Wear behaviour of SiC-Reinforced Metal Matrix Composites FeCrNiCuMo High Entropy Alloy Processed Through Powder Metallurgy | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Wear behaviour of SiC-Reinforced Metal Matrix Composites FeCrNiCuMo High Entropy Alloy Processed Through Powder Metallurgy Ramprabhu T, Vignesh P, Krishnakumar S, Anand GS, Bhuvaneswari CM, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3415717/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract A series of FeCrNiCuMo high-entropy alloys with different SiC (x = 10 and 15% wt. %) contents were designed, and their microstructure and tribological behaviour were investigated. The tribological behaviour and wear resistance of the composites were evaluated at a range of sliding speeds (20, 30, and 40 ms − 1 ) in a brake dynamometer for brake friction material applications. According to the estimates of volume loss, wear rate, and friction coefficient, the possible wear mechanisms were suggested in all cases. Additionally, SEM/EDS analysis was conducted on the worn surfaces and debris. With the increase in sliding speed, the wear rate increases due to the increased intensity of abrasive wear, oxidation wear, and plastic deformation-assisted wear. The materials possessed excellent braking performance and wear resistance. The values of average coefficient friction under A1 (20ms − 1 ), A2 (30ms − 1 ), and A3 (40ms − 1 ) sliding conditions were 0.23, 0.29, and 0.34, respectively. In comparison to the A3, the A1 exhibits a lower volume wear loss. As the sliding speed change, adhesive wear and abrasive wear become more prevalent, and fatigue wear also occurs. High entropy alloy SiC Microstructure Tribological properties Sliding speed & SEM Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 1. INTRODUCTION The performance of the brake system is largely impacted by the friction material properties, which are extremely difficult to forecast. In order to enhance brake performance and prolong the life of the brakes, the brake materials must have high wear resistance, low brake fade, constant friction, and vibration [ 1 , 2 ]. The microstructure of prepared materials has a significant impact on their mechanical properties, durability, wear resistance, as well as stability in engineering applications [ 3 ]. The demands are high for materials with as steady frictional coefficient, and low wear rates. With high temperature, braking pressure, and initial braking speed, the wear rate accelerates significantly [ 4 , 5 ]. In recent years, the unique compositions, microstructures, and adjustable properties of high-entropy alloys have attracted increasing attention. A compositionally complicated alloy design approach known as high entropy alloys (HEAs) has greatly increased the broad range of alloy systems that are currently accessible as well as yielded alloys with exciting structural and functional characteristics [ 6 ]. Accordingly, HEAs are described as having disordered solid solution structures with a minimum of four or five primary alloying elements in amounts ranging from 5 to 35 at% [ 7 , 8 ]. These alloys can exhibit a remarkable mixture of qualities, including outstanding specific strength, fracture toughness, ductility, and improved mechanical performance at higher temperatures. Also, these alloys provide strong resistance to corrosion, creep, as well as oxidation [ 9 ]. Further, it has become significantly popular among researchers to study the mechanical behavior and application of a high entropy CoCrFeMnNi alloy. There are several ways to prepare HEAs, including arc melting, mechanical alloying, laser cladding, and spark plasma sintering [ 10 ]. Many alloys and combinations that are impossible or difficult to produce using the standard melting and casting procedure can be formed through a special process called mechanical alloying [ 11 ]. According to previous research, an effective method for creating an alloy with homogeneous compositions and microstructures is powder metallurgy, which produces high-strength FeCrNiCuMo alloys with high entropies. Powders can be thoroughly mixed in a short amount of time without the microstructure becoming coarser [ 12 , 13 ]. A fine-grained structure, controlled form, and more homogenous composition may be achieved by the conventional solid mixing method of powder metallurgy, which also includes mechanical alloying and a subsequent consolidation process [ 14 , 15 ]. HEAs are the most intriguing choices for usage as an additive phase in ceramic matrix because of their exceptional characteristics and capacity to form the liquid phase during the sintering process [ 16 ]. The most common alloys utilized in tribology applications are nickel and other high entropy alloys. This is because of the formation of intermediate layers when it comes into contact with other sliding materials. By limiting the contact between the two sliding materials, these intermediary layers inhibit alloy wear. In particular, HEAs like Ti 0.8 CoCrCuFeNi and TiCoCrCuFeNi demonstrated some functional characteristics, including superconductive and superparamagnetic properties [ 17 , 18 ]. Importantly, due to the slow dispersion of the alloying components, these alloys exhibit good thermal stability. In contact sliding applications, such a characteristic is crucial to regulating friction-induced temperature [ 19 ]. However, depending on the operating temperature, the wear behavior and characteristics of intermediate layers fluctuate [ 20 ]. Moreover, to attain adequate mechanical characteristics, additional alloying elements must be added by lattice distortion or precipitation formation to strengthen the HEA. Among different alloys, substances like V, Mo, Cu, Nb, Al, Ti, etc. are capable of altering the crystalline structure, resulting in a considerable increase in strength [ 21 , 22 ]. Recent reports suggest that ceramic particles like SiC, TiC and NbC are being used as reinforcement in HEAs, which has a good impact on their mechanical characteristics and tribological behaviour. In particular, SiC ceramics exhibit a variety of exceptional physical-chemical characteristics, including great hardness and mechanical stability at high temperatures, outstanding thermal conductivity and strong resistance to oxidation and corrosion. The high-power electronics industry, as well as the automotive and aerospace sectors, use this low-density ceramic in a variety of structural ceramics applications [ 23 ]. The current work aims to improve the wear and frictional properties of the brake pad based on FeCrNiCuMo friction material with varying SiC (10 and 15 wt.%). Using a high entropy FeCrNiCuMoSiCx alloy at ambient temperatures, the present experiment aims to examine the sliding wear response. In conclusion, it is recommended that High Entropy Alloy Metal-matrix Composites (HEAMC's) developed in this study be used in aerospace applications. 2. MATERIALS AND METHODS 2.1 Powder Processing For brake pads, FeCrNiCuMo powders with equiatomic compositions (20%) were prepared by mixing powders of Fe, FeCr, Ni, Cu, and Mo with approximately 99% purity and powder characteristics [ 1 ]. The raw powders were mixed for 22h in a planetary ball-milling machine at a speed of 300 rpm, with steel balls of 8 mm in diameter and a mass ratio of 1:1 between the steel balls and the raw powder. Process control was achieved using De-Nature Spirit. As soon as the metallic powders had been mechanically alloyed in the ball mill, SiCx particles of different weights (x = 10 & 15 wt. %) were added without the use of balls, in order to avoid deforming, a mechanical alloying, or deformation, and then allowed to run for 2h. 2.2 Compaction and Sintering Cycle A uniaxial compaction setup with a capacity of 200 tons was used to compact the composite mix into a 3.2 mm thick pad. The hardened steel dies wall and punch surfaces were coated with graphite oil to facilitate easy ejection of the compact. After the compacted pads have been placed in the bell furnace and subjected to a specific temperature for a certain period of time, the compacted pads are then subjected to the load (165 T) and time (25s). Sintering takes place at 1000°C and lasts 210 minutes in this case. The process was carried out in a dry hydrogen atmosphere (Flow rate: 0.012 m 3 /min), and the temperature was raised at a controlled heating rate of 5.55°C per minute during the sintering process. 2.3 Sintered Density and Material Characterization By using Archimedes' principle as a basis for measuring the density of the composites in the compacted and sintered states. A standard metallographic technique was used to prepare samples for microstructure. The composites were studied using optical and scanning electron microscopes equipped with energy-dispersive spectrometers (EDS). SEM was used to measure the surface elemental composition and the topography of worn surfaces and loose wear debris. 2.4 Mechanical Properties In order to determine the hardness of the composites, the Vickers hardness tester was used. Five indentions were taken randomly and the average of them was reported as hardness. The load was 100 g, and dwell time was 15 seconds. Full-scale dynamometer tests were conducted using the main parameters listed in Table 1 . In an ultrasonic bath for 15 minutes, acetone was used to clean the pads and disc to a 1-mm finish. Using rivets, the pads were attached to the holder. Low-carbon alloy steel discs were used as rotors. We conducted 100 braking stops, using the computer-controlled data acquisition system to record information such as torque, friction coefficient, stopping distance, and time. A Digital (XB220A) electronic balance was used to measure the weight loss of pads (precision: 1 mg). The FeCrNiCuMo SiC x=10 is denoted as Mix-A and FeCrNiCuMo SiC x=15 is denoted as Mix-B. Table 1 Brake testing parameters Test Sliding speed (m/s) Brake energy absorbed by 2 pads (kJ) Rotor disc (rpm) Disc radius (mm) Brake load (N) Flywheel mass moment of inertia (Nms 2 ) A1 20 20.8 382 250 980 30.87 A2 30 55.6 573 A3 40 83.3 764 3. RESULTS AND DISCUSSION 3.1 Metallurgical Evaluation According to the optical image of FeCrNiCuMoSiC x (x = 10 & 15wt%) shown in Fig. 1 (a & b), the system is characterized by three distinct layers namely the friction material, the intermediate transition layer, and the steel backing plate. From Fig. 1 (a & c), the SiC is stable in the microstructure for Mix A. The SiC distribution in the matrix is uniform. The bonding appears to be strong and free from defects such as delamination, cracks, or interfacial products. In addition, it also enhanced the dimensional stability of the brake pad. There are no traces of defects, such as cracks, pores, or undesirable interfacial products, in the composite's bond with Ni-plated steel, as shown in Fig. 1 (a). The microstructure of the steel sheet is dominated by the ferrite phase, with some pearlite. The brake pads developed are not a homogenous material in Fig. 1 (b & d). The particle size of each element is not uniform in size and the distribution of the element is not well dispersed in the matrix. The Mix B materials towards either side of the interface were entirely different, crack, and de-bonding occurred frequently during actual applications. In order to overcome the poor joint, future optimization should be carried out in powder processing/ sintering for better usage of Mix-B. As for this paper Mix-A alone is carried out for mechanical and dynamometer tests. The mechanical and physical properties of Mix-A alloy were also determined. According to Ram et al.[ 18 ] the appearance of FCC peaks confirms the existence of a solid solution matrix. Intermetallics (FeNi 3 and CrNi 3 ) were discovered in FeCrNiCuMoSiC x=10 composite. The average hardness, porosity, and density of Mix-A after sintering reached 178 ± 4 HV, 5.84% and 6.34 g/cm 3 respectively. A decrease in wear loss is associated with an increase in hardness, according to the Archard relation. In addition, the composites have a higher hardness than the individual metallic elements. There is a possibility of strengthening the solidsolution [ 1 ]. The effect of alloy structure on the ability to resist wear at different brake energy and sliding speeds is apparent in this study. The HEAs show high wear that may be due to the relatively low hardness of these alloys [ 18 , 24 ]. 3.2 Wear behaviour The wear response of FeCrNiCuMo (SiC x=10 ) was tested for three different sliding speeds. Figure 2 presents the coefficient of friction (CoF) evolution for the 100 braking stops with varying sliding speeds. Wear mechanisms are affected by sliding speed, causing material deformation, changing friction interface temperatures, and affecting wear mechanism [ 25 , 26 ]. An increase in COF is observed with the increasing sliding speed of FeCrNiCuMo SiC X=10 . The coefficient of friction curves is typically characterized by two friction regimes as reported in literature [ 27 ]. The A1 and A2 alloys exhibit relatively large fluctuation whereas A3 alloy does a small fluctuation. Initially, the A1 shows a rapid and steep running in a stage where the friction coefficients rapidly increase up to a certain value. The second stage, where friction coefficients are observed to fluctuate significantly with increasing stops. There is a fluctuation in CoF, which can be attributed to lose wear debris. Sliding speed is affected by the stuck debris, which causes abrupt fluctuations in CoF when the debris interferes with the sliding. The smallest attainable CoF is due to the wear mechanism of oxidation wear in contrast to the delamination wear. The large fluctuation of the friction coefficient is caused by two reasons. The first is the periodic localized fracture of the surface layer [ 28 , 29 ]. The second is the periodic accumulation and elimination of debris on the worn surface. The coefficient of friction increases as the large debris accumulates on the worn surface while it decreases as the debris departs from the worn surface [ 30 ]. As for the small fluctuation of A3, it is due to its wear mechanism of oxidative wear, which results in small debris. Figure 3 shows the average coefficient of friction with varying sliding speed. In comparison, A3 and A2 show a higher coefficient of friction than A1. There is a high difference in the wear mass loss between A1 and A3 after friction testing. The results suggest that the A1 has better wear performance than the A3 does. A1 also shows the smallest mass loss, indicating a greater wear resistance. In accordance with the prevailing wear mechanisms at that sliding speed, as the sliding speed increases, the CoF increases. At the higher speed (40ms − 1 ), the friction between the two surfaces generates more energy, which causes the temperature to rise. In the Fig. 4 , the stopping distance and mean torque are shown as a function of sliding speeds. The mean torque increases with increase in the sliding speeds. As the sliding speed increases, more heat is dissipated in the form of frictional energy between the brake pad and rotor, which increases energy dissipation. In addition to dissipating energy, the braking system also experiences an increase in temperature, which may affect wear behavior. Additionally, high sliding speeds (40ms − 1 ) can create increased abrasive wear as contaminants and debris are present on the surface of the rotor. In consequence, particles are more likely to interact and enter the brake pad material at a faster rate, resulting in a greater loss of material and more rapid wear. Brake mean torque and sliding speed may also be affected by other factors like the brake pad and rotor material composition and properties as well as system design and operating conditions. During braking, the friction coefficient of the body determines the stopping distance of the body. A higher sliding speed leads to a larger mean break torque and a shorter stopping distance for FeCrNiCuMoSiC x=10 . Shorter stopping distances are seen at A1 as compared to A2 and A3. As a result of the higher oxygen content at A1 (20ms − 1 ) and the lower wear rate, the third body friction is enhanced and the stopping distance decreases. Considering these factors, it can be deduced that A1 sliding speed has a higher wear resistance and mean torque as well as a better braking performance than the A2 and A3. The higher temperatures cause the constituents to oxidize, which in turn causes mass loss. As a result, contact surfaces exhibit enhanced diffusion activity, which leads to deterioration in wear properties (Fig. 5 ). High sliding speeds cause delamination of particle/matrix if braking force is applied, resulting in significant mass loss. Beyond this sliding speed, the oxide scale thickness increases, cracking of the scales will accelerate faster. When the friction temperature rises, the material softens, weakening the particle/matrix interface and resulting in mass loss. Up to the critical speed, increasing the sliding speed facilitates the formation of oxides and a tribolayer at the wearing surface, thereby preventing the accumulation of wear per unit sliding distance until the critical speed is reached [ 31 ]. This suggests that the A1 is suitable for use as a brake pad wear protector, which is a practical application. The SEM technique to analyse the morphologies and compositions of the friction surface after braking tests and the corresponding results are shown in Fig. (6–8). Based on the wear pattern shown in Fig. 5 , the A1 (20ms − 1 ) exhibits a higher wear resistance than the other sliding speeds, with smooth surface and peeling area is less. The main wear mechanism is therefore suggested to be abrasive and slight fatigue wear. Fatigue, brittle fracture, or low deformation cause the loss of material in this method. Moreover, the wear debris between the two surfaces is also used as an abrasive, which is referred to as three-body abrasion [ 32 , 33 ]. According to the EDS results, the A1 surface showed a high oxygen content in the worn surface, indicating that an extent of oxidation wear had occurred on the surface and formation of hard oxide particles which are effective on the abrasive wear mechanism. The formation of a hard oxide layer leads to changes in the wear mechanism and a reduction in the effect of adhesion. However, the brittle characteristic of the oxide layer might be effective on this mechanism, as applied stress can break the oxide layer with a lower amount of deformation. When the sliding speed was changed to A2 (30ms − 1 ), the wear mechanism observed in Fig. 7 was found to be a combination of abrasive wear and severe adhesive wear. This led to a significant increase in wear loss and the area of the spalling pit on the surface. As the wear progressed, numerous pits and flakes started to appear on the worn surface, accompanied by noticeable internal cracks that had the potential to expand further [ 33 ]. The presence of hard particles within the spall pit was also observed. At this stage, the wear mechanism can be categorized as delamination wear, where significant deformation causes the formation of adhesion points. These adhesion points can detach subsequently due to shearing forces, resulting in the generation of debris. This phenomenon is commonly referred to as adhesive wear. Over time, the adhesion points can grow, leading to the peeling off the material matrix in the form of lamellae, under the influence of high shear forces. This process ultimately gives rise to severe delamination wear. Additionally, as the sliding speed increases, the brittle oxide layer becomes more vulnerable to breaking under the heat generated by friction. This transition from oxidative wear to adhesive wear further exacerbates the severity of the wear observed. In Fig. 8 it was found that the A3 (40ms − 1 ) displayed many plastic deformations and spalling which indicate that serious fatigue wear and adhesive wear occurred. Increasing the sliding speed caused the FeCrNiCuMoSiC 10 to develop large spalling pits and deep grooves. The repeated action of sliding at high speeds resulted in a gradual softening of the contact point of the friction surface, which in turn led to a gradual weakening of the surface's resistance to plastic deformation as the temperature of the friction surface. Spalling pits and grooves formed on the worn surface because of the peeled-off debris. According to Zhang et al. [ 34 ], continuous friction caused the worn surface to form more pits and grooves. Additionally, the EDS analysis revealed a notable presence of oxygen, indicating the formation of an oxide film on the surface during the wear process. Although the quantity of these oxide phases may not be substantial, the localized temperature rises from friction caused the surface to undergo oxidation. In the sliding speed of A2 and A3 there is a reduction in lamellar shedding, the worn surface becomes shallower, the oxide film deteriorates, and hard particles are evident. Wear occurs through abrasive and adhesive mechanisms currently. It appears the friction pair removed the oxide film from the composites, leaving behind the worn composites. Due to the shear force, the relatively soft matrix was quickly worn away because of the shear force, leaving behind the harder reinforced particles within the matrix and dividing the adhesion points into discontinuous points. The harder particles cause the abrasion of the matrix material, resulting in the formation of pits. These pits can cause an increase in the friction coefficient and further accelerate the wear rate. CONCLUSION We have developed successfully the FeCrNiCuMoSiC x=10 structure in the SiC composites using compaction and pressure sintering techniques. We have studied the microstructure and tribology behaviour of the composites. Our study leads to following important results. The microscopy analysis revealed that the FeCrNiCuMo SiC x=10 high entropy alloy has good interfacial bonding, free from defects such as cracks, pores, and undesirable interfacial products. and confirmed the uniform distribution of SiC particles. A proper braking system should be able to stop with a minimum stopping distance, wear rate and CoF at all sliding speeds. The A1 (20ms -1 ) sliding condition, got the excellent wear it wears rate, and average friction coefficient, were 1.298 x10 -7 mm 3 /N.m and 0.23, respectively. The wear mechanisms of A1 were recorded as abrasive and oxidation wear. There is no segregation of any element in wear tracks as suggested by the EDS analysis. The accumulation and compact debris are rich in oxides at the wear track, and the fine oxide particles formed in wear subsurface act to improve wear resistance. Declarations Conflict of Interest Dr. T Ram Prabhu declares that has no conflict of interest. Dr. P Vignesh declares that has no conflict of interest. S Krishnakumar declares that has no conflict of interest. Anand GS declares that has no conflict of interest. CM Bhuvaneswari declares that has no conflict of interest. Dr. SS Kale declares that has no conflict of interest. The authors have no affiliation with any other external organization/agency with a direct or indirect financial interest in the subject matter discussed in the manuscript entitled “ Wear behaviour of SiC-Renforced Metal Matrix Composites FeCrNiCuMo High Entropy Alloy Processed Through Powder Metallurgy ” that is submitted for Tribology Letters. Therefore, “ No potential conflict of interest ” is reported by the authors. 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(2023). doi.org/10.1016/j.matchemphys.2023.128207 Téllez-Villaseñor, M.A., León-Patiño, C.A., Aguilar-Reyes, E.A., Bedolla-Jacuinde, A.: Effect of load and sliding velocity on the wear behaviour of infiltrated TiC/Cu–Ni composites. Wear (2021). doi.org/10.1016/j.wear.2021.203667 Liu, Y., Ma, S., Gao, M.C., Zhang, C., Zhang, T., Yang, H., Wang, Z., Qiao, J.: Tribological properties of AlCrCuFeNi 2 high-entropy alloy in different conditions. Metall. Mater. Trans. A (2016). doi.org/10.1007/s11661-016-3396-8 Prabhu, T.R., Varma, V.K., Vedantam, S.: Tribological and mechanical behavior of multilayer Cu/SiC+ Gr hybrid composites for brake friction material applications. Wear (2014). doi.org/10.1016/j.wear.2014.06.006 Kumar, N.S., Prabhu, T.R., Mishra, R.K., Eswaraprasad, N., Shankar, G.S., Basavarajappa, S.: Analysis of dry sliding wear behavior of the nano composites using statistical methods with an emphasis on temperature effects. Meas. (2018). doi.org/10.1016/j.measurement.2018.06.064 Zhan, Y., Zhang, G.: Friction and wear behavior of copper matrix composites reinforce with SiC and graphite particles. Tribol. Lett. (2004). doi.org/10.1023/B:TRIL.0000017423.70725.1c Additional Declarations No competing interests reported. Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-3415717","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":239116828,"identity":"716c7a5b-2f3c-44ae-b68e-88eb26f19472","order_by":0,"name":"Ramprabhu T","email":"","orcid":"","institution":"Center for Military Airworthiness and Certification","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Ramprabhu","middleName":"","lastName":"T","suffix":""},{"id":239116829,"identity":"a2e7eb8a-1b7a-48be-9e27-f3ddd213bcb5","order_by":1,"name":"Vignesh P","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAABBklEQVRIiWNgGAWjYDACZjB5gIGBv//xgw8VIBHmBuK08EicYTOccQYkwkhACwNMC0MOgzRvG4hDQIvBcfZrDz78uZNnz3D2gAHvvNpo/naglh8V23BrOcxTbjiz7VkxD3NfwgPJbcdzZxxmbGDsOXMbpxbJZp40ad6Gw4k9DAcMDAy3HcttAGphZmwjoOXPH5CWBAOJxDnHcucT0sLPzH5MmoENpCXHQOJgQ03uBsJaeNgke9sOF/PcOJZm2HDsQO5GoJaD+PzCxn/8mcSPP4fz2PubDz/+U1OXO+/84YMPflTg1sLAwGMAIhOgvMNg8gAe9UDA/gBZSx1+xaNgFIyCUTAiAQAzTWHmZQy1TAAAAABJRU5ErkJggg==","orcid":"","institution":"Center for Military Airworthiness and Certification","correspondingAuthor":true,"submittingAuthor":false,"prefix":"","firstName":"Vignesh","middleName":"","lastName":"P","suffix":""},{"id":239116830,"identity":"1686e0eb-2652-4341-a506-073b56783baa","order_by":2,"name":"Krishnakumar S","email":"","orcid":"","institution":"Center for Military Airworthiness and Certification","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Krishnakumar","middleName":"","lastName":"S","suffix":""},{"id":239116831,"identity":"ec7a2cdc-9939-488a-986e-9991fbc5957a","order_by":3,"name":"Anand GS","email":"","orcid":"","institution":"Center for Military Airworthiness and Certification","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Anand","middleName":"","lastName":"GS","suffix":""},{"id":239116832,"identity":"8ae6bc1e-608e-4843-abb3-211756abaef0","order_by":4,"name":"Bhuvaneswari CM","email":"","orcid":"","institution":"Center for Military Airworthiness and Certification","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Bhuvaneswari","middleName":"","lastName":"CM","suffix":""},{"id":239116833,"identity":"0a5a5d05-6240-4b08-b8cc-e2989474c6b2","order_by":5,"name":"Kale SS","email":"","orcid":"","institution":"Center for Military Airworthiness and Certification","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Kale","middleName":"","lastName":"SS","suffix":""}],"badges":[],"createdAt":"2023-10-06 09:29:18","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3415717/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3415717/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":44599485,"identity":"b9669ffd-f7a2-4fc9-abf8-36e5df13f10a","added_by":"auto","created_at":"2023-10-13 20:42:13","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":662679,"visible":true,"origin":"","legend":"\u003cp\u003eOptical image of (a) Mix A: 1, 2 and 3 indicates back plate, Ni plated layer and composite respectively (b) Mix B where magnified image of (c) Mix A and (d) Mix B\u003c/p\u003e","description":"","filename":"floatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/6f9a98d2f689efd2d1119e69.png"},{"id":44599480,"identity":"193ce63c-be25-4d0c-8509-74d37754d4e0","added_by":"auto","created_at":"2023-10-13 20:42:08","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":53423,"visible":true,"origin":"","legend":"\u003cp\u003eCoefficient of friction vs number of stops of FeCrNiCuMo (SiC\u003csub\u003ex=10\u003c/sub\u003e) with varying sliding speed\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/81956f87f806f91eaaf9db5c.png"},{"id":44599477,"identity":"c9ba989a-1add-413b-95f7-b7aa621a12f6","added_by":"auto","created_at":"2023-10-13 20:42:08","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":41302,"visible":true,"origin":"","legend":"\u003cp\u003eVariation in CoF with varying sliding speed\u003c/p\u003e","description":"","filename":"floatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/c2ee6944d1327275e2a7377e.png"},{"id":44600704,"identity":"8dc8290b-20fb-47cb-b464-27ae0562fdf5","added_by":"auto","created_at":"2023-10-13 20:50:08","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":49922,"visible":true,"origin":"","legend":"\u003cp\u003eEffect of sliding speed on brake mean torque and stopping distance\u003c/p\u003e","description":"","filename":"floatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/57676716f46519c53c6ae712.png"},{"id":44599479,"identity":"6de84e4d-9dd1-4d36-a81c-e3091f84e10f","added_by":"auto","created_at":"2023-10-13 20:42:08","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":37680,"visible":true,"origin":"","legend":"\u003cp\u003eWear rate for FeCrNiCuMo (SiC\u003csub\u003ex=10\u003c/sub\u003e) varying sliding speed\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/e4e0da1a462c78eb275b42f0.png"},{"id":44599481,"identity":"98580a29-4d6f-45b1-9d71-4d41323041c1","added_by":"auto","created_at":"2023-10-13 20:42:08","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":548932,"visible":true,"origin":"","legend":"\u003cp\u003eSEM morphology of wear surface of A1 condition\u003c/p\u003e","description":"","filename":"floatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/4c08edfc564bd1609ac94ed0.png"},{"id":44600739,"identity":"69347bb0-7d79-43f8-9ee0-ac1e3086e2c1","added_by":"auto","created_at":"2023-10-13 20:50:13","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":711477,"visible":true,"origin":"","legend":"\u003cp\u003eSEM morphology of wear surface of A2 condition\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/afa5147f5e7b1682ebbdc7ae.png"},{"id":44599483,"identity":"deaf3286-66e7-476f-a4f6-4f584959092e","added_by":"auto","created_at":"2023-10-13 20:42:08","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":462233,"visible":true,"origin":"","legend":"\u003cp\u003eSEM morphology of wear surface of A3 condition\u003c/p\u003e","description":"","filename":"floatimage8.png","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/0298b88fb1809e16084e7d33.png"},{"id":44693726,"identity":"c022532c-f3fe-4acf-ad7c-77b83bfd1f7d","added_by":"auto","created_at":"2023-10-16 13:22:30","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2689523,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3415717/v1/7f564d87-d2a3-4e97-bcde-9532f57e3a83.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Wear behaviour of SiC-Reinforced Metal Matrix Composites FeCrNiCuMo High Entropy Alloy Processed Through Powder Metallurgy","fulltext":[{"header":"1. INTRODUCTION","content":"\u003cp\u003eThe performance of the brake system is largely impacted by the friction material properties, which are extremely difficult to forecast. In order to enhance brake performance and prolong the life of the brakes, the brake materials must have high wear resistance, low brake fade, constant friction, and vibration [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. The microstructure of prepared materials has a significant impact on their mechanical properties, durability, wear resistance, as well as stability in engineering applications [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. The demands are high for materials with as steady frictional coefficient, and low wear rates. With high temperature, braking pressure, and initial braking speed, the wear rate accelerates significantly [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e, \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. In recent years, the unique compositions, microstructures, and adjustable properties of high-entropy alloys have attracted increasing attention. A compositionally complicated alloy design approach known as high entropy alloys (HEAs) has greatly increased the broad range of alloy systems that are currently accessible as well as yielded alloys with exciting structural and functional characteristics [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]. Accordingly, HEAs are described as having disordered solid solution structures with a minimum of four or five primary alloying elements in amounts ranging from 5 to 35 at% [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e, \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. These alloys can exhibit a remarkable mixture of qualities, including outstanding specific strength, fracture toughness, ductility, and improved mechanical performance at higher temperatures. Also, these alloys provide strong resistance to corrosion, creep, as well as oxidation [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. Further, it has become significantly popular among researchers to study the mechanical behavior and application of a high entropy CoCrFeMnNi alloy. There are several ways to prepare HEAs, including arc melting, mechanical alloying, laser cladding, and spark plasma sintering [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. Many alloys and combinations that are impossible or difficult to produce using the standard melting and casting procedure can be formed through a special process called mechanical alloying [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. According to previous research, an effective method for creating an alloy with homogeneous compositions and microstructures is powder metallurgy, which produces high-strength FeCrNiCuMo alloys with high entropies. Powders can be thoroughly mixed in a short amount of time without the microstructure becoming coarser [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. A fine-grained structure, controlled form, and more homogenous composition may be achieved by the conventional solid mixing method of powder metallurgy, which also includes mechanical alloying and a subsequent consolidation process [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. HEAs are the most intriguing choices for usage as an additive phase in ceramic matrix because of their exceptional characteristics and capacity to form the liquid phase during the sintering process [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. The most common alloys utilized in tribology applications are nickel and other high entropy alloys. This is because of the formation of intermediate layers when it comes into contact with other sliding materials. By limiting the contact between the two sliding materials, these intermediary layers inhibit alloy wear. In particular, HEAs like Ti\u003csub\u003e0.8\u003c/sub\u003eCoCrCuFeNi and TiCoCrCuFeNi demonstrated some functional characteristics, including superconductive and superparamagnetic properties [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e, \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e]. Importantly, due to the slow dispersion of the alloying components, these alloys exhibit good thermal stability. In contact sliding applications, such a characteristic is crucial to regulating friction-induced temperature [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. However, depending on the operating temperature, the wear behavior and characteristics of intermediate layers fluctuate [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. Moreover, to attain adequate mechanical characteristics, additional alloying elements must be added by lattice distortion or precipitation formation to strengthen the HEA. Among different alloys, substances like V, Mo, Cu, Nb, Al, Ti, etc. are capable of altering the crystalline structure, resulting in a considerable increase in strength [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. Recent reports suggest that ceramic particles like SiC, TiC and NbC are being used as reinforcement in HEAs, which has a good impact on their mechanical characteristics and tribological behaviour. In particular, SiC ceramics exhibit a variety of exceptional physical-chemical characteristics, including great hardness and mechanical stability at high temperatures, outstanding thermal conductivity and strong resistance to oxidation and corrosion. The high-power electronics industry, as well as the automotive and aerospace sectors, use this low-density ceramic in a variety of structural ceramics applications [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. The current work aims to improve the wear and frictional properties of the brake pad based on FeCrNiCuMo friction material with varying SiC (10 and 15 wt.%). Using a high entropy FeCrNiCuMoSiCx alloy at ambient temperatures, the present experiment aims to examine the sliding wear response. In conclusion, it is recommended that High Entropy Alloy Metal-matrix Composites (HEAMC's) developed in this study be used in aerospace applications.\u003c/p\u003e"},{"header":"2. MATERIALS AND METHODS","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Powder Processing\u003c/h2\u003e \u003cp\u003eFor brake pads, FeCrNiCuMo powders with equiatomic compositions (20%) were prepared by mixing powders of Fe, FeCr, Ni, Cu, and Mo with approximately 99% purity and powder characteristics [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]. The raw powders were mixed for 22h in a planetary ball-milling machine at a speed of 300 rpm, with steel balls of 8 mm in diameter and a mass ratio of 1:1 between the steel balls and the raw powder. Process control was achieved using De-Nature Spirit. As soon as the metallic powders had been mechanically alloyed in the ball mill, SiCx particles of different weights (x\u0026thinsp;=\u0026thinsp;10 \u0026amp; 15 wt. %) were added without the use of balls, in order to avoid deforming, a mechanical alloying, or deformation, and then allowed to run for 2h.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Compaction and Sintering Cycle\u003c/h2\u003e \u003cp\u003eA uniaxial compaction setup with a capacity of 200 tons was used to compact the composite mix into a 3.2 mm thick pad. The hardened steel dies wall and punch surfaces were coated with graphite oil to facilitate easy ejection of the compact. After the compacted pads have been placed in the bell furnace and subjected to a specific temperature for a certain period of time, the compacted pads are then subjected to the load (165 T) and time (25s). Sintering takes place at 1000\u0026deg;C and lasts 210 minutes in this case. The process was carried out in a dry hydrogen atmosphere (Flow rate: 0.012 m\u003csup\u003e3\u003c/sup\u003e/min), and the temperature was raised at a controlled heating rate of 5.55\u0026deg;C per minute during the sintering process.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Sintered Density and Material Characterization\u003c/h2\u003e \u003cp\u003eBy using Archimedes' principle as a basis for measuring the density of the composites in the compacted and sintered states. A standard metallographic technique was used to prepare samples for microstructure. The composites were studied using optical and scanning electron microscopes equipped with energy-dispersive spectrometers (EDS). SEM was used to measure the surface elemental composition and the topography of worn surfaces and loose wear debris.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4 Mechanical Properties\u003c/h2\u003e \u003cp\u003eIn order to determine the hardness of the composites, the Vickers hardness tester was used. Five indentions were taken randomly and the average of them was reported as hardness. The load was 100 g, and dwell time was 15 seconds. Full-scale dynamometer tests were conducted using the main parameters listed in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. In an ultrasonic bath for 15 minutes, acetone was used to clean the pads and disc to a 1-mm finish. Using rivets, the pads were attached to the holder. Low-carbon alloy steel discs were used as rotors. We conducted 100 braking stops, using the computer-controlled data acquisition system to record information such as torque, friction coefficient, stopping distance, and time. A Digital (XB220A) electronic balance was used to measure the weight loss of pads (precision: 1 mg). The FeCrNiCuMo SiC\u003csub\u003ex=10\u003c/sub\u003e is denoted as Mix-A and FeCrNiCuMo SiC\u003csub\u003ex=15\u003c/sub\u003e is denoted as Mix-B.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003e\u003cem\u003eBrake testing parameters\u003c/em\u003e\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"7\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTest\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSliding speed (m/s)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eBrake energy absorbed by 2 pads (kJ)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eRotor disc\u003c/p\u003e \u003cp\u003e(rpm)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eDisc radius (mm)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003eBrake load (N)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e \u003cp\u003eFlywheel mass moment of inertia (Nms\u003csup\u003e2\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eA1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e20\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e20.8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e382\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\" morerows=\"2\" rowspan=\"3\"\u003e \u003cp\u003e250\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\" morerows=\"2\" rowspan=\"3\"\u003e \u003cp\u003e980\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\" morerows=\"2\" rowspan=\"3\"\u003e \u003cp\u003e30.87\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eA2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e55.6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e573\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eA3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e40\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e83.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e764\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"3. RESULTS AND DISCUSSION","content":"\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\n \u003ch2\u003e3.1 Metallurgical Evaluation\u003c/h2\u003e\n \u003cp\u003eAccording to the optical image of FeCrNiCuMoSiC\u003csub\u003ex\u003c/sub\u003e (x\u0026thinsp;=\u0026thinsp;10 \u0026amp; 15wt%) shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e (a \u0026amp; b), the system is characterized by three distinct layers namely the friction material, the intermediate transition layer, and the steel backing plate. From Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e (a \u0026amp; c), the SiC is stable in the microstructure for Mix A. The SiC distribution in the matrix is uniform. The bonding appears to be strong and free from defects such as delamination, cracks, or interfacial products. In addition, it also enhanced the dimensional stability of the brake pad. There are no traces of defects, such as cracks, pores, or undesirable interfacial products, in the composite\u0026apos;s bond with Ni-plated steel, as shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e(a). The microstructure of the steel sheet is dominated by the ferrite phase, with some pearlite. The brake pads developed are not a homogenous material in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e (b \u0026amp; d). The particle size of each element is not uniform in size and the distribution of the element is not well dispersed in the matrix. The Mix B materials towards either side of the interface were entirely different, crack, and de-bonding occurred frequently during actual applications. In order to overcome the poor joint, future optimization should be carried out in powder processing/ sintering for better usage of Mix-B. As for this paper Mix-A alone is carried out for mechanical and dynamometer tests. The mechanical and physical properties of Mix-A alloy were also determined. According to Ram et al.[\u003cspan class=\"CitationRef\"\u003e18\u003c/span\u003e] the appearance of FCC peaks confirms the existence of a solid solution matrix. Intermetallics (FeNi\u003csub\u003e3\u003c/sub\u003e and CrNi\u003csub\u003e3\u003c/sub\u003e) were discovered in FeCrNiCuMoSiC\u003csub\u003ex=10\u003c/sub\u003e composite.\u003c/p\u003e\n \u003cp\u003eThe average hardness, porosity, and density of Mix-A after sintering reached 178\u0026thinsp;\u0026plusmn;\u0026thinsp;4 HV, 5.84% and 6.34 g/cm\u003csup\u003e3\u003c/sup\u003e respectively. A decrease in wear loss is associated with an increase in hardness, according to the Archard relation. In addition, the composites have a higher hardness than the individual metallic elements. There is a possibility of strengthening the solidsolution [\u003cspan class=\"CitationRef\"\u003e1\u003c/span\u003e]. The effect of alloy structure on the ability to resist wear at different brake energy and sliding speeds is apparent in this study. The HEAs show high wear that may be due to the relatively low hardness of these alloys [\u003cspan class=\"CitationRef\"\u003e18\u003c/span\u003e, \u003cspan class=\"CitationRef\"\u003e24\u003c/span\u003e].\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e\n \u003ch2\u003e3.2 Wear behaviour\u003c/h2\u003e\n \u003cdiv class=\"BlockQuote\"\u003e\n \u003cp\u003eThe wear response of FeCrNiCuMo (SiC\u003csub\u003ex=10\u003c/sub\u003e) was tested for three different sliding speeds. Figure\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003e presents the coefficient of friction (CoF) evolution for the 100 braking stops with varying sliding speeds. Wear mechanisms are affected by sliding speed, causing material deformation, changing friction interface temperatures, and affecting wear mechanism [\u003cspan class=\"CitationRef\"\u003e25\u003c/span\u003e, \u003cspan class=\"CitationRef\"\u003e26\u003c/span\u003e]. An increase in COF is observed with the increasing sliding speed of FeCrNiCuMo SiC\u003csub\u003eX=10\u003c/sub\u003e. The coefficient of friction curves is typically characterized by two friction regimes as reported in literature [\u003cspan class=\"CitationRef\"\u003e27\u003c/span\u003e].\u003c/p\u003e\n \u003c/div\u003e\n \u003cdiv class=\"BlockQuote\"\u003e\n \u003cp\u003eThe A1 and A2 alloys exhibit relatively large fluctuation whereas A3 alloy does a small fluctuation. Initially, the A1 shows a rapid and steep running in a stage where the friction coefficients rapidly increase up to a certain value. The second stage, where friction coefficients are observed to fluctuate significantly with increasing stops. There is a fluctuation in CoF, which can be attributed to lose wear debris. Sliding speed is affected by the stuck debris, which causes abrupt fluctuations in CoF when the debris interferes with the sliding. The smallest attainable CoF is due to the wear mechanism of oxidation wear in contrast to the delamination wear. The large fluctuation of the friction coefficient is caused by two reasons. The first is the periodic localized fracture of the surface layer [\u003cspan class=\"CitationRef\"\u003e28\u003c/span\u003e, \u003cspan class=\"CitationRef\"\u003e29\u003c/span\u003e]. The second is the periodic accumulation and elimination of debris on the worn surface. The coefficient of friction increases as the large debris accumulates on the worn surface while it decreases as the debris departs from the worn surface [\u003cspan class=\"CitationRef\"\u003e30\u003c/span\u003e]. As for the small fluctuation of A3, it is due to its wear mechanism of oxidative wear, which results in small debris.\u003c/p\u003e\n \u003c/div\u003e\n \u003cp\u003eFigure\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003e shows the average coefficient of friction with varying sliding speed. In comparison, A3 and A2 show a higher coefficient of friction than A1. There is a high difference in the wear mass loss between A1 and A3 after friction testing. The results suggest that the A1 has better wear performance than the A3 does. A1 also shows the smallest mass loss, indicating a greater wear resistance. In accordance with the prevailing wear mechanisms at that sliding speed, as the sliding speed increases, the CoF increases. At the higher speed (40ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), the friction between the two surfaces generates more energy, which causes the temperature to rise. In the Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003e, the stopping distance and mean torque are shown as a function of sliding speeds. The mean torque increases with increase in the sliding speeds. As the sliding speed increases, more heat is dissipated in the form of frictional energy between the brake pad and rotor, which increases energy dissipation. In addition to dissipating energy, the braking system also experiences an increase in temperature, which may affect wear behavior. Additionally, high sliding speeds (40ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) can create increased abrasive wear as contaminants and debris are present on the surface of the rotor. In consequence, particles are more likely to interact and enter the brake pad material at a faster rate, resulting in a greater loss of material and more rapid wear. Brake mean torque and sliding speed may also be affected by other factors like the brake pad and rotor material composition and properties as well as system design and operating conditions.\u003c/p\u003e\n \u003cp\u003eDuring braking, the friction coefficient of the body determines the stopping distance of the body. A higher sliding speed leads to a larger mean break torque and a shorter stopping distance for FeCrNiCuMoSiC\u003csub\u003ex=10\u003c/sub\u003e. Shorter stopping distances are seen at A1 as compared to A2 and A3. As a result of the higher oxygen content at A1 (20ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) and the lower wear rate, the third body friction is enhanced and the stopping distance decreases. Considering these factors, it can be deduced that A1 sliding speed has a higher wear resistance and mean torque as well as a better braking performance than the A2 and A3.\u003c/p\u003e\n \u003cp\u003eThe higher temperatures cause the constituents to oxidize, which in turn causes mass loss. As a result, contact surfaces exhibit enhanced diffusion activity, which leads to deterioration in wear properties (Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e). High sliding speeds cause delamination of particle/matrix if braking force is applied, resulting in significant mass loss. Beyond this sliding speed, the oxide scale thickness increases, cracking of the scales will accelerate faster. When the friction temperature rises, the material softens, weakening the particle/matrix interface and resulting in mass loss. Up to the critical speed, increasing the sliding speed facilitates the formation of oxides and a tribolayer at the wearing surface, thereby preventing the accumulation of wear per unit sliding distance until the critical speed is reached [\u003cspan class=\"CitationRef\"\u003e31\u003c/span\u003e]. This suggests that the A1 is suitable for use as a brake pad wear protector, which is a practical application.\u003c/p\u003e\n \u003cp\u003eThe SEM technique to analyse the morphologies and compositions of the friction surface after braking tests and the corresponding results are shown in Fig.\u0026nbsp;(6\u0026ndash;8). Based on the wear pattern shown in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e, the A1 (20ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) exhibits a higher wear resistance than the other sliding speeds, with smooth surface and peeling area is less. The main wear mechanism is therefore suggested to be abrasive and slight fatigue wear. Fatigue, brittle fracture, or low deformation cause the loss of material in this method. Moreover, the wear debris between the two surfaces is also used as an abrasive, which is referred to as three-body abrasion [\u003cspan class=\"CitationRef\"\u003e32\u003c/span\u003e, \u003cspan class=\"CitationRef\"\u003e33\u003c/span\u003e]. According to the EDS results, the A1 surface showed a high oxygen content in the worn surface, indicating that an extent of oxidation wear had occurred on the surface and formation of hard oxide particles which are effective on the abrasive wear mechanism. The formation of a hard oxide layer leads to changes in the wear mechanism and a reduction in the effect of adhesion. However, the brittle characteristic of the oxide layer might be effective on this mechanism, as applied stress can break the oxide layer with a lower amount of deformation.\u003c/p\u003e\n \u003cp\u003eWhen the sliding speed was changed to A2 (30ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), the wear mechanism observed in Fig.\u0026nbsp;\u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003e was found to be a combination of abrasive wear and severe adhesive wear. This led to a significant increase in wear loss and the area of the spalling pit on the surface. As the wear progressed, numerous pits and flakes started to appear on the worn surface, accompanied by noticeable internal cracks that had the potential to expand further [\u003cspan class=\"CitationRef\"\u003e33\u003c/span\u003e]. The presence of hard particles within the spall pit was also observed. At this stage, the wear mechanism can be categorized as delamination wear, where significant deformation causes the formation of adhesion points. These adhesion points can detach subsequently due to shearing forces, resulting in the generation of debris. This phenomenon is commonly referred to as adhesive wear. Over time, the adhesion points can grow, leading to the peeling off the material matrix in the form of lamellae, under the influence of high shear forces. This process ultimately gives rise to severe delamination wear. Additionally, as the sliding speed increases, the brittle oxide layer becomes more vulnerable to breaking under the heat generated by friction. This transition from oxidative wear to adhesive wear further exacerbates the severity of the wear observed.\u003c/p\u003e\n \u003cp\u003eIn Fig. \u003cspan class=\"InternalRef\"\u003e8\u003c/span\u003e it was found that the A3 (40ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) displayed many plastic deformations and spalling which indicate that serious fatigue wear and adhesive wear occurred. Increasing the sliding speed caused the FeCrNiCuMoSiC\u003csub\u003e10\u003c/sub\u003e to develop large spalling pits and deep grooves. The repeated action of sliding at high speeds resulted in a gradual softening of the contact point of the friction surface, which in turn led to a gradual weakening of the surface\u0026apos;s resistance to plastic deformation as the temperature of the friction surface. Spalling pits and grooves formed on the worn surface because of the peeled-off debris. According to Zhang et al. [\u003cspan class=\"CitationRef\"\u003e34\u003c/span\u003e], continuous friction caused the worn surface to form more pits and grooves. Additionally, the EDS analysis revealed a notable presence of oxygen, indicating the formation of an oxide film on the surface during the wear process. Although the quantity of these oxide phases may not be substantial, the localized temperature rises from friction caused the surface to undergo oxidation.\u003c/p\u003e\n \u003cp\u003eIn the sliding speed of A2 and A3 there is a reduction in lamellar shedding, the worn surface becomes shallower, the oxide film deteriorates, and hard particles are evident. Wear occurs through abrasive and adhesive mechanisms currently. It appears the friction pair removed the oxide film from the composites, leaving behind the worn composites. Due to the shear force, the relatively soft matrix was quickly worn away because of the shear force, leaving behind the harder reinforced particles within the matrix and dividing the adhesion points into discontinuous points. The harder particles cause the abrasion of the matrix material, resulting in the formation of pits. These pits can cause an increase in the friction coefficient and further accelerate the wear rate.\u003c/p\u003e\n\u003c/div\u003e"},{"header":"CONCLUSION","content":"\u003cp\u003eWe have developed successfully the FeCrNiCuMoSiC\u003csub\u003ex=10\u003c/sub\u003e structure in the SiC composites using compaction and pressure sintering techniques. We have studied the microstructure and tribology behaviour of the composites. Our study leads to following important results. The microscopy analysis revealed that the FeCrNiCuMo SiC\u003csub\u003ex=10\u003c/sub\u003e high entropy alloy has good interfacial bonding, free from defects such as cracks, pores, and undesirable interfacial products. and confirmed the uniform distribution of SiC particles. A proper braking system should be able to stop with a minimum stopping distance, wear rate and CoF at all sliding speeds. The A1 (20ms\u003csup\u003e-1\u003c/sup\u003e) sliding condition, got the excellent wear it wears rate, and average friction coefficient, were 1.298 x10\u003csup\u003e-7\u003c/sup\u003e mm\u003csup\u003e3\u003c/sup\u003e/N.m and 0.23, respectively. The wear mechanisms of A1 were recorded as abrasive and oxidation wear. There is no segregation of any element in wear tracks as suggested by the EDS analysis. The accumulation and compact debris are rich in oxides at the wear track, and the fine oxide particles formed in wear subsurface act to improve wear resistance.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eConflict of Interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eDr. T Ram Prabhu declares that has no conflict of interest.\u003c/p\u003e\n\u003cp\u003eDr. P Vignesh declares that has no conflict of interest.\u003c/p\u003e\n\u003cp\u003eS Krishnakumar declares that has no conflict of interest.\u003c/p\u003e\n\u003cp\u003eAnand GS declares that has no conflict of interest.\u003c/p\u003e\n\u003cp\u003eCM Bhuvaneswari declares that has no conflict of interest.\u003c/p\u003e\n\u003cp\u003eDr. SS Kale declares that has no conflict of interest.\u003c/p\u003e\n\u003cp\u003eThe authors have no affiliation with any other external organization/agency with a direct or indirect financial interest in the subject matter discussed in the manuscript entitled \u0026ldquo;\u003cem\u003e\u0026nbsp;Wear behaviour of SiC-Renforced Metal Matrix Composites FeCrNiCuMo High Entropy Alloy Processed Through Powder Metallurgy\u003c/em\u003e\u0026rdquo; that is submitted for \u003cem\u003eTribology Letters.\u003c/em\u003e\u003cem\u003e\u0026nbsp;\u003c/em\u003eTherefore, \u0026ldquo;\u003cem\u003eNo potential conflict of interest\u003c/em\u003e\u0026rdquo; is reported by the authors.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData Availability\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eData is contained within the article\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003ePrabhu, T.R.: Effect of bimodal size particles reinforcement on the wear, friction, and mechanical properties of brake composites. Tribol.-Mater.Surf.Interfaces. (2016). doi:10.1080/17515831.2016.1262587\u003c/li\u003e\n\u003cli\u003eElzayady, N., Elsoeudy, R.: Microstructure and wear mechanisms investigation on the brake pad. J. Mater. Res. Technol. (2021). doi:0.1016/j.jmrt.2021.02.045\u003c/li\u003e\n\u003cli\u003eBoz, M., Kurt, A.: Effect of ZrSiO4 on the friction performance of automotive brake friction materials. JJ. Mater. Res. Technol. (2007)\u003c/li\u003e\n\u003cli\u003eVerma, P.C., Menapace, L., Bonfanti, A., Ciudin, R., Gialanella, S., Straffelini, G.: Braking pad-disc system: Wear mechanisms and formation of wear fragments. Wear (2015). doi:10.1016/j.wear.2014.11.019\u003c/li\u003e\n\u003cli\u003eJoseph, J., Haghdadi, N., Shamlaye, K., Hodgson, P., Barnett, M., Fabijanic, D.: The sliding wear behaviour of CoCrFeMnNi and AlxCoCrFeNi high entropy alloys at elevated temperatures. Wear (2019). https://doi.org/10.1016/j.wear.2019.03.002\u003c/li\u003e\n\u003cli\u003eSenkov, O.N., Miller, J.D., Miracle, D.B., Woodward, C.: Accelerated exploration of multi-principal element alloys with solid solution phases. Nat. Commun. (2015). doi:10.1038/ncomms7529\u003c/li\u003e\n\u003cli\u003eZhang, Y., Zuo, T.T., Tang, Z., Gao, M.C., Dahmen, K.A., Liaw, P.K., Lu, Z.P.: Microstructures and properties of high-entropy alloys. Prog. Mater. Sci. (2014). doi:10.1016/j.pmatsci.2013.10.00\u003c/li\u003e\n\u003cli\u003eMiracle, D.B., Senkov, O.N.: A critical review of high entropy alloys and related concepts. Acta Mater.\u003cem\u003e (\u003c/em\u003e2017). doi.org/10.1016/j.actamat.2016.08.081\u003c/li\u003e\n\u003cli\u003eWang, B., Huang, X., Fu, A., Liu, Y., Liu, B.: Serration behavior and microstructure of high entropy alloy CoCrFeMnNi prepared by powder metallurgy. Mater. Sci. 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(2004). doi.org/10.1023/B:TRIL.0000017423.70725.1c\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"
[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"High entropy alloy, SiC, Microstructure, Tribological properties, Sliding speed \u0026 SEM","lastPublishedDoi":"10.21203/rs.3.rs-3415717/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3415717/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eA series of FeCrNiCuMo high-entropy alloys with different SiC (x\u0026thinsp;=\u0026thinsp;10 and 15% wt. %) contents were designed, and their microstructure and tribological behaviour were investigated. The tribological behaviour and wear resistance of the composites were evaluated at a range of sliding speeds (20, 30, and 40 ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) in a brake dynamometer for brake friction material applications. According to the estimates of volume loss, wear rate, and friction coefficient, the possible wear mechanisms were suggested in all cases. Additionally, SEM/EDS analysis was conducted on the worn surfaces and debris. With the increase in sliding speed, the wear rate increases due to the increased intensity of abrasive wear, oxidation wear, and plastic deformation-assisted wear. The materials possessed excellent braking performance and wear resistance. The values of average coefficient friction under A1 (20ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), A2 (30ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), and A3 (40ms\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) sliding conditions were 0.23, 0.29, and 0.34, respectively. In comparison to the A3, the A1 exhibits a lower volume wear loss. As the sliding speed change, adhesive wear and abrasive wear become more prevalent, and fatigue wear also occurs.\u003c/p\u003e","manuscriptTitle":"Wear behaviour of SiC-Reinforced Metal Matrix Composites FeCrNiCuMo High Entropy Alloy Processed Through Powder Metallurgy","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2023-10-13 20:42:03","doi":"10.21203/rs.3.rs-3415717/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"
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