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The influence of hydrolysis time of gamma-methacryloxypropyltrimethoxysilane (MPS) at 1% in an aqueous solution (pH 4) on the silanization of 6063 aluminum alloy samples was studied. Analysis of silane layers by means of FTIR and contact angle measurement rendered 60 min of hydrolysis, 10 min of immersion, and 60 min of curing (100 °C) as the most adequate process to obtain proper silane&-substrate bonding. Formed silane coatings were also characterized by scanning electron microscopy (SEM) and their composition was determined by semi-quantitative X-ray energy dispersive spectroscopy (EDS). Samples silanized by different methods (including pretreatment with atmospheric pressure plasma (APPT)) were painted and the performance of polyester coatings was assessed with mechanical tests.