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Dielectric insulator materials containing nanometer-scale closed-cell pores with low dielectric constants (k < 2.2), good mechanical properties, and high dielectric breakdown strengths are required for future semiconductor devices. In this paper we present a novel method for preparing nanoporous polyorganosilicate films, which promise to satisfy the key requirements, via inorganic/organic polymer hybrid templating. The nanometer-scale inorganic/organic polymer hybrids are generated in situ upon heating mixtures of methylsilsesquioxane (MSSQ) prepolymer with star-shaped hydroxy-terminated poly(ε-caprolactone) (PCL) to ∼250 °C, causing chain extension and cross-linking of MSSQ. Subsequent heating to 430 °C results in the thermal decomposition and volatilization of PCL components from the vitrified poly(methylsilsesquioxane) (PMSSQ) matrix, leaving behind porous PMSSQ films with pores with the size …