液相法制备棒状Al2O3及Al2O3-ZrO2陶瓷复合粉体

doi:10.16085/j.issn.1000-6613.2021-0730

化工进展 ›› 2021, Vol. 40 ›› Issue (S2): 309-314.DOI: 10.16085/j.issn.1000-6613.2021-0730

液相法制备棒状Al₂O₃及Al₂O₃-ZrO₂陶瓷复合粉体

靳元勋¹(), 霍地¹(), 孙旭东¹^,²

^1.东北大学材料科学与工程学院，材料各向异性与织构教育部重点实验室，辽宁沈阳 110819
^2.东北大学佛山研究生院，广东佛山 528311

收稿日期:2021-04-07 修回日期:2021-05-07 出版日期:2021-11-12 发布日期:2021-11-12
通讯作者: 霍地
作者简介:靳元勋（1995—），男，硕士研究生，研究方向为陶瓷粉末制备。E-mail：1377225714@qq.com。
基金资助:
国家自然科学基金(51872033)

Preparation of rod-like Al₂O₃ and Al₂O₃-ZrO₂ ceramic composite powders in aqueous solution

JIN Yuanxun¹(), HUO Di¹(), SUN Xudong¹^,²

^1.School of Materials Science and Engineering, Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), Northeastern University, Shenyang 110819, Liaoning, China
^2.Foshan Graduate School of Northeastern University, Foshan 528311, Guangdong, China

Received:2021-04-07 Revised:2021-05-07 Online:2021-11-12 Published:2021-11-12
Contact: HUO Di

摘要/Abstract

摘要：

采用二乙三胺五乙酸（DTPA）为配合剂，以简易的液相法合成出微纳米纤维状Al和Al-Zr前体，煅烧处理制备了棒状α-Al₂O₃和Al₂O₃-ZrO₂复合陶瓷粉体。同时研究了DPTA∶Al³⁺质量比、反应温度与时间对陶瓷粉体形态的影响。利用X射线衍射（XRD）、热分析（TG/DSC）以及扫描电子显微镜（SEM）对粉体进行了表征。结果表明：较高的DTPA∶Al³⁺质量比以及较长的反应时间有利于制备高长径比的纤维棒状Al和Al-Zr配合物前体。合成纳米纤维状α-Al₂O₃和Al₂O₃-ZrO₂前体的最优条件是反应温度60℃，反应时间5.5h，DTPA∶Al³⁺比例为1.2∶1。相应地，该前体煅烧后可以制备出棒状α-Al₂O₃和Al₂O₃-ZrO₂复合陶瓷粉体。

关键词: 棒状粉体, α-Al₂O₃, Al₂O₃-ZrO₂, 液相法, 二乙三胺五乙酸

Abstract:

Using diethylenetriaminepentaacetic acid (DTPA) as coordination agent, the micro/nano Al and Al-Zr fibrous precursors were synthesized by a simple liquid synthesis method, and further calcined to make rod-like α-Al₂O₃ ceramic and Al₂O₃-ZrO₂ composite powders. The effects of mass ratio of DTPA to Al³⁺, reaction temperature and time on the morphology of ceramic powders were simultaneously studied. The powders were characterized by X-ray diffraction (XRD), thermal analysis (TG/DSC) and scanning electron microscope (SEM). The results show that higher mass ratio of DTPA to Al³⁺ along with longer reaction time are favorable for the preparation of fibrous Al and Al-Zr complex precursors with high aspect ratio. The optimized conditions to prepare the nanofibrous α-Al₂O₃ and Al₂O₃-ZrO₂ precursors are controlled the mass ratio with m(DTPA)∶m(Al³⁺)=1.2∶1 at 60℃ for 5.5h. Correspondingly, rod-shaped α-Al₂O₃ and Al₂O₃-ZrO₂ composite ceramic powders can be prepared by calcining these precursors.

Key words: rod-like powders, α-Al₂O₃, Al₂O₃-ZrO₂ composites, low-temperature liquid phase synthesis, diethylenetriaminepentaacetic acid(DTPA)

中图分类号:

TQ343.5

靳元勋, 霍地, 孙旭东. 液相法制备棒状Al₂O₃及Al₂O₃-ZrO₂陶瓷复合粉体[J]. 化工进展, 2021, 40(S2): 309-314.

JIN Yuanxun, HUO Di, SUN Xudong. Preparation of rod-like Al₂O₃ and Al₂O₃-ZrO₂ ceramic composite powders in aqueous solution[J]. Chemical Industry and Engineering Progress, 2021, 40(S2): 309-314.

图/表 7

图1 不同m(DTPA)∶m[Al(NO3)3·9H2O]比例时Al配合物前体SEM形貌

图2 不同温度和时间条件下Al配合物前体的SEM形貌

图3 铝前体的XRD图谱与热分析曲线

图4 棒状α-Al2O3的XRD图谱与SEM形貌

图5 不同时间与ZrO2含量条件下Al-Zr复合前体的SEM形貌

图6 棒状Al2O3-ZrO2复合粉体SEM形貌与XRD图谱

图7 棒状Al2O3-ZrO2复合陶瓷粉体的EDS分析

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液相法制备棒状Al₂O₃及Al₂O₃-ZrO₂陶瓷复合粉体

Preparation of rod-like Al₂O₃ and Al₂O₃-ZrO₂ ceramic composite powders in aqueous solution

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