高能球磨法制备铈锆铝复合氧化物的工艺

doi:10.16085/j.issn.1000-6613.2018-0777

化工进展 ›› 2018, Vol. 37 ›› Issue (10): 3958-3965.DOI: 10.16085/j.issn.1000-6613.2018-0777

高能球磨法制备铈锆铝复合氧化物的工艺

何秋梅¹, 鲁忠臣², 曾美琴³

1 广东水利电力职业技术学院机械工程系, 广东广州 510635;
2 华南理工大学机械与汽车工程学院, 广东广州 510640;
3 华南理工大学材料科学与工程学院, 广东广州 510640

收稿日期:2018-04-15 修回日期:2018-06-08 出版日期:2018-10-05 发布日期:2018-10-05
通讯作者: 何秋梅(1977-),女,副教授,研究方向为纳米材料。
作者简介:何秋梅(1977-),女,副教授,研究方向为纳米材料。E-mail:heqm@gdsdxy.edu.cn。
基金资助:
国家金属材料近净成形工程技术研究中心开放基金项目（2016002）。

Preparation process for ceria-zirconia-alumina composites by high energy ball milling

HE Qiumei¹, LU Zhongchen², ZENG Meiqin³

1 Department of Mechanical Engineering, Guangdong Polytechnic Water Resources and Electric Engineering, Guangzhou 510635, Guangdong, China;
2 School of Mechanical & Automotive Engineering, South China University of Technology, Guangzhou 510640, Guangdong, China;
3 School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640, Guangdong, China

Received:2018-04-15 Revised:2018-06-08 Online:2018-10-05 Published:2018-10-05

摘要/Abstract

摘要： 采用高能球磨法制备铈锆铝复合氧化物，运用XRD、SEM等方法研究CeO₂-ZrO₂-Al₂O₃复合催化材料分别在不同球磨时间、不同成分含量、不同焙烧温度和不同球磨工艺路线下的组织结构和稳定性能。结果表明：①随球磨时间的延长，各组元晶粒细化效果越来越明显，球磨30h，CeO₂晶粒约20nm，颗粒约200nm，但复合粉末一直未发生机械合金化。②经30h球磨的复合粉体，在1000℃以下具有良好的稳定性能，高温下有少量的ZrO₂溶入CeO₂中形成固溶体，CeO₂-ZrO₂和Al₂O₃之间表现出一定的协同稳定效应，而在1000℃以上相结构变化明显。③质量分数为18%的CeO₂和6%的ZrO₂的复合粉体颗粒比较细小，分布比较均匀，对γ-Al₂O₃的稳定化效果比较理想。④采用先将CeO₂和ZrO₂球磨30h，再添加Al₂O₃并继续球磨30h的高能球磨工艺，可制备出含大量CeO₂-ZrO₂固溶体的复合粉体，CeO₂-ZrO₂与γ-Al₂O₃相互改性作用更加理想。

关键词: 铈锆铝复合氧化物, 高能球磨, 制备工艺, 组织结构, 稳定性

Abstract: Ceria-zirconia-alumina composites were prepared by high energy ball milling. XRD and SEM were used to analyze the microstructure transformation and stability of CeO₂-ZrO₂-Al₂O₃ composite catalyst under the conditions of different milling time, content, calcination temperature and milling processes. The results indicated that:(1) The mechanical alloying of composite powders did not occur during milling process. But the effect of grain refinement was more and more obvious with the extending of milling time. The grain size of CeO₂ reached about 20 nm after milling for 30 h and the size of the particles was about 200 nm. (2) The milling composite powders showed good structural stability when roasted below 1000℃. In contrast, there would be a significant change in the phase structure when it was above 1000℃. Meanwhile, there was a small amount of ZrO₂ dissolving into CeO₂ to form solid solution with increasing calcination temperature. CeO₂-ZrO₂ and Al₂O₃ showed some synergistic and stabilizing effects with each other. (3) The particles of composites with 18% CeO₂ and 6% ZrO₂ were relatively small and well-distributed, which had the best stabilizing effect on γ-Al₂O₃. (4) Optimized the ball milling process:first, CeO₂ and ZrO₂ were milled for 30 h, then added Al₂O₃ to them and continuously milled for another 30 h. A composite powder containing a large amount of CeO₂-ZrO₂ solid solution could be prepared by this way. The interaction between CeO₂-ZrO₂ and γ-Al₂O₃ was more ideal.

Key words: ceria-zirconia-alumina composites, high energy ball milling, preparation process, microstructure, stability

中图分类号:

TQ426

何秋梅, 鲁忠臣, 曾美琴. 高能球磨法制备铈锆铝复合氧化物的工艺[J]. 化工进展, 2018, 37(10): 3958-3965.

HE Qiumei, LU Zhongchen, ZENG Meiqin. Preparation process for ceria-zirconia-alumina composites by high energy ball milling[J]. Chemical Industry and Engineering Progress, 2018, 37(10): 3958-3965.

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高能球磨法制备铈锆铝复合氧化物的工艺

Preparation process for ceria-zirconia-alumina composites by high energy ball milling

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