Nanocyrstalline phosphors were prepared through a Pechini-type sol-gel process. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), photoluminescence, and cathodoluminescence (CL) spectra were utilized to characterize the synthesized phosphors. XRD results reveal that the sample begins to crystallize at , and pure phase can be obtained at . FE-SEM images indicate that the -doped phosphors are composed of aggregated spherical particles with sizes ranging from . Under the excitation of UV light and low-voltage electron beams , the -doped phosphors show the characteristic emissions of the (, , transitions) with a yellow color. The CL intensity (brightness) of the -doped phosphor is higher than that of the commercial product (yellow) to some extent.