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A novel anhydrous preparation of silica (SiO₂)-encapsulated terbium (Tb³⁺) complex nanoparticles has been investigated. The SiO₂-Tb³⁺ nanoparticles are incorporated in electrospun polyvinylpyrrolidone hybrid nanofibers. Transmission electron microscopy confirms that Tb³⁺ complexes are uniformly and stably encapsulated in or carried by nanosilica. The influence of pH on the fluorescence of Tb³⁺ complexes is discussed. The properties, composition, structure, and luminescence of the resulting SiO₂–Tb³⁺ hybrid nanoparticles are investigated in detail. There is an increase in the fluorescence lifetime of SiO₂–Tb³⁺ nanoparticles and SiO₂–Tb³⁺/polyvinylpyrrolidone (PVP) hybrid nanofibers compared with the pure Tb³⁺ complexes. Due to the enhanced optical properties, the fluorescent hybrid nanofibers have potential applications as photonic and photoluminescent materials.