Core–sheath fibers with the core component being a luminescent nanocomposite and the sheath component being poly(vinyl pyrrolidone) were prepared via the method of co-axial electrospinning; the luminescent nanocomposite consisted of a silicone rubber matrix with the complex Eu(TTA)3phen (TTA: 2-thenoyltrifluoroacetone, phen: 1,10-phenanthroline) as the filler. The fluorescence spectra, fluorescence lifetimes, and Judd–Ofelt parameters of the prepared core–sheath fibers were investigated. The results indicated that the Eu(TTA)3phen complex was uniformly dispersed in the silicone rubber as molecular clusters and/or nanoparticles, leading to a high luminescence intensity and efficiency. Additionally, unlike the neat Eu(TTA)3phen complex and electrospun fibers of thermoplastic-based nanocomposites that had no appreciable difference in the fluorescence lifetime and luminescent quantum efficiency at 73 and 293 K, the prepared electrospun core–sheath fibers had a longer fluorescence lifetime and a higher luminescence quantum efficiency at 73 K due to the contribution of the silicone rubber matrix.
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