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Abstract: Ti3SiC2-based compound was synthesized by mechanical alloying (MA) using starting materials consisting of 3Ti/Si/2C/xAl (x =0, 0.1, 0.2, 0.3) powder mixtures, and the effects of Al on the MA synthesis of Ti3SiC2 were studied. Our results showed that, ball milling of the 3Ti/Si/2C powder mixture for 10h produced both powder form products of TiC, TiSi2 and Ti3SiC2, and bulk form products with Ti3SiC2 as the main phase. Adding a small amount of Al remarkably increased the ratio of Ti3SiC2 in the mechanically alloyed products (in both the powders and the bulks). When x =0.1, Ti3SiC2 content in the powders and bulks reached 76.8 and 85.9wt%, respectively, after being ball milled for 10h. Excessive Al, however, would reduce the content of Ti3SiC2 in the milled products. [Copyright &y& Elsevier]