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International Journal of Recent Technology and Engineering (IJRTE) ISSN: 2277-3878, Volume-8 Issue-3, September 2019

Tribological Behavior and Hardness Properties of Heat Treated Al 7075-Beryl-Graphene Hybrid Metal Matrix Composites

Shanawaz Patil, Mohamed Haneef

 mirror frames, house members, serving trays and cooking Abstract— The emerging technologies and trends of the utensils. Even in the field of engineering applications, the present generation require downsizing the unwieldy structures to aluminum and its alloys plays vigorous role as an aerospace, lightweight structures. Aluminum matrix composites are tailored space, and automotive components material of increasing candidate materials for aerospace applications due to their outstanding greater strength to weight ratio and low wear rate. In value because of its properties which includes diverse range this study, Al7075 -Beryl-Graphene hybrid composites are of uses are appearance, lightweight and has a low of developed by using stir casting process. Graphene weight range 2.7 to 2.8 gm/cm3 which is almost one-third of percentage was varied from 0 wt. % to 2 wt. % in steps of 0.5 wt. %. (7.83 gmcm3)[-,5]. One of the foremost usually used metal Whereas for Beryl 6 wt. % is used thorough out the study. The alloy for structural application is Al7075 due to its enticing casted specimens were heat-treated at T6 solutionizing wide-ranging properties like low density, improved strength, temperature of 530±5oC for 8 hours. After the heat treatment the specimen are quenched in boiling Water and Ice. The , toughness, and resistance to . Al7075 alloy microstructure of the newly developed hybrid MMCs has been has been extensively used in aircraft structure elements and investigated by TEM and SEM. The microstructural study reveals different stressed structural applications [6- 10]. the uniform distribution of reinforcement into matrix materials. The incorporation of particulate reinforced ceramic hard The hardness and wear behavior of matrix and hybrid composites particles like carbide, carbide, aluminum before and after heat treatment examined by Brinell hardness test and Pin-on-disc test machine respectively. The heat-treated oxides, silicates such as aluminum silicates Al7075-Beryl-Graphene hybrid composites significantly improved (Be3Al2 (SiO3)6), silicide (Si3N4), the hardness and low wear rate compared to base matrix Al7075 silicide (Mg2Si) etc. into the Al matrix enhance its properties alloy. like physical and mechanical properties of the composites and make them a low cost, inherent isotropic and better candidate Index terms: Al7075, Beryl, Graphene, SEM, TEM material for various engineering applications [11, 16]. Aluminum alloys are largely reinforced -with ceramic I. INTRODUCTION materials which are in the form of micron size particles, In the past five decades extensive attention has been fibers, or whiskers. Meanwhile, in the modern years dedicated to composite materials. Composite materials are nanomaterials were used as reinforcement in Al MMCs, created with mixture of two or more materials with owing to their higher surface to volume ratio, excellent and completely different properties to produce advanced new unique properties with respect to mechanical and physical, material. Stuff will offer superior and outstanding distinctive which are capable of meeting the requirement of applications physical and increased fascinating mechanical properties that [17-18]. notice applications in structural, automobiles, aerospace Nano materials like Graphene, nano-diamonds and carbon space, etc. The need for miniaturization and need for nanotubes exhibit outstanding mechanical, tribological, development of composite properties in engineering materials electrochemical and thermal properties owing to their calls for production of lightweight materials with multifarious efficient structures. Graphene has begun as a key class of characteristics required in the aerospace, automotive industry advanced and unique reinforcement material in aluminum with numerous possibilities for vehicle weight reduction. The alloys due to its high strength, large aspect ratio, improved hybrid metal matrix is one of the vital novelties in the growth thermal properties and high elastic modulus [19]. However, a of advanced materials. Amongst all the several metal matrix little research work has been revealed with Beryllium materials, aluminum and its alloys are extensively used in the aluminum silicate and Graphene as reinforcements in development of the metal matrix composites. Aluminum is the Al-MMC. Beryl is naturally occurring material and lightweight and second most plentiful metal available on the incorporation of Beryl in metal matrix composite exhibit wear earth. It has been most widely used and became an economic resistance and increase in hardness [20]-[24]. Speer et al. [25] competitor in the field of commercial applications such as have described the applications of aluminum-Beryllium metal matrix composites (AlBeMet). The AlBeMet composites Revised Version Manuscript Received on 30 May, 2018. materials are most broadly used in aerospace and structural Shanawaz Patil, PhD Research Scholar, VTU Belegavi and Assistant Professor, REVA University, Bengaluru, Karnataka, India, Email: applications. [email protected] Dr. Mohamed Haneef, Professor & Director (R&D), Ghousia College of Engineering, Ramanagara, Karnataka, India, Email: [email protected]

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4808 & Sciences Publication

Tribological Behavior and Hardness Properties of Heat Treated Al 7075-Beryl-Graphene Hybrid Metal Matrix Composites The AlBeMet material has excellent strength to weight Magnesium Oxide (MgO) 0.48 ratio, low weight, and thermal properties are outstanding Oxide (Na2O) 0.55 which perfect match for the high-temperature applications. Potassium Oxide (K2O) 0.004 AlBeMet material has a low CTE, high specific heat and high Oxide (MnO) 0.05 thermal conductivity these properties are favorable for Figure 1 depicts the SEM micrograph of Beryl powder and various space and aerospace applications. Many researchers Figure 2 shows the XRD patterns of Beryl particles used for [24-31] revealed that the liquid metallurgy route (stir casting) the present study. is one of the utmost extensively used and economical Graphene is basically an allotrope of carbon was first processing techniques for the fabrication particulate MMCs. studied in 1947 and found as the thinnest that stack together to In the present investigation, aluminum 7075 alloys as matrix form graphitic material. Graphene is strong nanomaterial and and Al7075/Beryl-Graphene MMCs were developed by using having thickness of 5-10nm with 10-micron lateral dimension stir casting with varying percentage of Graphene from and 20-30 layers particulate used here as reinforcement. The 0.5wt% to 2wt% in steps of 0.5 and fixed percentage (6wt. %) bulk density of Graphene is 480 kg/m3 and anorthic (triclinic) of Beryl. The present study meant to study the special effects crystal system. The SEM image of Graphene is shown in of T6 solutionizing on hardness and wear behavior of Figure 3. aluminum composites containing Graphene and Beryl reinforcement particles. The microstructural characterization of hybrid nanocomposites as cast and worn out surface is studied using SEM.

II. MATERIALS AND METHODS: In the present research, Beryl and Graphene are used as reinforcing materials and Al 7075 alloy (Al-Zn-Mg-Cu) matrix composites are chosen, as it offers excellent properties to meet desired expectations. 2.1 MATRIX MATERIAL:

Al7075 alloy has outstanding properties which to wide Fig. 1- SEM image of Beryl Particles usage in many engineering sectors, typically used in aircraft stringer application. The nominal chemical composition of the as-received Al 7075 matrix alloy is shown in Table I. TABLE 1: CHEMICAL COMPOSITION OF AL 7075 MATRIX ALLOY Elements Weight Percentage (Zn) 5.602 Magnesium (Mg) 2.506 (Cu) 1.598 (Cr) 0.253 (Ti) 0.18 Fig. 2- XRD Pattern of Beryl Particles (Fe) 0.106

Manganese (Mn) 0.0014 Silicon (Si) 0.052 Aluminum (Al) Balance 2.2 REINFORCEMENT MATERIAL Beryl, commonly known as Beryllium aluminum silicate and having a chemical formula (Be3Al2 (SiO3)6) is occurring mineral. The density of the mineral Beryl is 2700-2800 kg/m3 which is quite similar to the aluminum alloy, having a hardness of 7.5-8.5 on Moh’s scale. The particle size of reinforcement Beryl used here of 60 to 70 microns (µm). The chemical composition of Beryl is shown in Table 2. Fig. 3- SEM image of Graphene Particles TABLE 2: CHEMICAL COMPOSITION OF BERYL Elements Weight Percentage Silicon Oxide (SiO2) 62.12 Aluminum Oxide (Al2O3) 18.05 Beryllium Oxide (BeO) 8.24

Ferric Oxide (Fe2O3) 4.054 Oxide (CaO) 1.34

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4809 & Sciences Publication International Journal of Recent Technology and Engineering (IJRTE) ISSN: 2277-3878, Volume-8 Issue-3, September 2019

Fig. 5-Muffle Furnace Fig. 4 Stir Casting Process 2.3 PREPARATION OF THE HYBRID COMPOSITE: Al 7075, fixed 6wt% of Beryl particles and varying weight percentage of Graphene reinforcement were fabricated by liquid metallurgy route (Figure 4 stir casting method) by using 6 kW, 5 kg melting capacity, PID temperature controlled electrical furnace. Figure 4 shows the stir casting set up used for developing hybrid composite. Al7075 alloy is melted in the furnace to a temperature of 800oC. The preheated Graphene and Beryl particulates were poured slowly into vortex of molten metal. A mechanical stirrer was used to create vortex for the duration of 10 minutes and the stirring speed maintained was 300rpm. The melt is degassed by using commercially available tablets of Hexa-chloroethane Fig. 6- Hardness Samples (C2Cl6). Finally the liquid metal is poured into the preheated cast-iron molds. Table 3 shows the number of samples prepared during the present study for the investigation. The electric muffle furnace shown in Figure 5, was used for heat treatment (solutionizing T6 treatment). The specimens were heat-treated for a solutionizing temperature of 530±5oC for a duration of 8 hours and then quenched in boiling Water and Ice medium. Figure 6 shows the specimens used for the Brinell hardness test. The Brinell hardness tests were carried out as per the ASTM-E10 standard. A pin-on-disc apparatus shows in Figure 7 which contains counterpart of EN32 steel disc of hardness 60 HRC was employed to characterize the dry Fig. 7- Pin-On-Disc set up sliding wear analysis of the heat-treated and as-cast Al7075 alloy and hybrid composites as per ASTM G99 standard. Figure 8 depicts the test samples used for the wear test. TABLE 3: LIST OF SPECIMENS PREPARED Sample Al 7075 (wt. %) Beryl (wt. %) Graphene (wt. %) A 100 0 0 B 93.5 6 0.5 C 93 6 1 D 92.5 6 1.5 E 92 6 2

Fig. 8- Wear Samples

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4810 & Sciences Publication

Tribological Behavior and Hardness Properties of Heat Treated Al 7075-Beryl-Graphene Hybrid Metal Matrix Composites TABLE 3: WEAR TEST CONDITION c) ASTM Standard G-99 Pin Material Al7075, Al7075-6 Wt. % of Beryl-Varying Wt.% of Graphene Disc Material EN32 Pin Contact Area (mm2) 50.272 Track Diameter / Radius 100 / 50 (mm) Load (N) 10, 20, 30 Sliding Distance (m) 2000 Sliding Speed (m/sec) 3.5 Temperature Room Temperature Al7075+6wt. % of Beryl+1.5Wt. % of Graphene III. RESULTS d)

3.1 MICROSTRUCTURE BY SCANNING ELECTRON MICROSCOPE Figure 9 depicts the scanning electron microscope (SEM) micrographs of A7075-6wt. % of Beryl and varying weight percentage of Graphene. The SEM tests reveal that the structure, Beryl and Graphene are evenly dispersed in the matrix with no void and discontinuities observed. Presence of good interfacial bonding between the reinforcements and metal matrix composites with minimal porosity. The microstructural study of the samples was witnessed under a Al7075+6wt. % of Beryl+2Wt. % of Graphene scanning electron microscope (SEM) at numerous locations Fig. 9 SEM micrographs of Hybrid MMC across the composite's specimen to study the distribution of Beryl and Graphene particles in the Al7075. Figure 10 and 11 represents the EDS analysis and EDS spectrum for the heat-treated water quench of sample C (6 Wt. % of Beryl and 1Wt.% of Graphene) respectively and it confirms the presence of Beryl and Graphene in the Al7075 matrix. a)

Fig. 10 Selected area for EDS Analysis of heat-treated water quench for sample C

Al7075+6wt. % of Beryl+0.5Wt. % of Graphene b)

Fig. 11 EDS spectrum of heat-treated composites water quench for sample C Al7075+6wt. % of Beryl+1Wt. % of Graphene

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4811 & Sciences Publication International Journal of Recent Technology and Engineering (IJRTE) ISSN: 2277-3878, Volume-8 Issue-3, September 2019

3.2 TRANSMISSION ELECTRON MICROSCOPY: observed. Significant growth can be seen by the dispersion of TEM analysis carried out on JEOL 2000 FX-II TEM Beryl and Graphene ceramic reinforcement into matrix alloy. equipment. Figure 12 shows the TEM micrographs of as-cast Beryl is harder than the material [2] there is a mismatch in Al7075/6 Wt. % of Beryl/ 1Wt.% of Graphene TEM analysis coefficient of reinforcement’s particles results reveal the presence of stacked layers of Graphene and matrix alloy. [33-34]. From the test results it is inferred along with the Beryl particles and indicates good dispersion that 29.48% of enhancement in hardness of 6 wt. % of Beryl of reinforcement. The uniform distribution of Beryl and and 1 wt. % of Graphene for as-cast condition when compared Graphene are useful to enhance the mechanical and to base alloy. Figure 11 shows the effect of quenching media tribological properties of the hybrid MMC. TEM analysis on the Brinell hardness of Al7075 alloy and hybrid MMC’s. also shows the clear and clean transition region of The extreme hardness resulted in water quenching. An reinforcement and matrix. It also reveals that the improvement of 50.35% of hardness of 6 wt. % of Beryl and 1 Beryl-Graphene and matrix have clear and strong interfaces wt. % of Graphene for water quench condition when that lead to metallurgical bonding which results in drastic compared to Al7075 of as cast. The minimum improvement increase in mechanical and tribological properties. of hardness has resulted in ice quench samples. An improvement of 37.73% of hardness of 6 wt. % of Beryl and 1 wt. % of Graphene for ice quench condition when compared to base alloy of as cast. The enhancement in the hardness for the heat-treated samples is because of formation of precipitates of Copper (AlCu), Silicon carbide, Iron (Fe) and Magnesium (Mg). The further solutionizing treatment makes uniform refinement in crystal structure and sudden cooling help in retaining supersaturated solid solution in composites and hence exhibit increase in hardness for the heat-treated alloy. 3.4 DRY SLIDING WEAR BEHAVIOR Figure 14 depicts the weight loss of the composites on the different applied loads (10 N, 20 N & 30 N) for a constant sliding velocity of 3.5 m/s and sliding distance of 2000 m. The solutionizing behavior expressively reduces the wear loss of the as-cast alloy and its composites. The solutionizing treatment causes the formation of precipitation in the alloy and its composites which in turn decreases the weight loss and also the presence of Graphene and Beryl reinforcement,

protects the matrix alloy against wear, thus the wear loss Fig. 12 TEM micrographs of Hybrid MMC reduces. The wear loss of the hybrid composites was found a 3.3 HARDNESS smaller amount than that of the matrix material at all loads. A similar observation is observed in the study of Al5083/B4C MMCs [35] The wear loss is decreased as the increase in the weight

percentage of Graphene up to 1 wt. % of Graphene for as cast and as well as for solutionized hybrid composite. And also from wear test results, it is inferred that the wear loss for heat-treated Al7075 and its composites are much lower when compared to as-cast alloy and its composites. Figure 15 shows the test results of the effect of reinforcement on wear loss of Al7075 alloy and hybrid MMC’s for the water quench condition. Test results inferred that about 80.76% reduction of wear loss is observed in heat-treated Al7075 alloy/6wt. % of Beryl and 1 wt. % of Graphene for water quench condition. Figure 16 shows the test results of effect of reinforcement on wear Al7075 alloy and hybrid MMC’s for the ice quench condition. The test results inferred that about 76.92% reduction of wear loss is observed in heat-treated Al7075 Fig.13 Hardness with varying the Beryl and Graphene alloy/6wt. % of Beryl and 1 wt. % of Graphene for ice quench contntent under as-cast and heat-treated condition condition. Figure 13 shows the variation of Brinell hardness number with the addition of Beryl and Graphene varying weight percentage. With the addition of Beryl and Graphene particles into the Al7075 alloy, a severe growth in hardness is

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4812 & Sciences Publication

Tribological Behavior and Hardness Properties of Heat Treated Al 7075-Beryl-Graphene Hybrid Metal Matrix Composites environment causes the generation of heat due to friction which results in wide plastic deformation on Al 7075 alloy surface and tends to high wear loss when compared to hybrid composites. The incorporation of hard Beryl particles and Graphene decrease the progress of delamination mechanism which results in high wear resistance. However, further addition of Beryl particles and Graphene in the composites development of mechanically mixed layer which contains fragmented reinforcement particles and oxides of aluminum and iron acts as lubricating agents and offers wear resistance of hybrid composite as reported in previous works of literature [32], [33]. Figure 18 (i) shows spot EDS of heat-treated water quench Al7075-6wt.%Beryl and 1wt.% of Graphene hybrid MMCs. The EDS test results provide the presence of elements like Graphene, Mg, Cu, Zn, and Fe. The

Fig. 14 Wear loss with varying the Beryl and Graphene detailed elemental analysis is shown in Table 4 which gives for as-cast as a function of load the presence of intermetallic precipitates after solutionizing and quenching in both water and ice media.

a) Al7075 alloy at 30N b) Al7075+6wt.% of Beryl+0.5Wt. % of Graphene as cast

Fig. 15 Wear loss with varying the Beryl and Graphene Content for Water Quench as a function load

c) Al7075+6wt. % of d) Al7075+6wt.% of Beryl+1Wt. % of Graphene Beryl+1.5Wt. % of Graphene

e) Al7075+6wt.% of f) Al7075 heat-treated Beryl+2Wt. % of Graphene alloy- water quench

Fig. 16 Wear loss with varying the Beryl and Graphene Content for Ice Quench as function load 3.5 WORN OUT STUDIES Figure 17 shows the worn surfaces of the as-cast and heat-treated Al7075 alloy. The scratches, cracks and plastic deformation were found at surface of Al 7075 due to debris detached and adhered. While conducting the wear test, sliding

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4813 & Sciences Publication International Journal of Recent Technology and Engineering (IJRTE) ISSN: 2277-3878, Volume-8 Issue-3, September 2019

reinforcement. The hardness of the Al7075-Beryl-Graphene composites for the solutionized ice quench shows a maximum hardness of 116.8 BHN at 6 wt. % of Beryl and 1 wt.% of Graphene particulate showing improvement of 37.73% when compared to Al7075 matrix material without the addition of reinforcement. The weight loss is decreased as the increase in the weight percentage of Graphene. The least weight loss achieved for the 1 wt. % of Graphene for as-cast and heat-treated g) Al7075+6wt. % of h) Al7075+6wt. % of composites quenched with water and ice. The weight loss for Beryl+1Wt. % of Graphene Beryl+1Wt. % of heat-treated Al7075 alloy and its composites are much heat-treated – water Graphene heat-treated reduced than their corresponding cast alloy and its quench – Ice quench composites. A maximum of 80.76% reduction of wear Fig. 17 SEM micrographs, of worn-out surfaces of as-cast and heat-treated composites observed in heat-treated water quench Al7075 alloy/6wt. % of Beryl and 1 wt. % of Graphene. About 70.92% reduction of wear observed in heat-treated ice quench Al7075 alloy/6wt. % of Beryl and 1 wt. % of Graphene

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The hardness of Al7075-Beryl-Graphene composites for the solutionized water quench shows a maximum hardness of 127.5 BHN at 6 wt.% of Beryl and 1 wt.% of Graphene particulate showing improvement of 50.35% when compared to Al7075 matrix material without the addition of

Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4814 & Sciences Publication

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Published By: Retrieval Number C6868098319/2019©BEIESP Blue Eyes Intelligence Engineering DOI: 10.35940/ijrte.C6868.098319 4815 & Sciences Publication