Tetraethoxysilane and 2-hydroxybenzyl alcohol were allowed to undergo a sol-gel reaction under acidic conditions. These compounds underwent con densation independently to give hybrids consisting of silica and phenolic resin components, which are applicable as precursors for silicon carbide powders and fibers when they are prepared in the fibrous form. The spin-lattice relaxation time measurement for the hybrids using solid-state Si-29 NMR spectroscopy suggests that there is appreciable interaction between the silica and phenolic resin components in the hybrids through hydrogen bonding.