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In this paper, we report the synthesis of different silica materials via the acid-catalyzed sol–gel process at room temperature (25°C), using silane precursors with various alkyl chains (dimethyl, octyl and/or hexadecyl), in order to obtain thin films with anti-reflective and hydrophobic properties. Chemical, optical and structural properties of obtained silica materials were thoroughly characterized with various techniques such as FTIR and UV–Vis spectroscopy, AFM analysis, ellipsometric measurements, ESEM and TEM microscopy. Wettability of thin films was evaluated by water contact angle measurements. FTIR spectra of silica materials revealed that the intensity of the Si–O–Si characteristic bands varies depending on the precursor type. From AFM results, we found that the obtained films present a different microstructure as a function of the silica sol formulations. The hydrophobic character of the thin films increases with increasing the length of the hydrophobic chains following the order: dimethyl < octyl < hexadecyl. UV–Vis analysis of the coatings covered with silica materials presents a low reflectance (15.5%). The proposed method in this work has the potential to be a low-cost processing path of nanostructured anti-reflection transparent substrates.