放电等离子烧结制备高致密LiNbO3陶瓷的研究

硅酸盐通报 ›› 2023, Vol. 42 ›› Issue (6): 2190-2196.

所属专题：陶瓷

放电等离子烧结制备高致密LiNbO₃陶瓷的研究

侯俊峰^1,2, 张明哲^1,2, 田少华¹, 吴集思³, 江文莉^1,2

1.北方民族大学材料科学与工程学院,银川 750021;
2.碳基先进陶瓷制备技术国家地方联合工程研究中心,银川 750021;
3.南昌航空大学航空制造工程学院,南昌 330000

收稿日期:2023-03-27 修订日期:2023-03-27 出版日期:2023-06-15 发布日期:2023-06-25
作者简介:侯俊峰(1979—),男,博士,讲师。主要从事功能陶瓷材料的研究。E-mail:hou8635@yeah.net
基金资助:
宁夏回族自治区重点研发计划(2022BDE03005)

Preparation of High Density LiNbO₃ Ceramics by Spark Plasma Sintering

HOU Junfeng^1,2, ZHANG Mingzhe^1,2, TIAN Shaohua¹, WU Jisi³, JIANG Wenli^1,2

1. School of Materials Science & Engineering, North Minzu University, Yinchuan 750021, China;
2. National and Local Joint Engineering Research Center of Advanced Carbon Based Ceramics Preparation Technology, Yinchuan 750021, China;
3. School of Aeronautical Manufacturing Engineering, Nanchang Hangkong University, Nanchang 330000, China

Received:2023-03-27 Revised:2023-03-27 Online:2023-06-15 Published:2023-06-25

摘要/Abstract

摘要： 为解决LiNbO₃粉体烧结活性低、高温下Li元素烧失导致的烧结体致密度低的问题,采用固相反应法合成化学计量比的LiNbO₃粉体,通过还原处理增加其氧空位浓度,然后采用放电等离子烧结(SPS)技术对其进行烧结,制备出高致密LiNbO₃陶瓷。利用XRD、EPR、XPS、Raman光谱仪、SEM对LiNbO₃粉体及其陶瓷进行表征和分析,结果表明,LiNbO₃粉体经700 ℃还原处理后氧空位浓度显著增大,且氧空位出现在Nb—O八面体中O原子的晶格位置。随着SPS温度的升高,LiNbO₃陶瓷的相对密度呈先增大后减小的趋势,900 ℃时烧结体的相对密度达到最大,为98.19%。经800 ℃退火增氧处理后,LiNbO₃陶瓷由黑色转变为白色,氧空位缺陷被消除,LiNbO₃陶瓷相对密度为98.32%。本研究为高致密碱金属铌酸盐陶瓷的制备提供了新思路。

关键词: LiNbO₃, 氧空位, Nb—O八面体, 放电等离子烧结, 相对密度, 晶粒尺寸

Abstract: In order to solve the problem of low sintering density caused by low sintering activity of LiNbO₃ powders and loss on ignition of Li element at high temperature, LiNbO₃ powders with stoichiometric ratio were synthesized by solid phase reaction method. The oxygen vacancy concentration of LiNbO₃ powders increased by reduction treatment, and then high density LiNbO₃ ceramics were prepared by spark plasma sintering (SPS) technology. The phase composition, oxygen vacancy concentration and surface morphology of LiNbO₃ powders and the sintered body were characterized and analyzed by XRD, EPR, XPS, Raman spectroscopy and SEM. The results show that the oxygen vacancy concentration of LiNbO₃ powders increases significantly after 700 ℃ reduction treatment, and the oxygen vacancies generate at the lattice position of O atom in Nb—O octahedron. With the increase of SPS temperature, the relative density of LiNbO₃ ceramics shows a trend of increasing first and then decreasing. The relative density of sintered body reaches a maximum of 98.19% at 900 ℃. After annealing and oxygen increasing treatment at 800 ℃, the color of LiNbO₃ ceramics changes from black to white. At the same time, the oxygen vacancy defect of LiNbO₃ ceramics is eliminated and the relative density is 98.32%. This study provides a new idea for the preparation of high density alkali metal niobate ceramics.

Key words: LiNbO₃, oxygen vacancy, Nb—O octahedron, spark plasma sintering, relative density, grain size

中图分类号:

TB34
TQ174

侯俊峰, 张明哲, 田少华, 吴集思, 江文莉. 放电等离子烧结制备高致密LiNbO₃陶瓷的研究[J]. 硅酸盐通报, 2023, 42(6): 2190-2196.

HOU Junfeng, ZHANG Mingzhe, TIAN Shaohua, WU Jisi, JIANG Wenli. Preparation of High Density LiNbO₃ Ceramics by Spark Plasma Sintering[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2023, 42(6): 2190-2196.

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放电等离子烧结制备高致密LiNbO₃陶瓷的研究

Preparation of High Density LiNbO₃ Ceramics by Spark Plasma Sintering

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