Particulate-reinforced in situ metal matrix composites (MMCs) possess excellent properties such as high specific strength and modulus, elevated-temperature resistance, but are low in fabrication costs. Thus, their production is of special interest in the advanced materials research field. [1±7] The in situ production of MMCs involves the formation of the reinforcing phases through direct chemical reactions in the metallic matrices. Ceramic TiC, TiB 2 , Al 2 O 3 , and SiC, etc. have been widely used as reinforcements for the in situ MMCs, especially aluminum matrix composites. [1±4] Recently, the systems of Al-TiO 2 -X, where X is boron, [5,6] B 2 O 3 , [5,7] or carbon, [8] have been investigated to prepare (TiB 2 +Al 2 O 3 ) or (TiC+Al 2 O 3 ) reinforced aluminum composites. The present work will report the reaction process in the Al-TiO 2 -CB 4 system and the successful synthesis of an Al/(TiC+TiB 2 +Al 2 O 3 ) composite through the in situ reaction of this system in molten aluminum. Figure 1 shows the DSC curve of the Al-TiO 2 -CB 4 pellet heated to 1300 C and followed by cooling. During heating, an endothermic peak with the maximum at 674.4 C, corresponding to the melting of Al, and two exothermic peaks which overlap each other between 862 and 1020 C, can be observed. It is clear from the presence of phases revealed on the XRD patterns of the as-milled powder and this heated pellet (Fig. 3) that the two exothermic peaks are related to reactions between the starting materials to form the desired TiB 2 , TiC and a-Al 2 O 3 phases. During the cooling process, only an exothermic peak associated with the solidification of Al is present, indicating that the new phases formed are thermodynamically stable at the temperature of as high as 1300 C. To determine reactions at the exothermic peaks in Figure 1, pellets were heated in the DSC at the same rate to 948 and 1040 C respectively (Fig. 2a,b), and then subjected to XRD analysis.Compared with that in Figure 1, however, the DSC curves ending at 948 C and 1040 C (Fig. 2a,b) do not clearly show the small exothermic peak at the beginning of the exothermic event. While on the curve in Figure 2c, which was repeated for further comparison, a small peak appears after the large one, contrasting with Figure 1. Comparing the four DSC curves suggests that the exothermic events between 860 and 1040 C may be regarded as an exothermic peak. The starting, ending and the maximum temperatures of the exothermic peak during each run of heating are slightly different too. All these differences might be attributed to different density of each pellet.In the XRD pattern of the pellet heated to 948 C, TiAl 3 as well as TiC, TiB 2 , and a-Al 2 O 3 , are apparently detected. The presence of TiAl 3 suggests that the following reduction reaction of TiO 2 occurs:This has also been verified in previous DSC studies of the solidification of Al melting of Al 618°C 674.4°C 958.0 °C 900.3°C DSC (mW/mg) Temperature(°C)Fig. 1. DSC trace of the 70.4 %Al-24 %TiO 2 -5.6 %CB 4 pellet heated to 1300 C and f...