Composite ZrB 2 -MoSi 2 coating modified by Y 2 O 3 and Al was prepared by a new multi-chamber detonation accelerator (MCDS) on carbon/carbon composites. Postdeposition heat treatment of the samples at 1500 • C for 1 and 6 h was carried out in air. The effect of heat treatment on the microstructure and phase composition of the ZrB 2 -MoSi 2 coating was investigated by scanning electron microscopy and X-ray diffraction phase analysis. The as-sprayed coating presented as a dense lamellar structure, composed of m-ZrO 2 , t-ZrO 2 , some hexagonal ZrB 2 , and cubic Al phases. The m-ZrO 2 , c-ZrO 2 , and h-(α-Al 2 O 3 ) formed at 1500 • C. The coatings after heat treatment (1 and 6 h) exhibited a structure without cracks. The porosity (~1%) of the coating did not change after heat treatment. Thin, continuous, silica-rich film covered the surfaces of ZrO 2 and Al 2 O 3 particles, and could have played a role during heat treatment by acting as a grain lubricant for particle rearrangement.