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Strategies of bone tissue engineering and regeneration rely on bioactive scaffolds to mimic the natural extracellular matrix (ECM) as templates onto which cells attach, multiply, migrate, and function. For this purpose, hybrid biomaterials based on smart combinations of biodegradable polymers and bioactive glasses (BGs) are of particular interest, since they exhibit tailored physical, biological, and mechanical properties, as well as predictable degradation behavior. In this study, hybrid biomaterials with different organic−inorganic ratios were successfully synthesized via a sol−gel process. Poly(ε-caprolactone) (PCL) and tertiary bioactive glass (BG) with a glass composition of 70 mol % SiO₂, 26 mol % CaO, and 4 mol % of P₂O₅ were used as the polymer and inorganic phases, respectively. The polymer chains were successfully introduced into the inorganic sol while the networks were formed. Fourier transform …