
Ionics (2025) 31:7565–7593 7567

Fig. 2  Evolution and applications of LFP batteries

olivine structure of LFP allows easy movement of lithium further increased energy capacity and charging efficiency.
ions, providing good thermal stability and high safety. Fol- Currently, LFP batteries are increasingly dominant in the
lowing this discovery, intensive academic research was con- market, especially in China, for electric vehicles and large-
ducted to improve the initially low conductivity of LFP. In scale applications such as grid storage. LFP batteries are
the early 2000 s, significant breakthroughs occurred with gaining global acceptance due to their potential to support
carbon coating techniques and metal doping, which made carbon peaking and carbon neutrality goals in the transporta-
the material more efficient as a battery cathode. In 2003, tion sector, making them a more environmentally friendly
the company A123 Systems began commercializing the LFP option than other battery types. The installed capacity of
battery, and its use has expanded to applications such as in LFP batteries is predicted to reach 60% by 2024, making
electric vehicles (EVs) and portable power tools. them mainstream in the global power battery market. In
Between 2010 and 2020, the use of LFP batteries has addition, many studies have shown that LFP batteries have
been increasing, especially in energy storage systems and lower environmental impacts and better performance in life
electric vehicles, due to their lower cost and longer life cycle assessments, attracting more attention in the global
compared to other technologies such as ­LiCoO2. The use of industry [19].
cobalt in batteries, such as in LCO and NMC, despite offer- The future development of these batteries focuses on
ing high electronic conductivity and good low-temperature increasing energy density, reducing production costs, and
performance, has raised sustainability and ethical issues. tackling safety issues to compete with other technologies.
Limited cobalt reserves and uneven distribution lead to cost To meet these goals, bioinspiration emerges as a promis-
fluctuations and dependence on specific countries. In this ing strategy, offering innovative solutions to address the
context, cobalt-free materials such as LFP have become a inherent limitations of LFP batteries by mimicking natural
more attractive alternative, especially since they do not con- structures that enhance ion conductivity and facilitate faster
tain cobalt and offer better safety and capacity retention. ion transport. Bioinspired designs, such as porous or hier-
LFP has also been widely used in the energy storage and archical structures, can also improve the cycle stability of
electric vehicle (EV) markets, most notably with the intro- LFP, reduce volumetric expansion, and enhance electrode
duction of the “blade battery” by BYD in 2020. Although performance during repeated charge and discharge cycles
the energy density of LFP is still lower than that of NMC, [20]. Alongside these innovations, solid-state battery (SSB)
developments are underway to meet market demand. Reduc- technology has gained increasing attention due to its inher-
ing the use of cobalt in battery technology reduces environ- ent safety advantages, enhanced thermal stability, and the
mental impacts and helps address the growing Co resources potential use of lithium metal anodes for higher energy
crisis [18]. Developments in manufacturing techniques have density. Notably, the combination of lithium iron phosphate
7568 Ionics (2025) 31:7565–7593

(LFP) with solid-state electrolytes represents a particularly ions ­(Fe2+/Fe3+) in the olivine structure of the LFP, accord-
promising avenue. Solid-state LFP systems can effectively ing to the electrochemical reactions that occur through Eqs.
address safety issues typically associated with liquid elec- (1) and (2) [26]:
trolytes, such as flammability and leakage, while preserving
LFP’s key benefits, including structural stability, long cycle Charging ∶ LFP + xLi+ + xe → xFePO4 + (1 + x)LFP (1)
life, and environmental friendliness. This makes solid-state
LFP a strong candidate for safe and durable energy stor- Dicharging ∶ FePO4 + xLi+ + xe → xLFP + (1 − x) FePO4
age, particularly in electric vehicle applications where the (2)
risks of thermal runaway and fire hazards must be minimized Equations (3) and (4) each describe the reaction taking
[21–23]. place at the carbon anode [27, 28]:
Furthermore, carbon coating continues to be developed
to address the limitations of lithium iron phosphate (LFP) Charging ∶ 6C + xLi+ + e → Lix C6 (3)
cathode materials. Different types of carbon sources have
been utilized to enhance the electrochemical performance of Discharging ∶ Lix C6 + xLi+ + xe → 6C (4)
LFP, including organic compounds, polymers, and commer-
cially available carbon materials. Organic sources such as The overall chemical reaction for charging and discharg-
glucose, sucrose, and citric acid can produce homogeneous ing an LFP cell is given in Eq. (5) [29]:
amorphous carbon layers through in situ carbonization. This Charging∕discharging ∶ LFP + 6C ⇄ Li1−x FePO4 + LixC6
results in hard carbon that improves electrical conductivity, (5)
although it may face challenges related to coating uniformity
Schematic diagram illustrating the charging (Fig. 3a) and
and density. Additionally, polymers like starch and polyani-
discharging (Fig. 3b) processes in an LFP battery is depicted
line have been explored as functional carbon coatings [24].
in Fig. 3. In a LIBs, there are three main components that
Commercial carbon materials, such as carbon nanotubes
play a vital role: the anode, the cathode, and the electrolyte.
(CNTs), graphene, and carbon black, offer excellent con-
These three components work together to enable the flow
ductivity but often come with high costs and issues related to
of energy during the battery’s discharge and charge cycles.
poor dispersion. Super P, an affordable commercial carbon,
During the energy discharge process, lithium ions (Li⁺)
has shown effectiveness in forming uniform carbon coatings
move through the electrolyte from the anode to the cathode,
while providing competitive specific capacities and rate per-
while electrons (e⁻) simultaneously flow through an external
formance. Recently, asphalt has been used as a soft carbon
circuit, generating an electrical current that can be used by
precursor capable of creating thin, uniform, and conductive
electronic devices (Fig. 3a). Conversely, during the charge
graphitic carbon layers. This approach allows for the forma-
process, lithium ions (Li⁺) are released from the cathode and
tion of a core-shell architecture that enhances electrochemi-
move to the anode through the electrolyte medium. At the
cal performance, surpassing the performance of hard carbon
same time, electrons (e⁻) flow through an external power
derived from organic sources.
source to the anode, allowing energy to be stored in the bat-
Beyond the type of carbon sources used, the effectiveness
tery cell (Fig. 3b). This process enables continuous cycles of
of the carbon coating is greatly influenced by the synthesis
energy storage and discharge in a lithium-ion battery system,
method used. The chosen synthesis route affects carbon dis-
making it one of the most efficient and widely used energy
tribution, coating thickness, and interfacial interactions with
storage technologies [30].
LFP particles [25]. Therefore, this review will also cover
The crystal structure of ­LiFePO4, as illustrated in Fig. 4,
commonly used LFP synthesis techniques, including hydro-
belongs to the olivine mineral group. This structure consists
thermal synthesis, spray pyrolysis, sol-gel methods, solid-
of an oxygen framework arranged in a distorted hexagonal
state synthesis, dry emulsion methods, microwave heating,
(hcp) pattern, where 1/8 of the tetrahedral voids are filled by
carbothermal reduction, mechanochemical activation, and
phosphorus (P) atoms, and half of the octahedral voids are
co-precipitation technique.
filled by metal atoms, in this case lithium (Li) and iron (Fe).
During the charge and discharge cycles, lithium (Li⁺)
­LiFePO4 crystallizes in the Pnma space group. In its crys-
ions undergo repeated de-intercalation and intercalation
tal structure, the F
­ eO6 octahedra are arranged in the bc plane
processes between the anode and cathode. During charging,
with shared corners, while the linear chains of ­LiO6 octahedra
Li⁺ ions are released from the crystal structure of the lithium
share edges and are parallel to the b axis. These octahedral
iron phosphate (LFP) cathode and move through the elec-
chains are connected by phosphate tetrahedra that share cor-
trolyte toward the anode, usually graphite-based, where Li⁺
ners and edges, forming a solid and stable three-dimensional
ions are intercalated. Conversely, Li⁺ ions are re-intercalated
structure. The advantages of ­LiFePO4 as a cathode material
during discharging into the LFP cathode material. This pro-
have sparked many studies and discussions on its physical
cess is accompanied by changes in the oxidation state of iron
Ionics (2025) 31:7565–7593 7569

Fig. 3  Schematic diagram illustrating the charging (a) and discharging (b) processes in a lithium-ion battery

LFP synthesis method

Hydrothermal

Hydrothermal processing involves heterogeneous chemi-

cal reactions in aqueous solvents or under high tempera-
tures and pressures. This process is used to dissolve and
recrystallize materials that are usually difficult to dissolve
at atmospheric pressure conditions. The main advantages of
this technology lie in its ability to produce materials with
high purity, good crystal symmetry, and relatively efficient
and fast reaction times [34]. Hydrothermal processing is
an effective method for material synthesis because of its
environmentally friendly nature. This method is very suit-
able for the sustainable synthesis of materials ranging from
bulk single crystals to ultra-fine crystals and nanocrystals.
Zero-waste synthesis is becoming the future direction in
materials processing, with particular attention to protect-
ing the environment without increasing the impact of global
warming. Developments in hydrothermal technology have
significantly contributed to materials engineering [35, 36].
The advantage of hydrothermal synthesis is that most of
the materials involved in the reaction can be dissolved by
Fig. 4  The crystal structure of ­LiFePO4 [33]. Reproduced with per- heating the system under a certain pressure until it reaches
mission from Ref. [33]. Copyright 2013 Elsevier
a critical point. Hence, chemical reactions between reactants
can be maximized compared to solid-state processes. The
final product’s size, shape distribution, and crystallinity can
be conditioned and regulated precisely by adjusting param-
eters such as temperature, reaction time, type of solvent,
properties. Therefore, it is necessary to deepen the appropriate surfactant, and precursor. The reaction in hydrothermal syn-
synthesis process from various material sources in examining thesis can be carried out in a simple and easy process when a
the advantages and disadvantages of each process [31, 32]. dopant material is added. However, hydrothermal synthesis
7570 Ionics (2025) 31:7565–7593

also has several disadvantages, such as the need for costly Fig. 6b.1, b.2 was conducted to investigate the changes
autoclaves and safety concerns during the reaction process, in the valence state of Fe in the spent LFP sample and
long reaction times, and limitations in direct observation after the regeneration process (MA-1.2M-100-6h). In the
of the reaction process [37, 38]. Table 1 shows a summary spent LFP, ­Fe2+ was identified at 708.88 eV ­(2p3/2) and
of research on the synthesis of LFP using the hydrothermal 722.66 eV (­ 2p 1/ 2), while F ­ e 3+ was found at 710.81 eV
method. and 724.44 eV. After the regeneration process, the dis-
During hydrothermal synthesis, the fluid dynamics affect appearance of F ­ e 3+ peaks and the shift of the Fe 2­ p 3/ 2
the uniformity of reactant mixing in the autoclave. Insuf- binding energy to a lower value, as shown in Fig. 6b.2,
ficient flow causes a less uniform reaction, while more indicate that hydrothermal treatment with DL-malic acid
intensive mixing accelerates and produces a more uniform effectively reduced F ­ e3+ to F
­ e2+. This transformation was
product. For this reason, reactors with mixers or impellers also accompanied by morphological changes and elemen-
have been developed. Slow heating in a furnace prolongs tal redistribution. Figure 6c.1 shows the cycle performance
the reaction time, but the microwave-assisted hydrothermal of spent LFP and MA-1.2M-100-6h sample at 1C. The
method accelerates it through direct heating, enabling the cycling stability of spent LFP is relatively low. After 200
synthesis of LFP/C/graphene in 10–15 min at 200 °C. This cycles, its specific discharge capacity decreases from 98.9
method also lowers the synthesis temperature and improves to 86.1 mAh ­g−1, with a capacity retention of only 87.1%.
the crystallinity and electrochemical properties of the syn- In contrast, after improvement through the hydrothermal
thesized product, as shown in Fig. 5 [47]. process, the cycling stability of the MA-1.2M-100-6h sam-
Yang et al. [48] synthesized LFP using malic acid (MA) ple is significantly improved, with a Coulombic efficiency
at a Li concentration of 1.2 mol/L, a hydrothermal tem- exceeding 97.2% and capacity retention reaching 98.7%.
perature of 100 °C, and a reaction duration of 6 h (abbrevi- Figure 6c.2 shows the initial specific discharge capacities
ated by MA-1.2M-100-6h). The reaction was performed of the MA-1.2M-100-6h sample of 158.5, 155.3, 149.5,
in a 100 mL hydrothermal reactor with a mixture of 3 g 142.4, 131.8, 108.6, and 70.8 mAh ­g−1 at rates of 0.1, 0.2,
of spent LFP powder, LiOH⋅H2O, and DL-malic acid to 0.5, 1, 2, 5, and 10 C, respectively, close to the commercial
adjust the solution’s pH to 6.0. This process was ended by level. In addition, no significant capacity loss occurred
annealing at 650 °C for 3 h to produce regenerated cathode when the electric charge was reduced from 10 to 0.1C.
material. Figure 6a shows the apparent particle agglom- These results indicate that regeneration via the hydrother-
eration in MA-1.2M-100-6h LFP, which results in large- mal process can effectively improve the crystal structure
sized particles. This is because the stable high-pressure of spent LFP samples and improve L ­ i + diffusion, cycle
hydrothermal reaction process creates a uniform liquid performance, and reaction rate. Figure 6c.3 displays cyclic
phase environment, allowing the growth of LFP crystals voltammetry of the MA-1.2M-100-6h sample that shows
with smaller grain sizes. The XPS analysis presented in a low polarization voltage of 0.26 V, indicating that the

Table 1  Summary of research on the synthesis of LFP using hydrothermal method

Li precursor Fe precursor PO4 precur-sor Additive Cathode Crystal structure Discharge Columbic Ref.
capacity (mAh efficiency
­g−1) (%)

LiOH FeSO4. H3PO4 Ethylene glycol LFP 150 (C/5) - [39]

7H2O
LiOH FeSO4. H3PO4 C19H42BrN LFP Orthorhombic 130 (C/20) - [40]
7H2O
Li(CH3COO) FeSO4. (NH4)2 - LFP Orthorhombic 147 (C/10) 85 [41]
7H2O HPO4
LiOH FeSO4. H3PO4 - LFP Orthorhombic 135 (1C) 58.7 [42]
7H2O
LiOH.H2O FeSO4. H3PO4 Polyethylene glycol LFP Orthorhombic 118 (C/10) 70 [43]
7H2O
LiOH.H2O FeSO4. H3PO4 LFP - 139.5 (C/10) - [44]
7H2O
LiOH FeSO4. H3PO4 Multi-wall carbon nanotubes LFP/C - 160 - [45]
7H2O
LiNO3 FeCl2.4H2O NH4H2 Sucrose LFP/C - 130 (C/10) 86 [46]
PO4
Ionics (2025) 31:7565–7593 7571

Fig. 5  The methods and equipment used for hydrothermal synthesis of LIB’s cathode [47]. Reproduced with permission from Ref. [47]. Copy-
right 2023 Elsevier

MA-1.2M-100-6h sample has more efficient ­Li+ deinterca- across solar cells, electronics, and biomedical devices [53].
lation and higher charge-discharge reversibility [48]. Table 2 summarizes research on the synthesis of LFP using
the spray pyrolysis method.
Spray pyrolysis A schematic diagram of the spray drying device consist-
ing of an ultrasonic atomizer, a tube furnace, a negative ion
Spray pyrolysis is an economical technique for mass-pro- generator, and an air outlet pipe is illustrated in Fig. 7 [59].
ducing products with a high purity, uniform shape, with Lan et al. [59] reported the preparation of L ­ ifePO4 pow-
an average particle size of around 10–20 nm [49]. Spray ders by the ultrasonic spray drying method. The precursor
pyrolysis (SP) is a promising method for creating particles solution was atomized into mist droplets with an average
with adjustable properties such as size, shape, and composi- diameter of 3.9 µm, which were then dried in a high-tem-
tion [50]. Spray pyrolysis systems generally include a reser- perature tube furnace to form solid particles. The negative
voir for holding the precursor solution, a droplet generator, ion generator assisted in depositing the particles on the inner
a reactor, and a collection unit. The precursor solution is surface of the furnace. The furnace temperature was adjusted
atomized and transported by gas into the reactor, where the to 200 °C, 250 °C, 300 °C, and 350 °C to study the effect
droplets undergo evaporation and decomposition, forming of temperature on the memory effect of the synthesized
solid particles. The process of particle formation involves ­LiFePO4. In the initial step, 0.036 mol ­LiH2PO4, 0.036 mol
nucleation and growth of monomer precursors. Electric ­FeCl2.4H2O, 0.00108 mol LiOH.H2O, 15 mL hydrochloric
heating or flames are conventionally used to generate heat acid, and 0.85188 g sucrose were added to 50 mL of deion-
for evaporating solvents and decomposing precursors. Non- ized water, diluted to 200 mL, and stirred until evenly mixed.
traditional heating techniques like microwaves or lasers are This solution was then atomized using an ultrasonic atom-
employed to manipulate particle morphology [51, 52]. Spray izer at a frequency of 1.7 MHz and fed into a tube furnace
pyrolysis has made notable strides in depositing diverse with a gas flow of 5% H ­ 2/Ar at temperatures of 200 °C, 250
materials from precursor solutions while ensuring precise °C, 300 °C, and 350 °C. Before the synthesis process, the air
control over the resulting layers morphology, composition, in the furnace was replaced with 5% ­H2/Ar for 15 min. After
and structural characteristics. This method has become spray drying, the LFP precursor powder was milled for 1 h,
established in producing thin films and finds applications heated to 650 °C at 10 °C/min for 8 h, cooled naturally, and
7572 Ionics (2025) 31:7565–7593

Fig. 6  a SEM micrograph of the synthesized LFP labeled MA-1.2M- cific discharge capacities of the MA-1.2M-100-6h cell; and c.3 cyclic
100-6h; b.1 and b.2 XPS diagrams of the Fe 2p for the spent LFP voltammetry of the MA-1.2M-100-6h cell [48]. Reproduced with per-
and the MA-1.2M-100-6h sample; c.1 cycle performance of the spent mission from Ref. [48]. Copyright 2023 Elsevier
LFP and MA-1.2M-100-6h sample at a rate of 1 C; c.2 the initial spe-

Table 2  Summary of research on the synthesis of LFP using the spray pyrolysis method

Li precursor Fe precursor PO4 precursor Additive Cathode Crystal structure Discharge Columbic Ref.
capacity (mAh efficiency
­g−1)

LiNO3 Fe(NO3)3.9H2O H3PO4 Citric acid and sucrose LFP/C Orthorhombic 155 (1C) 93 [54]
LiNO3 Fe(NO3)3.9H2O H3PO4 Citric acid LFP/C Orthorhombic 150 (1C) 95 [55]
LiNO3 Fe(NO3)3.9H2O H3PO4 Ascorbic acid LFP/C Orthorhombic 150 (C/10) - [56]
Li(HCOO)·H2O FeCl2·4H2O H3PO4 - LFP Orthorhombic 158 (C/10) - [57]
LiNO3 Fe(NO3)3.9H2O H3PO4 Sucrose LFP/C Orthorhombic 118 (1C) 90 [58]
LiOH.H2O FeCl2·4H2O LiH2PO4 Hydrochlo-ric acid and LFP/C Orthorhombic 151 - [59]
sucrose
Li2CO3 Fe2O3 H3PO4 Glucose LFP/C Orthorhombic 142 (1C) 98 [60]
LiNO3 Fe(NO3)3.9H2O H3PO4 - LFP Orthorhombic - - [61]
Li(HCOO)·H2O FeCl2·4H2O H3PO4 Citric acid LFP/C Orthorhombic 140 (C/10) 81 [62]
Li(HCOO)·H2O FeCl2·4H2O H3PO4 Citric acid LFP/C Orthorhombic 137 (C/10) 98 [63]
Ionics (2025) 31:7565–7593 7573

Fig. 7  Schematic illustration of

a custom-designed spray drying
device for LFP synthesis [59].
Reproduced with permission
from Ref. [59]. Copyright 2021
MDPI

collected as the LFP sample. Increasing the spray drying the same, about 0.78 µm. Figure 8b shows the XRD pattern
temperature leads to the increase of Li-Fe dislocations. In consistent with the olivine ­LiFePO4 structure without impu-
the olivine LFP structure, these dislocations can block the rity phases. Rietveld refinement shows a good agreement
migration path of Li ions in the [010] direction and contrib- between the experimental data and the calculated results
ute to the decrease in the specific capacity of LFP. Various for the Pnma L­ iFePO4 phase group at all temperatures. The
methods, such as advanced electron microscopy, neutron specific capacity value of ­LiFePO4 decreases with increas-
or X-ray diffraction, and theoretical calculations have con- ing spray drying temperature, from 161.15 mAh g­ −1 for the
firmed this phenomenon [59]. spray drying temperature of 200 °C to 151 mAh g­ −1 for
Figure 8a shows SEM photographs of the L ­ iFePO4 pre- the spray drying temperature of 350 °C. Figure 8c shows
cursor powders synthesized at various temperatures, in the FTIR spectrum of ­LiFePO4, which features characteris-
which the particles were generally spherical, and the size tic bands at 469, 549, 640, 966, and 1055 c­ m−1. The band
ranged from 0.4 to 1.2 µm. At 300 °C and 350 °C, there are near 463 c­ m−1 is associated with O–P–O and O=P–O bend-
a small number of particles larger than 1.8 µm, while the ing vibrations, while the bands at 547 and 638 ­cm−1 cor-
average particle size at 200 °C, 250 °C, and 300 °C is almost respond to P–O–P stretching modes. The band at 966 ­cm−1

Fig. 8  SEM, XRD, and FTIR analysis results of synthesized LFP at various temperatures using the spray pyrolysis method: a SEM image, b
XRD diffractogram, and (c) FTIR spectra [59]. Reproduced with permission from Ref. [59]. Copyright 2021 MDPI
7574 Ionics (2025) 31:7565–7593

is attributed to P–O–P bending, whereas the band at 1043 regulate the speed of both hydrolysis and condensation reac-
­cm−1 is linked to the vibration of ­(PO4)3− units coordinated tions. These process parameters can be changed to produce
with metal ions. Notably, a blue shift of the 966 ­cm−1 band materials with different microstructures and surface chemi-
occurs with an increase in spray-drying temperature, indicat- cal properties. The subsequent process of “sol” allows the
ing enhanced formation of Li–Fe antisite defects. This find- manufacture of ceramic materials in various forms, such as
ing aligns with the XRD refinement results, which suggest films that can be deposited on substrates via the spin coating
an increase in structural disorder [59]. technique [68]. When the “sol” is poured into the mould, a
wet “gel” will form [66, 69]. ­LiFePO4/C composites can
Sol gel be prepared using the sol-gel method, which allows equal
control of the amount and distribution of L­ iFePO4 particles.
The sol-gel method comprises several stages, beginning with In addition, the carbon coating applied to the composites
the hydrolysis of alkoxides, the formation of a colloidal sus- increases their electronic conductivity, resulting in better-
pension, and the transition of the colloidal suspension into a performance materials. The sol-gel method provides higher
gel through a condensation process [64]. The sol-gel method precision control over particle formation, resulting in a more
is one of the most widely used synthesis techniques for pro- homogeneous ­LiFePO4 distribution and enhanced stability
ducing oxide-based materials and nanoparticles, owing to and efficiency of the composites [68]. Table 3 summarizes
its numerous advantages. This process can be carried out at research on the synthesis of LFP using the sol-gel method.
a short processing time, allowing for the synthesis of mate- A flowsheet of LFP powder synthesis via the sol-gel
rials with high purity and highly homogeneous structures. method using C ­ 6H5FeO7 and L ­ iH2PO4 as precursors accord-
Moreover, this method enables the production of high-qual- ing to Amri et al. (2022) is illustrated in Fig. 9 [78]. The
ity particles with uniform size and facilitates the simulta- sol-gel reaction is highly recommended for the synthesis of
neous synthesis of metal or metal oxide alloys in a single LFP in lithium-ion batteries because it offers several advan-
step by mixing precursors in specific ratios. Additional tages, such as better homogeneity through atomic mixing
advantages include flexibility in forming organic–inorganic and high purity of the product, a more comprehensive com-
hybrid materials, the ability to generate controlled poros- position range, more precise particle size control, and does
ity, and excellent thermal and chemical resistance [65, 66]. not require too stringent process conditions [78].
The presence of numerous hydroxyl groups facilitates the Zhang et al. [68] used ­FeC2O4·H2O, ­NH4H2PO4, and
formation of hydroxyapatite layers, enhancing the activity LiOH·H2O dissolved in deionized water with citric acid as a
of materials compared to those produced by other meth- complexing agent and sucrose as a carbon source to synthe-
ods [65, 67]. Numerous factors impact the hydrolysis and size LFP and LFP/C powder by the sol-gel method. The mix-
condensation reactions in the sol-gel process, including the ture was sonicated for 15 min, then stirred at 80 °C until the
reactivity of metal alkoxides, the ratio of water to alkox- water was evaporated. The resulting gel was heated at 200 °C
ide, solution pH, temperature, solvent properties, and the for 2 h under argon gas flow and then sintered at 750 °C for
incorporation of additives. Catalysts are also introduced to 6 h in an ­H2/Ar atmosphere. L­ iFePO4 was synthesized via a

Table 3  Summary of research on the synthesis of LFP using the sol-gel method
Li precursor Fe precursor PO4 precursor Additive Cathode Crystal structure Discharge Columbic Ref.
capacity (mAh efficiency
­g−1)

Li3PO4 Fe(III)-citrate and H3PO4 Citric acid LFP/C - 150 (C/10) - [70]
­C6H5FeO7
LiOH·H2O FeC2O4·H2O NH4H2PO4 Citric acid LFP/C Orthorhombic 163.5 (C/10) - [68]
Li(CH3COO)·2H2O Fe(NO3)3·9H2O H3PO4 Glycolic acid LFP/C - - - [71]
Li(CH3COO)·2H2O Fe(NO3)3·9H2O NH4H2PO4 Citric acid LFP/C Orthorhombic 138 (C/10) - [72]
LiOH·H2O FeCl2·4H2O NH4H2PO4 Glucose LFP/C Orthorhombic 143.4 (C/10) - [73]
LiNO3· FeC2O4·H2O H3PO4 Citric acid LFP/C - 148 (C/40) - [74]
2H2O
LiNO3· Fe(NO3)3·9H2O NH4H2PO4 Citric acid LFP/C - 152.8 (C/10) - [75]
2H2O
Li2CO3 and FeC2O4·H2O and (NH4)2 C6H10O4 LFP/C Orthorhombic 153 (C/5) - [76]
Li(CH3COO)·2H2O Fe(CH3COO)2 HPO4
Li2CO3 Fe3(PO4)2 NH4H2PO4 Graphite LFP/C Orthorhombic 168.8 (C/10) 98.8 [77]
Ionics (2025) 31:7565–7593 7575

Fig. 9  A flowsheet of LFP powder synthesis via sol-gel method using C
­ 6H5FeO7 and L
­ iH2PO4 as precursors [78]. Reproduced with permission
from Ref. [78]. Copyright 2022 Elsevier

sol-gel reaction with the materials milled and heated under crystal growth [79, 80]. This method is often used to pre-
similar conditions. Figure 10a shows the SEM results of LFP pare single crystals, polycrystalline solids of phosphates,
and LFP/C synthesized by Zhang et al. [68]. LFP particles transition metal arsenates, and monovalent cations. In the
synthesized by the sol-gel method were 1–2 mm in size with crystallization process, a temperature change accompanies
irregular shapes and agglomerates. Meanwhile, LFP/C has a phase change. This process consists of two main stages:
spherical particles with smaller dimensions, around 0.5–1 germination and crystal growth. Germination begins when
mm, and a more even distribution. The particle size and the system is not in a phase equilibrium and involves the
surface morphology affect the electrochemical properties of formation of crystal nuclei in the reaction mixture. Next,
the LFP and LFP/C cells. Smaller LFP/C particles accelerate crystal growth occurs through a series of stages, including
the diffusion of ­Li+, improving the electronic conductivity atomic reorganization, solid surface adsorption, diffusion,
[68]. Figure 10b compares the long-term performance of and placement of atoms in their final positions. The increase
LFP and LFP/C at 0.1C reported by Zhang et al. [68]. The of crystal layer formation on the surface causes a gradual
initial capacities of LFP/C and LFP were about 163.5 and increase in crystal volume [81, 82]. In addition, solid-state
132.8 mAh ­g−1, respectively. After 110 cycles, the capacity is an essential method for synthesizing inorganic materials
of LFP/C decreased by only 8.9%, while LFP decreased by for thermoelectric applications. Solid-state synthesis gener-
26.6%, indicating that LFP/C has a more stable capacity and ally involves heating, cooling, and solidification steps. Under
cycle. Figure 10c shows the cyclic voltammogram, with a certain synthesis conditions, structural or chemical devia-
sharper redox peak of LFP/C and a lower polarization of tions from the desired structure and composition may occur
LFP than that of LFP/C (80 mV compared to 100 mV), indi- [83, 84]. Table 4 summarizes research on the synthesis of
cating faster redox kinetics. The smaller potential interval LFP using the solid-state method.
in LFP/C indicates a more reversible electrochemical reac- Zhi et al. [89] synthesized LFP-1 by mixing nanoparti-
tion. Figure 10 d shows the Nyquist plots, where LFP/C has cles of F
­ ePO4 and L­ i2CO3 in solution, dried at 120 °C, and
a lower charge transfer resistance (Rct), indicating that the sintered at 700 °C for 12 h under nitrogen flow. Secondly,
presence of carbon enhances the material conductivity [68]. LFP-2 was prepared using nanoparticles of ­FePO4, ­Li2CO3,
and starch, with the mixture dispersed in solution. After
Solid‑state synthesis method starch gelatinization at 80 °C, the mixture was dried and
sintered at 700 °C for 12 h to produce L ­ iFePO4 composite.
The solid-state method can produce nanocrystal-sized Figure 11 shows the results of X-ray diffraction, particle
materials and is an approach that continues to be devel- size, scanning electron microscopy, and cell performance
oped. The conditions for forming suitable nanocrystals are analyses of the synthesized LFP by Zhi et al. [89]. Fig-
the absence of impurities, controlled particle shape, even ure 11a shows that the main phase of the LFP-2 sample
size distribution to prevent agglomeration, good stability, synthesized by the enhanced solid-state method was an
and high productivity. This method can prevent or reduce orthorhombic olivine structure (Pnma, JCPDS: 83–2092).
the agglomeration of particles caused by high-temperature However, the F ­ eP4 phase was also found in the LFP-1 sam-
reactions. The solid-state process in nanocrystal forma- ple, possibly due to poor mixing. Figure 11b shows the
tion is divided into three stages: diffusion, nucleation, and difference in particle size distribution of the two samples.
7576 Ionics (2025) 31:7565–7593

Fig. 10  a Comparison of the particle morphology of the synthesized LFP and LFP/C via sol-gel method, b charge-discharge curves, c cyclic vol-
tammogram, and (d) Nyquist plot of LFP and LFP/C cells [68]. Reproduced with permission from Ref. [68]. Copyright 2018 Elsevier

LFP-2 has a narrow distribution curve, indicating a more micrograph of the morphology of the LFP-1 and LFP-
homogeneous particle size, while LFP-1 has a broader 2. LFP-1 shows significant and irregular particles, while
curve due to excessive crystal growth. The particle sizes at LFP-2 had a uniform carbon layer. LFP-1 had an imperfect
D50 were 2.51 µm (LFP-1) and 1.39 µm (LFP-2), respec- layer, causing excessive crystal growth. Figure 11d shows
tively. The use of complex carbon sources in LFP-2 helps the TEM images of two ­LiFePO4/C samples. The LFP-2
suppress particle growth during sintering by producing sample demonstrates that the conductive carbon, produced
a more even carbon layer. Figure 11c compares the SEM by the carbonization of a complex carbon source, is evenly
Ionics (2025) 31:7565–7593 7577

Table 4  Summary of research on the synthesis of LFP using solid-state method

Li precursor Fe precursor PO4 precursor Additive Cathode Crystal structure Discharge Columbic Ref.
capacity (mAh efficiency
­g−1)

Li2CO3 FeC2O4·2H2O NH4H2PO4 - LFP Orthorhombic 85 (C/20) - [85]

Li2CO3 and FeC2O4·2H2O and (NH4)2 - LFP Orthorhombic 126 (C/10) - [76]
Li(CH3COO)·2H2O Fe(CH3COO)2 HPO4
LiF FeC2O4·2H2O NH4H2PO4 - LFP Orthorhombic 151 (C/15) - [86]
Li2CO3 FeSO4·7H2O NH4H2PO4 Na2CO3 LFP/C Orthorhombic 155.4 (C/10) - [87]
Li2CO3 FeC6H5O7.xH2O NH4H2PO4 - LFP/C Orthorhombic 154 (0.17C) 91 [88]
Li2CO3 FePO4 - PEG LFP/C Orthorhombic 155.2 (C/5) - [89]
6000
Li2CO3 FePO4 - Graphite LFP/C - 114 (C/5) - [90]
LiH2PO4 Fe3O4 - Sucrose LFP/C - 145.3 (C/10) - [91]
Li2CO3 FePO4 • ­xH2O H3PO4 Glucose LFP/C - 118 (C/10) 99 [92]

coated on the surface of the L ­ iFePO4 particles and distrib- produce high-performance LFP/C composites via solid-state
uted between the particles, forming a three-dimensional reactions remains an important approach without the need
conductive network that enhances the electronic conduc- for complicated separation processes [88].
tivity of the material. In contrast, the LFP-1 sample is only
partially coated with carbon from PEG6000, leading to Dry emulsion
low conductivity and excessive crystal growth. The con-
ductivity measurements using the two-point method show Dry emulsions are solid formulations that are physically and
values of 2.01 × 1­ 0−2 S/cm for LFP-1 and 1.35 × 1­ 0−1 S/ microbiologically stable. The preparation of dry emulsion
cm for LFP-2. Compared to pure L ­ iFePO4 (~10−9 S/cm), involves drying an oil-in-water emulsion containing a solid
this carbon-coated composite shows an increase in con- carrier, whereby the carrier provides a solid structure to the
ductivity by a factor of ­107–108, contributing to improved emulsion. This process creates a lipid-based formulation
electrochemical performance. Figure 11e shows both cells’ that is soluble both in vivo and in vitro, making it highly
charge/discharge curves at various rated capacities (C). efficient in various applications [93, 94]. Dry emulsions are
The discharge capacity of LFP-1 dropped drastically from formed when the aqueous phase evaporates, causing the oil
155.2 mAh g­ −1 (0.2 C) to 95.7 mAh ­g−1 (5 C) due to the droplets to approach and create a soft solid structure after
large particle size and low crystallization. At a rate of 5 passing a critical concentration [95]. The main advantage
C, LFP-1 also showed a more significant electrochemical of dry emulsions is their ability to produce a solid structure
polarization. Meanwhile, LFP-2 had a higher discharge with good droplet distribution and high stability. However,
capacity of 161.8 mAh g­ −1 (0.2 C) and 124.8 mAh g­ −1 this method has two drawbacks. First, the droplets in the
(5 C) with a stable voltage plateau, indicating a high dis- solid structure can deform under capillary pressure, leading
charge capability due to the increased electronic conduc- to deformation and potential coalescence of the oil droplets.
tivity and smaller particles. Figure 11f shows the cycling Second, the concentration distribution of the droplets can
performance curves at a rated capacity of 2 C. LFP-2 had be uneven, especially near the emulsion-air interface, thus
a better cycling performance, with no capacity decrease slowing down evaporation and affecting drying efficiency
after 110 cycles, while LFP-1 experienced a decrease. The [96, 97]. One of the challenges in this process is controlling
better performance of LFP-2 was attributed to the smaller droplet deformation and ensuring uniform drying throughout
particle size, better conductivity, and higher crystalliza- the sample. Uneven evaporation can lead to the formation of
tion [89]. an undesirable oil phase, so unique methods are needed to
Unlike solution-based synthesis methods, conventional ensure the stability of the final structure.
solid-state reactions allow stepwise heat treatment that Cho and Chung [98] used L ­ iNO 3, Fe(NO 3) 3.9H 2O,
removes organic matter and provides an effective way to and ­(NH4)2HPO4 as starting materials to synthesize LFP
add carbon sources such as sucrose, glucose, or polymer by dry emulsion method. The precursors were calcined
precursors. These carbon sources can directly form a con- under argon at a heating rate of 5 °C per minute at vari-
ductive layer on the surface of the formed crystal particles. ous temperatures. The precursors were calcined at differ-
Since the formation of a surface layer in solid-state reac- ent temperatures (650 °C, 750 °C, and 850 °C), and XRD
tions is simpler than that in solution methods, the strategy to and SEM analyses showed that increasing the calcination
7578 Ionics (2025) 31:7565–7593

Fig. 11  The results of XRD, particle size, SEM, and cell performance profile, f charge-discharge profile, e cycle performance profile. Repro-
analyses of the synthesized LPF by Zhi et al. [89]. a XRD diffrac- duced with permission from Ref. [89]. Copyright 2017 ECS
togram, b PSA, c SEM image, d TEM images, e charge-discharge

temperature resulted in more considerable crystal growth. shown in Fig. 12a, while the SEM micrographs for vari-
Characterization of olivine-type ­LiFePO4 synthesized by ous calcination temperatures are displayed in Fig. 12b.
dry emulsion reported by Cho and Chung [98] is depicted Increasing the calcination temperature increased the crys-
in Fig. 12. The XRD pattern of the synthesized LFP is tal growth. The particle size of the compound calcined at
Ionics (2025) 31:7565–7593 7579

Fig. 12  Characterization of synthesized LFP via dry emulsion method reported by Cho and Chung [98]. a XRD diffractogram, b SEM image, c
cell performance test result. Reproduced with permission from Ref. [98]. Copyright 2004 Elsevier

650 °C was less than 400 nm, while at 850 °C, the size capacity than that at 850 °C; therefore, the temperature of
ranged from 1 to 3 µm. The cycling performance of LFP 750 °C was regarded as the optimum temperature. At this
compounds at different calcination temperatures (650, temperature, with 40% carbon black, the initial discharge
750, and 850 °C) is shown in Fig. 12c, with the experi- capacity of 132.5 mAh g­ −1 increased to 151 mAh g­ −1 at
ments conducted at 3.0–4.0 V and a current density of the 10th cycle due to the increased conductivity. Over-
20 mA/g. The discharge capacity increased until the 10th all, the dry emulsion method offers excellent potential in
cycle before stabilizing. The compound calcined at 650 synthesizing small-particle LFP, with the results showing
°C had the lowest capacity despite its small particle size. stable cycling performance up to 700 cycles, making it a
The compound synthesized at 750 °C showed a higher promising method for energy storage applications [98].
7580 Ionics (2025) 31:7565–7593

Microwave heating Figure 13 illustrates the formation process of LFP/graphene

by precipitation and microwave heating conducted by Liu
Microwave heating has gained recognition across several et al. [103].
sectors in recent decades, including food processing, chemi- The microwave heating accelerates the reaction time and
cal engineering, and healthcare. In contrast to traditional the structure formation, while graphene on the surface of
heating techniques, microwave heating offers advantages LFP particles prevents the grain growth. Graphene helps
such as selective energy absorption, rapid heating rates, to organize the nanoparticles into microspheres and micron
improved energy efficiency, and volumetric heating. How- blocks. When the conductive electrolyte is introduced into
ever, a significant drawback remains in heating’s non-uni- the cathode material, the high surface area of the nanopar-
formity, primarily due to mixed modes within microwave ticles enhances the contact with the electrolyte. The size of
cavities. This issue limits the broader adoption of micro- the nanoparticles shortens the diffusion path of electrons
wave heating in diverse industries [99, 100]. Incorporating a and lithium ions, improves the conductivity, and ensures the
rotating system into microwave heating can enhance the uni- stability of the cathode structure during the intercalation and
formity of temperature distribution throughout the heating deintercalation of lithium ions.
process. Within this rotating system, the sample experiences Figure 14 illustrates SEM micrograph, charge-discharge
intensity variations of the electromagnetic field, ensuring test results for LFP/graphene and LFP/C, cycling perfor-
nearly equal absorption of microwave energy across all sam- mance test for LFP/graphene and LFP/C cells, and electron
ple parts [101]. The rotating system in microwave heating and lithium transfers for LFP/graphene and LFP/C accord-
shows that heating uniformity increases by 18 to 38% com- ing to Liu et al. [103]. As illustrated in Fig. 14a, ­LiFePO4/
pared to conventional microwave heating [102]. graphene forms microspheres that consist of tightly packed
Liu et al. [103] conducted one-step microwave synthe- nanoparticles. The microwave-assisted synthesis, along with
sis of micro/nanoscale ­LiFePO4/graphene cathode by dis- the wrapping of graphene, facilitates the formation of these
solving ­FeSO4·7H2O and ­H3PO4 in a mixture of deionized microspheres by limiting grain growth and promoting self-
water and ethylene glycol. This mixture was then mixed assembly. This unique morphology provides a high surface
with LiOH·H2O solution and GO suspension with a molar area, enhances contact with the electrolyte, and ensures
ratio of Li:Fe:P = 3:1:1. After 3 h of stirring, the solution structural stability during lithium intercalation cycles. Fig-
was evaporated at 80 °C for 12 h. The process was carried ure 14b displays the Raman spectra of L ­ iFePO4/graphene
out with sucrose as a carbon source for other samples. The and ­LiFePO4/C composites. The vibrational modes from
obtained precursors were then compacted into pellets and ­PO43− and the coupled motions of ­Fe2+–PO43− appear in
irradiated with microwaves at 1500 W and 2.45 GHz for 10 the ranges of 945–1058 ­cm−1 (P–O stretching), 587–626
min. The results were LFP/graphene and LFP/C composites. ­cm−1 (O–P–O bending), and below 400 c­ m−1 (lithium cage

Fig. 13  Illustration of the for-

mation process of LFP/graphene
by precipitation and microwave
heating according to Liu et al.
[103]. Reproduced with permis-
sion from Ref. [103]. Copyright
2020 FrontChem
Ionics (2025) 31:7565–7593 7581

Fig. 14  a SEM micrograph of LFP/graphene, b Raman spectra of and LFP/C cells, d electron and lithium transfers for LFP/graphene
LFP/graphene and LFP/C, c.1 charge-discharge test results for LFP/ and LFP/C [103]. Reproduced with permission from Ref. [103]. Cop-
graphene and LFP/C, c.2 cycling performance test for LFP/graphene yright 2020 Frontier in Chemistry

and Fe translations). The pronounced D band (~1310 ­cm−1) graphene has an initial discharge capacity of 166.3 mAh g­ −1
and G band (~1590 c­ m−1) are indicative of carbon struc- at 0.1 C, which drops to 156.1 mAh ­g−1 at 1 C and 132.4
tures, where the D band reflects disorder and the G band mAh ­g−1 at 5 C. At 10 C, the capacity reached 120.9 mAh
corresponds to ­sp2 C–C bonding. The lower ID/IG ratio ­g−1 with a constant voltage above 3 V. For LFP/C, the dis-
in ­LiFePO4/graphene (1.18 compared to 1.43) suggests a charge capacities were 154.8, 133.8, 121.6, 105.9, and 86.4
higher degree of graphitization, which enhances conductiv- mAh ­g−1 at 0.1, 1, 3, 5, and 10 C, respectively. The cycle
ity and improves electrochemical performance. Additionally, performance of LFP/graphene and LFP/C at electrical charge
the strong carbon signals help to suppress high-frequency rates from 0.1 to 10 C is shown in Fig. 14c.2. Although the
peaks from ­LiFePO4. capacity of LFP/graphene decreases with the increasing
The charge and discharge capacity profiles of LFP/gra- electrical charge rate, the capacity retention remains high,
phene and LFP/C at various electrical charge rates (0.1 which were 99.5%, 99.2%, 99.4%, 99.1%, and 97.1% at 0.1,
to 10 C) are shown in Fig. 14c.1. The cells were tested at 1, 3, 5, and 10 C, respectively, after ten cycles. For LFP/C,
room temperature within a voltage range of 2.7–4.2 V. LFP/ the retention capacities were 97.7%, 96.9%, 93.0%, 87.1%,
7582 Ionics (2025) 31:7565–7593

and 79.5%, respectively. This indicates that LFP/graphene of the composite, which plays a vital role in improving the
had a better cycling rate performance and stability due to the electrochemical performance of LFP. Studies have shown
high electrical conductivity of graphene. that the discharge capacity of the cell increases at a specific
The polarization of the LFP/C electrode occurs owing LFP synthesis temperature and decreases if the threshold
to the uneven distribution of carbon, making it difficult for temperature is exceeded [105]. Meanwhile, Wu et al. [106]
electrons to reach all reactive sites for ­Li+ ion intercalation, used an efficient carbon coating strategy to improve the elec-
as shown in Fig. 14d. In contrast, in LFP/graphene, the one- tronic conductivity of LFP, providing higher specific capac-
dimensional mobility of ­Li+ ions allows graphene to help ity and better rate performance in LFP electrodes. Jiang et al.
electrons reach the particles from different directions, reduc- [107] synthesized LFP/C via carbothermal reduction where
ing the polarization. Therefore, the LFP/graphene composite the synthesis was done using the ball milling method with
has higher electrochemical reactivity, with sharper peaks and heat treatment as illustrated in Fig. 15. Precursor materials
minor potential differences [103]. of ­FePO4, ­Li2CO3 (excess 5%), dopants (LiF, Mn, Nb), and
glucose as a carbon source were mixed with ethanol as a
Carbothermal reduction dispersant. The mixture was milled for 12 h at 400 rpm,
filtered, and dried at 80 °C. After milling and sieving, the
The carbothermal method has several advantages, including powder was calcined at 300 °C for 3 h in Ar atmosphere and
high purity, excellent dispersibility, and optimal sinterabil- then heated again at 700 °C for 7 h.
ity. Additionally, the particle size and morphology of the Figure 16a shows the XRD patterns of the as-synthesized
produced materials can be effectively controlled, making it LFP/C, LFP/C-F3, LFP/C-Nb1, and LFP/C-Mn3 matched
an ideal choice for producing consistent quality materials. with JCPDS PDF#40–1499 according to Jiang et al. [107].
The carbothermal method is also widely used in industrial All samples show similar XRD peaks, which can be indexed
production due to its low cost and capability for mass pro- to the orthorhombic crystal system (space group Pnma).
duction, which makes it an efficient and economical option The XRD peaks related to dopant elements did not appear
on a large scale [104]. LFP is known to have low electronic because the amount of dopant elements (F, Mn, Nb, and Mg)
conductivity, which is one of the main obstacles to improv- in the doped LFP samples was minimal. SEM micrographs
ing its performance as a cathode material in batteries. A of the doped LFP/C, LFP/C-F3, LFP/C-Nb1, and LFP/C-
strategy to overcome this problem is to add carbon during Mn3 precursors are shown in Fig. 16b. Doping did not cause
the synthesis process. Wang et al. [105] synthesized LFP/C significant changes in the particle morphology compared to
using ­FePO4 as the raw material and glucose as a conductive the undoped samples. The particle sizes range from 2 to 5
additive and reducing agent. Glucose pyrolysis helps convert µm, with secondary particles formed from the aggregation
­Fe3+ to ­Fe2+, while the remaining carbon from this process of primary particles. The charge-discharge values at 0.2 C
improves the electronic conductivity by controlling the mor- for the 1 st, 25th, 50th, 75th, and 100th cycles are shown in
phology and size of the synthesized LFP powder. As a result, Fig. 16c.1–c.4, as well as rate capability in Fig. 16c.5 and
the formation of carbon increases the surface conductivity cycling performance in Fig. 16c.6.

Fig. 15  Illustration of LFP/C

synthesis via carbothermal
reduction and ball milling
method performed by Jiang
et al. [107] Reproduced with
permission from Ref. [107].
Copyright 2024 MDPI
Ionics (2025) 31:7565–7593 7583

Fig. 16  a XRD patterns of the as-synthesized LFP/C, LFP/C-F3, Mn3, respectively. c.5 Rate capability variation and c.6 cycling per-
LFP/C-Nb1, and LFP/C-Mn3 reported. b SEM micrographs of the formance graphs of the doped LFP/C, LFP/C-F3, LFP/C-Nb1, and
doped LFP/C, LFP/C-F3, LFP/C-Nb1, and LFP/C-Mn3. c.1–c.4 LFP/C-Mn3 [107]. Reproduced with permission from Ref. [107].
Charge-discharge values at 0.2 C for the 1 st, 25th, 50th, 75th, and Copyright 2024 MDPI
100th cycles of the doped LFP/C, LFP/C-F3, LFP/C-Nb1, and LFP/C-

The discharge capacities for LFP/C, LFP/C–F3, LFP/C–Nb 1 has the best cycling performance, with a
LFP/C–Nb1, and LFP/C–Mn3 are 14.2 mAh ­g−1, 10.4 mAh capacity retention of 96.1% after 100 cycles, compared
­g−1, 6.9 mAh g­ −1, and 13.3 mAh g­ −1 at 0.2 C. Regarding rate to LFP/C–F3 (93.3%), LFP/C–Mn3 (90.9%), and LFP/C
performance, LFP/C–F3 shows the highest discharge capac- (90.1%). The XRD results show that F ­ − and ­Nb5+ doping
ity, while LFP/C has a lower capacity than LFP/C–Mn3 at 5 effectively improves the lattice structure, reduces the internal
C and 10 C. At 0.2 C, LFP/C–Nb1 and LFP/C–F3 show the resistance, and enhances the electrical conductivity, contrib-
highest capacities and good electrochemical performance. uting to the high rate and cycling performance [107].
7584 Ionics (2025) 31:7565–7593

Mechanochemical activation Kim et al. [112] used L ­ i 2CO 3, ­F eC 2O 4.2H 2O, and
­NH4H2PO4 as precursor materials for LFP synthesis via the
Mechanochemical activation (MA) is a process where mechanochemical activation (MA) method. The process
intensive grinding induces structural changes, amorphiza- involves high-energy ball milling, pressing the powder into
tion, and enhanced chemical reactivity in materials. MA is pellets, and thermal treatment at temperatures of 500 to 700
typically achieved through milling and is known for its low °C in a nitrogen atmosphere. For the LFP/C variant, acety-
energy consumption and operating temperatures, which lene black powder was added as a carbon source. Adding
helps reduce production costs and makes it environmen- carbon inhibits crystal growth, resulting in smaller particles
tally sustainable [108, 109]. In the MA process, chemical and increasing the material’s conductivity. The XRD dif-
and physical reactions occur, such as breaking down parti- fractogram of LFP synthesized by the MA method at vari-
cles into smaller sizes, phase transformation, new phases, ous temperatures, SEM micrographs, and voltage-specific
and surface formation. The interfacial process in the MA capacity profiles of the LFP cells reported by Kim et al.
process is described through two primary mechanisms: [112] is illustrated in Fig. 17. Based on the XRD diffrac-
adjusting surface characteristics and elevating the free togram in Fig. 17a, it was known that the crystal structure
energy within the surface region. MA enhances the num- of LFP begins to form at temperatures as low as 500 °C,
ber of functional groups by exposing latent groups within although with lower peak intensities compared to the sam-
the crystal structure and initiating targeted phase changes. ples from higher temperatures (600 °C and 700 °C). The
The activation energy necessary for chemical reactions XRD diffraction patterns revealed that all samples have an
is derived from external sources such as heat, light, and orthorhombic structure with the Pnma space group, consist-
electric potential [110, 111]. ent with the desired LFP phase. The diffraction peaks at

Fig. 17  a XRD diffractogram of LFP synthesized by MA method tures. c Voltage-specific capacity profiles of the fabricated LFP cells
at various temperatures reported by Kim et al. [112]. b SEM micro- (Reproduced with permission from Ref. [112]. Copyright 2017 Else-
graphs of the synthesized LFP by MA method at various tempera- vier
Ionics (2025) 31:7565–7593 7585

lower temperatures indicate that crystallization is not opti- Thus, although the difference in sintering temperature did
mal, but significant LFP crystals still form even at 500 °C. not significantly impact the charge and discharge voltage,
More extensive crystallization occurs at 600 °C, indicating the addition of carbon played a vital role in improving the
that this temperature is ideal for the LFP phase formation. electrochemical performance of the cells. The investigation
The temperature of 700 °C, although producing crystals with results show that the sintering temperature significantly
stronger XRD peak intensity, shows an increase in crystal affects the crystal structure, particle size, and morphology
size, which can impair the morphology and electrochemi- of LFP and LFP/C. A temperature of 600 °C was reported to
cal performance of the LFP cells. No impurity peaks were be optimal for obtaining materials with good crystallization,
detected in the XRD spectrum, indicating that the resulting small particle size, and well-distributed morphology [112].
material had a good purity. At higher temperatures, such as 700 °C, undesired particle
Figure 17b provides SEM micrographs of LFP and LFP/C growth occurs, reducing the specific surface area and nega-
particles synthesized at various temperatures. At 500 °C, tively affecting the electrochemical performance of the cells.
the LFP particles show a spherical morphology with nano- The addition of carbon effectively inhibited crystal growth,
sized and slight agglomeration due to the incomplete crys- producing particles with smaller sizes and better morphol-
tallization process at low temperatures. At 600 °C, the LFP ogy, which improved electronic conductivity and electro-
particles were observed to be more well-distributed and chemical stability [112]. A summary of research results on
uniform in size compared to those formed at 500 °C. This the synthesis of LFP through dry emulsion, microwave heat-
indicates that sintering at a temperature of 600 °C is optimal ing, carbothermal, and mechanochemical activation methods
for obtaining denser particles and more appropriate crystals. is given in Table 5.
However, at 700 °C, the particles experienced significant
growth, almost 4–5 times larger than the particles formed Coprecipitation
at 600 °C. This undesirable particle growth was caused by
excessive and rapid crystallization at higher temperatures, In the coprecipitation process, analyte ions precipitate under
which could reduce the specific surface area and worsen the supersaturation conditions by the presence of neutralizing
electrochemical performance of the LFP cells. Meanwhile, or chelating agents. The advantages of this method are the
adding carbon to the LFP/C sample significantly inhibited ease of obtaining pure inorganic reagents and the simplic-
particle growth. The particles produced at 600 °C remained ity of the process. High recovery and significant levels of
small and well-distributed without excessive agglomeration. pre-concentration can be achieved through this technique.
Carbon acts as a crystal growth inhibitor and helps create This method can also produce single metal oxide particles
more stable particles with a smoother morphology. At 700 or other compounds with high recovery. By controlling pro-
°C, despite the increase in particle size, the LFP/C sample cess parameters such as solution pH, temperature, stirring
still had a smaller particle size than pure LFP, which indi- speed, and reactant concentration, it is possible to achieve
cates that carbon is essential in controlling the morphology desired sizes and morphology for the resulting precipitates
and particle size during synthesis. [124]. While coprecipitation can efficiently capture a broad
As seen in the electrochemical performance testing spectrum of analytes, it also comes with disadvantages. The
result of the LFP and LFP electrodes synthesized by the resulting precipitate often contains a mass that is several
MA method in Fig. 17c, the initial discharge capacity meas- orders of magnitude greater than that of the analyte, poten-
urement shows a discharge plateau at around 3.4 V. The tially leading to significant contamination issues. Removal of
discharge capacities of LFP synthesized at 500, 600, and analytes from the precipitate matrix may require additional
700 °C were 74, 82, and 79 mAh ­g−1, respectively, while separation processes. Possible contamination and losses can
those of LFP/C samples prepared at the same temperature also occur in filtration and the precipitates dissolution [125,
were 84, 123, and 97 mAh ­g−1, respectively. This plateau 126]. Table 6 gives a summary of the research results on the
indicates the stability of the electrode during the discharge synthesis of LFP using the coprecipitation method.
process, without significant changes caused by variations in Figure 18 illustrates a synthesis of LFP powder for high-
synthesis temperature or carbon addition. This indicates that power LFP cathodes via coprecipitation method, according
although the sintering temperature can affect the structure to Hsieh et al. [134]. The precursor of F­ ePO4.xH2O was pre-
and morphology of the material, its effect on the discharge pared by the coprecipitation method, in which ­FeSO4.7H2O
voltage remains insignificant. However, adding carbon still was dissolved in deionized water to make a 2.0 M F ­ e2+ solu-
significantly improves electronic conductivity and reduces tion, and then equimolar ­H3PO4 was added. After stirring
the internal resistance in LFP/C materials. Carbon acts as for 0.5 h, concentrated H ­ 2O2 was slowly added. A white
an additional conductor that helps enhance electron transfer precipitate was formed when N ­ H3·2H2O was added as a
during the charge and discharge process, improving the cells’ neutralizing pH to adjust the pH at the range of 1–4. After
long-term cycling performance and fast charging capability. stirring for 0.5 h, the precipitate was separated, washed, and
7586 Ionics (2025) 31:7565–7593

Table 5  A summary of research results on the synthesis of LFP through dry emulsion, microwave heating, carbothermal, and mechanochemical
activation methods
Method Li precursor Fe precursor PO4 precursor Additive Cathode Crystal struc- Discharge Columbic Ref.
ture capacity efficiency
(mAh ­g−1)

Dry emulsion LiNO3 Fe(NO3)3. (NH4)2HPO4 Carbon LFP/C Orthorhombic 140 98 [113]
9H2O
LiNO3 Fe(NO3)3. (NH4)2HPO4 Carbon LFP/C Orthorhombic 120 96 [114]
9H2O
Microwave Li3PO4 Fe3(PO4)2· - Active carbon LFP/C Orthorhombic 161 (C/10) - [115]
heating 8H2O
Li2CO3 FePO4. - Glucose LFP/C Orthorhombic 162 (C/10) - [116]
4H2O
LiOH·H2O FeSO4· H3PO4 Ethylene LFP/C Orthorhombic 166.3 (C/10) 99.5 [103]
7H2O glycol, and
sucrose
LiOH·H2O FePO4. - Glucose LFP/C Orthorhombic 125 (C/10) 83.3 [117]
4H2O
Carbothermal LiOH·H2O FePO4. H3PO4 Glucose LFP/C Orthorhombic 142 (1C) 95.7 [118]
2H2O
Li2CO3 Fe2O3 (NH4)2HPO4 NH4F and LFPF/C Orthorhombic 139.7 (C/10) 95.4 [119]
­C6H10O5
Li2CO3 FePO4 - Glucose LFP/C Orthorhombic 144.1 (1C) - [105]
LiNO3 Fe(NO3)3. NH4H2PO4 Citric acid LFP/C Orthorhombic 142.6 (C/10) - [120]
9H2O
LiAc· (NH4)2Fe H3PO4 C42H70O35 LFP/C Orthorhombic 146 (C/10) - [106]
2H2O (SO4)2·
6H2O
Li2CO3 FeSO4· NH4H2PO4 Carbon LFP/C - 152 (C/10) - [121]
7H2O
Mechanoche- Li2CO3 FeC2O4. NH4H2PO4 C6H8O7 LFP/C Orthorhombic 139 (1C) - [122]
mical 2H2O
activation Li2CO3 LFP NH4H2PO4 V2O5 1-xLFP·xLi3V2 - 142.6 (C/10) 91 [123]
(PO4)3

Table 6  A summary of the research results on the synthesis of LFP using coprecipitation method
Li precursor Fe precursor PO4 precursor Additive Cathode Crystal structure Discharge capac- Columbic Ref.
ity (mAh ­g−1) efficiency

Li2CO3 FePO4 - C6H12O6 LFP/C Orthorhombic 162.8 (C/5) - [127]

Li2CO3 Fe2O3 H3PO4 Glucose LFP/C Orthorhombic 161 (C/10) 98 [60]
Li2CO3 Fe(NH4)2 NH4H2PO4 Glucose LFP/C Orthorhombic 159.6 (C/5) 95.5 [128]
(SO4)2 ·6H2O
LiOH.H2O FeSO4 H3PO4 Glucose LFP/C Orthorhombic 155.9 (C/10) 97.8 [129]
LiOH FeSO4· H3PO4 FeC2O4 LFP/C - 121 (1C) - [130]
7H2O
Li2CO3 FeSO4· NH4H2PO4 C6H12O6⋅H2O LFP/C Orthorhombic 157.79 (C/10) 96.74 [131]
7H2O
Li2CO3 FeSO4· H3PO4 Glucose LFP/C Orthorhombic 161.55 (C/10) 98.63 [132]
7H2O
CH3COO FeSO4· (NH4)H2PO4 - LFP Orthorhombic - - [133]
Li·2H2O 7H2O
Li2CO3 FeSO4· H3PO4 Glucose LFP/C - 162.1 (C/10) 96 [134]
7H2O
Ionics (2025) 31:7565–7593 7587

Fig. 18  Illustration of a synthesis of LFP powder for high-power LFP cathodes via coprecipitation method, according to Hsieh et al. [134].
Reproduced with permission from Ref. [134]. Copyright 2012 Elsevier

dried at 80 °C for 12 h. For the synthesis of C/LFP compos- pyrolysis of glucose under an inert atmosphere during the
ite, ­FePO4·2H2O and ­Li2CO3 were heated at 200 °C for 2 h. calcination process. Figure 19d shows the discharge capac-
Subsequently, the ­FePO4, ­Li2CO3, and glucose mixture was ity for 20 cycles of C/LFP cells whose cathode materials
soaked, dried, and calcined at 650 °C for 12 h in a nitrogen were synthesized at a pH range of 1–4. The C/LFP cathode
atmosphere [134]. synthesized at pH 3 exhibited the highest Coulombic effi-
XRD diffractograms of LFP synthesized by the copre- ciency (~96%) and a symmetric profile, reflecting the high
cipitation method at various pH are shown in Fig. 19a [134]. lithium-ion reaction reversibility. The discharge capacities
Except for LFP at pH 1, the other three samples show the at 0.1 and 5 C were about 162.1 and 119.7 mAh g­ −1, respec-
formation of highly crystalline LFP without any detectable tively. The improved performance was associated with the
impurity phases. The presence of impurities, such as ­Li3PO4, contribution of quasi-spherical nanoparticles and thin car-
may form due to large agglomeration, which requires a bon layers, which enhanced the electronic conductivity and
longer time for phase transformation. All the diffraction lithium-ion diffusion [134].
peaks in the LFP samples match the standard orthorhombic
olivine phase of LFP (JCPDS No. 83–2092), indicating good
crystallinity of the synthesized LFP. Figure 19b shows the Conclusion, challenges, and perspective
FE-SEM images of the C/LFP composites synthesized via
coprecipitation at pH 1, 2, 3, and 4, respectively. Based on This review discusses various synthesis methods for LFP
the observation results, the particle size and morphology of cathode materials, emphasizing cost-effectiveness, environ-
the LFP powders are like those of the ­FePO4 precursor. The mental impact, and particle uniformity. Mechanochemical
LFP powder produced at pH 3 maintains a spherical shape activation and carbothermal methods are highlighted as
with an average size of 200–400 nm, while other LFP sam- some of the most cost-efficient approaches, making them
ples tend to aggregate. This indicates that the F
­ ePO4 precur- suitable for scalable production with relatively low resource
sor plays an essential role in controlling the crystallization input. Additionally, sol-gel and spray pyrolysis methods pro-
and morphology of the synthesized C/LFP composites. vide economic benefits, particularly in terms of simplicity
Figure 19c.1, c.2 presents HR-TEM images of C/LFP and flexibility in operations.
nanoparticles synthesized via the coprecipitation method From an environmental perspective, hydrothermal and
at pH 3, captured at low and high magnifications, respec- coprecipitation methods are advantageous due to their low
tively. The images reveal that the C/LFP crystallites exhibit a energy requirements and minimal waste generation. Further-
quasi-spherical morphology with an average size of approxi- more, when optimized correctly, carbothermal and spray
mately 250 nm, comparable to that of F ­ ePO4 particles. The pyrolysis techniques contribute positively to sustainable
atomic-resolution HR-TEM image clearly displays lattice synthesis. Regarding particle uniformity, sol-gel, copre-
fringes with an interplanar spacing of 0.25 nm, which can cipitation, and microwave heating methods are particularly
be indexed to the (121) crystal plane of the orthorhombic effective, enhancing electrochemical performance through
LFP structure. The selected area electron diffraction (SAED) controlled morphology. While dry emulsion and solid-state
pattern, shown as an inset in Fig. 19c.2, presents distinct methods can also produce homogeneous particles, they may
diffraction spots characteristic of a single-crystalline LFP. have limitations regarding scalability. Selecting the appro-
In addition, a thin carbon coating with a thickness of about priate synthesis method involves balancing these three criti-
3–4 nm is observed on the particle surface, attributed to the cal factors based on specific application requirements.
7588 Ionics (2025) 31:7565–7593

Fig. 19  a XRD diffractogram. b FE-SEM. c.1 low and c.2 high magnification TEM images. d Battery test graph whose cathode synthesis using
co-precipitation method [134]. Reproduced with permission from Ref. [134]. Copyright 2012 Elsevier

Although LFP batteries exhibit lower energy density sity gap through various methods, such as surface treat-
compared to NMC and NCA batteries, they are expected to ments, nanostructuring, and doping with additional ele-
maintain a significant market share owing to their superior ments like manganese (Mn) to enhance performance.
safety, thermal stability, and the abundance of raw materials. Additionally, efforts to increase tap density could further
Innovations in packaging technology and advancements in improve energy density. Innovations in battery archi-
material modification methods offer considerable opportu- tecture, such as cell-to-pack (CTP) technology, are also
nities to improve the overall performance of LFP batteries. helping to enhance the competitiveness of LFP batteries.
Several challenges and future perspectives in the develop- 2. Waste management and environmental impact
ment of LFP technology that need to be addressed:   Some synthesis methods generate chemical waste
that must be carefully managed to prevent environmen-
1. Low energy density in LFP batteries tal damage. Future research should focus on developing
  LFP suffers from a lower energy density compared greener and more sustainable synthesis methods. Addi-
to other cathode technologies. This limitation restricts tionally, the batteries currently in use have a limited
their use, particularly in energy-intensive sectors where cycle life and usage duration. As a result, the amount of
both battery size and weight are crucial factors. Future end-of-life battery waste is expected to increase, high-
research should focus on addressing this energy den- lighting the need for effective processing solutions to
Ionics (2025) 31:7565–7593 7589

mitigate environmental issues. The processing and recy- transport sector: modelling ambitious scenarios. Energy Pol-
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Acknowledgements This study is part of Anisa Surya Wijareni’s 11. Hu J, Huang W, Yang L, Pan F (2020) Structure and performance
(first author) Ph.D. research. Anisa would like to thank the Indone- of the ­LiFePO4 cathode material: from the bulk to the surface.
sia Endowment Fund for Education (LPDP), the Ministry of Finance Nanoscale Royal Soc Chem 15036–15044. [Link]
Republic Indonesia, for granting the scholarship supporting her PhD 1039/​d0nr0​3776a
program. 12. Kim HJ, Krishna TNV, Zeb K, Rajangam V, Muralee Gopi CVV,
Sambasivam, S, Raghavendra KVG, Obaidat IM (2020) A com-
Author contribution Anisa Surya Wijareni: Writing – original draft, prehensive review of Li-ion battery materials and their recycling
Visualization & editing. Jotti Karunawan: Writing – review & edit- techniques. Electronics (Switzerland) 1–44. [Link] oi.​org/​10.​
ing, Validation, Supervision Zela Tanlega Ichlas: Review, Supervision 3390/​elect​ronic​s9071​161
Afriyanti Sumboja: Conceptualization, Review, Validation, Supervi- 13. Kim T, Song W, Son DY, Ono LK, Qi Y (2019) Lithium-Ion bat-
sion Mohammad Zaki Mubarok: Conceptualization, Writing, Review, teries: outlook on present, future, and hybridized technologies. J
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MacLean HL, Posen ID, McKechnie J (2023) Estimating the
Competing interest The authors declare no competing interests. environmental impacts of global lithium-ion battery supply
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