In situ formation of TiB2 in mullite matrix through the reaction of TiO2, boron and carbon has been studied. In hot-pressed and pressureless-sintered samples, in addition to TiB2, TiC was also found to be dispersed phases in mullite matrix. However, in the case of pressureless-sintered samples, mullite/TiB2 composite with 98% relative density can be obtained through a preheating step held at 1300゚C for longer than 3h and then sintering at a temperature above 1600゚C. Hot-pressed composite containing 30 vol% TiB2 gives a flexural strength of 427 MPa and a fracture toughness of 4.9 MPa m1/2. The composites were applied to the diffuser nozzle and the nozzle’s stress and the buckling are analyzed.