Sr 2 SiO 4 :Eu electrospun nanofibers were in situ synthesized successfully by calcination in this work. X-ray diffraction results confirmed that the calcined nanofibers were composed of the orthorhombic ␣Ј-Sr 2 SiO 4 phase. High resolution transmission electron microscopy and selected area electron diffraction indicated that the single Sr 2 SiO 4 :xEu electrospun nanofiber was polycrystalline with moderate orientation. Intense red and yellow emissions were observed in the calcined Sr 2 SiO 4 :xEu 3+ ͑Eu 2+ ͒ electrospun nanofibers. These nanofibers with intense visible emissions can be potentially applied in the fields of light-emittingdiode-based one-dimensional white light sources, displays, biological markers, etc.Nanomaterials, due to their particular chemical and physical properties compared with bulk materials, have gained wide attention in the past decades. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19] Compared with other techniques to produce one-dimensional nanomaterials, electrospinning has been studied widely for its convenience, efficiency, and low cost. 3-19 Among the preparations of micro-/nanofibers by electrospinning, great efforts have been focused on the luminescent electrospun nanofibers due to their potential applications in the fields of displays, biological markers, sensors, lab-on-a-chip, etc. 6-19 Moran-Mirabal et al. prepared ruthenium͑II͒ tris͑bipyridine͒/poly͑ethylene oxide͒ ͑PEO͒ electrospun nanofibers, which showed light emission at low operating voltages ͑3-4 V͒ approaching the bandgap limit of the organic semiconductor. 6 These light-emitting nanofibers exhibited an attractive feature for sensing applications and lab-on-a-chip integration. Song et al. studied the photoluminescent properties of the YBO 3 :Eu 3+ electrospun nanowires and nanotubes. 7 The chargetransfer excitation bands of Eu 3+ in the nanowires and nanotubes were blueshifted in contrast to those in bulk because of the variation in coordination environments. Bashouti et al. prepared CdSe nanorod-doped PEO electrospun nanofibers. 8 The emission spectra of the aligned CdSe nanorods showed a linear polarization, which is significantly important for polarized light sources in the visible and near-IR spectral regime. However, to our best knowledge, the work on yellow-emitting electrospun nanofibers is scarce, which is important to prepare a light-emitting diode ͑LED͒-based one-dimensional white light source.In the present work, we in situ synthesized Sr 2 SiO 4 :Eu 3+ ͑Eu 2+ ͒ nanofibers by electrospinning, and their photoluminescence properties were also studied for their composition and atmosphere dependencies. Due to the light-emitting source of nanofibers confined into a one-dimensional nanoscale, Sr 2 SiO 4 :Eu 3+ ͑Eu 2+ ͒ electrospun nanofibers may possess some peculiar optical properties, such as polarized luminescence, which can be potentially applied as linearly polarized light resources. 19,20 This study on yellow-emitting electrospun nanofibers may open another field of electrospun nanofibe...