Diamond & Related Materials 144 (2024) 111035

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Diamond & Related Materials

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Influence of graphene nanoplates and titanium diboride particulate on wear

and interfacial bonding properties of sintered aluminium alloy composites
J. Lokesh Kumar a, P. Gurusamy a, *, N. Gayathri b, V. Muthuraman c
a
Department of Mechanical Engineering, Chennai Institute of Technology, Chennai, Tamilnadu, India
b
Department of Mechanical Engineering, VelTech HighTech [Link] [Link] Engineering College, Chennai, Tamilnadu, India
c
Department of Mechanical Engineering, Vels Institute of Science, Technology and Advanced Studies, Chennai, Tamilnadu, India

A R T I C L E I N F O A B S T R A C T

Keywords: Graphene has been considered an appropriate reinforcing filler for aluminium/titanium metal matrix composites
Interface bonding due to its outstanding strength and stiffness and its exceptional thermal and electrical properties. The variable
Graphene nanoplates concentrations of graphene nanoplates (GNPs) was considered in this research, such as 2 %, 4 %, 6 % and 8 %, for
Wear resistance
determining wear properties and interface bonding aluminium alloy composites. The graphene-reinforced Al
Metal matrix composites
7075/10 % TiB2 hybrid nanocomposite samples were produced using ball milling and pressure-less vacuum
sintering process. The wear loss was investigated for all the variable graphene concentration samples with
respect to wear load and sliding distance by pin-on-disk method and optimum concentatrion of GNPs was ob­
tained by design of experimental (DOE) analysis. Further, Field Emission Scanning Electron Microscopy
(FESEM), Elemental mapping, Energy Dispersive X-ray (EDX), and microhardness tests were utilized to analyze
the graphene-reinforced Al 7075/10 % TiB2 hybrid nanocomposites, It was concluded that the wear resistance
and microhardness of Al/10 % TiB2/4 % GNPs increased by 71.3 % and 17.6 %, respectively, compared with
non-hybrid aluminium alloy materials. Moreover, a Transmission Electron Microscope (TEM) has been used to
investigate the interfacial strength of aluminium alloy composites. The wear loss characteristics was also opti­
mized using and central composite design (CCD) of response surface methodology (RSM).

1. Introduction ceramic particles such as graphite (Gr) and SiC to help solve these issues.
It was noted that graphene has lubricating properties, which lead to the
Aluminium alloys have significant properties and important perfor­ decreased porosity with increased Gr content [4]. Since Ali et al.
mance characteristics, such as high strength-to-weight ratio, high revealed its unique two-dimensional carbon nanomaterial nature, gra­
ductility, excellent corrosion resistance, good workability, good thermal phene has attracted a lot of attention. Being stronger than steel and
and electrical conductivity. Aluminium and its alloys are widely used in harder than diamonds, this material also has an amazing Young’s
the aeronautical, electronic, automotive, and aerospace industries. modulus of 1 TPa and high thermal conductivity. These remarkable
Additionally, stronger mechanical characteristics, corrosion resistance, physical and chemical properties make it stand out in the field [5].
wear resistance, and thermal conductivities are required for aluminium Because of these qualities, graphene has been chosen as an efficient
and its alloys in the application. It is insufficient to deal with these issues MMC reinforcement [6].
with composite aluminium reinforced with ceramic fibres and particu­ Gürbüz et al. demonstrated that the graphene, a single form of
lates. To maintain strength and wear resistance, increasing the fracture graphite added to sp-hybridized carbon atoms, was a two-dimensional
toughness of ceramic tool materials is still crucial. Thus, some novel substance. Additionally, graphene considered the desirable material
approaches and materials are required to strengthen aluminium and its due to its favorable tribological characteristics [7]. It was noted that the
alloys [1,2]. Furthermore, the researchers have investigated various increase in graphene content improves mechanical properties and de­
aluminium alloys and their influences on the mechanical properties [3]. creases the elongation as well as electrical properties. Also, the
In particular, aluminium alloy (AA) has lower wear resistance and lower aluminium/Gr alloy matrix exhibited a higher corrosion rate than pure
resilience to high temperatures. Researchers also have added AA to aluminium. The size and agglomeration of the graphene particles play a

* Corresponding author.
E-mail address: gurusamyp@[Link] (P. Gurusamy).

[Link]
Received 21 October 2023; Received in revised form 23 February 2024; Accepted 18 March 2024
Available online 24 March 2024
0925-9635/© 2024 Elsevier B.V. All rights reserved.
J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Table 1 lots of attention for automotive and high-temperature aerospace appli­

Materials specifications of a) Al7075, b) TiB2, c) GNPs. cations due to their appealing qualities, including high stiffness, high
Mechanical properties strength, strong corrosion and low density, and oxidation resistance
[13]. Titanium (Ti) has unique properties such as corrosion resistance,
Property Aluminium Titanium Graphene
(Al) diboride (TiB2) nanoplatelets (GNPs) high specific strength and biocompatible metal over steel. However, PM
Ti components are either undesirable in terms of their mechanical
Young’s modulus 69 ~1000 600–700
(GPa)
characteristics and performance or because of their expensive cost. Also,
Tensile strength 120–570 ~130 300–600 authors have reported that pressure-assisted techniques were utilized to
(MPa) provide good mechanical properties and higher densification of the Ti
Hardness (Vickers) 167–245 10–50 1800–2500 materials [14]. On the other hand, titanium matrix materials’ extensive
Fracture toughness 10–30 ~4 3–5
variety of applications are frequently constrained by their lacking
(MPa√m)
tribological performance. However, to effectively use new forms of high-
performance structural materials, they often need to be both strong and
robust and have good wear resistance. Titanium materials have low
Physical properties
wear resistance, which affects not only how they look on the outside but
Property Aluminium Titanium Graphene also where the cracks start growing and the degree to which quickly they
(Al) diboride (TiB2) nanoplatelets (GNPs)
fail in harsh situations or under complicated loads [15].
Density (g/cm3) 2.70 ~2.25 4.49 Further, authors has investigated on the various concentrations of
Melting point (◦ C) 660.32 ~3700 2980
graphene oxide (GO) reinforced Ti composites, which was fabricated by
Thermal 237–250 ~3000 ~35
conductivity (W/ a high temperature sintering method. It was reported that the increase of
mK) GO into the Ti matrix and temperature was attributed to a decrease in
Electrical 37.7 MS/m ~20,000 S/m Insulator the coefficient of friction [16]. Researchers have investigated the me­
conductivity (S/ chanical properties and interface reactions between nickel-coated gra­
m)
Coefficient of 23.1 ×
phene nanoflakes (Ni-GNFs)/Ti composites. It was concluded that 0.05
2.1 × 10− 6 /◦ C 7.8 × 10− 6 /◦ C
thermal 10− 6 /◦ C wt% GNFs addition with Ti exhibited 30.1 % yield strength enhance­
Specific heat 0.90 J/g◦ C ~2.10 J/g◦ C 0.51 J/g◦ C ment compared with pure Ti [17]. Moreover, hot sintering of titanium
capacity (J/g◦ C) matrix composites reinforced with carbon nanotubes (CNT) and gra­
phene oxide (GO) were shown to increase the yield strength and hard­
ness over pure titanium by 150 % and 74 %, respectively [18]. The
major role after the milling process to control the interfacial bonding of
consistent dispersion of graphene nanoplatelets (GNPs) was mainly
the Al alloy matrix [8]. Ramadan et al. Investigated graphene rein­
attributed to enhancing the mechanical properties of the titanium ma­
forcement in aluminium matrix composites with different contents upto
trix due to titanium carbide (TiC) formed in-situ has a pinning effect
0.8 wt%. It was represented that ball milling is prominently used to
[19]. Hu et al. Noted that graphene added to the copper leads to the
distribute the graphene uniformly with the formation of interlocked
lowest enhancement mechanical properties compared with graphene
microstructure in aluminium matrix composites [9]. Further, the au­
reinforced with Mg, Ti and Ni materials. Also, it was reported that the
thors have discussed how the amounts of graphene oxide (GrO) and
increased amount of graphene improves the hardness of nano­
multilayered graphene (MLG) applied to the silicon nitride ceramic
composites. However, the overdose of graphene has been attributed to a
matrix varied between 5 % and 30 wt%. It was pointed out that 5 wt%
reduction in the hardness strength of materials due to the aggregation of
graphene addition was attributed to higher hardness than 30 wt%
addition in the matrix [10]. Also, it has been pointed out by Cygan et al.
that the physical properties of silicon nitride composite were decreased Table 2
by the addition of 1 % graphene [11]. Researchers have found that Compositions of sintering composite materials (wt%).
graphene plays a major role in the aluminium alloy matrix for grain Symbol Al7075 TiB2 GNPs
refinement and interface bonding with the matrix, which might enhance A 100 – –
the fracture toughness. Furthermore, it was demonstrated that the AT 90 10 –
higher flexural strength and hardness were mostly due to the fine ATG2 88 10 2
ATG4 86 10 4
ceramic granules, high relative density, and stable graphene structures
ATG6 84 10 6
[12]. ATG8 82 10 8
Furthermore, titanium aluminide (TiAl)-based alloys have received

Fig. 1. Schematic diagram of fabrication process of Al/TiB2–GNPs composites using powder metallurgy method.

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 2. a) Ball milling process, b) compaction process, c) wear analysis.

Fig. 3. Sample pictures a) A, b) AT, c) ATG2, d) ATG4, e) ATG6, f) ATG8.

brittleness and electrical conductivity of titanium dioxide ceramic

Table 3 without degrading its microhardness, GNPs can be suggested as an
Parameters of wear test. excellent reinforcement. Also, it was represented that improving elec­
S. Parameter used Value trical and mechanical properties in TiO2/GNP composites revealed
no novel possibilities for reinforced ceramic matrix material in several
1 Temperature & humidity 28 ◦ C, 60–65 % improvements and wide-ranging industrial applications [24].
2 Counterpart material disc EN-31 Steel (Ø 40 mm × 8 mm Further, it was found that graphene is a perfect reinforcement ma­
dimensions thickness) terial in the development of aluminium matrix composites (AMCs)
3 Counterpart hardness 60 HRC
4 Load (N) 10 and 20 N
because of its superior all-around performance. Further, authors have
5 Sliding speed (m/s) 1 m/s noticed that the proportion of graphene and other microstructure
changes brought on by the added graphene significantly impact the
mechanical characteristics, electrical conductivity, tribological proper­
ties, thermal conductivity, and corrosion-resistant of the AMCs [25]. Sun
Table 4 et al. discussed the influence of nano-TiC and graphene reinforcing
Coded level values of parameters used for experimental design.
Al2O3-based ceramic-tool materials. It was found that the fracture
Parameters Ranges and actual values of coded levels toughness, flexural strength, and Vickers hardness can be attained to
− 1.682 − 1 0 1 1.682 their maximum levels using 0.5 vol% graphene with 10 % volume
percent nano-TiC [26]. Wang et al. discussed the grain refinement and
GNPs in % 0 2 4 6 8
Sliding distance (mm) 400 500 600 700 800 grain growth mechanism of Al2O3/WC/TiC/graphene ceramic compos­
Applied load (N) 5 10 15 20 25 ites. The growth of Tungsten carbide (WC) grains was shown to be more
strongly inhibited by graphene than by the growth of Al2O3 grains. The
grain refinements of Al2O3 and WC with Graphene were attributed to the
graphene [20].
pinning effect, intragranular structure and strong interface bonding,
Chen et al. studied the effect of graphene nanoplates (GNPs) in respectively [27]. However, the graphene is not properly dispersed
Al2O3/TiB2 ceramic tool materials. It was noted that including GNPs
during reinforcement in the metal matrix composite materials. Because
might increase the densification and enhance the mechanical charac­ agglomerate of grapheme particles due to its van der Waals forces.
teristics [21]. Also, it was found that uniform dispersion of graphene
Hence, proper ball milling could disperse the particle uniformly and
nanosheet (GNS) significantly restricts the dislocation movement and enhance interface reactions between matrix and reinforcements. How­
unusual grain growth in the Cu matrix. Meanwhile, the increase in GNS
ever, ball milling is expected to create an atomic bond between the
might reduce the mechanical performance of Cu matrix composites [22]. reinforcement and the metal matrix in addition to realizing the homo­
Lv et al. suggested that the research would provide new perspectives for
geneous dispersion of the reinforcement in the matrix [28].
fabricating graphene-based LTCC composite materials that function Furthermore, powder metallurgy technique was prominently used to
effectively [23]. The researchers have noted that the increase of manufacture aluminium nanocomposite samples, significantly

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Table 5
RSM model multilevel factorial design of experiments.
Std Run Coded value Original values Response

A: GNPs B: Sliding distance C: Applied load A: GNPs B: Sliding distance C: Applied load Wear loss
(%) (m) (N) (%) (mm) (N) (gm)

1 9 − 1 − 1 − 1 6 500 10 0.0676
2 7 1 − 1 − 1 2 700 10 0.008
3 3 − 1 1 − 1 6 700 10 0.0511
4 8 1 1 − 1 2 500 20 0.0801
5 17 − 1 − 1 1 6 500 20 0.0613
6 10 1 − 1 1 2 700 20 0.1081
7 14 − 1 1 1 6 700 20 0.1301
8 12 1 1 1 0 600 15 0.2651
9 18 − 1.68179 0 0 8 600 15 0.0648
10 4 1.68179 0 0 4 400 15 0.1292
11 5 0 − 1.68179 0 4 800 15 0.016
12 15 0 1.68179 0 4 600 5 0.1354
13 1 0 0 − 1.68179 4 600 25 0.0315
14 6 0 0 1.68179 4 600 15 0.1816
15 13 0 0 0 4 600 15 0.034
16 11 0 0 0 4 600 15 0.036
17 2 0 0 0 4 600 15 0.035
18 20 0 0 0 4 600 15 0.034
19 16 0 0 0 4 600 15 0.036
20 19 0 0 0 2 500 10 0.035

(2 %, 4 %, 6 % and 8 %) of graphene nanoplates (GNPs) have been used

Table 6
with aluminium composite materials for obtaining desirable mechanical
The density of various samples.
properties and wear resistance. Moreover, the influence of wear load
Sample types (10 N, 20 N and 30 N) and sliding distance (400, 600 and 800) on the
A AT ATG-2 ATG-4 ATG-6 ATG-8 wear loss of Al/TiB2/GNPs was investigated. Further research was car­
Density, g/cm 3
2.622 2.647 2.662 2.669 2.666 2.667
ried out to determine the effects of GNP concentrations on the micro­
hardness of Al7075/10 %TiB2 nanocomposites. The interfacial bonding
has been studied using scanning electron microscopy (SEM) and trans­
improving their microstructural and physicomechanical properties [29]. mission electron microscopy (TEM) analysis. Moreover, the wear loss
Researchers indicating that powder metallurgy (PM) was the prominent has been investigated by design of experiment (DOE) approach on
unique production process of creating materials and components using aluminium composite materials.
powders (metal or ceramic) as the raw material, which were then shaped
into the desired shape and dimensions and followed by sintered at high- 2. Experimental
temperature [30]. The powder metallurgy is green and can supply parts
of small sizes and complex shapes at a low-cost energy-saving technique 2.1. Materials
that, compared to conventional manufacturing, offers better perfor­
mance and greater design freedom, the most utilized technology in The aluminium (7075) materials were purchased from Parshwamani
automobile manufacturing [31]. The density level of a PM material can Metals Mumbai, India, with an average particle size of 80 μm. The
be increased, attributed to improving its qualities. However, while graphene nanoplatelets (15 nm) with purity percentage of 99.9+ % and
keeping the material’s porosity, the component’s performance could be Titanium diboride (TiB2) (3–8 μm) with purity percentage of 99 % were
enhanced by altering the alloying system and applying heat treatments. supplied from Reinste Nano Ventures New Delhi, India. The material
The pores’ sphericity has ensured the quality [32]. Moreover, the PM specification is shown in Table 1.
components have materials with dispersion-strengthening properties
that comprise insoluble nanosize phases [33]. Previous studies have
2.2. Methods
reported that aluminium/titanium matrix composites have significantly
high specific strength. However, it has poor wear resistance and inter­
Samples were prepared using a powder metallurgy process. The
facial bonding in the metal matrix composites, attributed to limiting
schematic diagram (Fig. 1) describes all the processes of producing
their applications. To reduce these limitations, graphene significantly
samples. The sintering process has 3 stages. At first, when the temper­
affects the grain refinement, wear properties and interfacial bonding in
ature rises, the aluminium (Al) phase melts. The molten Al phase
composite materials. However, among all of this research, researchers
gradually soaked the Ti/Gr fillers and filled the pores during the inter­
have focused less on the concentration of graphene nanoplates with
mediate stage. The fillers were gradually encircled by the Al phase in the
respect to interfacial bonding and wear properties. Besides, research
late stage, producing an intricate structure that densified the material
studies are required for titanium diboride (TiB2) reinforcement with
being composited.
various graphene concentrations. It is required to demonstrate how wear
caused the fundamental mechanisms of composites deterioration.
2.2.1. Ball milling
Moreover, the effect of variation of sliding distance on wear properties
Mechanical ball milling is effective at grinding, cold welding and
of metal matrix composites needs to be investigated to find appropriate
frequently employed to create alloys from powders [20]. Additionally,
wear behaviour. Further investigation is required for the manufacture of
graphene nanoplates and TiB2 dispersion in an aluminium metal powder
these nanocomposites using powder metallurgy methods.
matrix enhanced the composite strength. A planetary ball mill
The present investigation aims to enhance the wear resistance and
(FRITSCH, Germany) was used to combine Ti powder, Al powder, and
interfacial bonding of graphene nanoplates (GNPs) reinforced with
graphene platelets for 120 min at a speed of 125 rpm. The re­
Al7075/10 %TiB2 sintered nano composites. The various concentrations
inforcements were evenly distributed throughout the matrix and the

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 4. SEM and EDAX images of a) Al7075, b) graphene nanoplates, c) TiB2.

Fig. 5. Sintered samples of a) elemental analysis (EDAX) of Al + 10 % TiB2 + 4 % Gr, b) XRD analysis for ATG-4 and ATG-8.

strain hardening of the powder particles was initiated in the ambient amount of cold welding that occurred between the matrix and rein­
environment. The weight ratios of the powder combinations varied such forcement powders and between the powders and tungsten balls, stearic
as: Al, Al/10 wt% Ti (AT), Al/10 wt% Ti-2 wt% Gr (ATG2), Al/10 wt% acid was used as a process control agent. Ar gas was used to seal the
Ti-4 wt% Gr (ATG4), Al/10 wt% Ti-6 wt% Gr (ATG6), Al/10 wt% Ti-8 wt chromium steel vial to prevent the oxidation of the aluminium powder.
% Gr (ATG8), which is shown in Table 2. At room temperature (30 ◦ C),
these weighted powders were properly blended. A chromium steel vial is 2.2.2. Compaction and sintering
loaded with a predetermined amount of aluminium matrix and rein­ Circular H-13 steel dies were employed to prepare the composite
forcing powders in a 2:10 powder-to-ball ratio. In order to limit the samples. Zinc stearate and acetone were added to the punch and die’s

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 6. Graphene reinforced Al/TiB2 sintered samples for a) microhardness, b) wear loss vs. Gr content.

preferable for polishing the specimens for precise identification of pores

by SEM and TEM analysis. A field emission scanning electron micro­
scope (FESEM), Carl Zeiss Microscope of Model SIGMA (Carl Zeiss Mi­
croscopy GmbH, Germany), has been used to study the cracked surface
and crack propagation morphology of the sintered samples. A trans­
mission electron microscope (TEM, Talos F200, FEI, USA) was used to
study graphene’s wrapping and interfacial bonding effects on ceramic
grains. Further, Energy dispersive spectroscopy was used to analyze the
element distribution in the composites. TEM preparation of sintered
samples was prominently considered for TEM process. The process be­
gins by mixing 10 drops of G-1 epoxy resin and 1 drop of hardener on
weighing paper, ensuring thorough blending with a toothpick before
adding the composite powder containing aluminium, graphene nano­
particles, and titanium diboride. After mixing, the mixture is aged for a
Fig. 7. Graphene reinforced Al/TiB2 sintered samples for a) wear loss vs
applied load, b) wear loss vs. sliding distance.
night or a few days to eliminate bubbles, then cured either through
gentle heating or at room temperature to form a solid bulk material. This
material is then ground to a thin foil, from which 3 mm diameter TEM
contact surfaces in order to cause the green compacted composite
discs are punched. Subsequently, dimpling is performed to reduce
specimens to eject. A Uniaxial hydraulic pallet press (Hydraulic Press 40
thickness and ensure uniformity across the sample surface. Finally, ion
Tonne) was used to compact the combined particles at 600 MPa pressure
milling is conducted to achieve the required electron transparency for
at room temperature, which was shown in Fig. 2b. These cylindrical
TEM analysis. While this method has shown efficacy with metallic
pellets, which were made for sintering, had dimensions that complied
powders, its applicability to ceramic powders, including the composite
with ASTM standards: the diameter size of 10 mm and the height of 30
in question, may require additional optimization due to material-
mm. Following each compaction, Acetone was used to thoroughly clean
specific characteristics, necessitating preliminary trials and adjust­
the inner die walls and plungers, then zinc stearate was used to ensure
ments before proceeding with TEM sample preparation.
the die assembly operated as intended. Afterwards, green pellets were
sintered after cold compression at 450 ◦ C–470 ◦ C for 1 h under a con­
2.2.4. Design of experiments
stant argon gas flow (flow rate = 1 L/min) in the tube electric furnace.
To investigate the critical parameters to promote the wear loss,
The sintered samples were preserved in the furnace until they reached
design of experiment (DOE) has been used. Twenty experiments were
room temperature. The sintered samples are shown in Fig. 3.
carried out to find the wear loss. In each of the trial investigations, each
experiment was carried out 3 times. It was considered that RSM was
2.2.3. Characterization of composite samples
utilized to determine how variables affected the results. The RSM con­
Shimadzu’s Micro Vickers hardness testing apparatus (model-HMV-
sists of statistical and mathematical models that are used to optimize a
G21ST, Shimadzu Analytical (India) Pvt. Ltd., India) was used to
variety of processes and find the relationship between variables and
determine the hardness of composite materials. A diamond indenter
responses. Central composite design (CCD) is a type of RSM method with
with an applied force of 0.1 kg for a 15-s period was used to evaluate the
a high predictability of response and used for fitting second order model
micro-Vickers hardness of composite materials that had been manufac­
response [46]. Table 4 indicates RSM experimental model, each element
tured in accordance with ASTM E384-17 at 4 separate locations in the
is modified over 3 levels: high (+1), low (1) axial points (labeled as
samples. The sample’s hardness was then determined with standard
±1.682), and center (marked as level 0). ANOVA has prominently used
deviations for better accuracy by the average of 4 measurements. All of
to determine the analytical parameters, and the statistical software
the sintered samples were polished to a grit of 2000 before being cleaned
package design expert 11.0, USA, was utilized for regression analysis of
ultrasonically with acetone and ethanol. The wear test was conducted by
experimental data [34] and to depict the response surface. RSM exper­
pin-on-disk wear test (Ducom Instrumetns Pvt. Ltd., India) for all the
imental data was obtained, which was shown in Table 5.
types of samples using by, shown in Fig. 2c. Table 3 shows the param­
eters considered for wear testing of samples.
The specimens were prepared to investigate the surface morphology
of aluminium hybrid alloy composites. The diamond grit (3 μm) was

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 8. Wear track imges of a)ATG-2, b) ATG-4, c) ATG-6, d) ATG-8.

Table 7
ANOVA model analysis.
Source Sum of squares df Mean square F-value p-Value Comment

Model 0.0785 9 0.0087 18,549.42 <0.0001 Significant SD: 0.0007

A—GNPs 0.0049 1 0.0049 10,481.06 <0.0001 Mean: 0.0770
B—Sliding distance 0.0170 1 0.0170 36,188.54 <0.0001 C.V. %: 0.8909
C—Applied load 0.0273 1 0.0273 57,956.60 <0.0001 R2: 0.9999
AB 0.0039 1 0.0039 8304.83 <0.0001 R2(adj): 0.9999
AC 0.0056 1 0.0056 11,986.03 <0.0001 R2(pred): 0.9999
BC 0.0036 1 0.0036 7696.36 <0.0001 AP: 530.4653
A2 0.0069 1 0.0069 14,666.69 <0.0001
B2 0.0030 1 0.0030 6308.71 <0.0001
C2 0.0092 1 0.0092 19,542.10 <0.0001
Residual 4.705E− 06 10 4.705E− 07
Lack of fit 7.048E− 07 5 1.410E− 07 0.1762 0.9602 Not significant
Pure error 4.000E− 06 5 8.000E− 07
Cor total 0.0785 19

3. Results and discussion attributed to improve the hard reinforcement, while adding graphene
particles with Al alloy matrix, which lead to decrease the diffusion at the
3.1. Determination on surface morphology and density Al/TiB2/graphene interfaces. Consequently, this could be affected the
densification behaviours of the sintered nanocomposites. However, the
Al/TiB2/GNPs composites’ apparent density was calculated using the presence of graphene, with >4 %Gr concentrations, increases the in­
Archimedes method. It depends on various variables, including rein­ tensity of Al-graphene interfaces and, as a result, reduces the obstacles to
forced powder quantity, sintering temperature, time, reinforced powder the Al particle’s diffusion, demonstrating this observed reduction in
amount, distribution of particle sizes, shape, and interparticle friction, densification behaviour of the sample [8]. Also, previous studies was
the tendency for particle agglomeration, and packing density during reported that the high aspect ratio of GNPs increased the glass’s vis­
shaping [7]. Homogeneous dispersion and embedding are restricted cosity, preventing the samples’ densification; therefore, while
after 4 % graphene, as shown in Table 6. This may be caused by the increasing GMPs concentration was attributed to decrease the densities
flakes of graphene’s propensity to agglomerate. The Al and agglomer­ of the sintered sheets [23].
ated graphene leads to high friction between the particles during PM Fig. 4(a–c) indicates the received materials’ surface morphology and
processing. elemental analysis. It was observed in SEM analysis that Aluminium,
Further, it was represented that aluminium particle contact area TiB2 and Graphene were found in the sintered composites, and they are
decreased by agglomerated graphene, which might be increasing the evenly distributed in the composites. Also, In the EDX analysis, the peak
porosity and reducing the hardness values. These results can be indicated respective element was represented in the materials.

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 9. Surface response plots for various parameters.

Fig. 10. Surface response plots of a) diserability and b) predictable.

Additionaaly, similar aluminium peak was introduced on Al 7075 3.2. Elemental chracterization
analysis. Fig. 4b indicated that the additional oxygen peak introduced on
Graphen nanoplates. The elemental analysis has been determined by EDX analysis, illus­
trated in Fig. 5a. The atomic and weight percentage of Al + 10 % TiB2 +

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Table 8 3.3. Microhardness of composite

Results obtained from ANOVA analysis.
Parameters Ranges and actual values of coded levels Results The hardness measurement for all the types of samples was indicated
in Fig. 6a. The Al + 10 % TiB2 + 4 % Gr (ATG4) sample microhardness
− 1.682 − 1 0 1 1.682
was 17.64 % higher than the pure aluminium sintered component. It was
GNPs in % 0 2 4 6 8 5.059921 represented that the increase in graphene was attributed to increased
Sliding distance (mm) 400 500 600 700 800 527.6291
Applied load (N) 5 10 15 20 25 10.45838
hardness. In contrast, the microhardness is significantly decreased with
the increase of graphene above 4 %. This might be due to the nano­
particles impeding the movement of dislocations and uniform distribu­
4 % Gr (ATG4) hybrid composites was indicated. The peaks of Al, B, Ti, C tion of nanoparticles in the alloy materials. Also, high-density TiB2
and O elements are evident from EDX analysis. It was reported that particles were attributed to the increased hardness value of aluminium
graphene and titanium particle reinforcement with aluminium composite materials. In contrast, hardness might be decreased due to an
confirmed in the hybrid composites. An XRD technique is prominently increase in graphene particles [8,35]
used or analysing structure of prepared sintered sample. Fig. 5b shows
that characteristic peaks existed corresponding to aluminium cubic
crystal structure for ATG4 and ATG8 samples. It was revealed that the 3.4. Influence of loading and graphene concentration
phase of pure Al found at 2θ = 38.56◦ , 44.52◦ , 65.16◦ , 78.27◦ and
82.51◦ . It was noted that the increase of graphene contents was attrib­ Fig. 7a depicts how the applied load affects the wear loss of all
uted to decrease the peak intensities and slightly increase their broad­ manufactured samples. It was observed that the wear loss was an
ness [8]. On the other hand, the peak indicated at 2θ = 26.61◦ for increasing trend with an increase in applied load for all aluminium
graphite and 2θ = 34.22◦ , 61.15 and 68.12 for TiB2. Further, silicon was composites. It was shown that the wear loss of hybrid composites in­
indicated at the peak of 57.04◦ . Also, it was noticed that no intermetallic creases gradually as the load increases. This might be due to the sig­
phase was present in TiB2 graphene reinforced aluminium alloy com­ nificant amount of delamination and plastic deformation that happened
posite materials. on the mating surface is the cause of this increase in wear loss [24,35].
Consequently, the fracture toughness was significantly decreased for
non-hybrid (A) and hybrid composites (AT, AG2, AG6 and AGT8),
leading to an increase in wear loss. It could be concluded that ATG4

Fig. 11. SEM analysis of sintered samples a) A, b) AT, c) ATG2, d) ATG4, e) ATG6, f) ATG8.

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 13. FESEM elemental mapping of sintered samples of ATG8.

Fig. 12. FESEM elemental mapping of sintered samples of ATG4. aluminium composite by optical microscopes. Fig. 8(a–d) shows that
wear track images of all the graphene reinforced sintered samples. Fig. 8
composite materials have high wear resistance over other hybrid com­ (a, c, and d) noticed that more ploughing marks at a deeper depth result
posite materials. in larger and more pronounced asperity changes under plastic defor­
Fig. 7b reported the influence of sliding distance on the wear loss of mation, increasing the amount of losses on the sample surface. On the
aluminium hybrid composite materials. It was represented that the wear other hand, the weak spots that initiated the crack and eventually
loss is minimum for the Al + 10 % TiB2 + 4 % Gr hybrid sintered sample resulted in the removal of the upper surface in terms of fake-looking
compared with other hybrid samples. Because of The presence of wear debris are the damaged asperities and some damaged area on
graphite particles, which are released during sliding conditions and the worn surface caused by the formation of a void around the particle
establish a protective turbo-layer between the surfaces of the pin and [36]. Additionally, it was discovered that the asperities can pierce the
counter disc, allows for this improvement. Moreover, wear resistance is sample and create grooves by sliding between two contact surfaces.
increased with the increase of graphene concentration. However, wear However, Fig. 8b showed that less wear loss was observed as a mini­
resistance is reduced after adding 4 % graphene particles in aluminium mum, which could be attributed to graphene particles producing
composite materials, as shown in Fig. 6b, because increasing graphene lubricating films on aluminium alloy composites. Also, it was noticed
concentration might be distributed heterogeneously in aluminium that the absence of deep grooves and slower rate of wear indicate
composite materials. Also, the disbanding might occur by the effect of reduced damage to the area. This could be reduced plastic deformation
large numbers of Gr-Gr contacts [35]. This might lead to introduce pores on the subsurface, which was attributed to preventing subsurface cracks
in AGT6 and AGT8 composite materials. This could be evident from SEM on the sintered sample surfaces [37].
analysis.
In addition, the graphene might be pulled away from the matrix
grains’ interfaces, avoiding direct contact and functioning as a lubricant. 3.5. Design of experiment analysis
Further, the remaining GNPs and the TiC are interlinked to form the
brittle structure because the TiC forms in situ at the interface between The model’s significance is indicated by its F-value of 18,549.42, as
the TiB2 matrix and the GNPs. This may lower the wear rate by mini­ shown in Table 7. The likelihood of such a large F-value, which results
mizing the local depth of penetration of the abrasive particles in the from noise, is only 0.01 %. When the P-value is <0.0500, model terms
composites [15]. are considered significant in this context. Notably, A, B, C, AB, AC, BC,
Wear track images were observed for graphene reinforced A2, B2, and C2 are important terms in this situation. Terms that have a

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J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

Fig. 14. Fractography analysis of sintered samples a) ATG2, b) ATG4, c) ATG6, d) ATG8.

value higher than 0.1000 are regarded as not significant. Reducing the that error in percentage is within the desirable values. The optimum
number of irrelevant terms in a model (apart from those necessary for results were obtained from design of experimental analysis were shown
hierarchy) may improve performance overall. With an F-value of 0.18, in Table 8. It was represented that GNPs, sliding disdance and applied
the lack of fit is negligible in comparison to pure error. Importantly, a load were 5.06 %, 527.6 mm and 10.4 N, respectively. The optimum
significant F-value for Lack of Fit indicates that there is a 96.02 % results were in good agreement form experimental analysis.
probability that the F-value is noise. Therefore, a non-significant lack of
fit is indicative of a well-fitting model.
3.6. Interface bonding analysis
Moreover, Table 7 shows that there is a reasonable agreement when
the marginal difference between the adjusted R2 (0.9999) and the pre­
This study used SEM to investigate the interface bonding of sintered
dicted R2 (0.9999) is <0.2. It is advised that the signal-to-noise ratio, as
and wear-fractured samples. Also, TEM was used to find the particles’
determined by Adeq Precision (AP), be at least 4 [34]. A 530.465 ratio
interface bonding with the aluminium matrix. Interface bonding be­
indicates a positive signal. This model’s strong signal makes it possible
tween the metal matrix and reinforcement is important in load transfer
to explore the design space [34]. The suggested models show a high
and contact, thermal resistance. Fig. 11(a–f) indicated that all the type
degree of consistency when these criteria are compared to the values in
samples. Fig. 10b indicates TiB2 particles are dispersed in the grain
the ANOVA table. Strong agreement between calculated and observed
boundaries and aluminium alloy matrix. Fig. 11(c–f) observed that sig­
results within the experimental range is further highlighted by the
nificant pores and graphene agglomeration has occurred in graphene-
elevated coefficient values. The determination coefficient (R2 > 0.99)
added aluminium alloy matrix materials. This might be due to inho­
and adjusted determination coefficient (R2adj. > 0.99) values,
mogeneous graphene dispersed aluminium alloy matrix materials.
approaching 1, underscore this robust agreement.
Moreover, increased graphene content also contributes to increased
Fig. 9(a–c) indicates the two dimensional fitted response of influence
particle agglomeration and filling of interstitial spaces between Al par­
of variables such as percentage of GNP, sliding velocity and applied wear
ticles during milling, which results in increased porosity contents in the
load on wear loss in the Al/TiB2 composite materials. 2D plots were
sintered nanocomposite, which results in less interface bonding between
developed for determining the optimum solution for reducing the wear
the particles with the aluminium matrix [8]. As seen in Fig. 10(e and f).
loss. It was represented that form Fig. 8a, Wear loss is greatly enhanced
However, Fig. 9d observed that the graphene phase and TiB2 in the ATG-
after 1 coded value for optimum GNPs percentage and 0 coded value for
4 sample have good interface contact with the aluminium matrix, which
optimum sliding distance. The optimal applied wear load has been be­
was attributed to increased interface bonding.
tween 0 and − 0.5 coded values for reading the wear loss. It was
FESEM elemental mapping was utilsed to represent the distribution
demonstrated that optimum sliding distance and wear load could be
of reinforcement elements in the aluminium sintered composites. Fig. 12
<0 coded values. Consequently, it was evident from the perturbation
(a, b) shows the elements such as aluminium, titanium, boron and car­
graph (Fig. 9d). The optimal GNPs percentage could be between o to 1
bon were distributed uniformly in the Al 7075 alloy sintered composites.
coded values. Consequently, The required GNPs percentage could be
Also it can be concluded that TiB2, and graphene exists in the sintered
between 4 and 6 % for decreasing the wear loss in the Al/TiB2 composite
composites. Consequently, wear resistance was significantly increased
materials.
for graphene reinforced aluminium composites. The graphene is uni­
Fig. 10(a, b) noted that predicted a wear loss for sliding distance and
formly dispersed, as shown by the arrows in Fig. 12a, to effectively
GNPs percentage are slight variations with desirable values. It was noted
prevent agglomeration and fully evident high performance in alumi,ium

11
J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

adding more graphene and nano-TiB2. Furthermore, High GNP con­

centration and ease of agglomeration resulted in numerous pores
(shown by red circles) at the grain boundary, which reduced the me­
chanical characteristics. Also, it was indicated that the matrix grains
were firmly anchored and tightly linked to the GNPs, which is advan­
tageous for increasing fracture toughness. [21]. On the other hand, the
high concentration of graphene leads to adverse effects on mechanical
properties due to weakness of interface bonding.
Solid-state diffusion is necessary for the development and expansion
of interparticle bonding. Mechanical characteristics and microstructure
are significantly influenced by diffusion bonding. Therefore, carefully
choosing alloy particles are crucial for regulating grain development and
densification [39]. Additionally, a greater interfacial area between
aluminium particles is provided by the appropriate quantity of evenly
distributed GNPs. At the grain borders, these GNPs perform as two-
dimensional barriers. They minimize dislocation movement during
plastic deformation and limit grain development during sintering [40].
The selective area diffraction (SAED) pattern plays a major role in
determining the layer and lattice parameters of the material being
studied [41]. The SAED pattern seen when looking at graphene nano­
plates is shown in Fig. 15(a–d). The SAED pattern for the ATG-6 and
ATG-8 samples shows graphene-related diffraction spots. Back-folding
of edges, intrinsic rotational stacking faults, or overlapping domains of
graphene layers could be the cause of multiple spots in the pattern [42].
The ATG-2 sample’s SAED pattern shows both spots and rings; the rings
are related to a-C because of the carbon content, while the spots are
diffraction results of graphene nanoplates. Only diffraction rings are
visible in the ATG-4 sample’s SAED pattern, indicating that it is an a-C
film. Interestingly, the presence of monolayer graphene nanoplates is
confirmed by the inner ring of the pattern exhibiting more intense spots
than the outer ring. This observation is consistent with SAED pattern
characteristics [43]. Fig. 15 (e-h) shows the GNPs limit the migration of
dislocations and grain development in the Al matrix. When the GNPs
content in the Al matrix is smaller (4 wt%GNPs), the uniform dispersion
prevents grain development and dislocation movement while providing
strong mechanical characteristics. However, the mechanical character­
istics are reduced as the GNPs concentration rises (6 wt% and 8 wt%
GNPs) due to inadequate interfacial bonding. In particular, Fig. 15f in­
dicates TiB2 and graphene particles were enclosed with aluminium alloy
Fig. 15. TEM analysis of wear fractured samples a) ATG2, b) ATG4, c) ATG6, matrix materials, leading to improved interface bonding of alloy mate­
d) ATG8. rials through a crack pinning mechanism [26]. Consequently, this could
be attributed to preventing the crack growth propagation, leading to the
alloy composites. Further, it was indicated that The ultra-fine grain enhanced fracture toughness of aluminium alloy composite material.
boundary was achieved through the critical role of graphene nanoplates Furthermore, Graphene nanoplates exhibiting folds and wrinkles [44]
(GNPs) reinforcement, which greatly improved the composite’s prop­ are shown in Fig. 15(e–h). These nanoplates’ ability to fold can have a
erties. This phenomenon confirms that aluminium and nanographene detrimental effect on the composite material’s overall strength and
successfully bonded at their interface during the sintering process, a stiffness [38]. Point defects [45] may also be a contributing factor to the
finding that is corroborated by HR-TEM analysis [38]. The sintering graphene layer’s tendency to wrinkle.
process produced a slightly elongated grain boundary, as shown in
Fig. 13a, which effectively closed micropores and addressed other sur­ 4. Conclusion
face defects. The microstructure of the composites exhibits a conspicu­
ous presence of graphene, which is observed to have contributed to a The present investigation was carried out to determine the wear and
refined grain structure as observed in the FESEM elemental mapping. interface bonding behaviour of sintered aluminium metal matrix com­
Fig. 14(a–d) reported the fractography analysis of wear-fractured posites. The ball mill, compaction and sintering processes were carried
sintered samples. The Interface bonding behaviour has been investi­ out to produce six types of aluminium/TiB2/GNPs samples. The micro­
gated for graphene-added aluminium alloy composite samples such as hardness of 4 wt% graphene nanoplates (ATG4) samples were reported
ATG-2, ATG-4, ATG-6 and ATG-8. A strong interface was observed in 4 to be 2.3 %, 2 % and 11 % higher than 6 wt%, 8 wt% and 2 wt% GNPs
% graphene aluminium alloy materials, possibly due to graphene being samples, respectively. Also, it was reported that the wear resistance of 4
fully dispersed in aluminium alloy [28]. On the other hand, A graphene- wt% graphene nanoplates (ATG4) samples were increased by 41.4 %,
induced strong bonding contact led to graphene breaking and bridging 59.6 % and 65.6 % compared to 6 wt%, 8 wt% and 2 wt% GNPs samples,
cracks, whereas a weak bonding interface led to graphene pulling away respectively. This might be because the graphene nanoplates provide
from the crack and guiding it [26]. It was noticed that graphene break more interfacial bonding with titanium and aluminium alloy. Moreover,
might consume more fracture energy, which could enhance the inter­ the wear loss has significantly increased with the increase of wear load
facial strength of aluminium composites. Nano-TiB2 also induced crack and sliding distance. The interface bonding of GNPs and TiB2 particles
deflection and crack branching. Similarly, more pores could be found by aluminium alloy materials was observed by SEM and TEM analysis. It
was reported that strong interface bonding has been achieved by 4 wt%

12
J. Lokesh Kumar et al. Diamond & Related Materials 144 (2024) 111035

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J. Lokesh Kumar: Investigation, Data curation. P. Gurusamy: [17] Y.X. Ge, H.M. Zhang, X.W. Cheng, Q.B. Fan, Z.H. Zhang, X.N. Mu, et al., Interface
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