T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... 433–440 EFFECT OF B 4 C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR PERFORMANCE OF AZ91 COMPOSITES PRODUCED WITH HOT PRESSING VPLIV DODATKA B 4 C NA MIKROSTRUKTURO, TRDOTO IN SUHO DRSNO OBRABO VRO^E STISKANIH KOMPOZITOV AZ91 Tuba Özdemir Öge 1* , Mecit Öge 2 , Volkan Murat Yýlmaz 3 , Firdevs Banu Özdemir 4 1 Bartýn University, Vocational School of Health Services, Aðdacý Campus, 74100, Bartýn, Turkey 2 Bartýn University, Faculty of Engineering, Department of Mechanical Engineering, Kutlubey-Yazýcýlar Campus, 74100, Bartýn, Turkey 3 Bartýn University, Central Research Laboratory, Kutlubey-Yazýcýlar Campus, 74100, Bartýn, Turkey 4 Beykent University, Department of Health Programmes, Buyukcekmece Premises, 34550, Istanbul, Turkey Prejem rokopisa – received: 2018-06-27; sprejem za objavo – accepted for publication: 2019-01-08 doi:10.17222/mit.2018.127 AZ91-B4C composites were fabricated with varying reinforcement ratios (5 w/%,10w/%,20w/% and 50 w/% B4C) via powder metallurgy and hot pressing to examine their microstructure, hardness and dry-sliding-wear performance. Powder compositions were verified with XRD and the microstructure of the sintered composites was evaluated using SEM (Scanning Electron Microscope) and EDS analyses. Hardness measurements and dry-sliding-wear tests were performed to evaluate the effect of reinforcement addition on the hardness and wear performance of the fabricated composites. Hot pressing of the composite with 50 w/% B4C required a significantly higher sintering pressure at the same sintering temperature. Increasing the B4C addition resulted in increased hardness values for all the composites, whereas the lowest worn volume and coefficient of friction were obtained with 10 w/% B4C. Keywords: metal-matrix composites, particle size, boron carbide, AZ91, material characterization, SEM, hardness, dry sliding wear Avtorji so izdelali AZ91-B4C kompozite z razli~no vsebnostjo oja~itvene faze (5, 10, 20 in 50) w/% B4C s pomo~jo postopkov metalurgije prahov in vro~ega stiskanja. Sledila je preiskava njihove mikrostrukture, dolo~itev trdote in odpornosti proti obrabi zaradi suhega (nemazanega) drsenja. Sestavo prahu so verificirali z rentgensko strukturno analizo (XRD) in ovrednotili mikrostrukturo sintranih kompozitov z vrsti~nim elektronskim mikroskopom (SEM) ter energijsko disperzijsko spektroskopijo (EDS). Meritve trdote in preizkuse obrabe s suhim drsenjem so izvedli zato, da bi dolo~ili vpliv dodatka oja~itvene faze na izdelane kompozite. Vro~e stisnjen kompozit s 50 w/% B4C je zahteval znatnovi{ji tlak stiskanja pri enaki temperaturi sintranja. Pove~anje vsebnosti dodatka B4C je povi{alo trdoto vseh kompozitov, medtem ko je najmanj{i volumen delcev obrabe in najmanj{i koeficient trenja imel kompozit z 10 w/% B4C. Klju~ne besede: kompoziti s kovinsko osnovo, velikost delcev, borov karbid, AZ91, materialna karakterizacija, SEM, trdota, suha drsna obraba 1 INTRODUCTION Composites are among the most preferred material types as they provide a combination of the desired characteristics of different materials. Metal-matrix composites (MMCs) constitute a major portion in com- posite materials. They are generally composed of two constituents, namely the metal matrix and the reinforce- ment. 1 The main reason for the production of MMCs is to improve the strength, elastic modulus and other me- chanical properties of the matrix material via combining the characteristics of metals such as toughness and ductility with the high strength and elastic modulus of ceramics through various methods such as powder metallurgy. 2 Powder metallurgy is a cost-efficient and effective way of obtaining composites with particle or whisker reinforcement. 3 Prior to the production of MMCs with various powder-metallurgy techniques, ma- trix and reinforcement particles are mixed via various methods. A wide variety of materials can be used as the matrix, thus, composite materials with a wide range of elastic moduli, strengths, and thermal expansion coeffi- cients can be produced. Due to their superior properties, such as high hardness, refractoriness and wear resist- ance, hard particulates such as B 4 C SiC, Al 2 O 3 , MgO are widely used as reinforcing agents in MMCs. 4 Various studies have been introduced on the effect of varying the amount of reinforcement material on the microstructure and wear resistance of the metal-matrix composite fabricated. Wang et al., studied the micro- structure and properties such as porosity, hardness and wear resistance of magnesium matrix composites rein- forced with 2 w/%,5w/% and 7.5 w/% fine TiB 2 ( 7 μm) particulates. 5 They reported an increase in the hardness of the composites with increasing TiB 2 content, although the increase in hardness was significantly lower in the case of 7.5 w/% fine TiB 2 as a result of its rela- tively higher porosity content. Yavas and Goller investi- Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 433 UDK 620.1:669.721.5:661.665.3 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 53(3)433(2019) *Corresponding author e-mail: tuba2111@gmail.com gated the effect of B 4 C addition (0–5 w/%) on the properties of a TZM alloy produced with spark plasma sintering. They also reported a significant increase in the Vickers hardness of TZM (from 1.9 to 7.8 GPa) by the addition of 5 w/% B 4 C to the TZM. 6 Liu et al. studied the effects of B 4 C addition (1, 2, 3, 5, 7 and 9) w/% on the microstructure and properties of porous alumina ceramics produced with direct selective laser sintering. They used boron carbide to improve the sintering beha- vior of alumina and they reported a maximum com- pressive strength for the sintered samples in the case of 7 w/% B 4 C addition. 7 In their research on the effect of in-situ reinforcement on the aging and mechanical behavior of an AZ91 metal-matrix composite, Sahoo and Panigrahi studied the age-hardening kinetics of AZ91 and TiC-TiB 2 /AZ91 composites with different characteri- zation tools, and related the enhanced age hardening kinetics to the presence of a high dislocation density that acted as nucleation sites for Mg 17 Al 12 precipitates. 8 The effect of SiC nanoparticles on manufacturing, micro- structure and hardness of Mg-SiC nano-composites was studied by Penther et al., who used 1 and 10 /% SiC nano-composites. Reportedly, the nanoparticles pin the grain boundaries and trigger dynamic recrystallization of the Mg matrix. 9 As mentioned above, the related studies on the use of B 4 C as a reinforcing agent, generally involve minor weight fractions of reinforcement material. The present research, on the other hand, aims to examine the addition of a relatively higher weight fraction (50 %) and to pro- vide a further insight into the hot-pressed AZ91-B 4 C combination on which a scarce number of studies have been encountered, despite their wide applicability in fabrication of composites. In this regard, the microstruc- ture, hardness and dry-sliding-wear performance of metal-matrix composites reinforced with varying weight fractions of B 4 C(5w/%,10w/%,20w/% and 50 w/%) were investigated. The produced samples were investi- gated by means of Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDS), and then they were subjected to dry-sliding-wear tests under a 5-N load at room temperature, to gain an insight into the dry-sliding-wear performance of the composites produced with hot pressing. 2 MATERIALS and METHODS 2.1. Powder preparation and characterization AZ91 was granted by the Esan Company in bulk form. AZ91 magnesium alloy ingot (8 kg) with 637 mm × 139 mm × 70 mm dimensions was initially cut into smaller pieces with a band-sawing machine, and the obtained pieces were machined on a numerical control vertical mill to obtain the material in chip form. Following the machining operation, the obtained chips were ground to obtain finer particles. The particles obtained after fine milling of the AZ91 ingot were sieved with consecutive mesh sizes (150 μm, 200 μm and 250 μm) and those obtained under 150 μm mesh size were subjected to a particle size distribution analysis. Boron carbide was purchased in powder form from the Bor Optik Engineering R&D Company. The chemical analysis results provided by this supplier show that the boron carbide powder includes 77.96 w/% boron, 20.70 w/% carbon, and 0.31 w/% Fe, and 0.22 w/% boron oxide. The chemical composition of AZ91 and boron car- bide were provided from the suppliers. AZ91 alloy’s composition is Mg (88–90.50 %), Be (0.0005–0.0015 %), Al (8.50–9.50 %), Cu (Max. 0.025 %), Ca (Max. 0.010 %), Zn (0.45–0.90 %), Mn (0.17–0.40 %), Ni (Max. 0.001 %), Fe (Max. 0.004 %), Si (Max. 0.050), Sn (Max. 0.010 %), Zr (Max. 0.010 %), Pb (Max. 0.010 %), Ti (Max. 0.010 %), P (Max. 0.010 %). 10 Both powders were subjected to particle size distribu- tion analysis using a Malvern Mastersizer 3000 device. In the particle size distribution analysis, all the particle size measurements were done in wet mode. Deagglome- ration and dispersion of the particles was further ensured through ultrasonic treatment (of 120 s) prior to measure- ment. In the particle size distribution analysis, AZ91 magnesium alloy’s refractive index was 0.900 and dis- persant refractive index of water was 1.330. The specific surface area was 88.46 m 2 /kg. The uniformity of the con- centration was 0.716. The boron carbide refractive index was 1.570 and the dispersant refractive index of water was 1.330. The specific surface area was 2147 m 2 /kg. The uniformity of concentration was 8.126. The compo- sitions of powders were verified using a RIGAKU SmartLab TM X-ray Diffractometer. 2.2. Fabrication of composites with hot pressing In this work, the metal-matrix composites were ob- tained via hot pressing of AZ91 and boron carbide powders using a MSE Technology-HP-1200 hot-pressing machine. B 4 C + AZ91 composite powders were prepared by mixing5%B 4 C, 10 % B 4 C, 20 % B 4 C and 50 % B 4 C via powder metallurgy. Powder mixtures in 6 gr weight were homogeneously mixed and placed in a mold and subjected to a pressure of 10 MPa, 15 MPa and 45 MPa in the hot-pressing machine for a period of1hat515°C, as given in Table 1. The diameter of the fabricated B 4 C+AZ91 composite samples is 15 mm. After cooling down, the sintered samples were cold mounted and ground with 120, 320, 600 and 1000 grit-size SiC papers prior to microhardness measurements and dry-sliding- wear tests. 2.3. Sample characterization and wear tests Hardness data was acquired using a Qness Q10 (Aus- tria) hardness tester. The average of five micro-hardness measurements and the resulting standard deviations were T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... 434 Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 calculated. To avoid a large scattering of the measured values the highest possible indentation load (HV0.5) was used with 15 s dwelling time. Scanning Electron Micro- scope (SEM) micrographs and EDS results of the sample cross-sections were obtained using a TESCAN MAIA3 XMU scanning electron microscope. EDS spectra were obtained by taking at least three measurements on the SEM micrographs. Dry-sliding-wear tests were carried out on a recipro- cating pin-on-disk tribometer (Turkyus) using a WC abrader ball (6-mm diameter and 1800-HV hardness) in an atmospheric environment at room temperature. The test parameters were 100-m sliding distance, 0.03-m/s sliding speed and 5-N load (Table 2). The oscillation distance on the test rig was 10 mm. Frictional forces in grams were obtained from the load cell that instant- aneously transfers the friction data (with 1 second inter- vals) to the software of the test rig on a computer system. The obtained frictional forces were used to derive the coefficient of friction graphs using the load parameter. Table 2: Wear parameters Parameters Values 1 Load 5 N 2 Sliding speed 0.03 m/s 3 Sliding distance 100 m The maximum Hertzian contact pressure was calcul- ated as 787.8 MPa using the following Equation (1) and Equation (2): 11 a F v E v E RR = − − − ⎡ ⎣ ⎢ ⎤ ⎦ ⎥ + ⎡ ⎣ ⎢ ⎤ ⎦ ⎥ 3 11 4 11 1 2 1 2 2 2 12 3 (1) where a is the radius of the contact area; E 1 and E 2 are the moduli of elasticity, v 1 and v 2 are the Poisson’s ratios, and R 1 and R 2 are the radii of the sphere (tung- sten carbide spherical abrader with 6 mm) and the flat surface (AZ91+B 4 C metal matrix composite, R is consi- dered %), respectively. P F a max = 3 2 2 π (2) where P max is the maximum contact pressure at the centre of the circular contact area, F is the applied load and a is the radius of the contact area from Equation (1). The wear volume (volume loss) after each test was measured using a 3D optical profilometer (Huvitz-HDS 5800). The area measurements were taken from two different representative cross-sectional planes that were obtained via five different 3D optical profilometer measurements (Figure 1). The average of the resulting ten area measurements (in square millimeters) was multi- plied by the 10-mm oscillation distance to evaluate the approximate wear volumes on each sample surface. T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 435 Table 1: The composite materials and their physical properties No. Material M i (g) M s (g) h (mm) T s (°C) Press (MPa) 1 AZ91+ B 4C (% 5) 5.7 g + 0.3 g 4.8 g 17.9 mm 515 (°C) 10 MPa 2 AZ91+ B 4 C (% 10) 5.4 g + 0.6 g 4.8 g 17.3 mm 515 (°C) 10 MPa 3 AZ91+ B 4 C (% 20) 4.8 g + 1.2 g 5.5 g 19.7 mm 515 (°C) 15 MPa 4 AZ91+ B 4C (% 50) 3.0 g + 3.0 g 5.8 g 21.6 mm 515 (°C) 45 MPa Mi: Initial mass amount; Ms: Final mass amount; h: Height of samples; Ts: Sintering temperature; Press: Applied press on samples Figure 1: 2D and 3D profilometer images of AZ91+ B 4 C (%5) 3 RESULTS AND DISCUSSION 3.1. Powder characterization results The particle size analysis results of boron carbide and AZ91 particles used are given in Figure 2 and Figure 3. The results for B 4 C were obtained as 1.23 μm in Dv (10), 4.01 μm in Dv (50) and 127 μm in Dv (90) as given in Figure 2. The results for AZ91 powders were obtained as 40.3 μm in Dv (10), 126 μm in Dv (50) and 318 μm in Dv (90) as given in Figure 3. Dv (10), Dv (50) and Dv (90) correspond to the 10 %, 50 % and 90 % cumulative percentages, which are commonly used in cumulative particle size distribution analysis. D V (50) refers to the maximum particle dia- meter under which 50 % of the sample volume exists, thus it is also referred to as the median particle size. It is possible to observe the significant changes in the main particle size and the extreme points of distribution result- ing from the presence of fine or oversized particles/ agglomerates by monitoring these three parameters. 12 The uncommon distribution of B 4 C particle size, shown in Figure 2, is due to the irregular shapes of B 4 C parti- cles, which is also reported by Liu et al. 7 As seen in Figure 3, the AZ91 particles exhibit a relatively more even distribution and this is attributed to the sieving pro- cess, which enabled AZ91 particle sizes to be confined within a specific mesh interval. The XRD analysis results of the boron carbide and AZ91 magnesium alloy powders are shown in Figure 4. The peaks belonging to B 4 C (Figure 4a) and aluminium magnesium (Figure 4b) verify the compositions of the powders obtained from the suppliers. 3.2. SEM and EDS results Figure 5a to 5d shows the 500× and 1000× SEM micrographs of AZ91+B 4 C composites with 5 %, 10 %, 20 %, 50 % B 4 C addition, respectively. In Figure 5a, the presence of B 4 C particles is clearly visible in the darker tones. In the figure the particle boundaries of the matrix material are clearly disting- uished in the first three samples (Figures 5a to 5c) and they become indistinct in the case of 50 w/% reinforce- ment ratio (Figure 5d). This significant difference in Figure 5b is ascribed to the formation and accumulation of dislocations which result in increased grain refine- ment exerted by the hard B 4 C particulates on the matrix particles as a result of sintering conditions, hence the for- mation of smaller grains. A similar effect was observed by Singh et al. who synthesized an Al-MWCNT com- posite to examine the effect of powder milling and rein- forcement addition on sintering kinetics and mechanical properties. 13 During the EDS analysis, spectrum measurements were taken from at least three different points on the specimens and the most representative spectra are shown in Figure 6. T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... 436 Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 Figure 4: Qualitative analysis results by XRD of a) boron carbide and b) aluminum magnesium Figure 3: Particle size analysis result of AZ91 powder sieved under 150 μm mesh size Figure 2: Particle size analysis result of boron carbide powder The EDS results show that Mg, O, C, B, Al and Zn elements are present in the composition of the alloy. In addition to these elements, remarkable weight fractions of oxygen are observed in all the composite samples. This is attributable to the oxidation of the B 4 Ca n d Al-Mg composite to a considerable extent on the outer surfaces of composites during the hot sintering process, which took place under atmospheric conditions. As also stated by Çelik and Seçilmiº, particularly Al and its alloys easily react with oxygen to become more stable. 14 3.3. Microhardness measurement results Figure 7 shows the Vickers hardness values of the produced composites. As shown in the figure, the hard- ness of the produced composites was found as 60.62 HV, 61.38 HV, 65.65 HV and 72.56 HV for 5 w/%,10w/%, 20 w/% and 50 w/% B 4 C addition respectively, which is indicative of increasing hardness by B 4 C addition. Such contributing effect of hard particulate addition on the hardness of fabricated composites has been re- peatedly reported in various studies. Topçu et al. evaluated the effect of B 4 C addition (up to 20 w/%) and sintering temperature on the hardness of the fabricated samples. They attributed the increase in hardness with increasing reinforcement ratio to the dispersion strengthening effect. 15 Likewise, in their research on the effect of particulate reinforcement and heat treatment on the hardness and wear properties of nanocomposites, Sameezadeh et al. reported a considerable increase in the hardness of all composites as compared to the base alloy. T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 437 Figure 5: 500× and 1000× SEM micrographs of composites with a) 5 w/%,b)10w/%, c) 20 w/%,d)50w/% B 4 C addition Figure 7: Microhardness measurements of the samples Figure 6: EDS spectra of: a) AZ91 + B 4 C( 5w/%), b) AZ91+B 4 C (10 w/%), c) AZ91+B 4 C (20 w/%), d) AZ91+B 4 C (50 w/%) Reportedly, hard particulates in the composite matrix act as a barrier against dislocation movements within the matrix, thus showing higher resistance against the indenter of the microhardness device. 16 In the present research the same contributing trend of reinforcement addition on hardness is also encountered, although to an unexpectedly lesser extent. There is a considerable difference between 5 w/% and 50 w/% B 4 C addition, and yet the hardness increased by nearly 19 % (Figure 7). We describe this as follows. Related studies on the utilization of B 4 C and other reinforcing agents generally involve the use of hard particulates at lower ratios (generally under 25 %). The current research, however, involves the use of a significantly higher amount, which is 50 %. Sintering is the consolidation of loose or weakly bonded powders with or without pres- sure at high temperatures which are close to their melting points. 17 During sintering, hard particulates pin dislocations in the matrix, thus restricting their move- ment, which improves the hardness of the matrix ma- terial through grain refinement. Yin et al. reported such grain refinement and consequent improvement in hard- ness in which case B 4 C was the matrix material that was reinforced with Ti 3 SiC 2 and Si particles via spark plasma sintering. 18 However, this applies up to a certain weight fraction of the reinforcing agent for the same sintering conditions. In the present case, in which the hard parti- culates and matrix material have the same weight frac- tion, a higher sintering pressure was required to achieve the same structural integrity with that of the samples having a lower reinforcement ratio. As also proposed by Xiong et al. 19 densification of B 4 C particulates is a challenging process as a result of its strong covalent bonding and low self-diffusion coefficient. This also arises from the high electron density in inter-atomic regions for B 4 C, 20 hence the reported sintering pressures in Table 1. Although we applied a significantly higher sintering pressure (45 MPa) for the sample with 50 w/% reinforcement, this certainly fell short as we applied the same sintering temperature for all four samples, which in turn resulted in a relatively low difference between the hardness values gained by lowest and highest reinforce- ment ratios. 3.4. Wear test results Figure 8 shows the worn volumes of the composites with 5, 10, 20 and 50 w/% B 4 C addition. As shown in the graph, the worn volumes of the fabricated composites decreased with increasing B 4 C addition for the first two samples and increased with increasing reinforcement ratio after the second sample. The decrease in wear volumes of the first two compo- sites (with 5 w/% and 10 w/% B 4 C) is consistent with Archard’s equation, which states that higher hardness results in lower wear rates. Archard, in 1953, formulated this phenomenon with the following equation for wear: Wk ps H = n (2) As indicated by the equation, the volume of the ma- terial removed (W) is directly proportional to the sliding distance (s), normal pressure (p) and the dimensionless wear coefficient (k), and inversely proportional to the hardness of the surface being worn away (H). 21 In addi- tion to Archard’s approach, hard reinforcement materials are also reported to affect the contact area between sliding counterparts which leads to reduced wear rates during sliding. 22 Turan et al. likewise evaluated the effect of B 4 C and SiC particle reinforcements on the wear pro- perties of magnesium matrix metal composites. 23 They also reported that, increasing B 4 C addition decreased the specific wear rates under a 5-N load. In another research, Uthayakumar et al. also reported an increase in the wear resistance of Al–SiC–B 4 C hybrid composites with the addition of SiC and B 4 C particles. 24 The other two samples, however, exhibited increased wear volumes with increasing B 4 C amount and sample 4 with 50 w/% reinforcement ratio displayed the lowest wear resistance. Such a compromise in wear perform- ance despite increasing hardness in the composites with reinforcement addition is also reported by other re- searchers. Çelik and Seçilmiº proposed that, although increasing reinforcement ratio continuously increases the hardness and other mechanical properties of composites, T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... 438 Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 Figure 9: Friction-coefficient graphs of samples (S1: 5 w/% B 4 C addition, S2: 10 w/% B 4 C addition, S3: 20 w/% B 4 C, S4: 50 w/% B 4 C addition) Figure 8: Worn volume graph of samples (S1: 5 w/% B 4 C addition, S2: 10 w/% B 4 C addition, S3: 20 w/% B 4 C, S4: 50 w/% B 4 C addition) wear performance is improved only up to a certain volume fraction. 14 Likewise, Baradeswaran and Elaya Perumal reported in their research related to the influ- ence of B 4 C on tribological and mechanical properties of Al7075/B 4 C composites that the best wear performance was obtained by 10 w/% B 4 C addition among (5, 10, 15, and 20) w/% B4C addition, which is quite the same case with the current study. 25 We further propose that, such an increase in the worn volume in the samples with 20 and 50 w/% B 4 C addition is attributable to the need for higher sintering conditions (sintering temperature and pressure) to obtain the same structural integrity with the samples having lower B 4 C ratios, as also mentioned in the previous Section 3.3 Microhardness Measurement Results. Despite the significantly higher sintering pres- sure, the adverse effect of using the same sintering tem- perature for all samples, on the structural integrity of sample 4 (50 w/% reinforcement), manifested itself to quite a larger extent in the case of wear, as sample 4 ex- hibited the highest wear volume (Figure 8). Figure 9 shows the coefficient of friction (COF) values belonging to the composites with 5 w/%,10w/%, 20 w/% and 50 w/% B 4 C addition. Friction-coefficient values of all samples were found to vary between 0.075 and 0.5. In the graph, Sample 2 exhibits the lowest COF and Sample 4 exhibits the highest COF, which is indi- cative of the same trend with wear volumes. In the evaluation of COF values, however, factors other than hot-pressing conditions should be taken into account as COF can be governed by a few other phenomena. During sliding wear, the relative sliding motion of two surfaces that are in contact by the effect of an applied load results in a shear stress, which induces the occurrence of a fric- tional force. The resulting frictional force depends on various variables including the sliding speed, applied load, the contact area between the surfaces, the tempera- ture rise induced by friction and the various characteris- tics of mating surfaces. 26 During friction, the exerted normal and shear stresses generate frictional heat which results in the deformation and fracture of asperities, leading to material exchange between the abrader surface and the worn surface, and in turn inducing the formation of a mechanically mixed layer (MML) along with the formation of a boron oxide layer that arises from the oxidation of B 4 C. In their research, Uthayakumar et al. reported the formation of such a tribo-layer that occurred during the wear test of Al–SiC–B 4 C hybrid composites. 24 These together play an important role in the reduction of COF and wear through protecting the material from sub-surface and surface deformation. 24,26 As stated by Singh et al., when this mechanically mixed layer be- comes significantly thick, it becomes unstable as the cracks easily form at the subsurface and propagate through the mixed layer, leading to severe wear, which is also referred to as seizure. Reportedly, the formation and thickening of MML happens very fast or does not happen at all with increased load and sliding-speed con- ditions. 26 In the present research, the only variable during the wear tests was the reinforcement ratio and we ascribe the decreasing trend of COF until 10 w/% reinforcement to the maintenance of this layer; and the subsequent in- creasing trend to the fast-formation or non-formation of this mechanically mixed layer, with increasing B 4 C content. A similar case was encountered by Çelik and Seçilmiº, who investigated the wear behavior of Al matrix composites reinforced with different B 4 C addi- tion. 14 As also elaborated earlier, the sample with 50 w/% lacks structural integrity and ductility as compared to the other samples, thus failing to maintain this lubricating layer due to its relatively more brittle structure. 4 CONCLUSIONS Metal-matrix composites with AZ91 (matrix) and varying B 4 C addition (5 w/%,1 0w/%,2 0w/% and 50 w/%) were fabricated by powder metallurgy and hot pressing and subjected to SEM and EDS analyses and dry-sliding-wear tests to evaluate the effect of B 4 C addition on the microstructure, hardness and wear per- formance of the sintered composites. As a result, the following conclusions are drawn: As compared to the other three composites, hot pressing of the composite with 50 w/% B 4 C required a significantly higher sintering pressure (10–15 MPa vs. 45 MPa) at the same sintering temperature (515 °C) than the other composites. High weight percentages of oxygen were found in the EDS analyses as a result of the high affinity of Al and Mg to oxygen. Increasing B 4 C addition resulted in increased hard- ness values for all composites, although the rate of in- crease in hardness is significantly lower than the increase in reinforcement ratio. The lowest wear volume and coefficient-of-friction values were obtained with 10 w/% B 4 C, whereas the highest values were obtained with 50 w/% B 4 C. Acknowledgment The authors acknowledge the help of Lecturer Halil EªGÝN in Bartin University Central Research Laboratory Application and Research Center for XRD and SEM analyses. The valuable help of Res. Asst. Fatih AYDIN in Karabuk University-MARGEM is also acknowledged. Conflicts of Interest: The authors declare no conflict of interest. 5 REFERENCES 1 T. Ozdemir, The mean grain size determination by ultrasonic velocity technique in basic boron carbide of ceramic metal composites, Afyon Kocatepe University (Master’s Thesis), 2006 T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440 439 2 M. Kök, Fabrication of 2024 aluminium alloy metal matrix com- posites reinforced with Al2O3 particles, Science and Engineering Journal, 4 (2001) 2, 131–142 3 J. M. Torralba, C. E. da Costa, F. Velasco, P/M aluminum matrix composites: an overview, J. Mater. Process. Technol., 133 (2003), 203–206, doi:10.1016/S0924-0136(02)00234-0 4 S. M. R. Mousavi, S. M. Abarghouie Seyed Reihani, Investigation of friction and wear behaviors of 2024 Al and 2024 Al/SiCp composite at elevated temperatures, J. Alloys Compd. 501 (2010), 326–332, doi:doi.org/10.1016/j.jallcom.2010.04.097 5 Y. Wang, H. Y. Wang, K. Xiu, H. Y. Wang, Q. C. Jiang, Fabrication of TiB2 particulate reinforced magnesium matrix composites by two-step processing method, Mater. Lett. 60 (2006) 12, 1533–1537, doi:10.1016/j.matlet.2005.11.065 6 B. Yavas, G. Goller, Investigation the effect of B4C addition on pro- perties of TZM alloy prepared by spark plasma sintering, Int. Journal of Refractory Metals and Hard Materials, 58 (2016), 182–188, doi:10.1016/j.ijrmhm.2016.04.020 7 R-Z. Liu, P. Chen, J-M. Wu, S. Chen, A-N. Chen, J-Y. Chen, S-S. Liu, Y-S. Shi, C-H. Li, Effects of B4C addition on the microstructure and properties of porous alumina ceramics fabricated by direct selective laser sintering, Ceramics International, 44 (2018), 19678–19685, doi:10.1016/j.ceramint.2018.07.220 8 B. N. Sahoo, S. K. Panigrahi, Effect of in-situ (TiC-TiB2) reinforce- ment on aging and mechanical behavior of AZ91 magnesium matrix composite, Materials Characterization, (2018), doi:10.1016/ j.matchar.2018.03.002 9 D. Penther, A. Ghasemi, R. Riedel, C. Fleck, S. Kamrani, Effect of SiC nanoparticles on manufacturing process, microstructure and hardness of Mg-SiC nanocomposites produced by mechanical milling and hot extrusion, Materials Science & Engineering A 738, (2018), 264–272, doi:10.1016/j.msea.2018.09.106 10 https://www.esanmagnezyum.com/Download/images/AZ91-TDS- EN.pdf, 19.11.2018 11 J. E. Shigley, C. R. Mischke, R. G. Budynas, Mechanical Engineering Design, 7 th ed., McGraw Hill, New York 2004, 161–166 12 https://www.cif.iastate.edu/sites/default/files/uploads/Other_Inst/ Particle%20Size/Particle%20Characterization%20Guide.pdf, 19.11.2018 13 L. K. Singh, A. Bhadauria, T. Laha, Al-MWCNT nanocomposite synthesized via spark plasma sintering: effect of powder milling and reinforcement addition on sintering kinetics and mechanical properties, J Mater Res Technol, (2018), doi:10.1016/j.jmrt.2018. 03.005 14 Y. H. Çelik, K. Seçilmiº, Investigation of wear behaviours of Al matrix composites. reinforced with different B4C rate produced by powder metallurgy method, Advanced Powder Metallurgy, 28 (2017) 12, 2218–2224, doi:10.1016/j.apt.2017.06.002 15 I. Topcu, H. O. Gulsoy, N. Kadioglu, A. N. Gulluoglu, Processing and mechanical properties of B4C reinforced Al matrix composites, J. Alloy Compd., 482 (2009), 516–521, doi:10.1016/j.jallcom.2009. 04.065 16 M. Sameezadeh, M. Emamy, H. Farhangi, Effects of particulate rein- forcement and heat treatment on the hardness and wear properties of AA 2024-MoSi2 nanocomposites, Materials and Design, 32 (2011), 2157–2164, doi:10.1016/j.matdes.2010.11.037 17 J. Rojek, S. Nosewicz, M. Mazdziarz, P. Kowalczyk, K. Wawrzyk, D. Lumelskyj, Modeling of a sintering process at various scales, Procedia Engineering, 177 (2017), 263–270, doi:10.1016/j.proeng. 2017.02.210 18 S.-P. Yin, Z-H. Zhang, X.-W. Cheng, T.-J. Su, Z.-Y. Hu, Q. Song, H. Wang, Spark plasma sintering of B4C-TiB2-SiC composite ceramics using B4C,Ti3SiC2and Si as starting materials, Ceramics Interna- tional, 44 (2018), 21626–21632, doi:10.1016/j.ceramint.2018.08.245 19 Y. Xiong, X. Du, M. Xiang, H. Wang, W. Wang, Z. Fu, Densification mechanism during reactive hot pressing of B4C-ZrO2 mixtures, Journal of the European Ceramic Society, (2018), doi:10.1016/ j.jeurceramsoc.2018.05.016 20 V. Domnich, S. Reynaud, R. Haber, A. M. Chhowalla, Boron car- bide: structure, properties, and stability under stress, J. Am. Ceram. Soc., 94 (2011) 11, 3605–3628, doi:10.1111/j.1551-2916.2011. 04865.x 21 A. Zmitrowicz, Wear patterns and laws of wear–Areview ,J.Theo. App. Mech., 44 (2006) 2, 219–253 22 X. Jiang, N. Wang, D. Zhu, Friction and wear properties of in-situ synthesized Al2O3 reinforced aluminum composites, Trans. Non- ferrous Met. Soc. China, 24 (2014), 2352–2358, doi:10.1016/ S1003-6326(14)63356-2 23 M. E. Turan, H. Zengin, E. Cevik, Y. Sun, Y. Turan, H. Ahlatci, Wear behaviors of B4C and SiC particle reinforced AZ91 magnesium matrix metal composites, World Academy of Science Engineering and Technology International Journals of Materials and Metallurgical Engineering 10 (2016) 9, 1224–1227 24 M. Uthayakumar, S. Aravindan, K. Rajkumar, Wear performance of Al-SiC-B4C hybrid composites under dry sliding conditions, Mater. Des., 47 (2013) 456–464, doi:10.1016/j.matdes.2012.11.059 25 A. Baradeswaran, A. Elaya Perumal, Influence of B4C on the tribo- logical and mechanical properties of Al 7075–B4C composites, Composites Part B: Engineering, 54 (2013), 146–152, doi:10.1016/ j.compositesb.2013.05.012 26 M. Singh, B. K. Prasad, D. P. Mondal, A. K. Jha, Dry sliding wear behaviour of an aluminium alloy–granite particle composite, Tribo- logy International, 34 (2001), 557–567 T. Ö. ÖGE et al.: EFFECT OF B4C ADDITION ON THE MICROSTRUCTURE, HARDNESS AND DRY-SLIDING-WEAR ... 440 Materiali in tehnologije / Materials and technology 53 (2019) 3, 433–440