Materials and Design 57 (2014) 1–9

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Effect of shoulder diameter to pin diameter (D/d) ratio on tensile strength and ductility of friction stir processed LM25AA-5% SiCp metal matrix composites
P. Vijayavel a, V. Balasubramanian a,⇑, S. Sundaram b
a b

Centre for Materials Joining and Research (CEMAJOR), Department of Manufacturing Engineering, Annamalai University, Annamalai Nagar 608 002, Tamil Nadu, India Department of Manufacturing Engineering, Annamalai University, Annamalai Nagar 608 002, Tamil Nadu, India

a r t i c l e

i n f o

a b s t r a c t
Stir casted LM25AA-5% SiC Metal Matrix Composites (MMCs) consists of cast product dendrites and large agglomerated reinforced particle. The agglomeration of SiC creates difference in properties along the composite system. During loading it creates different stress field which causes failures in the composite material. Friction Stir Processing (FSP) is a novel processing technique facilitate by the frictional heat generation between the tool and the workpiece. FSP can triumph over the poor properties due to large sized and unevenly distributed SiC particle in the Al matrix. In this investigation, five different shoulder diameters to pin diameter (D/d) ratio is used for processing the composite material. Tensile properties and hardness of the friction stir processed material were evaluated and correlated with the macro and microstructure signatures. The characterization of processed composite material is carried out using optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX) and X-ray diffraction technique (XRD). The effect of different D/d ratio (2, 2.5, 3, 3.5, 4) on microstructural formation, particle size and distribution in the matrix were analysed and found that the D/d ratio of 3 yielded higher tensile and hardness properties. Ó 2013 Elsevier Ltd. All rights reserved.

Article history: Received 5 June 2013 Accepted 4 December 2013 Available online 20 December 2013 Keywords: Metal matrix composites Friction stir processing Microstructure Tensile properties Ductility

1. Introduction Stir Casted LM25 Aluminium (Al) based Metal Matrix Composites (MMCs) have the beneficial properties of both metals and ceramics like high strength to weight ratio, high specific modulus, high fatigue strength, corrosion resistance, attractive thermal and electrical characteristics, etc. [1,2]. This favourable characteristic makes the composite to apply in the wide range of application in ship building, aerospace, transportation, etc. Despite of its beneficial properties, the quality of the composite materials was inherently affected by the fabrication process itself. The composite material is suffered from porosity, uneven distribution of reinforcement particle, etc. which have an effect on the service of the composite materials. These composites also suffered from low ductility and toughness due to incorporation of the uneven distribution of hard ceramic reinforcement. The quality fabrication of composite materials were limited due to the difficulty in achieving a uniform distribution of the reinforcement material,

⇑ Corresponding author. Tel.: +91 4144 239734 (O), +91 4644 241147 (R); fax: +91 4144 239734/238080. E-mail addresses: (P. Vijayavel),, (V. Balasubramanian), mfg.sundaram@ (S. Sundaram).
0261-3069/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.

wettability between the two main substances, porosities in the cast metal matrix composites, chemical reaction between reinforcement material and the matrix alloy. Friction Stir Processing (FSP) is an emerging processing technique which can eradicate the above said problem [3–5]. The solid-state nature of FSP leads to several advantages over other processing techniques involving melting methods such as plasma spraying and high-energy electron beam irradiation, laser surfacing as problems associated with cooling from the liquid phase are avoided [6]. Issues such as porosity, solute redistribution, solidification cracking and liquation cracking especially in Al based MMCs, interfacial reaction between matrix and reinforced particle do not arise during FSP [7]. In general, FSP has been found to produce a low concentration of defects and is very tolerant of variations in parameters and materials [8,9]. Many researchers hardly reported the various process parameters of FSP and their various influencing characteristic on the metallurgical aspect, material flow behaviour and particle distribution [10–12]. But the effect of shoulder diameter to pin diameter (D/d) on the particle size, distribution and defect free processed zone formation was not yet studied. To reveal that, an attempt is made to study the effect of shoulder diameter to pin diameter (D/d) ratio on tensile strength and ductility of friction stir processed LM25-5% SiCp metal matrix composites.

the tensile specimens were extracted from the friction stir processed zone and tested using universal testing machine at a constant loading of 1. An indigenously designed and developed computer numerically controlled FSW machine (22 kW: 4000 r/min: 6 ton) was used for friction stir processing. / Materials and Design 57 (2014) 1–9 SiC 5% Reinforcement 2. Non consumable tool made of super high-speed steel was used for experimentation.1 Ni 0. since the matrix is Al.1 Ti 0.6 Si 7. . The fine mirror polished surface was achieved by rotating velvet cloth polish. Three specimens were prepared from each experimental condition and the specimens were tested and the average of tensile strength value for each experimental condition and the specimens were tested and shown in figure Table 4. These sample preparation should be carried out to enable the view of microstructural signatures such as grain size. The specimens were rigidly clamped using fixtures in order to eradicate misalignment of specimen during processing. the surface oxide layer can also be removed during polishing. The chemical composition and mechanical properties of the above MMC were evaluated and presented in Tables 1 and 2. Microhardness was measured along normal direction Elongation in 50 mm gauge length (%) 2 Reduction in cross sectional area (%) 6. 1a. Details of tensile test specimen. 0. Vijayavel et al. The tensile specimens were extracted from the friction stir processed zone and the schematic extraction is shown in Fig. The specimens used for metallographic study were extracted from the friction stir processed zone using wire cut electric discharge machining (WEDM) process.2 Table 1 Chemical composition (wt%) of LM25 Al & 5% SiCp MMCs. The surface of the composite was polished in order to maintain the flatness of the surface which enables the full contact of shoulder surface. 2000 and 2500. Since the composite have hard SiC particle. 1000. A cotton bud dipped in the Keller reagent etchant was used for microscopic examination. Cu 0. Initially the tool is allowed to plunge slowly into the material until the shoulder surface touches the workpiece surface. grain orientation. In addition.49 N (HV) 68 (a) Scheme of extraction of tensile specimen (b) Dimension of tensile specimen (c) Photograph of tensile specimen (Before Test) (d) Photograph of tensile specimen (After Test) (e) Photographs of elongated specimen at each condition Fig. The FSPed specimen were polished using the varying grit sequence of 500.5 kN/min rate. 1. The specimens were rinsed with the running water and cleaned with acetone. less preheat create tool damage.2 Mg 0. SiC distribution in Al matrix. Experimental work Al matrix is reinforced with 5% SiC particles by stir casting method and thus produced composite material was prepared into plates of size 200 Â 100 Â 12 mm for friction stir processing. As per the ASTM: B557M. A dwell period Table 2 Mechanical properties of the LM25 Al & 5% SiCp MMCs.581 Microhardness @ 0.5 Fe 0.2% Yield strength (MPa) 143 Ultimate tensile strength (MPa) 155 of 30 s is maintained to achieve the preheat zone.2 Al Balance P.3 Zn 0.5 Mn 0. The tool is ramped at a constant rate of 40 mm/min to create the defect free processed zone. 1500.

5–7. The fractured surfaces of tensile test specimens of friction stir processed zone have been analysed using SEM to reveal the fracture surface morphology. / Materials and Design 57 (2014) 1–9 Table 3 FSP Parameters and Tool Dimensions used in this investigation. 3. 4 3 7. Vijayavel et al. 3c. Despite of its defect. L (mm) Tool shoulder diameter.2 Plain taper Super high speed steel Table 5 Tensile properties of FSP region. crack.2 2. F (kN) Pin length. S (mm/min) D/d ratio Axial force.4 kN which is near equivalent to the defected FSP specimens. During tensile loading the defect in the FSP region act as the failure initiator. Fig. Yielding can represent that the materials undergoes ductile mode of failure while loading.5 Tunnel defect in the RS 4 Tunnel defect in the RS . Macrostructure and microstructure FSP zones are prone to defects like pin hole. Results 3. etc.2 22 5. pores can be observed in which it may occur due to the necking. 3d shows the fractograph of processed zone at D/d ratio 3.P. due to insufficient and excess heat input [14]. The failures were ductile type failure since the characteristic fine dimples were observed.5. the FSP can result higher tensile properties than the base material. Process parameters Tool rotational speed. The continuous load displacement curve which shows no signatures of upper and lower yielding point. cavity. 3. kissing bond. The macrographs of the processed zone for five different D/d ratios Top surface Observation Tunnel defect in the RS 2. Fractographs for five different D/d was displayed in Fig. 30 mA is allowed to pass to the material to reveal the phase proportion formed if any (see Tables 3 and 5). 3. N (rpm) Traverse speed. d (mm) Pin profile Tool material Values 1000 40 2.2. 3.5 Tunnel defect in the RS 3 No defect 3.5.2 5.4 mm below from the top surface of the processed zone using Vickers microhardness testing machine under 0. tunnel. The operating parameter of 40 kV voltage. The base material can withstand the load of 2.5 3 3.5 2.4 3 at 2. 3. At D/d ratio 2 and 4.3 7.49 N load. Tensile strength The load–displacement curves of tensile specimen of different D/d ratio are shown in Fig. 2.5406 Å wavelengths is allowed to scan the workpiece for XRD experimentation. The shoulder diameter has greater influence on the loading and displacement curve since the agglomeration of SiC particle create a stress field around it and the brittle nature of SiC does not allow to redistribute the stress while Table 4 Macrostructure of FSP region. D/d Cross sectional macrostructure AS 2 RS yielding. Cu Ka1 X ray of 1. Cup and cone like failure can be observed in Fig. 3a shows the base material fractograph in which flat cleavage fracture surface and fine dimples are present. It can be clearly evident that the presence of agglomerated SiC particle will reduce the ductility of the MMCs [13].5 4 Tensile strength (MPa) 162 174 192 154 151 Elongation in 20 mm gauge length (%) 2. D (mm) Pin diameter. 2. D/d ratio 2 2.1. Fig.

Of the five D/d ratio used to fabricate the joints. 2. SEM fractrographs of tensile specimen. Vijayavel et al. the specimen were analysed using SEM (Scanning Electron Microscope). The microstructural features of FSP zone observed under SEM are displayed in Fig.5 (d) D/d ratio 3 (e) D/d ratio 3. 5. From the macrostructure analysis. A noticeable change in microstructure from base material to processed zone is observed. The stir zone is characterized by relatively fine recrystallized grain with fine sized evenly distributed SiC particle in the Al matrix. 3. The microstructural difference between the base material and the stir zone is clearly evident in Fig. are presented in Table 4. Load displacement curve.4 P. The friction stir process involves in highly non-uniform material flow. (a) base material (b) D/d ratio 2 (c) D/d ratio 2. Microstructures of processed zone for five different D/d ratio are displayed in Fig. . / Materials and Design 57 (2014) 1–9 Fig.5 (f) D/d ratio 4 Fig. the variation in the processed zone size. In order to get the clear understanding of the size and distribution of SiC particles in FSP region. D/d ratio of 3 produced defect free processed zone. shape and the location of defects inferred that the formation of defect free FSP zone is a significant function of tool rotation speed. 6. but also by the tool parameter. The processed zone signatures are not only affected by the process parameter that dictate the overall temperature. 4.

7 represents the measured hardness values in the FSP region. Discussion Fig.1. / Materials and Design 57 (2014) 1–9 5 D/d ratio used. As the D/d ratio increases. Optical micrographs of friction stir processed region.3.P. 5. Of the The excess heat generation enables the forward pin movement rather than the material flow to the rear due to aforementioned Fig. Vijayavel et al. . Microhardness Fig. 4. The optimum heat input for defect free joint is achieved at D/d ratio of 3. 4. This results in proper material flow and formation of fine recrystallized grains with and homogenous distribution of hard SiC particle in the FSPed region. 3. it can be inferred that the shoulder diameter has appreciable influence on the formation of grain size of the Al matrix and distribution of SiCp reinforcement. the D/d ratio of 3 yielded finer and uniform distribution of SiCp reinforcement in the Al matrix than their counterparts. 4. Interface microstructure. Effect of D/d ratio on tensile properties From the SEM micrographs. the hardness values increases to extent and then decreases when the frictional contact area is further increased.

which is a result of the stir action of the rotating pin during FSP [16]. Thus the defect free specimen yields better tensile properties. excess amount of heat is generated which leads to turbulent type of material flow which results in the occurrence of defects in the processed zone. At lower D/d ratio. process. Fig. This creates an inadequacy for the entire filling of material at the rear of the pin which was also clearly noted in the macrograph. The addition and distribution of SiC particle creates high dislocation density in the composite system. Since the total tensile specimen is extracted from the FSP region.6 P. 6. The enhancement of the tensile properties of FSPed composites is attributed to the following reasons: well spreading of reinforcement in the al matrix. 7. Thus optimum heat generation and subsequent material flow yields the good tensile strength. / Materials and Design 57 (2014) 1–9 (a) base material (b) D/d ratio 2 (c) D/d ratio 2.5 (d) D/d ratio 3 (e) D/d ratio 3. Vijayavel et al. At higher D/d ratio. less amount of heat is generated which is insufficient for the better material transport. From the results the tool shoulder diameter has a major effect in the formation of defect free joints. The defects thus created in the stir zone act as the stress raiser and the fracture initiator when subjected to tensile loading [15]. This will impede the dislocation movement while loading or deformation. Thus during tensile loading the strain localization occur at the middle of the specimen. This . SEM micrographs of friction stir processed region. The dislocation cannot cut through the hard SiC particles so that the dislocation is bow around the SiC particle and passes through the SiC. there is no considerable variation in the properties. Thus during tensile loading the strain localization occur at the middle of the specimen. Average microhardness of friction stir processed region.5 (f) D/d ratio 4 Fig. Since the total tensile specimen is extracted from the FSP region. there is no considerable variation in the properties.

Effect of D/d ratio on macrostructure and microstructure Material flow in the processed zone is influenced by the extrusion process. As the D/d ratio increases both hydrostatic pressure beneath the shoulder and the temperature in the stir zone increases. The tool pin propels the material flow which creates severe plastic deformation. / Materials and Design 57 (2014) 1–9 7 (a) Base materials (b) D/d ratio 2 (c) D/d ratio 2.5 (d) D/d ratio 3 (e) D/d ratio 3. and grain growth by heat generation [18]. (f) D/d ratio 4 might be the possible reason for the increment of ductility and tensile properties of FSPed MMCs. 8. The shoulder diameter and the pin diameter have a greater influence in creating the driving force for the material flow. where the material is extruded under the shoulder diameter (D) and around the tool pin. the thickness of deformed aluminium lamellae. Vijayavel et al. EDAX results. Tool probe affects microstructure by two facts: shattering or fragmentation of matrix grains and alumina particles. and material flow stress in turn depends on the axial force.2.5 Fig. The shoulder force is directly responsible for the plunge depth of the tool pin into the work piece and load characteristics associated with friction stir processing.P. thus the area subjected to friction is low which result in less heat generation due to friction. and material flow patterns highly depend upon the geometry of the tool. At higher D/d ratio the processed zone get wider and the angular volume . Due to insufficient heat generation at lower D/d ratio resulted defects in the processed zone because of insufficient coalescence of transferred material. The mechanism of onion ring formation in the processed zone of composite is due to the degree of material mixing and reinforcement break ups. Defect-free processed zones are indicative of efficient material flow around the pin tools [17]. processing temperature. 4. At lower D/d ratio the shoulder diameter is low.

6c) due to the (a) Base material (b) D/d ratio 2 (c) D/d ratio 2. Of the five D/d ratio levels used to processing. 9. the D/d ratio must be optimized to get FSP Zone with good consolidation of metal and without widening or narrowing of processed zone.5 Fig. the FSPed plate with D/d ratio of 2. XRD results. (f) D/d ratio 4 . exhibited the same pattern but the microstructure consists of slightly finer than the FSPed plate made with 2 kN (Fig. / Materials and Design 57 (2014) 1–9 subjected to stirring is high. But FSPed plate with D/d ratio of 3 consists of fine.8 P.5 (d) D/d ratio 3 (e) D/d ratio 3. 6b).5. Even though uniform distribution in the MMCs. Hence. 6a). Vijayavel et al. the FSPed plate with an D/d ratio of 2 resulted pin hole defect at the top of the retreating side due to insufficient material flow and the microstructure consists of coarse eutectic SiC particles (Fig. eutectic SiC particles with uniform distribution throughout the MMCs (Fig. Similarly.

Microstructure of D/d ratio 3 shows a significant breakup of SiC particles and dendrite. Huang JC. Si (ICDD card No. Fig. Mechanical properties of friction stir processed 2618/Al2O3/20p metal matrix composite. [10] Ma ZR. Johannes LB. Ke Liming. Hsieh PJ. This may be the reason for higher FSPed strength of the FSPed plate with D/d ratio of 3 compared to their counter parts. Thus increase D/d ratio from 2 to 3 increases the heat generation. Scripta Mater 2005. [20] Akramifard HR. Microstructure and mechanical property of multi-walled carbon nanotubes reinforced aluminum matrix composites fabricated by friction stir processing. [14] Sharma SR. Mater Des 2013. Since the processing is carried out in the solid state no such formation of solidification products were observed. Mater Des 2014. Shamanian M. As the spindle speed further increased. On the thermo-mechanical loads and the resultant residual stresses in friction stir processing operations. the presence of SiC particle and its distribution in the Al matrix decide the hardness.37:458–64. Shivpuri R. Deep cup forming by superplastic punch stretching of friction stir processed 7075 Al Alloy. Mahoney MW. Friction stir welding and processing. Base material shows lowest average hardness values because it consists of softer SiC free zone and hard SiC agglomerated zone. Senthil kumar for his constant support. Scripta Mater 2004. Kokabi AH.351: 148–53. Influence of reinforcement proportion and matrix composition on pitting corrosion behaviour of cast aluminium matrix composites (A3xx. Though the fact.14(5):775–82. Mishra RS.P. the D/d ratio of 3. Ho NJ. On the role of pin geometry in microstructure and mechanical properties of AA7075/SiC nano-composite fabricated by friction stir welding technique. Microstructure and mechanical properties of Cu/SiC metal matrix composite fabricated via friction stir processing. Mater Sci and Eng A 2003. Effect of friction stir processing on fatigue behavior of A356 alloy. High strain rate superplasticity in friction stir processed Al–Mg–Zr alloy. Mishra RS. Scripta Mater 2005. The average of hardness value is accounted for the study. Mater Des 2014. The superior hardness in the processed zone is due to: even distribution of reinforced particles in the pure matrix as a hard phase and the refinement of grains in processed zone [20]. [13] Cavaliere P. Mater Sci and Eng A 2007. Grimes R.53:1455–60. Viejo F.32:2034–41. Acta Mater 2006. Huang Chunping. It is due to the material flow at plastic condition and heat generation during FSP.45:343–8. Materials Park (OH): ASM International. Acknowledgments The author wish to place their sincere thanks to University Grants Commission (UGC) for financial support under the scheme of Rajive Ganthi National Fellowship (RGNFS) and N. This may be one of the reasons of obtaining similar chemical constituents. [12] Dutta A.36:1657–65. Vijayavel et al. All spectrum observed are bit similar like appearance. [19] Dolatkhah A. [3] Mishra RS. the grain structure is refined by dynamic recovery and dynamic recrystallization mechanisms [19]. .51:237–41. 2007. Ramulu M.53:201–6. [15] Ma ZY. Cavitation in superplastic 7075 Al Alloys prepared via friction stir processing. Investigation of microstructure. 03-065-2869).58:884–8. even distribution of SiC reinforced particle in the Al matrix enabled by the optimized frictional heat generation by the shoulder contact are the reasons for superior tensile properties and microhardness of the processed zone. CIRP Ann Manu Tech 2008. 01-077-2109) (see Fig. Parvin Nader. Al–Al3Ti nanocomposites produced in situ by friction stir processing. Praveen C. Mishra RS. Charit I. World Acad Sci. surface and subsurface characteristics in titanium alloy friction stir welds of varied thicknesses weld joint.54:838–44. It is due to the fact that high amount of heat will generated due to the rubbing of shoulder with the work piece. This makes the tool to break up the hard SiC particle into small and evenly distributed in the matrix. was identified as the better tool dimensions which yielded defect free micro and macrostructure in FSP region and yielded a maximum tensile strength of 192 MPa and microhardness of 112 HV. At D/d ratio of 3 the heat input attains to an optimum level. Golbabaei P. [17] Bahramia Mohsen.51:2569–3551. Friction stir processing of AM 60B magnesium alloy sheets. This creates turbulent flow of material which in turns affects the distribution of SiC with decrease of hardness. Chang CP. Eng Technol 2011. a uniform distribution of smaller SiC particles in the aluminium matrix were observed. [9] Chuang CH. Kao PW. De Marco PP.53:519–27. Effect of rotational speed and probe profile on microstructure and hardness of AZ31/Al2O3nanocomposites fabricated by friction stir processing.54:5241–9. Pasta S. / Materials and Design 57 (2014) 1–9 9 sufficient flow of softened material. Arrabal R. References [1] Pardo A. [6] Cavaliere P. Storjohann D. Besharati Givi Mohammad Kazem. [4] Santella ML. Mater Des 2012. The reference sources for the matching peaks are as follows Al (ICDD card No. Merino MC. [7] Edwards P. Fratini L. The various intensity of peaks were observed at the diffraction angles (2h). 5. [16] Liu Qiang. 4. Molaiekiya F. Sabbaghian M.462:393–7. Esmailzadeh M. the higher friction coefficient increases generate higher heat input. Dehghani Kamran. Conclusions From this study following conclusions are derived: (1) Of the five tool dimensions used to friction stir process. [8] Hsu CJ. Merino S.3. [18] Azizieh M. Colin Sterling J. (2) Presence of very fine recrystallized microstructure.395:173–9. Mishra RS. Chang CY.45:1750–64. 8 shows the spectrums observed in EBSD analysis. Mater Des 2011.x/SiCp). Fabrication and analysis of bulk SiCp reinforced aluminum metal matrix composites using friction stir process. [5] Buffa G. EngstromT. Scripta Mater 2005. Pan IY. This is the reason why the average hardness at D/d ratio of 3 is higher. Effects of friction stir processing on mechanical properties of the cast aluminum alloy A319 and A356. Investigating effects of process parameters on microstructural and mechanical properties of Al5052/SiC metal matrix composite fabricated via friction stir processing. [11] Su Jain Qing. XRD results show the presence of Si. Using friction stir processing to fabricate Mg Al Zn intermetallic alloys. Effect of D/d ratio on microhardness Heats generated due to increase in D/d ratio (increase in shoulder diameter) have the greater influence on the hardness of the material. Ma ZY. breakups of SiC particles to fine and equal size. Mater Sci and Eng A 2005. During FSP. SiC (ICDD card No. Liu Fencheng. Xing Li. Besharati Givi MK. Abachi P.57:287–90. Acta Mater 2003. Carbonerasa M. [2] Puviyarasan M. Composites Part A 2005. In general. 9). Friction stir processing of large area bulk UFG aluminium alloy. Corros Sci 2005. The heat input is sufficient to make material which results in break ups and evenly distribution of SiC particle. Mahoney MW. Tracy Nelson W. SiC dispersed uniformly throughout the matrix. Sci Technol 2009. higher heat input soften the material and grains get coarser which in turns decreases the hardness. 01089-2224).52:135–40.