尿素共沉淀法制备Nd：YAG纳米粉体

Preparation of nanoscaled Nd:YAG powders by the urea co-precipitation method

采用共沉淀方法,以Nd_2O_3、Y_2O_3和Al(NO_3)_3·9H_2O为起始原料,尿素为沉淀剂,制备Nd:YAG纳米粉体,粉体经XRD、TG-DTA、FESEM以及激光散射等测试手段对其结构和形貌进行测试研究。XRD表明,前驱体在900℃煅烧3 h出现了YAG相和YAM中间相,在1000℃及其以上煅烧3 h后已完全转变成YAG相,且随着煅烧温度升高,衍射峰逐步增强,900℃～1200℃煅烧的Nd:YAG晶格常数值从1.2012 nm变化到1.1994 nm,颗粒度从31 nm变化到96 nm,激光粒度仪也给出了类似的变化趋势。TG-DTA结果表明当前驱体加热到1200℃时,粉体总重量损失约为43%。对前驱体进行了水洗和乙醇洗两种洗涤,比较发现乙醇洗涤更有利于Nd:YAG纳米粉体的分散,这些实验结果可为制备优良YAG透明陶瓷粉体提供参考。

Nd：YAG nanoscaled powders were prepared by the co-precipitation method with Nd2O3, Y2O3 and Al（NO3）3·9H2O as the starting materials and CO（NH2）2 as the precipitator. The structure and morphology of the powders were investigated by XRD, TG-DTA, FESEM and laser particle analyzer. XRD patterns show that YAG phase and intermediate phase YAM were detected in the sample from the precursor calcined at 900℃ for 3 hours, the precursor completely transformed to YAG phase when it was calcined at 1000℃ for 3 hours, and the intensity of YAG X-ray diffraction peaks increased with the increase of calcination temperature. Lattice parameters of Nd：YAG phase calcined at 900℃- 1200℃ changed from 1.2012 nm to 1.1994 nm, and the particle size ranged from 31-96 nm. The similar variation was given by a measure of laser particle analyzer. The TG-DTA results indicate that the mass loss value was about 43% when the precursor was heated up to 1200℃. Suspension was washed with distilled water and alcohol, respectively. The comparison results show that alcohol is more effective for the well-dispersion of the nano-sized Nd：YAG powders. The results provid references for preparing good powders of YAG transparent ceramics.