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A hybrid material of polystyrene (PS)–ZrO2 was developed by the sol–gel technique and deposited by spin-coating on AM60 and AM60–AlN nanocomposite surfaces to enhance corrosion resistance in marine environments. PS–ZrO2 with an average thickness of ≈305 ± 20 nm was dispersed homogeneously, presenting isolated micro–nano-structure defects with air trapped inside, which led to an increase in roughness (≈4 times). The wettability of the coated substrates was close to the hydrophobic border (θCA=90°–94°). The coated samples were exposed for 30 days to SME solution, simulating the marine–coastal ambience. The initial pH = 7.94 of the SME shifted to more alkaline pH ≈ 8.54, suggesting the corrosion of the Mg matrix through the coating defects. In the meantime, the release of Mg2+ from the PS–ZrO2-coated alloy surfaces was reduced by ≈90% compared to that of non-coated. Localized pitting attacks occurred in the vicinity of Al–Mn and β-Mg17Al12 cathodic particles characteristic of the Mg matrix. The depth of penetration (≈23 µm) was reduced by ≈85% compared to that of non-coated substrates. The protective effect against Cl ions, attributed to the hybrid PS–ZrO2-coated AM60 and AM60–AlN surfaces, was confirmed by the increase in their polarization resistance (Rp) in 37% and 22%, respectively, calculated from EIS data.