The paper presents the issues of metal surface treatment in fibre metal laminates (FML) to obtain high adhesion at the metal–composite interface. Aluminium 2024-T3 and titanium Grade 2 were analysed. The metal surface modifications were carried out by mechanical (sandblasting, Scotch-Brite abrasion), chemical (P2 etching, phosphate-fluoride process), electrochemical (chromic and sulphuric acid anodizing), and plasma treatment, as well as the application of sol-gel coatings. In terms of surface geometry, the analysis included roughness and 3D surface topography examination. The morphology was examined using scanning electron and atomic force microscopy. The surface free energy and its components (polar and dispersive) were determined using the Owens–Wendt method. The novelty of this study is the determination of the effect of different surface treatments on the surface free energy, topography, and morphology in terms of the possible appropriate adhesion in fibre metal laminates. Chromic acid anodizing is still the most effective in enhancing the expected adhesion. A suitable technique may be the use of P2 etching of aluminium. It results in low roughness, numerous micro-irregularities, and the presence of porosity. The obtained test results show that the application of sol-gel coating increases the surface free energy and may increase the adhesion.

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