The synthesis of the hydrophobic silica layer was conducted using the sol–gel method by reacting silica precursor trimethylchlorosilane (TMCS) and tetraethylorthosilicate (TEOS) with variations in the precursor composition ratio (TMCS:TEOS) of 10:90, 25:75, 50:50, 75:25, and 90:10 and then calcined at various temperatures. The TMCS‐TEOS silica thin layer has a significant influence on the surface hydrophobicity of the glass. The higher the number of TMCS precursors, the greater the contact angle produced. The highest contact angle produced was 98° at a TMCS‐TEOS ratio of 75:25 and without calcination. The TMCS‐TEOS silica thin layer contact angle decreased with increasing calcination temperature. The hydrophobicity of the TMCS‐TEOS silica thin layer could withstand temperatures up to 300°C. Quantitative analysis of FTIR spectra's peak area shows that with the increasing TMCS, the ratio of silanol/siloxane decreases. Gas sorption analysis shows that the TMCS‐TEOS thin layers' pore sizes are in the mesoporous region, and the pore shapes are cylindrical at all TMCS:TEOS ratios and calcination temperatures.