COMPOSITES SCIENCE AND TECHNOLOGY

Composites Science and Technology 67 (2007) 12751279 www.elsevier.com/locate/compscitech

Short communication

Development of ultrane grain aluminiumgraphite metal matrix composite by equal channel angular pressing
M. Saravanan, R.M. Pillai *, K.R. Ravi, B.C. Pai, M. Brahmakumar
Materials and Minerals Division, Regional Research laboratory (CSIR), Industrial Estate PO, Pappanamcode, Thriuvananthapuram 695 019, Kerala, India Received 14 August 2006; received in revised form 22 September 2006; accepted 4 October 2006 Available online 16 November 2006

Abstract Al5 vol% graphite particulate composite was subjected to equal channel angular pressing (ECAP) at room temperature up to four passes. A signicant grain renement, down to the submicron level of 300 nm was achieved. Hardness enhancement of more than two fold was observed with only a marginal dierence along the perpendicular and parallel directions of pressing. Further, the strength of the composites was increased by more than two folds. ECAP at room temperature has resulted in a more rapid and signicant grain renement and strengthening in Algraphite composite. 2006 Elsevier Ltd. All rights reserved.
Keywords: E. ECAP; A. Metalmatrix composites; B. Strength

1. Introduction Equal channel angular pressing (ECAP) is a novel technique for producing ultra ne grain structure in submicron levels without change in the billet shape or dimensions by introducing a large amount of shear strain into the materials [14]. Till date, this technique has been used in a wide range of materials including pure metals [514], alloys [1520], intermetallics [21,22] and metal matrix composites [2328]. This process is well suited for aluminum alloys and is capable of producing ultra ne grain structures with grain sizes falling between 200 and 500 nm. However, there appears to be only limited number of investigations carried out on aluminium metal matrix composites (MMCs) with 6061 alloy as the matrix and Al2O3 [2327] and SiC whiskers [28] as the reinforcement. It has been observed that ECAP of Al MMCs signicantly improves the homogeneity of reinforcement distribution in the matrix [23] and renes the matrix grain size into submicron level [26].

Strength of the Al 6061Al2O3 composite has been observed to increase by almost a factor of two by ECAP [25]. There has been little or no breaking of Al2O3 in 6061 AlAl2O3 composites after subjecting to 12 ECAP passes [24]. However, the average length of SiC whiskers has been found to reduce from 42 to 4.2 lm during ECAP of 6061 AlSiC whisker composites [28]. Further, all of the reported studies on Al MMCs have been done at elevated temperatures except one [27]. However, there is no work reported till date on ECAP of Al - graphite composite, wherein graphite is soft in nature compared to Al2O3 and SiC. Further, there is a possibility of performing ECAP of Algraphite particle (Grp) composite at room temperature due to its soft and self lubricating nature. Therefore, an attempt has been made to subject Al5 vol.% Grp composite to ECAP at room temperature for developing ultrane grain structure. 2. Experimental details Al5 vol.% Grp composite prepared by stir casting route [29] was chosen for this investigation along with unreinforced pure Al for comparison. Graphite particles used

Corresponding author. Tel.: +91 471 2515270: fax: +91 471 2491712. E-mail address: rmpillai_rrl@yahoo.com (R.M. Pillai).

0266-3538/$ - see front matter 2006 Elsevier Ltd. All rights reserved. doi:10.1016/j.compscitech.2006.10.003

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have an average particle size of 65 lm. Samples (12 12 55 mm) machined out of Al5 vol.% Grp composites and unreinforced pure Al cylindrical castings were subjected to ECAP at room temperature using a die having an internal channel bent through an angle (U  90) and the outer arc of curvature (W  20) to impose maximum strain and obtain homogeneous microstructure in the material [4,30,31 and 32]. These die angles introduce a strain of 1 on each pass of billet through the die [33]. Among the three deformation routes commonly used namely, (1) route A (without rotation between passes), (2) route BC (90 rotation in the same direction between passes) and (3) route C (180 rotation between passes), route BC was chosen in this investigation because of its maximum eciency in generating rened equiaxed grains [4,8 and 34]. It is to be noted that Al5 vol.% Grp could sustain a maximum of four passes at room temperature beyond which cracking of the samples started. Samples (10 10 2 mm) were cut from the centre of the specimens and polished for optical metallography and atomic force microscopy and later thinned by twin-jet electro polishing method as thin foils for TEM observations. Microhardness was measured using a Vickers diamond pyramidal indentor with an imposed load of 200 g on polished 10 10 5 mm samples. Tensile test was carried out at room temperature and a strain rate of 2 103 s1 on samples (gauge length of 18 mm and gauge diameter of 4.5 mm) machined parallel to the pressing direction of Al5 vol.% Grp composites. 3. Results and discussion 3.1. Microstructure Fig. 1(a) and (b) show the typical microstructures of unreinforced pure Al and Al5 vol.% Grp composite prior to ECAP respectively. Large grains were observed in unreinforced pure Al (150 lm) and Al5 vol.% Grp composite (35 lm). Fig. 2(a) and (b) show the AFM image of unreinforced pure Al and Al5 vol.% Grp composite after eight and four passes of ECAP, respectively. Fig. 3(a) and (b)

show the TEM microstructures together with the SAED patterns for unreinforced pure Al and Al5 vol.% Grp composite samples perpendicular to the pressing direction after eight and four passes respectively. It is important to note that there is a signicant dierence in the microstructures of unreinforced pure Al and Al5 vol.% Grp composites. In unreinforced pure Al, there are well dened grain boundaries and a relatively small number of intergranular dislocations after eight passes. On the other hand, in Al 5 vol.% Grp composite, grain boundaries are not well dened but rather poorly delineated and irregularly shaped or curved in general after four passes. Further, the non-uniform contrast with in the grains in Fig. 3(b) is indicative of a highly strained structure. SAED pattern (Fig. 3(b)) of the Al5 vol.% Grp composites subjected to four ECAP passes also reveals an array of many very small grains having random distribution of orientations. Figs. 2 and 3 also show that grain size of the Al5 vol.% Grp has been rened to around 300 nm perpendicular to the pressing direction after four ECAP passes against 620 nm in unreinforced pure Al even after eight ECAP passes. Fig. 3(c) shows that the grain size of the Al5 vol.% Grp has been rened around 400500 nm parallel to the pressing direction after four ECAP passes. Grain renement achieved in Al 5 vol.% Grp composite after four ECAP passes is equal to or higher than that observed in earlier studies [25 and 26] conducted in 6061 Al10 vol.% Al2O3 composites. Han and Langdon [26] have found in 6061 Al10 vol.% Al2O3 composites that the grain size has been reduced to 300 nm after eight ECAP passes at 533 K. Valiev et al. [25] have observed a reduction in grain size up to 600 nm after 10 ECAP passes at 673 K. These results clearly indicate that room temperature ECAP of Al5 vol.% Grp composites has resulted in more rapid formation of submicron grains (300 nm) with only four ECAP passes and lesser volume fraction reinforcement (5 vol.%). Since annihilation and absorption of dislocations into grain boundaries are higher at elevated temperatures, room temperature pressing ensures the potential for achieving ner grains more rapidly [35].

Fig. 1. Optical microstructures of (a) unreinforced pure Al and (b) Al5 vol.% Grp composite prior to ECAP.

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Fig. 2. AFM microstructures of (a) unreinforced pure Al and (b) Al5 vol.% Gr composite after eight and four passes, respectively.

Fig. 3. Transmission electron micrograph and SAED pattern of (a) unreinforced pure Al after eight passes and Al5 vol.% Grp composite after four passes (b) perpendicular and (c) parallel to the pressing direction.

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3.2. Hardness The increase in hardness for Al5 vol.% Grp composite after ECAP is shown in Fig. 4 and compared with that of unreinforced pure Al. It can be observed that Al5 vol.% Grp composite work hardens rapidly during the rst ECAP pass and thereafter at a slower rate. It also shows that the microhardness value has increased from 400 to 850 MPa after four ECAP passes, registering 112% increase. Moreover, only a marginal dierence exists between the hardness values measured perpendicular and parallel to the pressing direction (Fig. 5). 3.3. Tensile properties The strength of Al5 vol.% Grp composite after four ECAP passes is shown in Fig. 6 and compared with those of unpressed Al5 vol.% Grp and 6061 Al10 vol.% Al2O3 composites after eight ECAP passes at 533 K [26]. The strength has increased from 97 to 249 MPa after four ECAP passes with approximately two and half fold increase. Despite the soft nature and less amount of the reinforcement in AlGrp composites compared to 6061 AlAl2O3 composites [26], the strength achieved is higher than that of the latter. Further, it is achieved at room temperature. Hence, a rapid high degree of strengthening is possible in Algraphite composite after ECAP at room temperature. These results show that room temperature ECAP of Al5 vol.% Grp composite imparts better grain renement and strengthening with in four passes compared to other studies in composites carried out with high volume percent reinforcement and at higher temperature pressing.
800

Hardness (MPa)

600

400

200

0 Perpendicular to the pressing direction Parallel to the pressing direction

Fig. 5. Comparison of hardness perpendicular and parallel to the pressing direction after four passes in Al5 vol.% Grp composites.

250

200 Tensile strength (MPa)

150

100

50

0 Unpressed Al - 5 vol % Grp composites Al - 5 vol % Grp composites after 4 ECAP passes 6061 Al - 10 vol % Al2O3 composites after 8 ECAP passes [26]

900 800

Vickers Hardness (MPa)

700 600 500 400 300 200 100 0 0 2 4 6 8

Fig. 6. Comparison of strength in unpressed and ECAP processed Al 5 vol.% Grp and ECAP processed 6061 Al10 vol.% Al2O3 composites.

4. Conclusions In the present work, ECAP of Al5 vol.% Grp composite has been successfully carried out up to four passes at room temperature. A signicant grain renement, down to the submicron level of 300 nm, is achieved in AlGrP composite. Hardness enhancement of more than two fold was observed with only a marginal dierence along the perpendicular and parallel directions of pressing. Further, the strength of the composites is increased more than two folds by ECAP. ECAP results in more rapid and signicant grain renement and strengthening in AlGrP composite at room temperature.

99.5 % pure Al Al - 5 vol % Grp composites

Number of passes

Fig. 4. Comparison of variation in hardness with number of passes in Al 5 vol.% Grp composite and unreinforced pure Al.

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Acknowledgements The authors thank the Director, Regional Research Laboratory, Thiruvananthapuram, for the award of CSIR diamond jubilee Research Internship to the rst author and the members of the mechanical engineering section for the fabrication of die. References
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