Crosslinking of polycarbosilane (PCS) with divinylbenzene (DVB) is readily accomplished using heterogeneous catalysis with platinum chloride in heptane to provide a silicon carbide precursor that produces a ceramic with significantly reduced oxygen content. The ceramic yield after crosslinking increased from 47% to between 72% and 78%; however, crosslinking may be influenced by dehydrogenative silylation of hydroxyl groups. Solid-state C-13 NMR spectroscopy of the crosslinked PCS showed peaks assignable to the aromatic group at 144 and 126.7 ppm. Monitoring of the crosslinking reaction by H-1 NMR spectroscopy indicated 40% consumption of the vinyl bonds of DVB within 10 min and complete consumption within 16 h. Infrared spectroscopy showed no increase in the peak at 3,650 cm(-1) due to O-H stretching in Si-OH, demonstrating that hydrosilylation crosslinking is a highly effective non-oxidative crosslinking technique.