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2222材料工程  2022, Vol. 50 Issue (6): 97-106    DOI: 10.11868/j.issn.1001-4381.2021.000401
  研究论文 本期目录 | 过刊浏览 | 高级检索 |
并流共沉淀法合成Dy2O3-ZrO2纳米粉体
程慧聪1, 王雅雷1,*(), 李阿欣1, 刘怀菲2,*(), 武囡囡1, 刘蓉1
1 中南大学 粉末冶金国家重点实验室, 长沙 410083
2 中南林业科技大学 材料科学与工程学院, 长沙 410004
Synthesis of Dy2O3-ZrO2 nano powders by cocurrent coprecipitation
Huicong CHENG1, Yalei WANG1,*(), Axin LI1, Huaifei LIU2,*(), Nannan WU1, Rong LIU1
1 State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083, China
2 School of Materials Science and Engineering, Central South University of Forestry and Technology, Changsha 410004, China
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摘要 

采用并流化学共沉淀法合成了Dy2O3掺杂ZrO2(DySZ)纳米粉体材料,系统研究稳定剂掺杂量、阳离子浓度、反应系统pH值和煅烧温度对粉体材料物相组成、晶体结构和微观形貌的影响。结果表明:不同合成工艺条件下,DySZ粉体材料均具有纳米尺度特征,球形颗粒尺寸为10~30 nm,Dy2O3的掺杂可以起到稳定晶型的作用; 稳定剂掺杂量对DySZ粉体的物相组成具有明显影响,掺杂量为10%(质量分数)时可合成单一四方相结构的DySZ粉体; DySZ粉体材料的四方度和微观形貌对稳定剂掺杂量、阳离子浓度、反应体系pH值和煅烧温度均不敏感,但其平均晶粒尺寸随稳定剂掺杂量、阳离子浓度和反应体系pH值的升高略有降低,随煅烧温度的提高而显著增加。

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程慧聪
王雅雷
李阿欣
刘怀菲
武囡囡
刘蓉
关键词 Dy2O3-ZrO2粉体并流共沉淀法晶体结构微观形貌    
Abstract

Nano-sized Dy2O3 doped ZrO2 powders (DySZ) were synthesized by cocurrent co-precipitation method. The effects of Dy2O3 content, cation concentration, pH value and calcination temperature on the phase composition, crystal structure, grain size and micromorphology of DySZ powders were investigated. Results show that under different synthesis conditions, the spherical DySZ powders have nano scale characteristics with a size range of 10-30 nm, Dy2O3-doping can promote the DySZ stabilized as tetragonal structure. The doping amount of stabilizer has a significant effect on the phase composition of DySZ powder. Single tetragonal DySZ can be obtained with 10%(mass fraction) Dy2O3-doping. No significant effect can be found between the tetragonality, microstructure of DySZ powders and the stabilizer content, cation concentration, pH value as well as calcination temperature. The average grain size exhibits a slight decrease with the increase of stabilizer content, cation concentration and pH value. Meanwhile, the elevated calcination temperature can promote the crystal growth of DySZ.

Key wordsDy2O3-ZrO2 powders    cocurrent coprecipitation method    crystal structure    micromorphology
收稿日期: 2021-04-28      出版日期: 2022-06-20
中图分类号:  TQ174  
  TB383  
基金资助:国家科技重大专项(2017-Ⅵ-0020-0092);湖南省教育厅科学研究项目(19C1913)
通讯作者: 王雅雷,刘怀菲     E-mail: yaleipm@csu.edu.cn;huaifei011@126.com
作者简介: 刘怀菲(1983—),女,讲师,博士,主要从事高温热防护涂层材料的研究,联系地址:湖南省长沙市天心区韶山南路498号中南林业科技大学材料科学与工程学院(410004),E-mail: huaifei011@126.com
王雅雷(1982—),男,副研究员,博士,主要从事高性能碳基复合材料、粉末冶金材料的研究,联系地址:湖南省长沙市岳麓区麓山南路932号中南大学粉末冶金国家重点实验室(410083),E-mail: yaleipm@csu.edu.cn
引用本文:   
程慧聪, 王雅雷, 李阿欣, 刘怀菲, 武囡囡, 刘蓉. 并流共沉淀法合成Dy2O3-ZrO2纳米粉体[J]. 材料工程, 2022, 50(6): 97-106.
Huicong CHENG, Yalei WANG, Axin LI, Huaifei LIU, Nannan WU, Rong LIU. Synthesis of Dy2O3-ZrO2 nano powders by cocurrent coprecipitation. Journal of Materials Engineering, 2022, 50(6): 97-106.
链接本文:  
http://jme.biam.ac.cn/CN/10.11868/j.issn.1001-4381.2021.000401      或      http://jme.biam.ac.cn/CN/Y2022/V50/I6/97
Fig.1  并流共沉淀法合成DySZ粉体工艺流程图
Mass fraction of Dy2O3/% Cation concentration/
(mol·L-1)
pH value Calcination
temperature/
Holding time/h
5-15 0.5 11 800 2
10 0.1-0.9 11 800 2
10 0.5 7-11 800 2
10 0.5 11 500-800 2
Table 1  DySZ粉体合成工艺参数
Fig.2  不同稳定剂掺杂量合成DySZ粉体的XRD图谱
(a)全谱; (b)27°~32°特征区域; (c)72°~76°特征区域
Fig.3  DySZ粉体材料的四方度与晶粒尺寸随稳定剂含量的变化
Fig.4  不同稳定剂掺杂量合成DySZ粉体的微观形貌
(a)5%;(b)7.5%;(c)10%;(d)12.5%;(e)15%
Fig.5  不同阳离子浓度合成10DySZ粉体的XRD图谱
Fig.6  10DySZ粉体材料的四方度与晶粒尺寸随阳离子浓度的变化
Fig.7  不同阳离子浓度合成10DySZ粉体的微观形貌
(a)0.1 mol/L; (b)0.3 mol/L; (c)0.5 mol/L; (d)0.7 mol/L; (e)0.9 mol/L
Fig.8  不同反应系统pH值合成DySZ粉体的XRD图谱
Fig.9  10DySZ粉体材料的四方度与晶粒尺寸随pH值的变化
Fig.10  不同反应体系pH值合成10DySZ粉体的微观形貌
(a)pH=7;(b)pH=8;(c)pH=9;(d)pH=10;(e)pH=11
Fig.11  10DySZ前驱体的TG-DSC曲线
Fig.12  不同煅烧温度合成10DySZ粉体的XRD图谱
Fig.13  10DySZ粉体材料的四方度与晶粒尺寸随煅烧温度变化
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