This study investigated polysiloxane hybrid sol-gel coatings synthesized from tetraethyl orthosilicate (TEOS), 3-(trimethoxysilyl)propyl methacrylate (MAPTMS) and two different precursors, i.e., methyl- or ethyl- methacrylate (MMA or EMA), as corrosion protection of aluminium alloy 7075-T6. The hypothesis was that the additional alkyl group might affect the chemical properties and, consequently, the corrosion properties. Synthesis of the sols proceeded in two steps, each involving either MMA or

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... EMA in the same molar ratio. The resulting sols, siloxane-(poly(methyl methacrylate-co-MAPTMS)) or siloxane-(poly(ethyl methacrylate-co-MAPTMS)), were applied on aluminium alloy followed by characterization in terms of chemical structure and composition, topography, wettability, adhesion and corrosion resistance in 0.1 M sodium chloride solution. The chemical properties of sols, monoliths and coatings were investigated using Fourier transform infrared spectrometry, solid state nuclear magnetic resonance spectrometry, X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry. Coatings were similar in terms of surface topography, while the wettability of the coating with EMA showed 6° greater water contact angle compared to the coating with MMA. Both coatings were shown, by electrochemical impedance spectroscopy in 0.1 M NaCl solution, to act as barriers to protect the underlying substrate in which coating with EMA exhibits better protection properties after 2 months of immersion. Adhesion tests confirmed the highest grade of adhesion to the substrate for both coatings. Testing in a salt-spray chamber demonstrated excellent corrosion protection, where coatings remaining intact after more than 600 h of exposure.