高纯多晶LaB6纳米块体阴极材料的制备及表征

doi:10.3724/SP.J.1077.2008.01199

无机材料学报

高纯多晶LaB₆纳米块体阴极材料的制备及表征

周身林, 刘丹敏, 张久兴

北京工业大学材料学院新型功能材料教育部重点实验室, 北京 100022

收稿日期:2007-12-28 修回日期:2008-03-11 出版日期:2008-11-20 网络出版日期:2008-11-20

Fabrication and Characterization of High-purity Nanostructured Bulk LaB₆ Polycrystal Cathode Material

ZHOU Shen-Lin, LIU Dan-Min, ZHANG Jiu-Xing

The Key Laboratory of Advanced Functional Materials, Ministry of Education, College of Materials Science and Engineering, Beijing University of Technology, Beijing 100022, China

Received:2007-12-28 Revised:2008-03-11 Published:2008-11-20 Online:2008-11-20

摘要/Abstract

摘要： 采用放电等离子烧结技术, 以氢直流电弧法制备的La-LaH₂纳米粉末为原料, 制备了高纯LaB₆多晶纳米块体热阴极材料. 系统研究了LaH₂的脱氢反应、SPS合成LaB₆的烧结反应式, 并用XRD、SEM、TEM和AFM对LaB₆烧结块体的相与结构进行了表征. 实验结果表明, LaH2在796.4℃时发生脱氢反应; SPS制备得到了单相LaB₆纳米多晶块体, 纯度达到99.867%, 相对密度达到99.2%, 和其他烧结方法相比, 样品显微硬度及抗弯强度等性能显著提高. 晶体为大小均匀, 形态规则完整的等轴晶, 50MPa, 烧结温度1250～1350℃范围内平均晶粒尺寸为120nm, 随烧结温度的升高, 晶粒尺寸逐渐增大.

关键词: 放电等离子烧结, 多晶LaB₆, 纳米块体, 热阴极

Abstract: La-LaH₂ nanopowders were prepared by hydrogen arc plasma method, and then the mixed nanopowders of La-LaH₂ and B were in situ sintered by Sparkle Plasma Sintering (SPS) method in oxygen free system. High-purity LaB₆ polycrystal nanostructured bulk was successfully synthesized by SPS. The dehydrogenation of LaH₂ nanopowders and the reaction equation of sintering LaB₆ were studied. The phase and microstructure of LaB₆ bulks were characterized by using XRD, SEM, TEM and AFM techniques. The results show that the dehydrogenation temperature of LaH₂ nanopowders is 796.4℃. The sintered body is single-phase LaB₆, which has a high purity of 99.867%, and its relative densities is up to 99.2%. The hardness and bend strength of the sintered LaB₆ are much better than those of LaB₆ prepared by other sintering methods. The crystals of LaB₆ bulk are equiaxed crystals, the average grain size of the bulks sintered at 50MPa and 1250-1350℃ is about 120nm. The grains are homogeneous and integrated, and the grain size increases with the raising of sintering temperature.

Key words: spark plasma sintering (SPS), polycrystal Lanthanum hexaboride, nanostructured bulk, hot cathode

中图分类号:

周身林,刘丹敏,张久兴. 高纯多晶LaB₆纳米块体阴极材料的制备及表征[J]. 无机材料学报, DOI: 10.3724/SP.J.1077.2008.01199.

ZHOU Shen-Lin,LIU Dan-Min,ZHANG Jiu-Xing. Fabrication and Characterization of High-purity Nanostructured Bulk LaB₆ Polycrystal Cathode Material[J]. Journal of Inorganic Materials, DOI: 10.3724/SP.J.1077.2008.01199.

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高纯多晶LaB₆纳米块体阴极材料的制备及表征

Fabrication and Characterization of High-purity Nanostructured Bulk LaB₆ Polycrystal Cathode Material

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