La2Zr2O7 Powder with Pyrochlore Structure by Molten Salt Synthesis
摘 要
以氧化锆和氧化镧为反应原料, 以氯化钾-氯化锂为熔盐介质, 采用熔盐法制备了烧绿石结构锆酸镧(La2Zr2O7)粉体, 研究了反应温度和熔盐含量对该粉体纯度的影响, 并分析了其显微结构。结果表明:La2Zr2O7粉体除了由原料直接反应合成外, 还有部分是由La2O3与熔盐先生成中间产物LaOCl, 该中间产物再与ZrO2反应而生成; La2Zr2O7相的生成量随反应温度的升高而增加, 随熔盐含量的增加先增后减; 当熔盐与反应原料的质量比为3∶1时, 在1 200 ℃下反应3 h后可以合成纯La2Zr2O7相的粉体, 其形貌与原料ZrO2粉体的基本相似, 呈无规则颗粒状, 晶粒大小为80~200 nm。
Abstract
The La2Zr2O7 powders with pyrochlore structure were synthesized by the molten salt method with zirconium oxide and lanthanum oxide as reaction materials and with potassium chloride and lithium chloride as reaction media. The influences of reaction temperatures and molten salt content on the powder purity were investigated and the microstructures of the prepared powders was analyzed. The results show that apart from that directly prepared by the reaction materials, the La2Zr2O7 powders were also synthesized by the reaction of ZrO2 powder with intermediate product of LaOCl produced by the reaction of La2O3 powder with molten salts. The production of La2Zr2O7 phase increased with the increase of the reaction temperature and first increased then decreased with the molten salt content increase. Pure La2Zr2O7 powder was obtained under the condition of reaction at 1 200 ℃ for 3 h with the mass ratio of molten salt to reaction material of 3∶1. The morphology of the prepared La2Zr2O7 powder was similar to that of raw material ZrO2 powder, showing an irregular particle shape with grain sizes of 80-200 nm.
中图分类号 TQ174 DOI 10.11973/jxgccl201606012
所属栏目 新材料 新工艺
基金项目 “973”计划前期研究专项(2014CB660802); 国家自然科学基金面上资助项目(51272188, 51472184, 51472185); 湖北省自然科学基金重点资助项目(2013CFA086); 湖北省科技支撑计划对外科技合作项目(2013BHE002)
收稿日期 2015/11/25
修改稿日期 2016/4/26
网络出版日期
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备注黄仲(1990-), 男, 湖北咸宁人, 硕士研究生。
引用该论文: HUANG Zhong,LI Sai-sai,TAN Cao,LIU Jiang-hao,LU Li-lin,ZHANG Shao-wei,ZHANG Hai-jun. La2Zr2O7 Powder with Pyrochlore Structure by Molten Salt Synthesis[J]. Materials for mechancial engineering, 2016, 40(6): 55~58
黄仲,李赛赛,谭操,刘江昊,鲁礼林,张少伟,张海军. 熔盐法合成烧绿石结构La2Zr2O7粉体[J]. 机械工程材料, 2016, 40(6): 55~58
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参考文献
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【4】GUO X,ZHANG J.First principles study of thermodynamic properties of lanthanum zirconate[J].Materials Today:Proceedings,2014,1(1):25-34.
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【6】TONG Y,ZHU J,LU L,et al.Preparation and characterization of Ln2Zr2O7 (Ln=La and Nd) nanocrystals and their photocatalytic properties[J].Journal of Alloys and Compounds,2008,465 (1):280-284.
【7】CHEN D,XU R.Hydrothermal synthesis and characterization of La2M2O7 (M=Ti, Zr) powders[J].Materials Research Bulletin,1998,33(3):409-417.
【8】ARUNA S T,SANJEEVIRAJA C,BALAJI N,et al.Properties of plasma sprayed La2Zr2O7 coating fabricated from powder synthesized by a single-step solution combustion method[J].Surface & Coatings Technology,2013,219:131-138.
【9】RAO K K,BANU T,VITHAL M,et al.Preparation and characterization of bulk and nano particles of La2Zr2O7 and Nd2Zr2O7 by sol-gel method[J].Materials Letters,2002,54(2):205-210.
【10】MAO Y,GUO X,HUANG J Y,et al.Luminescent nanocrystals with A2B2O7 composition synthesized by a kinetically modified molten salt method[J].Journal of Physical Chemistry C,2009,113(4):1204-1208.
【11】WANG X,ZHU Y,ZHANG W.Preparation of lanthanum zirconate nano-powders by molten salts method[J].Journal of Non-Crystalline Solids,2010,356(20):1049-1051.
【12】LI Z S,LEE W E,ZHANG SW.Low-temperature synthesis of CaZrO3 powder from molten salt[J].Journal of the American Ceramic Society,2007,90(2):364-368.
【13】HUANG Z,LIU J H,DENG X G,et al.Low temperature molten salt preparation of molybdenum nanoparticles[J].International Journal of Refractory Metals & Hard Materials,2016,54:315-321.
【14】ZHANG S W,JAYASEELAN D D,BHATTACHARYA G,et al.Molten salt synthesis of magnesium aluminate (MgAl2O4) spinel powder[J].Journal of the American Ceramic Society,2006,89(5):1724-1726.
【15】LI Z S,ZHANG S W,LEE W E.Molten salt synthesis of LaAlO3 powder at low temperatures[J].Journal of the European Ceramic Society,2007,27:3201-3205.
【16】CHERGINETS V L,DEINEKA T G,DEMIRSKAYA O V,et al.Potentiometric investigation of oxide solubilities in molten KCl-NaCl eutectic:the effect of surface area of solid particles on the solubilities [J].Journal of Electroanalytical Chemistry,2002,531:171-178.
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