In-situ Al 2 O 3 /TiAl 3 intermetallic matrix composites were fabricated via squeeze casting of TiO 2 /A356 composites heated in the temperature range from 700 ЊC to 780 ЊC for 2 hours. The phase transformation in TiO 2 /A356 composites employing various heat-treatment temperatures (700 ЊC to 780 ЊC) was studied by means of differential thermal analysis (DTA), microhardness, scanning electron microscopy (SEM), electron probe microanalysis (EPMA), and X-ray diffraction (XRD). From DTA, two exothermic peaks from 600 ЊC to 750 ЊC were found in the TiO 2 /A356 composites. The XRD showed that Al 2 O 3 and TiAl 3 were the primary products after heat treatment of the TiO 2 /A356 composite. The fabrication of in-situ Al 2 O 3 /TiAl 3 composites required 33 vol pct TiO 2 in Al and heat treatment in the range from 750 ЊC to 780 ЊC. The hardness (HV) of the in-situ Al 2 O 3 /TiAl 3 composites (1000 HV) was superior to that of nonreacted TiO 2 /A356 composites (200 HV). However, the bending strength decreased from 685 MPa for TiO 2 /A356 composites to 250 MPa for Al 2 O 3 /TiAl 3 composites. It decreased rapidly because pores occurred during the formation of Al 2 O 3 and TiAl 3 . The activation energy of the formation of Al 2 O 3 and TiAl 3 from TiO 2 and A356 was determined to be about 286 kJ/mole.