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Journal of Materials Processing Technology 211 (2011) 1614–1619

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Journal of Materials Processing Technology
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A novel technique for development of A356/Al2 O3 surface nanocomposite by friction stir processing
Y. Mazaheri ∗ , F. Karimzadeh, M.H. Enayati
Department of Materials Engineering, Nanotechnology and Advanced Materials Institute (NAMI), Isfahan University of Technology, Isfahan 84156-83111, Iran

a r t i c l e

i n f o

a b s t r a c t
A356/Al2 O3 surface nanocomposite was produced by friction stir processing (FSP) method. X-ray diffractometery, optical and scanning electron microscopy, microhardness and nanoindentation tests were used to characterize the samples. The results indicated that the uniform distribution of Al2 O3 particles in A356 matrix by FSP process can improve the mechanical properties of specimens. The hardness and elastic modulus of the as-received A356, the sample treated by the FSP without Al2 O3 particles, surface microand nanocomposite specimens were about 75 Hv and 74 GPa, 69 Hv and 73 GPa, 90 Hv and 81 GPa, 110 Hv and 86 GPa, respectively. © 2011 Elsevier B.V. All rights reserved.

Article history: Received 8 October 2010 Received in revised form 18 April 2011 Accepted 30 April 2011 Available online 8 May 2011 Keywords: A356 Surface nanocomposite Friction stir processing Nanoindentation

1. Introduction Conventional Al matrix composites (AMCs) reinforced with ceramic particulates, especially Al2 O3 exhibit high strength, hardness and elastic modulus (Tjong, 2007). AMCs are one of the advanced engineering materials that have been developed for weight-critical applications in the aerospace, and more recently in the automotive industries due to their excellent combination of high specific strength and better wear resistance as demonstrated (Surappa et al., 1982). AMCs have been widely studied since the 1920s (Sethi, 2007). A survey of the previous studies indicates that a homogenous dispersion of fine particles in a fine grained matrix is beneficial to the mechanical properties of AMCs (Shorowordi et al., 2003). Dispersion of the nano-reinforcements in a uniform manner is a critical and difficult task. There are several methods to fabricate particulate reinforced Al or Mg based composites, including stir casting, squeeze casting, molten metal infiltration, and powder metallurgy (Lee et al., 2006). It should be pointed out that the existing processing techniques for forming surface composites are based on liquid phase processing at high temperatures. In this case, it is hard to avoid the interfacial reaction between reinforcement and metal matrix and the formation of some detrimental phases. Furthermore, critical control of processing parameters is necessary to obtain ideal solidified microstructure in surface layer. Obviously,

∗ Corresponding author. Tel.: +98 9173047580; fax: +98 3113912752. E-mail addresses:, yoosef (Y. Mazaheri). 0924-0136/$ – see front matter © 2011 Elsevier B.V. All rights reserved. doi:10.1016/j.jmatprotec.2011.04.015

if processing of surface composite is carried out at temperatures below melting point of substrate, these problems can be avoided. Recently, a lot of attention has been paid to friction stir processing (FSP) as a new surface modification technique (Su et al., 2005). Though FSP has been basically advanced as a grain refinement technique, it can be readily used for fabricating surface composites. FSP induces intense plastic deformation and mixing of material in the processed zone in which the true strain can be as high as 40 (Ma, 2008). In this way, it is possible to incorporate the ceramic particles into the metallic substrate plate, to form the surface composites. Mishra et al. (2003) reported the first result on the fabrication of AlSiCp surface composite via FSP. In this way SiC powder was added into a small amount of methanol and mixed, and then applied to the surface of Al plates to form a thin layer of SiC particle. The coated aluminum plates were then subjected to FSP. Additional research efforts were dedicated to fabricating the surface/bulk composites via FSP with improved particle predeposition methods. One of the methods is to produce one or two grooves along the FSP direction to pour the particles inside. Morisada et al. (2006a,b) reported the fabrication of SiC particles and multiwalled carbon-nanotubesreinforced AZ31 surface composites via FSP, using this method. With deeper grooves being cut, Lee et al. (2006) demonstrated a successful fabrication of bulk composites via FSP. More recently, Dixit et al. (2007) successfully dispersed nitinol (NiTi) particles in Al1100 matrix via FSP. They used four small holes drilled below the surface of the Al1100 plate to load the NiTi powders. Subjecting the powder-filled plate to FSP produced an Al1100/NiTi composite with improved mechanical properties. It is important to note that the fabrication of the surface/bulk composites is achieved under a solid-state condition. No interfacial reaction occurs between the

2.02 Table 2 HVOF parameters for A356–Al2 O3 composite powder. . 2. 1(c). According to above researches. Mechanical milling was carried out in a high energy planetary ball mill (Retsch PM100).%) Al Rem Si 7.% Al2 O3 composition. (c) TEM image of nanosized alumina. Experimental procedure microscopy (SEM). 1. (b) microsized alumina. To overcome this drawback. The microstructure and mechanical properties of the composite surfaced layer were evaluated in details. Scanning electron The A356 chips and Al2 O3 powder particles were mixed to achieve A356–5 vol.26 Mn 0. Microscaled (␮-Al2 O3 ) and nanoscaled alumina (nAl2 O3 ) powder particles had an angular and nearly spherical shape with a size distribution of 50–100 ␮m and 20–40 nm.1. respectively. Samples preparation 2. transmission electron microscopy (TEM) micrographs and Corresponding selected area diffraction pattern (SADP) of as-received materials are shown in Fig. Morphology of: (a) A356 chips. nominally at room temperature and under Ar atmosphere up to 12 h. 1.Y. Mazaheri et al. in this research a new technique was used to incorporate nano-sized Al2 O3 into A356 aluminum alloy to form particulate composite surface layer. 2. reinforced materials and processing way. The milling media consisted of twenty 20 mm diameter balls confined in a 500 ml volume vial. / Journal of Materials Processing Technology 211 (2011) 1614–1619 Table 1 Chemical composition of A356 bars.07 Cu 0.44 Fe 0. However. Several ring patterns and the absence of preferred orientation in the SADP confirmed that the used alumina particles are nanosized. A356 chips were irregular in shape with a size distribution of 200–300 ␮m. Parameters Oxygen flow rate Fuel gas flow rate Spray distance Powder rate Number of passes Unit l min l min−1 mm g min−1 −1 1615 Value 750 175 350 35 3 reinforcing particles and the metallic matrix. See Fig. surface composites were attempted by changing base materials. some drawbacks have been revealed when each of these techniques are applied. Materials The specimens used for the FSP experiments were A356-T6 10 mm × 50 mm × 250 mm bars. The agglomeration of the reinforced particles especially in case of nanosized powder is the major limitation of these methods. Residual machining chips of A356 and micro and nanosized ␣-Al2 O3 powders with purity of 99.44 Mg 0. The chemical composition of samples is given in Table 1. Element Composition (wt.05 Ti 0.9% were used for producing A356/Al2 O3 composite powders. The ball and vial materials Fig. and good interfacial bonding is achieved.

2. 2).5 ml HCl and 10 ml nitric acid in 87. The concept of development design of A356/Al2 O3 surface composites. The samples were prepared according to standard metallographic practice and etched with Keller’s reagent (1 ml 48% HF. / Journal of Materials Processing Technology 211 (2011) 1614–1619 Fig. This method is capable of measuring elastic moduli of the surface composites because of the relatively small volume being tested. The composite powders were deposited onto the grit blasted A356-T6 substrates by HVOF spraying (Metallization Met Jet III). 3. 3. The hardness and elastic modulus of as-received A356. Indeed. The average of three measurements for each point was calculated and reported as microhardness value. The FSP tool was made of H13 steel (Fig. CSM Instruments) with a Berkovich diamond indenter (B-J87). Transverse sections were examined by optical microscopy (OM) and SEM in a Philips XL30. In order to take the repeatability into account. Thus. In all FSP experiments tool rotation rate. respectively. 1. 2. The XRD patterns were recorded in the 2Â range of 20–100◦ (step size of 0. FSPed sample (no Al2 O3 ) and surface composites were evaluated from the load-penetration depth curves obtained in nanoindentation tests using a nanoindentation tester (NHTX S/N: 01-03119. Ball to powder weight ratio was 6:1 and rotation speed of vial was 300 rpm. Mazaheri et al. the test results were acquired from the average of four indentations. any adverse effects of porosity. The phase composition of the as-received and as-milled powders were analysed by X-ray diffraction (XRD. . respectively. 200 mm min−1 and 2◦ . Analysis techniques Cross-sectioning of the friction stir processed (FSPed) samples in planes perpendicular to the processing direction was performed for metallographic analysis. The spraying parameters are presented in Table 2.05◦ and time per step of 1 s). were hardened high carbon and chromium steels. Fig.5 ml distilled water for 30 s).1616 Y. (a) Dimensions (in mm) and (b) picture of the FSP tool. The as-milled powders were sieved in order to separate 25–63 ␮m fraction which is suitable for high velocity oxy-fuel (HVOF) spraying. The concept of development of A356/Al2 O3 surface composites design in this study is schematically shown in Fig. The hardness and elastic modulus were calculated by a standard procedure according to the method of Oliver and Pharr (1992). can be avoided.3. The hardness profile along the cross-section of FSPed samples was also determined by microhardness test using a Vickers indenter at the load of 100 g and dwell time of 5 s. The total powder mass was 200 g and 0.3 wt. the properties measured from nanoindentation are the true properties of the surface composite layers.% stearic acid was added as a process control agent (PCA). commonly obtained in bulk property measurements. Philips X’Pert-MPD) using Cu K␣ radiation ( = 0.15406 nm) generated at 40 kV and 30 mA. traverse speed and tilt of the spindle towards trailing direction were kept constant in this study to be 1600 rpm. Then plates with preplaced composite coatings were subjected to FSP. The indentations were made to a maximum load of about 70 mN and under loading and unloading rate of 140 mN/min.

Y. 5 shows the cross-sectional images of the coatings and surface composites. The XRD patterns of powder particles as-received and after 12 h of milling time are shown in Fig. Mazaheri et al. The as-milled powders were sieved in order to separate 25–63 ␮m fraction and used for spraying. Fig. Fig. After 3 passes. a coating thickness of about 200 ␮m was achieved. and no defects were visible. Nanosized Al2 O3 particles were found to be distributed within this region due to the occurrence of vigorous stirring during the process. (c) A356–nAl2 O3 composite coating and (d) A356/Al2 O3 surface nanocomposite. The surface composite layers appeared to be very well bonded to the aluminum alloy substrates. 4. 3. 5(b) and (d) shows optical micrographs of interface zone between surface composite layers and A356-T6 substrates after FSP. Structural evolution A356–Al2 O3 composite powder was prepared by 12 h ball milling of A356 machining chips and nanosized as well as microsized Al2 O3 powder. respectively. Cross-sectional microstructure of: (a) A356–␮Al2 O3 composite coating. 4. The XRD patterns of as-received ␣-Al2 O3 . Al2 O3 peaks was difficult to be detected due to the decrease in intensity and/or overlapping with higher intensity peaks related to A356. which is attributed to the low volume fraction of the Al2 O3 phase and the fine size of the powder in the A356–Al2 O3 powder mixture. 6 shows SEM images obtained from the surface micro and nanocomposite fabricated by the FSP. The friction stirred zones were typically about the size of the rotating pin. A356 and as-milled A356–Al2 O3 composite powders for 12 h. All the diffraction peaks from the A356 matrix are clearly seen. Composite coatings were deposited by HVOF process on A356-T6 substrates. 5(a) and (c). / Journal of Materials Processing Technology 211 (2011) 1614–1619 1617 Fig. all the expected diffraction peaks of Al2 O3 are not clearly observed. So that after 12 h milling. micrographs of the coatings revealed good homogeneity and uniformity and high-quality contact with substrates.1. Results and discussions 3. Fig. 6(a) and (b) are the broken Si particles dispersed in the Al matrix and Fig. namely width and depth of 4 and 5 mm. (b) A356/Al2 O3 surface microcomposite. 5. The coated specimens were then subjected to FSP. these peaks have a low intensity in the diffraction pattern. Because of the stability of alumina no other reaction product in the compositions was found. As can be observed in Fig. In comparison to the diffraction peaks from A356. The dark particles in Fig. . however. The composites consist only of ␣-Al2 O3 and A356 peaks.

3. Others have also found that FSP had a softening effect on A356. the thermo-mechanically affected zone (TMAZ) and the stir zone (SZ).8 ± 0. The hardness profile was measured along the centerline of the cross-section of the processed zone.2. Load versus penetration depth curves of as-received A356.7 ± 0. As reported in literature studies (Ma et al. Ma et al.5 86 MPa Vickers Vickers GPa Dimension . The information presented in the publications (Chen and Kovacevic. respectively. Fig. 6. 7. Mazaheri et al.8 ± 1. FSP generates sufficiently high temperatures..8 ± 2. some softening could also take place in these zones. at least in some locations. The hardness profiles along the cross section of the FSPed A356-T6 (no Al2 O3 ) and surface composite layers. 8.. 1600 rpm—200 mm min−1 ). / Journal of Materials Processing Technology 211 (2011) 1614–1619 Fig. Therefore. On the other hand FSP causes intense plastic deformation resulting in significant microstructural refinement of the processed zone increasing the hardness value.6 ± 1. The average hardness values of the BM and SZ were about 80 and 67 Hv. to affect re-solutionizing of the hardening phases in heat treatable Al alloys reducing the hardness value. The microstructure of FSPed samples are composed of four primary zones: the base metal (BM). 2008).6 ± 1.7 ± 2.9 79. microhardness profile shows a general softening and reduction of hardness in the stirred zone in contrast to that of the as-received A356-T6 in spite of smaller grain size.4 89.1618 Y. Fig.2 66. SEM micrograph of: (a) A356–␮Al2 O3 and (b) A356–nAl2 O3 surface composite. 2003.1 74 FSPed sample (no Al2 O3 ) 750 68. the white particles are Al2 O3 particles identified using energy dispersive spectroscopy (EDS). According to the previous microstructural results. For the FSPed A356-T6 with no alumina powder.1 109. the heat affected zone (HAZ). FSPed sample (no Al2 O3 ) and surface composite layers using nanoindentation technique.9 ± 1. Mechanical characterization Fig. 2003) indicate that. In addition. the effect of FSP on the distribution of hardness on the any sample is justifiable. FSPed sample (no Al2 O3 ) and surface composite layers. the heat generated by FSP can increase the temperature of TMAZ and HAZ leading to the full/partial dissolution of the hardening precipitates in heat treatable alloys.9 73 Microcomposite 978 89. 7 shows the hardness profile along the crosssection of samples under the same FSP condition (Â = 2◦ .6 81 Nanocomposite 1196 109. it seems that the softening of the stirred zone was result of dissolution of strengthening precipitates during FSP. Parameter Value As-received A356 HIT HV (nanoindentation) HV (microhardness) EIT 783 74. As can be seen the decrease in hardness for TMAZ and HAZ was Table 3 Mechanical characterizations of as-received A356. 2007.

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