UDK 66.018.95:669.71:620.18:620.17 ISSN 1580-2949 Izvirni znanstveni članek MATER. TEHNOL. 35(3-4)99(2001) M. VUKČEVI] ET AL.: THE CORRELATION BETWEEN THE PROPERTIES AND THE TYPE OF ... THE CORRELATION BETWEEN THE PROPERTIES AND THE TYPE OF REINFORCEMENT IN Al-MATRIX POWDER-METALLURGY COMPOSITES KORELACIJA LASTNOSTI IN VRSTE OJAČITVE V MATIČNIH KOMPOZITIH IZDELANI PO METODI METALURGIJE PRAHU Mira Vukčevi}, Kemal Deliji}, DarkoVuksanovi} Faculty of Metallurgy and Inorganic Technology, University of Montenegro, Cetinjski put b.b., 81000 Podgorica, Crna gora, Yugoslavia e-mail: miravŽcg.ac.yu Prejem rokopisa - received: 2001-01-03; sprejem za objavo - accepted for publication: 2001-03-20 Al-SiC particles (Al-SiCp) composites were fabricated by the admixture method using an Al-coated reinforcement and atomised matrix powder. The microstructure of the samples in the hot-pressed condition with the homogeneously dispersed reinforcement was monitored. The use of a coated reinforcement to make composites by powder metallurgy (PM) methods was found to yield superior mechanical properties than the use of a mixture of reinforcement and matrix powder. The coated-reinforcement sample had lower porosity, increased hardness and a higher compressive yield strength. The coating diminished direct reinforcement-reinforcement contact and promoted sintering with a resulting low porosity. Key Words: composites, coated-reinforcement, metal matrix Kompoziti Al-SiC (SiCp) so bili izdelani po metodi aditivnega mešanja iz ojačitve, prekrite z aluminijem, in vodno atomizi-ranega prahu. Mikrostruktura je bila preiskana po vročem stiskanju zlitine z enakomerno porazdeljeno ojačitvijo. Uporaba prekriteojačitveza izdelavo kompozita po P/M-metodi dajeboljšemehanskelastnosti kot uporaba zmesi prahu ojačitvein matične kovine. Manjša je poroznost, večja je trdota in večja je tlačna meja tečenja. Prekritje je zmanjšalo kontakt med zrni ojačitvein omogočilo sintranjez majhno poroznostjo. Ključne besede: Al-kompoziti, prekrita ojačitev, kovinska matica 1 INTRODUCTION Theincorporation of silicon-carbideparticles (SiCp ) in metal-matrix composites (MMCs) results in improved wear resistance, thermal resistance, hardness, yield strength, etc. These properties increase the utility of metals, which are traditionally known for being ductile, moderately hard, having good tensile strength and moderate thermal resistance. SiCp havefound themost important application in aluminum-matrix composites. Extensive reviews of the deformation mechanisms that occur during the incorporation of fibres, particles and whiskers into the metal matrices have been presented in literature, with using of short fibres, preform infiltration, extrusion and squeeze casting 1,2. Spray casting is a well-established technique in powder metallurgy (PM), that uses fibre reinforcement 3,4. Theuseof a different reinforcement technique, the so-called "coated-reinforcement method" 5, has been used to make copper-matrix composites, as well as copper-matrix and silver-matrix composites for use as brushes. In recent years, the coated-reinforcement method has been used by the Specialty Metal Products Division of AMETEK inc. to make Cu-Mo composites. Classical methods of conventional PM that use filler and metal matrix powder have been restricted to a low filler contact with an increasing filler volume fraction. In sintering processes, the working temperature is below the melting point of the matrix, but the reinforcement usually has a higher melting point than the matrix. Because of this, excessive reinforcement-reinforcement contacts lead to a composite with inferior properties due to ineffective reinforcement-reinforcement sintering at the relatively low processing temperature (lower than that required for reinforcement-reinforcement sintering). The ineffectively sintered reinforcements constitute defects in the composite. Reinforcement-reinforcement contact leads to a higher porosity level. The flow of the softened metal matrix, could be prevented and the intersticies would not be filled during sintering. This paper describes a solution to the problem that uses reinforcements coated with aluminum to eliminate the possibility of direct reinforcement-reinforcement contacts. The properties of the corresponding composites made by the coated-reinforcement method and by the admixture method were compared. It was found that the composites with aluminum-film-coated SiC particles were superior (compressive strength, hardness, electrical conductivity) to the corresponding composites made by theadmixturemethod. 2 EXPERIMENTAL TheAl-SiCp composites containing up to 15 wt% of reinforcement were fabricated by two methods. The first MATERIALI IN TEHNOLOGIJE 35 (2001) 3-4 99 M. VUKČEVI] ET AL.: THE CORRELATION BETWEEN THE PROPERTIES AND THE TYPE OF Table 1: Chemical composition of aluminum alloy (wt.%) Tabela 1: Kemična sestava aluminijeve zlitine (mas.%) Element Content Si 11.01 Cu 1.32 Be 0.25 Fe 0.97 Mo 0.15 Ni 0.90 Co 0.17 Mg 1.24 Mn 0.04 Al Balance Table 2: Chemical composition of SiCp filler (wt.%) Tabela 2: Kemična sestava polnila SiCp (mas.%) Element Cgraphite Simetal TiO2 Fe2O3 Al2O3 CaO MgO SiC Content 0.12 1.88 0.14 0.50 0.14 0.13 0.04 96.65 is the Al-coated method (using SiC particles coated with a thin film of aluminum), and thesecond is the admixture method (based on mixing Al powder and SiC particles). Thechemical composition of theAl-Si alloy used in this study is given in Table 1. The powder with a mean particle diameter (d50) of 150 µm (Figure 1) was madeby therotating-electrode process. The SiC particles used in this experiment were made in RUSE fertilizer factory in Slovenia. The chemical composition of SiC is shown in Table 2. TheSiCp was prepared by sieving six fractions: -30 µm, +30-75µm, +75-100 µm, +100-125 µm, +125-150 µm and over 150 µm. Thegranulation of -30 µm was used in the experiment. After mechanical preparation, the SiCp was chemically treated with a concentrated HCl solution for 30 min to eliminate metallic elements. In order to make the coated reinforcement, a thin aluminum film was deposited on thesurfaceof theSiCp using physical deposition. The matrix powder was kept under a vacuum of 10-4 Pa, then exposed to the flow of argon until the pressure reached 1Pa. The argon was ionized, the ions were accelerated by voltage of 2 kV towards theAl cathode. Thealuminum ions werethrown from the cathode and deposited on the powder surface. Thedeposition was uniform, becausetheparticles, so the number of particles which were not covered on the both sides was negligible. Mixing of the coated-reinforcement and the Al-Si-matrix powder was carried out in a ball mill. All the specimens were cold pressed in a graphite die to form a cylindrical green compact of 8-mm diameter and 10.5-mm heigh. The samples were pressed in a Carver Inc. Auto "C" series automatic hydraulic press, model 388. The preform was exposed to a pressure of 153 MPa during 25 min of cold pressing, then heated together with thediefor 20 min at 470 °C. TheSemi-solid system was subsequently hot pressed (380 °C) in the same die, for 10 min upon thepressureof 115 MPa. For thecomparison, thecorresponding composites madeby theadmixture method were fabricated under the same processing conditions. In both cases, the filler content varied as follows: 2, 5, 10, 15 wt%. ThePM routefor both methods is shown in Figure 2. Composite testing involved the following: density measurement, metallographic investigation, mechanical testing (compressive yield strength, compressive rupture strength, compressive deformation) and hardness testing. Themicrostructural characterisation was donewith a scanning electron microscope SEM JEOL JSM-840. Mechanical testing was carried out on a FPZ HECKERT RAUENSTEIN 100/1 standard testing machine. Hardness testing was done with standard Brinell hardness equipment (Detroit Testing machine) HB 2.5/1000/30. Figure 1: Scanning electron micrograph (SEM) of Al-Si powder Slika 1: Posnetek praha Al-Si v vrstičnem elektronskem mikroskopu (SEM) Figure 2: PM technique for coated filler and admixture methods Slika 2: PM-tehnika za prekrito polnilo in za konsolidacijo z mešanjem 100 MATERIALI IN TEHNOLOGIJE 35 (2001) 3-4 M. VUKČEVI] ET AL.: THE CORRELATION BETWEEN THE PROPERTIES AND THE TYPE OF 3 RESULTS 3.1 Microstructural analysis Figure 3 shows SEM micrographs of polished sections of the Al-SiCp composites. At the lower part of the cylindrical testing specimen the SiC particles are uniformly dispersed within the matrix (Figure 3a). Near the top surface of the testing cylinder SiC particles were found at the original droplet boundaries, producing cell-typemicrostructure(Figure 3b). This is attributed to the presence of excess liquid phase in the upper part of the form and the rejection of SiC particles by the solidification front6. Electron microscopy confirmed that, for low reinforcement contents, there is no apparent microstructural difference between the composites made by the two methods. Composites made by both methods arenearly efreeof pores, with thedistribution of the reinforcement depending on the specimen’s height. We found that the weight per cent of the aluminum film formed on the SiC particles, under the same deposition conditions, increased with a decrease in the SiC particlesize. This is dueto thelarger surfacearea of Figure 4: SEM micrograph of aluminum-plated SiC particle Slika 4: SEM-posnetek zrn SiC, prekritih z aluminijem thesmaller sizeof SiC particles. Figure 4 shows a micrograph of an aluminum-plated SiC particle. Theaveragealuminum film thickness was 2-3 µm. A scanning electron micrograph of a metal-matrix composite after hot pressing is shown in Figure 5. The dark parts with irregular shapes are the pores which are located among SiC particles. During the hot pressing and pressure action the SiC particles cracked easily. This phenomenon can be observed in Figure 5a. Thelarger theparticlesize, thehigher thepossibility of cracking. Figure 5b reveals that there is more porosity in the composites without coatings. In thecaseof composites made by the admixture method, SiC particles peel off easily during the process. The peeling of particles is due to the weak interfacial bonding between the SiCp and the matrix. It appears that the bonding is weak between the Al matrix and the noncoated reinforcement, but strong in the case of the coated reinforcement. 3.2 Physical and mechanical properties The density of the sintered composites was measured using thebuoyancy method (ASTM B328-92). The porosity was determined by: Vp=1-p/p0 (1) Figure 3: SEM of MMCs with 10 ?/o SiCp coated filler; a) dispersed-structure type; b) cell type Slika 3: SEM-posnetek MMCs z 10 vol.% SiCp prekritega polnila; a) struktura disperznega tipa; b) celična mikrostruktura where: Vp is theporevolumefraction, ? the measured density, ?0 theoretical density. For the measurement of the electrical conductivity, standard four-probe testing was used. Measured properties are given in Table 3. Table 3 shows that the measured physical properties of the differently processed composites are almost the same for a small reinforcement content (2 wt%). In the case of composites with a higher reinforcement content the coated method appears to be supperior to the conventional admixture method. MATERIALI IN TEHNOLOGIJE 35 (2001) 3-4 101 M. VUKČEVI] ET AL.: THE CORRELATION BETWEEN THE PROPERTIES AND THE TYPE OF Figure 5: SEM of 15 ?/o SiC matrix after hot processing; a) coated-filler compact; b) admixture-method compact Slika 5: SEM posnetek 15 vol.% SiC matice po vročem procesiranju; a) stisnjenec s prekritim polnilom; b) stisnjenec z dodatkom polnila 3.3 Mechanical properties The dependence of composite hardness on the of SiCp content is presented in Figure 6. The hardness increases with increasing SiCp content for both methods of composite preparation. The composites produced by the coated-rein-forcement method show an improvement in the hardness (up to ?5%) in thecaseof thehigher reinforcement content. Theinfluenceof SiCp content on the compressive yield stress is presented in Figure 7. Thecompressive yield stress increases with increasing content of reinforcement in composites made by both methods. The Table 3: Properties of Al-matrix composites Tabela 3: Lastnosti kompozitov z aluminijevo matico Figure 6: Influence of SiCp content on hardness of MMCs Slika 6: Vpliv vsebnosti SiCp na trdoto MMCs Figure 7: Influence of SiCp content on compressive yield strength Slika 7: Vpliv vsebnosti SiCp na tlačno mejo tečenja use of the coated reinforcement means higher values of compressive yield stress, compared to the composites madeby theadmixturemethod. All the specimens were compressed without fracturing, but small cracks developed on the specimen surface. Because the composites show ductile behaviour, the values for compressive strength may only bee arbitrary values, dependent on the degree of distortion Composite Al/SiCp 2% wt. of SiCp Al/SiCp 5% wt. of SiCp Al/SiCp 10% wt. of SiCp Al/SiCp 15% wt. of SiCp Property Admix Coated Admix Coated Admix Coated Admix Coated Porosity vol. % 0.18 0.18 0.21 0.20 0.27 0.22 0.42 0.37 El.Cond. MS/m 21.2 21.2 17.8 18.5 16.32 17.9 14.98 15.21 102 MATERIALI IN TEHNOLOGIJE 35 (2001) 3-4 M. VUKČEVI] ET AL.: THE CORRELATION BETWEEN THE PROPERTIES AND THE TYPE OF Figure 8: Influence of SiCp content on the compressive strength at 35% of thecompressivestrain ratio Slika 8: Vpliv vsebnosti SiCp na tlačno trdnost pri tlačnem razmerju 35 % that is regarded as effective failure for the material. The dependenceof the compressive strength at 35% of the compressivestrain ratio, on theSiCp particles content is shown in Figure 8. It increases with the increasing content of SiC particles, and MMCs made by the coated-reinforcement method show insignificantly higher levels of compressive strength compared to the composites made by theadmixturemethod at thesamelevel of compressive strain. 4 DISCUSSION Thedensity of theof theAl-SiCp composites decreases with an increase in reinforcement volume fraction under thesameprocessing conditions. This is becauseof theformation of porosity resulting from diffusivelimitation of thematrix atoms bonded by the SiCp. Theporosity was mainly formed among theSiC particles as shown in Figure 5. In thecaseof noncoated reinforcement, clustering can occur more easily than in the case of coated reinforcement. This can lead to the formation of porosity after hot pressing. The densification of the composites can be improved by increasing the sintering pressure. In that case, the rupture of the SiC reinforcement takes place more easily at high volumefractions. A higher reinforcement volume fraction and a higher porosity can hinder the electrical conductivity of the composites. The conductivity of a coated-reinforcement compositeis higher than theconductivity of the admixture-method composite, due to the lower porosity and more efficient bonding of the Al-SiCp interface. The hardness and compressive yield strength are higher for composites made by the coated-reinforcement method. The poor mechanical properties of the MATERIALI IN TEHNOLOGIJE 35 (2001) 3-4 admixture-method composite is due to the ineffective bonding between the contacting reinforcement units. The bonding strength between the Al matrix and the reinforcement unit will be reduced in this case and more brittlefracturecan beinitiated in thesecomposites. That can make these composites weaker than those made by the coated-reinforcement method. The strength of the coated-reinforcement composites is better, the densification is higher, the interfacial bonding better, as is theability to inhibit crack propagation. 5 CONCLUSIONS The coated-reinforcement method was found to be a successful way to produce MMCs. 1. Thequasi-uniform surfaceof an aluminum film can be formed on SiC particles by physical deposition. The film’s depth increased with decreasing SiC particlesize 2. Densification, strength, hardness and electrical conductivity increasein thecaseof coated reinforcement method. 3. The level of porosity appears to be higher in the admixture-method composites and it increases with an increasing volume fraction of reinforcement. 4. The coated-reinforcement method is effective for making composites with an increase in reinforcement content relative to the admixture method, because of the improved reinforcement-matrix bonding. The coating process does not increase the composite price much compared to the improvement in properties, because it does not depend on the amount of reinforcement, wheras some properties do. In the case of an electrically conducting reinforcement there is the possibility of using an electroplating process to coat the reinforcement, in some other cases electroless plating could be used. These are relatively cheap processes when compared to the contribution they maketo thecompositeproperties. 6 REFERENCES 1 1. T. Zhang, J. R. G. Evans, M. Bevis: Control orientation in short fibre-reinforced metal matrix composites, The International Journal of Powder Metallurgy, 32, (1996) 4, 331 2 G. Mott, P. K. Liaw: Correlation of mechanical and ultrasonic properties of Al/Sic metal matrix composites, Metallurgical Transactions, 19A (1988) 2233 3 Q. Zhang, R. H. Rangel, E. J. Lavernia: Nucleation phenomena during coinjection of ceramic particulates into atomised metal droplets, Acta Materialia, 44 (1996) 9, 3693 4 C. Park, M. Ho Kim, A. Lawley: Microstructure and wear response of spray cast Al-Si/SiCp composites 5 P. Yih, D. L. Chung: Powder metallurgy fabrication of Metal matrix composites using coated fillers, The International Journal of powder metallurgy, 32 (1995) 4, 335 6 M. Gupta, F. A. Mohamed, E. J. Lavernia: The effects of solidification phenomena on the distribution of SiC particulates during spray atomisation and co-deposition, International Journal of rapid solidification. 6 (1991) 247 103