铝源种类对熔盐法制备超细ZnAl2O4粉体的影响

人工晶体学报 ›› 2021, Vol. 50 ›› Issue (12): 2347-2353.

铝源种类对熔盐法制备超细ZnAl₂O₄粉体的影响

黄德鹏¹, 许欢¹, 刘江波², 付应文¹, 周振鹏¹

1.九江学院材料科学与工程学院,九江 332005;
2.浙江自力高温科技股份有限公司,绍兴 312000

收稿日期:2021-09-06 出版日期:2021-12-15 发布日期:2022-01-06
通讯作者: 许欢,博士,讲师。E-mail:xuhuan_wust@126.com
作者简介:黄德鹏(2001—),男,江西省人。E-mail:3249937731@qq.com
基金资助:
江西省高等学校大学生创新创业训练计划(S202011843003);江西省教育厅科学技术研究项目(GJJ201833);省部共建耐火材料与冶金国家重点实验室开放基金(G202006)

Influences of Alumimum Source Types on Preparation of Ultrafine ZnAl₂O₄ Powders by Molten Salt Method

HUANG Depeng¹, XU Huan¹, LIU Jiangbo², FU Yingwen¹, ZHOU Zhenpeng¹

1. School of Materials Science and Engineering, Jiujiang University, Jiujiang 332005, China;
2. Zhejiang Zili High Temperature Technology Co., Ltd., Shaoxing 312000, China

Received:2021-09-06 Online:2021-12-15 Published:2022-01-06

摘要/Abstract

摘要： 本文以Al(OH)₃、煅烧Al₂O₃和纳米Al₂O₃为铝源,在KCl和LiCl的混合熔盐介质中,800~1 200 ℃温度范围内保温3 h合成超细ZnAl₂O₄粉体。采用XRD、SEM、激光粒度仪和比表面分析仪等重点分析了铝源种类对ZnAl₂O₄粉体合成温度、产物物相组成以及显微形貌的影响。在此基础上探讨了反应温度、熔盐与原料的质量比(W_s/W_r)对粉体合成的影响。结果表明:铝源种类显著影响ZnAl₂O₄的开始形成温度和粉体性能,相比于煅烧Al₂O₃,以Al(OH)₃和纳米Al₂O₃为铝源生成ZnAl₂O₄的速率较快,在900 ℃时即可合成出单相ZnAl₂O₄。以煅烧Al₂O₃粉为铝源,当W_s/W_r为3∶1时,在1 000 ℃合成ZnAl₂O₄粉体的分散性最佳,而温度过高易造成粉体团聚长大。适当的W_s/W_r有利于ZnAl₂O₄的生成,当W_s/W_r为4∶1时合成的ZnAl₂O₄粒径最小。ZnAl₂O₄粉体均在一定程度保持着初始铝源的尺寸和形貌,表明熔盐法合成ZnAl₂O₄的机理主要遵循着“模板合成机理”。

关键词: ZnAl₂O₄, 熔盐法, 熔盐介质, 铝源种类, 物相组成, 显微形貌

Abstract: In this paper, ZnAl₂O₄ powders were synthesized by molten salt method at 800~1 200 ℃ for 3 h in the mixed molten salt medium of KCl and LiCl using Al(OH)₃, calcined Al₂O₃ and nano-Al₂O₃ as different aluminum sources respectively. The effects of aluminum source types on the synthesis temperature, phase composition and microstructure of the synthesized products were mainly analyzed by XRD, SEM, laser particle size analysis, and specific surface analysis. On this basis, the effects of reaction temperature and the mass ratio of molten salt to raw material (W_s/W_r) on the synthesis of ZnAl₂O₄ powders were discussed. The results show that the type of aluminum source significantly affect the formation temperature of ZnAl₂O₄ and powder performances. Compared with calcined Al₂O₃, the speed of ZnAl₂O₄ formation is faster with Al(OH)₃ and nano-Al₂O₃ as the aluminum sources, and the pure phase ZnAl₂O₄ can be synthesized at 900 ℃. When calcined Al₂O₃ is used as an aluminum source, and the W_s/W_r ratio is 3∶1, the as-synthesized ZnAl₂O₄ powder exhibits best dispersibility, but higher temperatures easily lead to the agglomeration of powders. The formation of ZnAl₂O₄ can be promoted by the appropriate W_s/W_r ratio, and the particle size is the smallest when the W_s/W_r ratio is 4∶1. The ZnAl₂O₄ still retains the initial size and morphology of original Al₂O₃ raw material, indicating that the synthesis of ZnAl₂O₄ by molten salt method is mainly followed the “template synthesis mechanism”.

Key words: ZnAl₂O₄, molten salt method, molten salt medium, aluminum source type, phase composition, microstructure

中图分类号:

TB383.3

黄德鹏, 许欢, 刘江波, 付应文, 周振鹏. 铝源种类对熔盐法制备超细ZnAl₂O₄粉体的影响[J]. 人工晶体学报, 2021, 50(12): 2347-2353.

HUANG Depeng, XU Huan, LIU Jiangbo, FU Yingwen, ZHOU Zhenpeng. Influences of Alumimum Source Types on Preparation of Ultrafine ZnAl₂O₄ Powders by Molten Salt Method[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2021, 50(12): 2347-2353.

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铝源种类对熔盐法制备超细ZnAl₂O₄粉体的影响

Influences of Alumimum Source Types on Preparation of Ultrafine ZnAl₂O₄ Powders by Molten Salt Method

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