Engineering Failure Analysis 151 (2023) 107426

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Engineering Failure Analysis

journal homepage: www.elsevier.com/locate/engfailanal

High-temperature dry sliding wear behavior of hybrid aluminum

composite reinforced with ceria and graphene nanoparticles
Dinesh Kumar *, Surjit Angra, Satnam Singh
Department of Mechanical Engineering, National Institute of Technology, Kurukshetra 136119, India

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

Keywords: Wear and friction occur naturally in the mating surfaces of moving machine parts. Overcoming
Hybrid aluminum nanocomposites friction can waste as much as 30 percent of the energy used. The last ten years have seen research
Cerium oxide on optimizing the amount of a particular nanoparticle additive for a certain tribological feature.
Graphene nanoplatelets
The primary goal of this study is to improve tribological materials by combining two types of
Dry sliding wear
Elevated temperature
nanoparticles as reinforced to an aluminum base alloy. Hybrid Aluminum Nanocomposites
(HANCs) made of cerium oxide or ceria nanoparticles (CeO2) and graphene nanoplatelets (GNPs)
reinforced in Al-6061 alloy were subjected to a wear test at temperatures ranging from 250 ◦ C to
1000 ◦ C at different loads ranging from 15 N to 60 N, and the sliding velocity and distance held
constant at 3 m/s and 2000 m, respectively. The nanocomposites were characterized using
Scanning Electron Microscopy (SEM) and Energy-Dispersive Spectroscopy (EDS). The wear rate of
the Al-6061/3CeO2/3GNPs was found to be superior and the same is confirmed by the worn-out
surface and wear debris analysis. At different high temperatures and at various loads; abrasion,
adhesion oxidative, plastic deformation, and delamination wear were observed as wear mecha­
nisms during the dry sliding wear test. However, there were challenges encountered during the
wear test, such as extreme operating conditions, realistic modeling, test standardization, and
multiscale wear analysis.

1. Introduction

Aluminum is a lightweight and highly versatile metal that is widely used in various industries due to its desirable properties. One of
the key advantages of aluminum is its low density, making it lightweight and easy to handle. This characteristic, coupled with its high
strength-to-weight ratio, makes aluminum an excellent choice for applications where weight reduction is crucial, such as in the
aerospace industry for aircraft and spacecraft construction [1]. It’s important to note that the selection of materials for automotive
applications involves considering various factors, including weight, strength, cost, manufacturability, and specific performance re­
quirements for each component. Aluminum and its alloys remain widely used in the automotive industry due to their overall favorable
properties and benefits, but careful consideration is given to selecting the most suitable materials for different applications within a
vehicle [2]. The disadvantage of being less sufficient mechanical and tribological properties in aluminum and its alloys, metals were so
effective in the application of various engines. In addition, the increased rejection rates were caused by high adhesion wear experi­
enced with Al-6061 alloys [3]. The excellent mechanical and tribological properties of aluminum-metal-matrix composites, nowadays,
these composites are being used more and more for various tribological applications. The majority of these applications are found in

* Corresponding author.
E-mail address: [email protected] (D. Kumar).

https://doi.org/10.1016/j.engfailanal.2023.107426
Received 7 May 2023; Received in revised form 17 June 2023; Accepted 22 June 2023
Available online 24 June 2023
1350-6307/© 2023 Elsevier Ltd. All rights reserved.
D. Kumar et al. Engineering Failure Analysis 151 (2023) 107426

the automotive sector [4]. These composite materials hold the edge on the competing bodies due to low densities, higher load-carrying
capacities, and higher strength-to-weight ratios. With these improved mechanical and tribological properties, aluminum matrix
composites are now being investigated in a large number of research projects. This is due to the fact that these composites contain solid
ceramic particles as a strengthening agent, they are a good contender for various applications in Internal Combustion Engines (ICE)
such as pistons, brake rotors, and cylinder liners [5]. The reinforcement has effects on the performance of a composite depending on its
shape, concentration, and distribution of particles. In tribological tests, two bodies are allowed to slide past each other, which results in
complex interactions between the bodies. The cylinder liner, piston ring, and broken rotor are listed as some applications, in which
operating temperatures can be about 0.8% above melting temperature, and aluminum alloys strengthened by first- and second-stage
reinforcing increase the operating temperature range [6]. Out of the above-mentioned applications, wear resistance on cylinder liner-
piston ring application was considered for the current work at real working conditions. The fabricated HANCs specimen (Pin) acts as
cylinder liner materials and the piston ring was considered as steel disc on wear test apparatus (Pin-on-disc). Many researchers have
found that operating parameters, including the temperature, load, and sliding velocity at a local interface, influence how much wear
occurs between the tribe pairs [7–9]. The novel feature of this study is the examination of HANCs based on Al-6061 and reinforced with
higher weight percentages of CeO2 and GNPs (varying from 1 wt% to 3 wt% for each reinforcement). Cerium oxide or graphene
nanoplatelets were used as a sole reinforcement or in combination with SiC [10], Al2O3 [11], B4C [12], CNT [13], TiB2 [14], etc. The
literature that discusses Al-6061 in conjunction with CeO2 and GNPs is very rare, and the highest weight percent of CeO2 and GNPs that
may be employed is just two percent [15–21]. High-temperature tribological tests were performed in this study with different loads.
During testing, a considerable amount of wear occurs, along with plastic deformation and material pull-outs. The wear resistance to
adherence in Aluminum Metal Matrix Composites (AMMCs) may be improved by making sure the nano-cerium oxide and graphene
nanoplatelets are evenly distributed in the matrix phase. Reducing the wear caused by adhesion will eventually reduce the amount of
wear caused by scraping and fusion in produced composites. Due to the fact that tribo-pair contact interfaces are more wear resistance,
which is caused by adding nano-cerium oxide and graphene nanoplatelets as reinforcements, the probability of increment of wear
resistance of HANCs specimen was noted. In the alloying matrix, nano-cerium oxide and graphene nanoplatelets encourage the for­
mation of tribomechanical mixing films during the sliding interface, assisting in the reduction of scoring wear failures.

2. Materials and method

2.1. Raw materials

The commercial Al-6061 alloy was chosen for this study as matrix material with composition as mentioned in Table 1.
Al-6061 alloy consists of superior properties such as; ductility, strength-to-weight ratio (SWR), formability, and wear resistance,
which progressively makes Al-6061 alloy widely applicable to marine manufacturing industries, aerospace sector, automotive segment
and nuclear industries. In order to strengthen the hybrid composite, GNPs and CeO2 were utilized as nano-reinforcements. The density
and melting temperature of the base alloy and the reinforcements are illustrated in Table 2.
The CeO2 and GNPs have a purity level of 99.9% and 99.5%. These nano-reinforcements have a particle size distribution of 25 nm
and 3 nm, respectively.

2.2. Samples preparation

The stir-casting method is used to fabricate the HANCs specimens. The addition of CeO2 and GNPs reinforcements to the base
matrix (Al-6061) was done in 1 wt% to 3 wt%. proportions during stir casting process. Matrix and reinforcing material properties were
provided by the manufacturer i.e., Nano Research Lab Jharkhand (India). Fig. 1 shows schematic representation of the stir die casting
procedure and work plan.
The Muffle furnace preheated the GNPs and CeO₂ reinforcements at 350 ◦ C for 45 min. The drying and gassing off of reinforcing
particles are aided by the preheating process. After chopping the Al-6061 into ingots, about 800 g were introduced to the furnace,
which was already heated to 850 ◦ C. When the metal in the furnace was molten, the reinforcements were added and mixed with a
stirrer that had steel blades. After removing the stirrer, the produced melted material (nanocomposite mixture) was left in the furnace,
which was further kept for 5 min at a constant temperature of 800 ◦ C. The slurry was then put into the casting vessel and then
withdrawn from the mould. This method was used to prepare the four HANCs group of samples representing the various compositions.
In Table 3, we can see the matrix and reinforcement wt.% combinations that was created by following the above-mentioned procedure.

Table 1
Composition of base alloy.
Element Weight Percentage

Silicon 0.51
Magnesium 0.797
Copper 0.219
Iron 0.257
Manganese 0.043
Chromium 0.157
Aluminum balanced

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Table 2
Properties of Al-6061, graphene and cerium oxide nano-reinforcements.
Matrix / Reinforcement Density Melting Point

Al-6061 alloy 2.71 g/cm3 750 ◦ C

GNPs 7.2 g/cm3 2400 ◦ C
CeO2 2.3 g/cm3 3670 ◦ C

Fig. 1. Flow chart of sample preparation and investigation.

3. Experimental setup

3.1. High temperature dry sliding wear test

High-temperature wear was measured on HANCs specimens using the pin-on-disc tribometer (Manufactured by DUCOM In­
struments, Bohemia, United States) as shown in Fig. 2. The wear test specimens were prepared according to ASTM G99-95 as used in
references [22–24]. As samples, 8 mm square pins with a 20 mm height were used in this study. On a pin-on-disc apparatus, wear
specimens are tested using a steel disc with a diameter of 200 mm and a hardness of 68 Rockwell C. Emery sheets with grits ranging
from 220 to 2000 were used to polish the specimen’s surface. Dry wear tests were performed at varying applied load of 15 N-60 N with
an interval of 15 N under elevated temperatures of 250 ◦ C, 500 ◦ C, 750 ◦ C, and 1000 ◦ C. The sliding distance of 2000 m, 3 m/s sliding
velocity, and 30 min as testing time was kept constant for the wear testing. The digital weighing machine manufactured by Gold-tech
HD (India), capable of measuring weight to within 0.001 g, was used to take pre- and post-test measurements. Analyses of the worn
surfaces of the specimens were performed using SEM (JSM-6390LV, JOEL USA).

Table 3
Nomenclature of the stir-casted specimens.
Nomenclature CeO₂ (wt.%) GNPs (wt.%) Al-6061 (wt.%)

K1 0 0 100
K2 1 3 96
K3 3 1 96
K4 3 3 94

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D. Kumar et al. Engineering Failure Analysis 151 (2023) 107426

Fig. 2. High-temperature tribometer (courtesy: BBSBEC Fatehgarh Sahib, Punjab, India): (a) Graphical representation of the apparatus, (b) Pin and
disc apparatus with components, and (c) Pin-on-disc apparatus wear and friction monitor.

Fig. 3. Morphological characteristics of the test samples before the tests (a) K1, (b) K2, (c) K3 and (d) K4.

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4. Results and discussions

4.1. Morphology of prepared HANCs specimens

The materials of stir-casted HANCs samples that contained varied amounts of reinforcing particles were characterized by the use of
SEM examination. Fig. 3 consists of the morphology of specimens K1, K2, K3, and K4 sequentially (a, b, c, and d, respectively).
Fig. 3a displays a scanning electron micrograph of a cast specimen of Al-6061 alloy (K1 specimen). Casing faults led to the for­
mation of certain pores and voids in the K1 specimens that were examined. As can be seen in Fig. 3b, the agglomeration of rein­
forcement particles led to a deterioration of the specimen’s metallographic characteristics. It was found that the particles in the K3
specimen were densely clustered together, and there were some cracks developed, as shown in Fig. 3c.
As can be seen in Fig. 3d, the combination of graphene nanoplatelets and cerium oxide to the Al6061 matrix material produced a
uniform dispersion and smooth texture. As can be observed in Fig. 3d, a fine dendritic structure is present in specimen K4.

4.2. Evaluation of the wear

In addition to the material type, the applied load found to be most relevant, important, and influencing parameter in determining
the weight loss during wear test of the material. Fig. 4 depicts the mean values (with the standard deviations) of the wear rate under the
various loads: 15 N, 30 N, 45 N, and 60 N while operating at the different temperatures: 250 ◦ C, 500 ◦ C, 750 ◦ C, and 1000 ◦ C. The wear
rates of K1, K2, K3, and K4 specimens were measured under varying loads and temperature, the rate of wear was shown to be reduced
when a greater weight percentage of reinforcement particles was present.
Even though specimen K4 had a larger weight percentage of reinforcing particles, the wear rate was shown to rise when it was
subjected to higher loads and temperatures. The hardness after conducting the wear test at elevated temperatures decreases and thus
the wear rate increased at elevated temperatures. Because of the clustering of reinforcing particles and the creation of cracking, which
both contribute to an increase in wear rate, same behavior was observed at different loads for a specimen that was classified as being in
the K2 and K3 category. Because of the even distribution of GNPs and CeO₂ throughout the Al-6061 alloy matrix material, the K4
specimens exhibited the lowest wear rate when compared to the other types of specimens. During the course of the investigation, we
found no cracks.
The Vickers hardness tester (ASTM E-92 standard) was used to measure the K1, K2, K3, and K4 specimens’ hardness (three
repetition on each sample was carried out to analyze the mean hardness value) after wear test at elevated temperature. This was done
in order to validate the wear behaviour that was observed for these specimens. According to the observation, hardness of HANCs
increased due to enhancement in reinforcements, and that it reaches its maximum value (111.7 VHN) for the K4specimen that contains
the highest i.e., six weight proportions of reinforcements (3 wt% of CeO₂ and 3 wt% of GNPs), as shown in Fig. 5.

Fig. 4. Wear rates of the test specimens under different elevated temperatures and loads (a) 15 N, (b) 30 N, (c) 45 N and (d) 60 N.

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Fig. 5. Mean values for hardness on different temperatures.

Fig. 6 represents the reinforcements effect on the SWR as well as the coefficient of friction for specimens K1, K2, K3, and K4. The
SWR is at its highest possible value for specimen K4, which has the highest weight proportions of nano-reinforcements.
In order to determine the grain size DeXel imaging-metallography was utilized, the ASTM E1382-97 standard was referred to this
analysis [25–27]. For the purpose of determining the grain size, a total of sixteen specimens from the stir-casted specimens were cut.
These specimens had a square size of 8 mm and a height of 20 mm. There were four specimens for each designation. In order to
determine the average grain size of each specimen, the line intercepting method was used three times, and then the results were tallied.
Using the micrograph, ten parallel lines were drawn across the image in a horizontal fashion. The number of grain boundaries that
came into contact with the horizontal line was automatically counted, and the grain size was recorded. four replicants were used on
each specimen in order to obtain an accurate reading of the mean grain size with same procedure, which can be seen in Fig. 7.

4.3. Morphology of worn-out surfaces

Fig. 8 presents the microscopic examination of the worn-out surfaces. Figs. 8, 9, 10, and 11 show photo-micrographs of the wear
track of the composites under various loads and temperatures.
Figs. 8, 9, and 10 exhibit stir-cast composite tracks with more debris, whereas Fig. 11 shows a uniform wear track with lesser debris.
K4 specimen shows maximum hardness and strength to weight ratio with improved grain size and interfacial bonding. After wear test,
we can also say that lower wear rate was also observed in the K4 specimen under various loads and temperatures. Keeping in mind the
fact, we have analyzed the worn-out surface behavior of K4 specimen at varying range of load and temperature. Fig. 8 displays the
worn-out surfaces of K4 specimen at 250 ◦ C under load range of (15 N-60 N) in the gap of 15 N. Fig. 8 (a, b, c, and d) represents the

Fig. 6. Reinforcement effect on the Strength-to-Weight Ratio (SWR) as well as the Coefficient of Friction (COF).

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Fig. 7. Representation of measured mean average grain size with standard deviations.

Fig. 8. Morphological characteristics of worn-out surfaces of K4 specimen under 250 ◦ C temperature at different loading conditions.

behavior of worn-out surfaces and wear mechanism was recorded as; 8(a) plowing wear under 15 N; 8(b) cracks, pits and holes were
noted under 30 N; 8(c) smearing wear under 45 N; 8(d) plastic deformation wear mechanism at 60 N during dry sliding wear test under
250 ◦ C.
Previous studies by various investigators found that wear tests with a duration of 5 to 60 min [28–30]; the present study employed a
time duration of 30 min. Before and after the wear test, the pin and disc were cleaned with a paper towel and acetone, following ASTM
G99-95 as indicated in the references [31–33]. Direct contact between the pin and the disc is necessary for an acceptable wear rate
[34], which necessitates cleaning per ASTM G99-95. The worn surfaces of the K4 specimen are shown in Fig. 9 when the temperature is
500 ◦ C and the load is between 15 N and 60 N. Fig. 9 shows the results of a dry sliding wear test conducted at 500 ◦ C on a sample of the
worn surfaces: 9(a) micro-ploughing wear mechanism at 15 N; 9(b) production of delaminated layers at 30 N; 9(c) plastic deformation
at 45 N; and 9(d) fused material and abrasive wear mechanism detected at 60 N. Fig. 10 shows the results of a dry wear test conducted
at 750 ◦ C on a K4 specimen, which revealed (a) fretting wear, (b) delamination, (c) particle peeled-off with flaky pits, and (d) adhesive
fracture wear mechanism. In this study, a brush was used to repeatedly remove the wear debris that had accumulated between the
counterpart and the steel disc throughout the wear test.
Fig. 11 shows the worn-out surface characterization of K4 specimen at 1000 ◦ C and a variety of loads, which were as follows: 11 (a)
layer-like delamination happens at 15 N; 11 (b) shattered particles and groves develop at 30 N; 11 (c) formation of groves and crater
happens at 45 N; 11 (d) fine and shallow grooves occur at 60 N. With a higher density (compared to the as-cast (Al-6061 alloy) sample)

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Fig. 9. Morphological characteristics of worn-out surfaces of K4 specimen under 500 ◦ C temperature at different loading conditions.

Fig. 10. Morphological characteristics of worn-out surfaces of K4 specimen under 750 ◦ C temperature at different loading conditions.

and a stronger interfacial bond between the reinforcing particles and the matrix material, the stir-casted sample has a lower wear
weight loss, which results in enhancement of wear resistance. In addition, harder materials and less weight loss may be expected from
denser stir-casted samples, which exhibit surface deformation resistance during wear testing.

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Fig. 11. Morphological characteristics of worn-out surfaces of K4 specimen under 1000 ◦ C temperature at different loading conditions.

4.4. Morphology of wear debris produced during the wear test

The wear mechanism in the composites were investigated by Scanning Electron Microscopy (SEM) of the wear debris generated
during dry sliding wear test operated at different loading conditions and temperatures.
After completing the wear test, the wear debris were collected, and these debris were then examined using SEM for the K4

Fig. 12. Wear debris of K4 specimen under 250 ◦ C at different loading conditions: (a) 15 N, (b) 30 N, (c) 45 N. and (d) 60 N.

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specimen, which produces at 250 ◦ C, 500 ◦ C, 750 ◦ C, and 1000 ◦ C temperatures. K4 HANCs showed the least wear, which is why the
wear debris of K4 specimen at various weights and temperatures was examined. Fig. 12 showed the wear debris of the Al6061 alloy
under various loads (15 N, 30 N, 45 N, and 60 N) at an increased temperature of 250 ◦ C. Fig. 12 showed the analysed delaminated,
micro-cracked, wear tracks, fused, and agglomerated debris.
Fig. 13 shows the wear debris of the Al6061 alloy by different loads (15 N, 30 N, 45 N, and 60 N) at a high temperature of 500 ◦ C.
This Figure depicts severe wear operating under various loads and at a temperature of 500 ◦ C as oxidised, bigger flake type, plate-like
wear shocks, and huge coarse molten debris were gathered.
The oxidized debris was analyzed through EDS and SEM analysis confirms the development of Al2O3 as illustrated in Fig. 14. The
confirmation of the development of Al2O3 suggests that the aluminum in the debris has reacted with oxygen during the oxidation
process. Aluminum oxide is a common product of aluminum oxidation and forms a protective layer on the surface of aluminum when
exposed to oxygen in the air. This layer provides corrosion resistance and prevents further oxidation of the underlying aluminum.[35].
Fig. 15 represents the wear detritus of Al-6061 alloy under numerous loads (15 N, 30 N, 45 N, and 60 N) under 750 ◦ C elevated
temperature. Corrugated debris, wear tracks on debris, small flaky debris, and small melted debris were noticed at 750 ◦ C when tested
under different loading conditions.
Fig. 16 demonstrates the wear detritus of Al-6061 alloy under various loads (15 N, 30 N, 45 N, and 60 N) under 1000 ◦ C elevated
temperature. Small flaky, fine equiaxed, smeared, and small fractured debris were found when operated at various loads under 1000 ◦ C
temperature during wear test. The less in size and finer in shape, wear debris were observed when compared to wear debris produced
under 250 ◦ C, 500 ◦ C, and 750 ◦ C elevated temperatures, which shows mild wear because of its higher hardness (K4 specimen).

5. Recommendations for preventive measures

General preventive methods to decrease system and component wear and failures:

1. Lubrication reduces friction and wear in mechanical systems. Lubricate moving components to reduce friction and wear.
2. Maintain a regular schedule and examine for wear and failure spots. This permits prompt repairs or replacements before cata­
strophic failures.
3. Choose materials that fit the application and environment. To avoid failures, choose materials based on strength, corrosion
resistance, temperature resistance, and wear resistance.
4. Train operators and maintenance staff to follow suitable practises. This helps detect early wear and failure and take action.
5. Test and monitor regularly to identify wear and deterioration. Ultrasound, vibration analysis, and thermography are non-
destructive testing procedures that may predict problems.

Fig. 13. Wear debris for the K4 specimen under 500 ◦ C at different loading conditions: (a) 15 N, (b) 30 N, (c) 45 N. and (d) 60 N.

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Fig. 14. EDS and SEM analysis of wear debris for K4 specimen produced after wear test.

Fig. 15. Wear debris of K4 specimen under 750 ◦ C at different loading conditions: (a) 15 N, (b) 30 N, (c) 45 N. and (d) 60 N.

6. Conclusions

The wear behavior of HANCs specimens at various loads (15 N, 30 N, 45 N, and 60 N) against a hardened steel disc were obtained
under various temperatures (250 ◦ C, 500 ◦ C, 750 ◦ C, and 1000 ◦ C). The main conclusions are mentioned as follows:

1. The stir-cast nano-composite (K4 specimen) with addition of 3 wt% of each reinforcement, reduces the wear rate (tested on Pin-on-
disc apparatus) compared to base matrix material (Al-6061 alloy) at various loads and temperatures.

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Fig. 16. Wear debris of K4 specimen under 1000 ◦ C at different loading conditions: (a) 15 N, (b) 30 N, (c) 45 N. and (d) 60 N.

2. K4 specimen reinforced with 3 wt% of CeO2 and GNPs showed the lowest wear rate, which was measured at 0.297, 0.41, 0.547, and
0.401 mm3/N-m under various loads of 15 N, 30 N, 45 N, and 60 N, respectively, compared to other specimens at elevated
temperatures.
3. Fine grain size of 6 nm has been observed from metallography analysis in K4 HANCs specimen. The reduction in grain size
improved the hardness and mechanical properties of the specimen, which increases the wear resistance of the K4 specimen.
4. SEM morphology of worn-out surfaces confirms plowing, pits, holes, cracks, smearing, plastic deformation, micro-ploughing,
fretting and delamination as surface defects following the wear test at elevated temperatures.
5. Delaminated, agglomerated, corrugated, oxidized, fused, small plates, small flaky, large flaky, small melted debris were observed
with wear and cracks on debris during SEM analysis of the debris collected after wear test at various loads and temperatures.
6. The abrasion, adhesion, delamination, plastic deformation and oxidative wear mechanism were the caused behind the wear
phenomenon of HANCs specimen at different loads and various elevated temperatures.

Research and development of new materials that can withstand even higher temperatures and exhibit superior wear resistance was
the key focus of the current study. This includes exploring novel alloys, coatings, and composites with enhanced properties for high-
temperature wear applications. Further advancements in surface engineering techniques, such as thermal spray coatings, ion im­
plantation, and surface modification processes, will play a vital role in improving wear resistance and extending the service life of
components operating at high temperatures. Continuous improvement of testing methodologies and equipment will be crucial to
accurately simulate real-world conditions and achieve more representative wear test results, enabling advancements in industries such
as aerospace, energy, automotive, and manufacturing.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to
influence the work reported in this paper.

Data availability

Data will be made available on request.

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Acknowledgments

The authors are thankful to National Institute of Technology Kurukshetra for the material, facilities and guidance to conduct the
research.

Data and code availability

Not applicable.

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