尿素共沉淀法制备Nd:YAG纳米粉体

J4 ›› 2010, Vol. 27 ›› Issue (1): 110-115.

尿素共沉淀法制备Nd:YAG纳米粉体

李冬青丁丽华张庆礼邵淑芳宁凯杰殷绍唐

中国科学院安徽光学精密机械研究所安徽省光子器件与材料重点实验室，安徽合肥，230031

出版日期:2010-01-28 发布日期:2009-12-30
通讯作者: 张庆礼（1973-），男，研究员，云南会泽县人，主要从事光学晶体生长及其性能研究。 E-mail:zql@aiofm.ac.cn
作者简介: 李冬青（1982-），男，硕士生，山东滕州市人，主要从事激光陶瓷制备及其性能研究。 E-mail: ldq7289@aiofm.ac.cn
基金资助:
国家自然科学基金(50772112, 50872135)，安徽省优秀青年科技基金资助项目( 08040106820)

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

LI Dong-Qing, DING Li-Hua, ZHANG Qing-Li, SHAO Shu-Fang, NING Kai-Jie, YIN Shao-Tang

Anhui Provincial Key Laboratory of Optical Devices and Materials, Anhui Institute of Optics and Fine Mechanics，Chinese Academy of Sciences， Hefei 230031 China

Published:2010-01-28 Online:2009-12-30

摘要/Abstract

摘要：

采用共沉淀方法，以Nd2O3、Y2O3和Al(NO3)3?9H2O为起始原料，以尿素为沉淀剂，制备Nd:YAG纳米粉体，制备的粉体经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小时出现了YAG相和YAM中间相，在1000℃及其以上煅烧3小时后已完全转变成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1.2012nm变化到1.1994nm，颗粒度从31nm变化到96nm，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。

关键词: 材料, 纳米粉体, 尿素共沉淀法, Nd:YAG, 颗粒度

Abstract:

Nd:YAG nanoscaled powders were prepared by 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 showed 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 calcination temperature increase. Lattice parameters of Nd:YAG phase calcined at 900-1200℃ changed from 1.2012 to 1.1994nm, and the particle size ranged from 31-96nm. The similar variation was given by a measure of laser particle analyzer. The TG-DTA results indicated 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 showed that alcohol was more effective for the well-dispersion of the nano-sized Nd:YAG powders. These experimental results provided references to prepare good powders of YAG transparent ceramics.

Key words: materials, nanoscaled powders, urea co-precipitation, Nd:YAG, particle size

李冬青丁丽华张庆礼邵淑芳宁凯杰殷绍唐. 尿素共沉淀法制备Nd:YAG纳米粉体[J]. J4, 2010, 27(1): 110-115.

LI Dong-Qing, DING Li-Hua, ZHANG Qing-Li, SHAO Shu-Fang, NING Kai-Jie, YIN Shao-Tang. Preparation of nanoscaled Nd:YAG powders by the urea co-precipitation method[J]. J4, 2010, 27(1): 110-115.

参考文献

[1] Wang Baosong, Jiang Haihe, Zhang Qingli, et al. Analysis on the temperature field of LD array pumped Nd:GGG disc laser in heat-capacity mode [J]. Chinese Journal of Quantum Electronics (量子电子学报),2007,24(6):688-693 (in Chinese).
[2] Zhang Qingli, Shao Shufang, Su Jing, et al. Study on raw material preparation method, crystal growth and structure of the scandium-containing garnet Nd:GSGG [J]. Chinese Journal of Quantum Electronics (量子电子学报), 2005, 22(4): 559-564 (in Chinese).
[3] Sun Dunlu, Zhang Qingli, Wang Zhaobing, et al. Study on the spectral characteristics of Nd:GSGG laser crystal [J]. Chinese Journal of Quantum Electronics (量子电子学报), 2005, 22(4): 570-573 (in Chinese).
[4] Lu J, Murai T, Takaichi K, et al. 72W Nd:Y3Al5O12 ceramic laser [J]. Appl. Phys. Lett., 2001, 78(23): 3586-3588. [5] Xu Guogang, Zhang Xudong, He Wen, et al. The study of surfactant application on synthesis of YAG nano-sized powders [J]. Powder Technology, 2006 163:202-205.
[6] Li Jiang, Pan Yubai, Zhang Junji, et al. Synthesizing yttrium aluminum garnet(YAG) nano-podwer by co-precipitation method[J]. Journal of the Chinese Ceramic Society(硅酸盐学报), 2003, 31(5): 490-493 (in Chinese). [7] Su Chunhui, Song Qiong, Zhang Huashan, et al. Neodymium-doped yttrium aluminum Garnet transparent laser ceramics prepared by co-precipitation method [J]. Journal of the Chinese Rare Earth Society(中国稀土学报), 2006, 24(1): 56-60 (in Chinese).
[8] Li Xia, Liu Hong, Wang Jiyang, et al. Preparation and properties of YAG nano-sized powder from different precipitation agent [J]. Opt. Mater.,2004, 25: 407–412.
[9] Piao Xianqing, Lu Liping, Liu Jinghe, et al. Preparation of Yb:YAG transparent laser ceramic with CO(NH2)2 co-precipitation method[J]. Journal of Functional Materials and Devices (功能材料与器件学报), 2004, 10(2): 264-268 (in Chinese).
[10] Sordelet D, Akinc M. Preparation of spherical, monosized Y2O3 precursor particles [J]. J. Coll. Int. Sci., 1988, 122(1): 47-59.
[11] Ye Yun, Zhou Guangming, Li Qiaoling, et al. Development of ferrite nanocrystalline microstructures during sintering[J]. Mechanical Management and Development (机械管理开发), 2006,(3):1-3 (in Chinese).
[12] Teng Fei, Ning Guiling, Tian Zhijian, et al. Measurement of size distribution of ultrafine particles by laser light scattering method [J]. Chinese Journal of Light Scattering (光散射学报), 2004, 16(2): 172-176 (in Chinese).

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