溶胶-凝胶法制备Y_2O_2S:Eu^(3+),Mg^(2+),Ti^(4+)红色长余辉发光粉及其发光特性

Synthesis and Luminescence Properties of Red Long Afterglow Phosphor Y_2O_2S:Eu^(3+),Mg^(2+),Ti^(4+) by Sol-Gel Process

以金属硝酸盐和钛酸丁酯为原料,乙酰丙酮为螯合剂,采用溶胶-凝胶法制备了Y2O2S:Eu3+,Mg2+,Ti4+红色长余辉发光粉体。采用X射线衍射仪、扫描电子显微镜和荧光分光光度计对不同温度合成的样品性能进行测试与表征。结果表明:干凝胶在600℃保温2 h生成了立方相的前驱体Y2O3:Eu3+,Mg2+,Ti4+。前驱体在1050～1150℃硫化后的产物为Y2O3与Y2O2S的混合相,在1 200℃时,硫化生成纯相的Y2O2S:Eu3+,Mg2+,Ti4+,产物平均粒径约为150nm,1300℃时再次出现Y2O3相。与高温固相法相比,溶胶-凝胶法制备的样品主激发峰出现蓝移,主发射峰位于616nm和626nm处,对应于Eu3+的5D0→7F2跃迁;硫化温度为1200℃时,样品的余辉时间为40min。

The red long afterglow phosphor Y2O2S：Eu3＋,Mg2＋,Ti4＋ material was synthesized by a sol-gel method using metal nitrate and tetrabulyl titanate as raw materials, aeetyl acetone as a eomplexing agent. The performance of samples synthesised at different temperatures was investigated by X-ray diffraction, scanning electron microscopy and fluorophotometer technique, respectively. The precursor of Y2O2S：Eu3＋,Mg2＋,Ti4＋ with a cubic crystal structure was obtained via the calcinations of the dry gel at 600 ℃ for 2 h. When the precursor was sulfurized at 1 050-1 150 ℃, the product was a mixture of Y2O3 and Y2O2S. The pure phase of Y2O2S：Eu3＋,Mg2＋,Ti4＋ was obtained at 1 200 ℃ and the average particle size was approximately 150 nm, the phase of Y2O3 appeared again at 1 300 ℃. The main peaks of excitation spectra of the samples synthesized by sol-gel method showed blue-shift, compared to the sample obtained by solid-state reaction method, and the main peaks of emission spectrum at 616 and 626 nm were ascribed to 5D0 to 7F2 transition of Eu3＋; The afterglow time of the sample was 40 min at the sulfurization temperature of 1200 ℃.