光谱学与光谱分析, 2016, 36 (12): 4063, 网络出版: 2016-12-30  

燃烧法合成La2Zr2O7粉及其光谱性能

Preparation of La2Zr2O7 Powder with Combustion Method and Its Spectral Properties
作者单位
1 上海应用技术学院化学与环境工程学院, 上海 201418
2 Regenia AB, Stockholm 10691, Sweden
摘要
以La2O3, Zr(NO3)4和甘氨酸为原料, 采用燃烧法合成La2Zr2O7粉。 分别用发射光谱法(ICP-AES)、 能谱法(EDAX)、 X衍射法(XRD)、 红外光谱法(IR)和热重-差热法(TG-DTA)等对La2Zr2O7粉进行表征。 分别研究了热处理温度对La2Zr2O7粉的X衍射谱和红外光谱的影响。 La2Zr2O7粉的ICP-AES和EDAX分析结果表明, 用燃烧法可合成出La2Zr2O7粉。 不同温度热处理后La2Zr2O7粉的XRD分析结果表明, 当热处理温度为600 ℃时, 出现一个衍射峰, 且衍射峰较宽, 该结构为半晶型结构; 提高热处理温度, 衍射峰逐渐尖锐, 峰形变窄, 衍射峰逐渐增多; 热处理温度在750~800 ℃范围, 可得到烧绿石结构的La2Zr2O7粉。 在650~750 ℃热处理后La2Zr2O7粉的红外光谱分析结果与XRD分析结果相同, 热处理温度为750 ℃时, 可得到烧绿石结构的La2Zr2O7粉。 La2Zr2O7粉的TG-DTG分析结果表明, 在120~1 600 ℃范围, La2Zr2O7粉的结构稳定。
Abstract
La2Zr2O7 powder was prepared with combustion method with La2O3, Zr(NO3)4 and glycine as raw materials. La2Zr2O7 powders were characterized with ICP-AES, EDAX, XRD, IR and TG-DTA techniques, respectively. Effects of heat treatment temperature on the XRD spectra and IR spectra of La2Zr2O7 powders were studied. The X-ray diffraction pattern of La2Zr2O7 powder after heat treatment at 600 ℃ has one diffraction peak, and the diffraction peak is quite broad, therefore, the crystal structure of the La2Zr2O7 powder is semi-crystal structure. With the increase of heat treatment temperature, diffraction peaks become gradually sharp and increase. The crystal structure of the La2Zr2O7 powders after heat treatment in 750~800 ℃ are pyrochlore structure. Analysis results of IR spectra of La2Zr2O7 powders after heat treatment in 650~750 ℃ show that the crystal structure of the La2Zr2O7 powders after heat treatment at 750 ℃ is pyrochlore structure, and the analysis results of XRD and IR are the same. Analysis results of TG-DTG of La2Zr2O7 powders show that the crystal structure of the La2Zr2O7 powders are stability in 120~1 600 ℃.

刘小珍, 张骋, 陈捷, 沈钦伟, 郭玲玲, 谢广. 燃烧法合成La2Zr2O7粉及其光谱性能[J]. 光谱学与光谱分析, 2016, 36(12): 4063. LIU Xiao-zhen, ZHANG Cheng, CHEN Jie, SHEN Qin-wei, GUO Ling-ling, XIE Guang. Preparation of La2Zr2O7 Powder with Combustion Method and Its Spectral Properties[J]. Spectroscopy and Spectral Analysis, 2016, 36(12): 4063.

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