Hydrophobically modified silica nanocomposites have been prepared using a low temperature sol–gel process. In this study, an alkyltriethoxysilane derivative, hexdecyltrimethoxysilane (HDTMS), was co-condensed with tetraethoxyorthosilicate (TEOS) with and without a cross-linking agent, 3-glycidoxypropyltrimethoxysilane (GPTMS), to produce the modified composites. The hydrophobic properties were determined using contact angle measurement. FESEM observations revealed a semispherical nanostructure of the composites with grain size of about 50–75nm in diameter. The chemical modification was studied by FTIR and EDX, whereas the physicothermal properties were analyzed by DSC and TGA. These long-chain alkyl modified silica nanocomposites are promising materials for use in hydrophobic and water-resistant applications.