The poor hydrolytic stability of silane interphase greatly limits the use of fiber reinforced composites (FRC) in demanding applications in which the FRC part is permanently exposed to a moist environment such as in prosthetic dentistry and orthodontics. To improve hydrolytic stability of the interphase between the matrix composed of a blend of triethyleneglycol dimethacrylate (TEGMA) and bisphenol A glycidylmethacrylate (Bis-GMA) monomers and glass or alumina oxide fibers, a two-step hydrosilylation procedure was employed. The process consisted of creating hydride intermediate on the fiber surface followed by hydrosilylation reaction attaching the unsaturated organic monomer (Bis-GMA) forming stable-Si-C bonds. Infrared spectroscopy (FTIR) confirmed formation of the hydride intermediate on the surface and then, attachment of the appropriate organic compound in the second step. The amount of deposited interphase and its stability was significantly enhanced compared to standard silanization treatment. Fracture surfaces were observed by scanning electron microscopy (SEM) before and after environmental exposure proving that the most stable interfacial bond was obtained with the two-step treated fibers. It was concluded that hydrosilylation provides a viable alternative to silanization for both glass and ceramic fibers in composites intended for applications requiring enhanced hydrolytic stability of the composite parts. (C) Koninklijke Brill NV, Leiden, 2012