溶剂热法制备氧化锆纳米粉体及其发光性能

Preparation and Luminescence of ZrO_2 Nanopowders Via Solvothermal Method

以乙醇为反应介质通过溶剂热法合成了氧化锆纳米粉体。采用X射线衍射(XRD)、透射电镜(TEM)及荧光光谱(PL)等测试技术对产物相组成、形貌结构及发光性能进行了表征。XRD结果表明,以KOH为沉淀剂制备的凝胶前躯体经140℃溶剂热反应3小时后所得的产物粉体由单一的四方相ZrO2组成,随着反应温度的升高单斜相ZrO2含量逐渐提高。TEM测试结果表明,不同温度合成的ZrO2纳米粉体形貌没有显著差异,产物粉体均为球形颗粒且可观察到较为明显的团聚现象。PL谱测试结果表明,140℃溶剂热合成的氧化锆粉体在250nm的紫外光激发下在402nm和625nm处分别有一个较强的宽发射峰和一个弱发射峰。

Zircoflia nanoparticles were＇synthesized via solvothermal method, and their compsition, morphology and luminescent property have been investigated. XRD results showed that the phase compositions of the products synthesised at various temperatures have significant difference, product synthesised at 140℃ composed of pure tetragonal zirconia, and the volume fraction of monoclinic zircoma were enhanced with increased reaction temperature. Nevertheless, there was little difference among the TEM photographs of ZrO2 nanoparticles synthesised at different temperatures, nanopowders were all spherical and showed obvious aggregation. The luminescence properties of ZrO2 nanopowders synthesised at 140℃ were investigated and the results show that, under 250 nm excitation, there was a strong and broad emission peak at 402nm and a broad excitation peak relative weak emission peak at 625 nm,respectively.