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“通过硝酸盐改性的醇盐合成路线制备的La2Zr2O7陶瓷无定形前体中Zr局部环境的XAFS研究

"XAFS study of Zr local environment in amorphous precursors of La2Zr2O7 ceramics prepared by a nitrate-modified alkoxide synthesis route
课程网址: http://videolectures.net/slonano07_ion_xsz/  
主讲教师: Elena Ion
开课单位: 约瑟夫·斯特凡学院
开课时间: 2008-02-12
课程语种: 英语
中文简介:
我们通过硝酸盐改性的醇盐溶胶凝胶合成路线制备了La2Zr2O7。将脱水的硝酸镧与正丁醇锆在2-甲氧基乙醇中混合并回流3小时。将获得的液体缓慢干燥。在150℃下,样品自燃。根据XRD,粉末在加热至700oC时为无定形,并在800oC发生结晶。该粉末由约70nm尺寸的纳米颗粒的易碎附聚物组成。通过EXAFS分析,我们研究了从溶胶转变为无定形粉末后的Zr和La局部环境,以了解亚纳米级上组成金属原子的分布。我们观察到,溶胶和在150 oC干燥并在500 oC加热的前体粉末的Zr EXAFS光谱相似,这表明在液态无定形固体转变过程中,Zr原子的局部环境没有受到影响,Zr – O – Zr连接它们已经在溶胶中形成,甚至可以在加热到500 oC的粉末中保存。在溶胶或无定形粉末中未观察到La-O-Zr键。 LZ溶胶的La EXAFS光谱类似于脱水硝酸镧(LN sol)的光谱,而在干燥和加热的粉末的光谱中,注意到第二个峰消失了。无法建立La La或La Zr关联。由于在合成的早期阶段没有确定La和Zr物种之间的联系,因此当可进行长距离扩散并导致纯烧绿石相时,物种之间的反应以固态反应进行。拟议的合成路线,允许在纳米级别的物种很好的混合。
课程简介: We prepared La2Zr2O7 by the nitrate-modified alkoxide-based sol-gel synthesis route. The dehydrated lanthanum nitrate was mixed with zirconium n-butoxide in 2-methoxyethanol and refluxed for 3 h. The obtained liquid was slowly dried. At 150oC, the sample self-ignited. According to XRD, the powder was amorphous upon heating up to 700oC and crystallization took place at 800oC. The powder was composed of friable agglomerates of about 70 nm sized nano-particles. By EXAFS analysis we investigated the Zr and La local environment upon transition from the sol to the amorphous powder in order to learn about the distribution of the constituent metal atoms at the sub-nanometer level. We observed that the Zr EXAFS spectra of the sol and the precursor powder dried at 150 oC and heated at 500 oC were similar, indicating that the local environment of Zr atoms was not affected during the liquid-amorphous solid transition, Zr – O – Zr links were formed already in the sol and preserved even in the powder heated at 500 oC. No La – O – Zr links in the sol or in the amorphous powder were observed. The La EXAFS spectrum of the LZ sol is similar to the spectrum of dehydrated lanthanum nitrate (LN sol), while in the spectra of dried and heated powder, vanishing of the second peak was noticed. No La-La or La-Zr corelation could be established. Since no link, between La and Zr species, was confirmed in the early stages of the synthesis, the reaction between the species proceeded as a solid-state reaction when long range diffusion became available leading to the pure pyrochlore phase. The proposed synthesis route, allowed a very good mixing of the species at the nanometre level.
关 键 词: 硝酸盐; 路线; 光谱
课程来源: 视频讲座网
最后编审: 2019-09-28:yuh
阅读次数: 53