采用静电纺丝技术制备了聚乙烯吡咯烷酮PVP/［Y(NO3)3+Al(NO3)3+Eu(NO3)3］复合纤维，将其进行热处理，得到了YAlO3:Eu3+发光纳米纤维。采用X射线衍射(XRD)、扫描电镜(SEM)、荧光光谱等技术对样品进行了表征。PVP/［Y(NO3)3+Al(NO3)3+Eu(NO3)3］复合纤维经1200 ℃焙烧2 h后，获得了YAlO3:Eu3+纳米纤维，属于正交晶系，空间群为Pnma。用Shapiro-Wilk方法检验了纤维直径分布情况，在95%的置信度下，纤维直径属于正态分布。PVP/［Y(NO3)3+Al(NO3)3+Eu(NO3)3］复合纤维表面光滑，纤维分散性较好，有很好的长径比，尺寸均一，平均直径为(152.9±26.0)nm；YAlO3:Eu3+纳米纤维的平均直径为(106.7±20.2)nm。在234 nm的紫外光激发下，YAlO3:Eu3+纳米纤维的主要发射峰位于590 nm和609 nm处，分别属于Eu3+的5D0→7F1跃迁和5D0→7F2跃迁，Eu3+ 掺杂离子浓度对YAlO3:Eu3+发射峰的峰型与位置均没有影响，当Eu3+ 掺杂离子浓度为5%时，YAlO3:Eu3+ 纳米纤维发光最强。

PVP/［Y(NO3)3+Al(NO3)3+Eu(NO3)3］ composite nanofibers are prepared via electrospinning, and YAlO3:Eu3+ nanofibers are fabricated by calcination of the prepared composite fibers. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and fluorescence spectroscopy. Pure phase YAlO3:Eu3+ nanofibers are obtained by calcination of the relevant composite fibers at 1200 ℃ for 2 h and YAlO3:Eu3+ nanofibers belong to orthorhombic system with space group Pnma. The diameters of fibers analyzed by Shapiro-Wilk method obey normal distribution under the confidence of level 95%. The surfaces of as-prepared composite fibers are smooth with a good aspect ratio, dispersion and uniform size. The diameters of PVP/［Y(NO3)3+Al(NO3)3+Eu(NO3)3］ fibers and YAlO3:Eu3+ nanofibers are (152.9±26.0)nm and (106.7±20.2)nm, respectively. Fluorescence spectra analysis manifests that YAlO3:Eu3+ nanofibers emit the predominant emission peaks at 590 nm and 609 nm under the excitation of 234 nm ultraviolet ray, attributed to the transitions of 5D0→7F1 and 5D0→7F2 energy levels of Eu3+, respectively. The doping concentrations of Eu3+ have no effect on the shape and wavelength of the emission spectra of YAlO3:Eu3+, and the luminescent intensity reaches a maximum at about 5% of Eu3+.