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The rare earth-doped luminescent materials have many outstanding luminescent properties which the other type luminescent materials owing to the special electronic configuration of the rare earth ions. The rare earth-doped luminescent material, possessing the properties of high brightness, long afterlow, adjustable wavelength scale, non-radiation and non-pollution, has been a popular subject of luminescent materials field.In this dissertation, sol-gel method was applied to prepare the precursor solution with a certain viscosity, and electrospinning technique was used to fabricate PVP/[Ca（NO3）+Al（NO3）3] and PVP/[Ca（NO3）2+Al（NO3）3+Eu（NO3）3+Nd（NO3）3],PVP/[Sr（NO3）2+Al（NO3）3] and PVP/[Sr（NO3）2+Al（NO3）3+Eu（NO3）3+Dy（NO3）3] composite microfibers, and the optimum preparative conditions were obtained. CaAl2O4, SrAl2O4, CaAl2O4: Eu2+ , Nd3+ and SrAl2O4 Eu2+ , Dy3+ nanofibers were obtained by calcination of the above relevant composite fibers.The samples were characterized by modern analytical methods, such as, field-emission scanning electron microscope （FESEM）, transmission electron microscope （TEM）, X-ray diffraction （XRD）, Fourier transform infrared spectrometer （FTIR）, fluorescence spectrophotometer, etc. The results showed that composite fibers had good dispersion and large aspect ratio, and the average diameter was 200nm. The mean diameter of CaAl2O4, SrAl2O4, CaAl2O4: Eu2+, Nd3+ and SrAl2O4: Eu2+, Dy3+ nanofibers was in the range of 50-100 nm, and had good properties of long afterlow.
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