This study focuses on the synthesis and characterization of Zirconium(IV) Propoxide (ZTP), Colloidal Silica (CS), and Methyltrimethoxysilane (MTMS)-derived non-stick hard coatings prepared via the sol–gel method. In the synthetic procedure, two different solutions were prepared separately based on the different hydrolysis rates of the silicon (SolS) and zirconium (SolZ) components. Polydimethoxysilane (PDMS) and Fluoralkylsilane (FAS) were used as hydrophobicity-promoting agents. The solution was applied onto aluminum surface, which was afterward dried and densified at 250 °C. The final solution was characterized by FTIR spectroscopy to determine the Zr–O–Si hetero-bonding and Si–O–Si and Zr–O–Zr homo-bonding. Coatings were analyzed by their hardness, hydrophobicity, and gloss. A homogeneous solution and crack-free hybrid coating was obtained. FTIR results showed that homo- and hetero-bonding between Zr and Si elements were obtained from a precipitation-free solution. Measured contact angles varied between 100° and 112°, and these results were evaluated according to the surface and gel structure. Highlights A crack-free, hydrophobic, hard hybrid thin films were synthesized using ZTP, MTMS and CS via sol–gel method. ZTP increased the contact angle of the film surface. Precipitation-free SolS solution was obtained due to the reactions between methyl groups in MTMS and the colloidal silica particles. PDMS and FAS components further increased the wetting angle of the hybrid film up to a specific ratio. FTIR results showed that Zr–O–Si hetero-bonding and Si–O–Si, Zr–O-Zr homo-bonding were obtained as result of the precipitation-free solution.