Polymer derived ceramics have been widely being explored as high
temperature structural components in aerospace as rocket nozzles, nose tip
and leading edges of reusable launch vehicles. Polycarbosilane (PCS) was modified by a condensation reaction with zirconium acetylacetonate [Zr(acac)4] to form polyzirconocarbosilane (PZrCS). A series of PZrCS were synthesized, which could be transformed into SiZrC ceramic phases on pyrolysis. The ceramic yield of PCS was significantly improved by the introduction of zirconium into the system. The XRD patterns of the PZrCs show the characteristic peaks of SiC at 1300 C and at 1500 C the characteristic peaks of ZrC and ZrO 2 were observed. The carbothermal reaction in PZrCS was completed at 1650 C and the resulting ceramic was non-oxide SiC/ZrC phase. The SEM images proved that the increase in concentration of zirconium in the final ceramic decreases the surface uniformity. HRTEM analysis of PZrCS heat treated at 1650 C shows the evolution of oxide free ZrC/SiC phase with compatible grain boundaries without stacking fault. It could be concluded that the technique of introducing ultra-high temperature ceramic phases into the SiC matrix is an effective approach to improve the high-temperature performance of silicon based ceramics.