D. MANICKAM et al.: EXPERIMENTAL INVESTIGATION OF LM25 ALLOY REINFORCED WITH SiC, Gr ... 395–398 EXPERIMENTAL INVESTIGATION OF LM25 ALLOY REINFORCED WITH SiC, Gr AND MOA PARTICLES EKSPERIMENTALNE RAZISKAVE NA Al ZLITINI LM25, OJA^ANI Z DELCI SiC, GRAFITA IN PEPELA MORINGE Dhanashekar Manickam, Senthil Kumar Velukkudi Santhanam * , Karthikeyan Sivagnanam Anna University, Department of Mechanical Engineering, Chennai 600025, Tamil Nadu, India Prejem rokopisa – received: 2018-03-09; sprejem za objavo – accepted for publication: 2018-12-20 doi:10.17222/mit.2018.038 An experimental investigation was performed on an LM25 aluminium alloy reinforced with silicon carbide (SiC), graphite (Gr) and moringa oleifera ash (MOA) particles. The composites with different proportions such as 5 w/% of SiC, 5 w/% of SiC + 1 w/% of Gr, 5 w/% of SiC + 3 w/% of Gr, 5 w/%SiC+1w/% MOA, and 5 w/% of SiC + 3 w/% of MOA were produced with the stir-casting method. The effects of the reinforcement particles on density, micro-hardness, grain size, porosity, particle distribution and microstructure were studied. A characterization study was made using optical microscopy (OP) and scanning electron microscopy (SEM). Based on the hardness and density results, the MOA-reinforced composites had better hardness and decreased porosity when compared to the Gr-reinforced composites. The MOA particles exhibited a homogeneous distribution in the matrix whereas the Gr particles had a few cluster formations. Keywords: LM25 aluminium alloy, moringa oleifera ash, stir casting, mechanical properties Avtorji opisujejo eksperimentalne raziskave na Al zlitini LM25, oja~ani z delci silicijevega karbida (SiC), grafita (Gr) in pepela moringe (MOE, angl.: Moringa Oleifera Ash). Kompoziti so vsebovali razli~ne dele`e posameznih delcev, to je: 5 w/% SiC, 5 w/%SiCin1w/% Gr, 5 w/% SiC in 3 w/% Gr, 5 w/% SiC in 1 w/% MOA, 5 w/% SiC in 3 w/% MOA. Kompozite so izdelovali s tehniko vme{avanja delcev v talino Al zlitine. Avtorji so nato raziskovali vpliv oja~itve (dodanih delcev) na gostoto, mikrotrdoto, velikost kristalnih zrn, poroznost in ostalo mikrostrukturo zlitine. Analize so izvedli z opti~no (OP) in vrsti~no elektronsko mikroskopijo (SEM) ter rentgensko strukturno analizo (XRD). Iz rezultatov meritev mikrotrdote in gostote ugotavljajo, da imajo z MOA oja~ani kompoziti bolj{o trdoto in manj{o poroznost v primerjavi z Gr oja~animi kompoziti. Delci MOA so enakomerno porazdeljeni v kovinski osnovi zlitine, medtem ko so se delci Gr zdru`evali oziroma tvorili skupke. Klju~ne besede: zlitina na osnovi aluminija LM25, pepel moringe, postopek litja z vme{avanjem delcev v talino Al zlitine, mehanske lastnosti 1 INTRODUCTION Aluminium-based composites with bio-organic parti- cles as the reinforcement are a topic of interest for the researchers due to their low costs and improved mecha- nical properties. To date, researchers have investigated the effects of various natural wastes used as reinforce- ment particles such as fly ash, 1,2 rice-husk ash, 3 bean-pod ash, 4 bamboo-leaf ash, red mud, groundnut-shell ash, 5 melon-shell ash 6 and bagasse ash 7 as the substitutes for the commercial reinforcement particles for producing cost-effective and new composite materials. Mazahery Ali et al. 8 examined the impact of nano-SiC particles incorporated in the A356 alloy and concluded that SiC particles enhanced the mechanical properties of compo- sites. Liang-Jing Fan 1 studied the behaviour of fly-ash particles in the Al–3Mg melt at 850 °C and various durations such as (0, 10, 20, 30 and 40) h, and observed that the Si released from the fly ash and Mg undergoes a reduction reaction to form the Mg 2 Si phase. During a longer reaction, porous fly-ash particles decompose completely and decrease the porosity. Rajan 2 examined the significance of fine-ash particles in an aluminium alloy at a very high temperature of 1200 °C; he found that the fly-ash particles undergo interfacial reactions with SiO 2 and Al 2 O 3 , yielding the MgAl 2 O 4 phase. Atuanya 4 utilized the bean-pod ash as the reinforcement and showed there was a better interparticle bond strength in an Al–Cu–Mg alloy. Kenneth 5 investigated the effects of groundnut-shell ash (GSA), rice-husk ash and bam- boo-leaf ash along with silicon carbide as the rein- forcement particles in an Al–Mg–Si alloy. GSA com- posites produced the highest mechanical properties among the ash particles. Abdulwahab 6 utilized the melon-shell ash with 5, 10, 15, and 20-% additions using the vortex method and observed a refined surface and better particle-matrix interface bond. Mohammed Imran 7 attempted a study with sugarcane bagasse-ash and graphite particles as the reinforcement in the Al7075 alloy and observed an increase in the hardness with an increase in the reinforcement. A composite with natural waste used as the reinforcing particles needs to have the proper mix ratio to obtain improved properties. In this experimental study, the stir-casting method was em- ployed to manufacture particle-reinforced composites. To the best of the author’s knowledge, moringa oleifera ash particles have not been used as the reinforcement Materiali in tehnologije / Materials and technology 53 (2019) 3, 395–398 395 UDK 620.1:669.715:546.281’261 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 53(3)395(2019) *Corresponding author e-mail: vssk70@gmail.com (Senthil Kumar Velukkudi Santhanam) particles with an LM25 alloy. Based on a literature survey, we can say that meagre information is available on multiple particles used with the LM25 alloy and the use of MOA as reinforcement particles. An experimental investigation was conducted on the LM25 alloy rein- forced with two different secondary reinforcements, i.e., Gr and MOA particles, and a comparative study of their effects on the physical, microstructural and mechanical properties of the composite materials was made. 2 EXPERIMENTAL PART The LM25 alloy was selected as the matrix; its che- mical composition is specified in Table 1. Silicon car- bide (SiC), graphite (Gr) and moringa oleifera ash (MOA) particles were the primary and secondary reinforcements. Dried moringa oleifera was calcined at 750 °C for 5 h. The ash obtained was mixed with a 2.5 mol NaOH solution and boiled at 75 °C for 3 h with magnetic stirring. Then the filtered precipitate was dried andmixedwitha2%HClsolution, refluxing at 75 °C for 4 h. Finally, the precipitate was collected, cleaned and dried at 110 °C for 10 h. 4 The synthesized ash particles were free from impurities and surface treated. The key elements present in the moringa oleifera ash were analysed and their values in w/% are shown in Table 1. The LM25 alloy was melted to 800 °C in an electric furnace and a hexachloroethane degasser was used to remove dissolved hydrogen. 9 Particle wettability in the melt was improved with an inclusion of 1 w/% of pure Mg. The reinforcement particles were preheated to 250 °C to remove moisture and a chromium-coated A310 stainless-steel stirrer was added at periodic inter- vals, stirring the melt at a varying speed of 450–700 min –1 . A higher stirring speed caused a homogeneous distri- bution of the particles 10 and a variation in the speed helped to limit the particle settlement at the bottom. The steel die was preheated to 250 °C to maintain a uniform cooling rate. Specific notations were determined for the composites such asA–(5w/% SiC),B–(5w/% SiC + 1 w/%MOA),C–(5w/% SiC + 3 w/%MOA),D–(5w/% S i C+1w/ %G r )a n dE–( 5w/% SiC + 3 w/% Gr). Density measurements were made using the Archime- dean principle and comparing the weights of the samples immersed in air and distilled water. 8 The rule-of-mix- tures relation, as given in Equations (1, 2), was applied to calculate the theoretical density and porosity %, respectively. The hardness was measured using a Vickers hardness-testing machine operated at a load of 200 gm, and the average of ten measurements from different points on a sample was taken. An XRD peak analysis performed with an X’PERT-PRO X-ray diffractometer operated at a scanning rate of 0.02 °min –1 , wavelength of 0.15406 nm, generator setting of 45 kV and 40 mA was used to study the metallurgical changes. The composites were mirror polished and etched using Keller’s reagent prior to optical and SEM examinations. d th = d m × V m + d r1 × V r1 + d r2 × V r2 (1) Porosity = dd d th mc th − ×100 (%) (2) Here d th ,d mc ,d m ,d r1 ,d r2 stand for the theoretical den- sity, measured density, matrix density, reinforcement 1 density and reinforcement 2 density while V m ,V r1 ,V r2 stand for the volume fraction of the matrix, reinforce- ment 1 and reinforcement 2, respectively. 3 RESULTS AND DISCUSSION 3.1 Density, porosity and Vickers hardness An addition of moringa oleifera ash particles to the composites decreases the density but the porosity forma- tion is minimal when compared to the graphite-mixed composites. An increase in the addition of Gr particles leads to an increase in the porosity %, which agrees with the result of the study by Mishra. 11 From Table 2,itis clear that the porosity increases as the w/% of graphite increases owing to the poor wettability and the graphite particles being clustered near the silicon carbide parti- cles. On the contrary, the MOA particles exhibit a better wettability with the matrix; thereby the porosity % is minimal. From Table 2, it is clear that the hardness de- creases with an increase in the graphite and MOA particles. Single-reinforcement composite A exhibits a higher hardness compared to the ones with dual rein- forcements. The MOA-reinforced composites have a higher hardness than the Gr-reinforced ones because of the formation of the strengthening phase Mg 2 Si and the microstructural refinement. This grain refinement is ascribed to the increase in the hardness of the MOA-rein- forced composites. 3.2 Microstructural characterization Figure 1 (a–f) shows the microstructures of the LM25 alloy and composites A, B, C, D and E, respect- ively, consisting of Al dendrites and eutectic Si. The microstructure examination reveals the dispersed MOA particles at the primary -aluminium grain interface. Composites B and C show no evidence of a cluster formation of the MOA particles. The average grain size D. MANICKAM et al.: EXPERIMENTAL INVESTIGATION OF LM25 ALLOY REINFORCED WITH SiC, Gr ... 396 Materiali in tehnologije / Materials and technology 53 (2019) 3, 395–398 Table 1: Chemical compositions of the LM25 alloy and MOA particles Elements Cu Si Mg Mn Fe Ti Ni Zn Pb Sn Al LM25 alloy (w/%) 0.02 6.99 0.48 0.02 0.22 0.18 0.01 0.04 <0.001 0.001 Balance Elements SiO 2 Al 2O 3 Fe 2O 3 TiO 2 P 2O 5 CaO MgO Na 2OK 2OS O 3 MOA particles (w/%) 1.22 0.024 0.045 <0.001 0.03 0.33 0.24 0.11 1.07 0.19 and circularity were measured using the ImageJ analysis software 12 and the values are given in Table 2. The circularity value is high for the MOA-particle-reinforced composites when compared to the base alloy and the other composites. The circularity is used to define the roundness of the grains (cylindrical shape) and a higher value provides a better strength. The grain shape has an effect on Young’s modulus due to the difference between the volume fractions of the grain boundaries with different grain shapes. 13 Figure 2 (e, f) depicts SEM images of the compo- sites, displaying the formation of particle clusters for the graphite-reinforced composites. Figures 2c and 2d show a better wettability of the MOA particles with the matrix, which hinders the growth of the secondary dendrite arm spacing; as a result, finer grains are formed. The MOA particles act as grain refiners and similar results were observed by Kanth et al. 14 who studied the effect of fly ash/SiC particles reinforcing Al-Zn alloy based compo- sites fabricated with the stir-casting method. As shown in Equation (3), Si and Mg react to form Mg 2 Si strength- ening precipitates in the MOA composites, which was confirmed with an XRD analysis as shown in Figure 3. The composites reinforced with SiC and Gr particles favour the formation of a brittle Al 4 C 3 compound accord- ing to Equations (4, 5), and graphite particles have a weak interface bonding with the matrix, which ultima- tely decreases the material properties. Si + 2Mg Mg 2 Si (3) 4Al+3C Al 4 C 3 (4) D. MANICKAM et al.: EXPERIMENTAL INVESTIGATION OF LM25 ALLOY REINFORCED WITH SiC, Gr ... Materiali in tehnologije / Materials and technology 53 (2019) 3, 395–398 397 Figure 1: Optical microstructures of the stir-cast alloy and composites a) LM25 alloy, b) composite A, c) composite B, d) composite C, e) composite D, and f) composite E at 500 × mag./25 μm (the insert graph at a magnification of 100 ×/100 μm) Figure 2: SEM images of the LM25 alloy and composites: a) LM25 alloy, b) composite A, c) composite B, d) composite C, e) composite D, and f) composite E Table 2: Density, porosity, micro-hardness, grain size and circularity values for the LM25 alloy and the composites S. No. Composite Theoretical density (g/cm 3 ) Measured density (g/cm 3 ) Porosity (%) Vickers hardness (Hv) Average Grain size in μm 2 Circularity % 1 LM25 alloy 2.66 2.7 0.54 67.5 47.78 0.24 2 A 2.70 2.68 0.71 91 40.3 0.62 3 B 2.45 2.42 1.41 84 35.68 0.66 4 C 2.06 1.99 3.21 77 34.78 0.66 5 D 2.62 2.5 4.41 80.5 48.05 0.57 6 E 2.51 2.32 7.62 71 38.1 0.53 4Al + 3SiC Al 4 C 3 + 3Si (5) Figure 3 shows XRD plots for the prepared compo- sites and the patterns exhibit a complete particle distri- bution in the matrix. From the XRD results, it is observed that the moringa ash particles influenced the aluminium phase as the peak intensity is reduced and the overall intensity peaks are reduced in Composites B and C. The XRD results also confirm that there was no for- mation of secondary phases. The aluminium peaks for Composites B and C (with moringa oleifera ash parti- cles) are shifted to higher 2 values in comparison to the LM25 alloy. This result is similar to that obtained by Praveen 15 who fabricated aluminium-matrix composites with bamboo leaf ash particles. 4 CONCLUSIONS Moringa oleifera ash reinforced composites enhance the evolution of Mg 2 Si precipitates and grain refinement. Graphite reinforced composites contain Al 4 C 3 precipi- tates, which retard the material properties because of their brittle nature. The moringa oleifera ash reinforced composites exhibit a decrease in the porosity % when compared to the graphite reinforced composites. The po- rosity of the moringa oleifera ash reinforced composites was reduced by 81.5 % compared to the graphite rein- forced composites. Composite A with a single reinforce- ment shows a higher hardness of 91 Hv, followed by Composite B with MOA particles. An increase in the se- condary reinforcement particles decreased the hardness of the composites. 5 REFERENCES 1 L.-J. Fan, S. H. 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MANICKAM et al.: EXPERIMENTAL INVESTIGATION OF LM25 ALLOY REINFORCED WITH SiC, Gr ... 398 Materiali in tehnologije / Materials and technology 53 (2019) 3, 395–398 Figure 3: XRD patterns of the LM25 alloy and composites: a) LM25 alloy, b) composite A, c) composite B, d) composite C, e) composite D, and f) composite E