并流共沉淀法合成Dy2O3-ZrO2纳米粉体

doi:10.11868/j.issn.1001-4381.2021.000401

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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 words： Dy₂O₃-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

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

1	GUO L , LI M , YE F . Phase stability and thermal conductivity of RE₂O₃ (RE=La, Nd, Gd, Yb) and Yb₂O₃ co-doped Y₂O₃ stabilized ZrO₂ ceramics[J]. Ceramics International, 2016, 42 (6): 7360- 7365. doi: 10.1016/j.ceramint.2016.01.138
2	黄巧玲. 氧化钇稳定氧化锆粉体的制备与表征[D]. 长沙: 湖南大学, 2015.
2	HUANG Q L. Preparation and characterization of yttria stabilized zirconia powders[D]. Changsha: Hunan University, 2015.
3	梁明德, 于继平, 张鑫, 等. 高温热障涂层陶瓷层材料研究进展[J]. 热喷涂技术, 2013, 5 (2): 1- 9. doi: 10.3969/j.issn.1674-7127.2013.02.001
3	LIANG M D , YU J P , ZHANG X , et al. Progress in ceramic materials for high temperature thermal barrier coatings[J]. Thermal Spray Technology, 2013, 5 (2): 1- 9. doi: 10.3969/j.issn.1674-7127.2013.02.001
4	任继文, 彭蓓, 张鸿海, 等. 钇稳定氧化锆纳米粉体烧结工艺的研究[J]. 材料工程, 2009, (2): 38- 42. doi: 10.3969/j.issn.1001-4381.2009.02.009
4	REN J W , PENG B , ZHANG H H , et al. Research on the sintering processing of the yttria stabilized zirconia nano-powders[J]. Journal of Materials Engineering, 2009, (2): 38- 42. doi: 10.3969/j.issn.1001-4381.2009.02.009
5	袁佟, 邓畅光, 毛杰, 等. 等离子喷涂-物理气相沉积制备7YSZ热障涂层及其热导率研究[J]. 材料工程, 2017, 45 (7): 1- 6.
5	YUAN T , DENG C G , MAO J , et al. Preparation and thermal conductivity of 7YSZ thermal barrier coatings prepared by plasma spray-physical vapor deposition[J]. Journal of Materials Engineering, 2017, 45 (7): 1- 6.
6	LIU H , LI S , LI Q , et al. Investigation on the phase stability, sintering and thermal conductivity of Sc₂O₃-Y₂O₃-ZrO₂ for thermal barrier coating application[J]. Materials & Design, 2010, 31 (6): 2972- 2977.
7	LIU H , LI S , LI Q , et al. Microstructure, phase stability and thermal conductivity of plasma sprayed Yb₂O₃, Y₂O₃ co-stabilized ZrO₂ coatings[J]. Solid State Sciences, 2011, 13 (3): 513- 519. doi: 10.1016/j.solidstatesciences.2010.11.043
8	苏正夫, 刘怀菲, 王雅雷. La₂O₃和Y₂O₃掺杂ZrO₂复合材料的高温相稳定性、抗烧结性及热导率[J]. 复合材料学报, 2015, 32 (5): 1381- 1389.
8	SU Z F , LIU H F , WANG Y L . High temperature phase stability, sintering resistance and thermal conductivity of La₂O₃ and Y₂O₃ doped ZrO₂composites[J]. Acta Materiae Compositae Sinica, 2015, 32 (5): 1381- 1389.
9	张丹华, 王璐, 郭洪波, 等. 多元稀土氧化物掺杂二氧化锆基陶瓷材料的热物理性能[J]. 复合材料学报, 2011, 28 (2): 179- 184.
9	ZHANG D H , WANG L , GUO H B , et al. Thermophysical properties of multiple rare earth oxide co-doped zirconia-based ceramic materials[J]. Acta Materiae Compositae Sinica, 2011, 28 (2): 179- 184.
10	REN X , ZHAO M , FENG J , et al. Phase transformation behavior in air plasma sprayed yttria stabilized zirconia coating[J]. Journal of Alloys and Compounds, 2018, 750, 189- 196. doi: 10.1016/j.jallcom.2018.03.011
11	李凤梅. 稀土在航空工业中的应用现状与发展趋势[J]. 材料工程, 1998, (6): 10- 13.
11	LI F M . Application and development trend of rare earth in aviation industry[J]. Journal of Materials Engineering, 1998, (6): 10- 13.
12	郭源源, 吴基球. CeO₂-Y₂O₃共稳定纳米四方多晶氧化锆粉体的制备与研究[J]. 中国陶瓷, 2007, 43 (5): 3- 6. doi: 10.3969/j.issn.1001-9642.2007.05.001
12	GUO Y Y , WU J Q . Preparation and study of TZP nano-powder doped by ceria/yttria multi-stabilizer[J]. China Ceramics, 2007, 43 (5): 3- 6. doi: 10.3969/j.issn.1001-9642.2007.05.001
13	RAHAMAN M , GROSS J , DUTTON R , et al. Phase stability, sintering, and thermal conductivity of plasma-sprayed ZrO₂-Gd₂O₃ compositions for potential thermal barrier coating applications[J]. Acta Materialia, 2006, 54 (6): 1615- 1621. doi: 10.1016/j.actamat.2005.11.033
14	VOROZHTCOV V A , STOLYAROVA V L , SHILOV A L , et al. Thermodynamics and vaporization of the Sm₂O₃-ZrO₂ system studied by Knudsen effusion mass spectrometry[J]. Journal of Physics and Chemistry of Solids, 2021, 156, 110156. doi: 10.1016/j.jpcs.2021.110156
15	GUO L , GUO H , GONG S , et al. Improvement on the phase stability, mechanical properties and thermal insulation of Y₂O₃-stabilized ZrO₂ by Gd₂O₃ and Yb₂O₃ co-doping[J]. Ceramics International, 2013, 39 (8): 9009- 9015. doi: 10.1016/j.ceramint.2013.04.103
16	GUO L , LI M , ZHANG C , et al. Dy₂O₃stabilized ZrO₂ as a toughening agent for Gd₂Zr₂O₇ ceramic[J]. Materials Letters, 2017, 188, 142- 144. doi: 10.1016/j.matlet.2016.11.038
17	王刚, 滕佰秋, 王志宏, 等. 航空发动机上可磨耗封严涂层的应用及需求[J]. 热喷涂技术, 2012, 4 (1): 20- 23. doi: 10.3969/j.issn.1674-7127.2012.01.006
17	WANG G , TENG B Q , WANG Z H , et al. The development of abradable coatings for aeroengine[J]. Thermal Spray Technology, 2012, 4 (1): 20- 23. doi: 10.3969/j.issn.1674-7127.2012.01.006
18	SPORER D, REFKE A. Processing and properties of advanced ceramic abradable coatings[C]// Beijing: International thermal spraying Conference. 2007.
19	QULCK L , WHEATLEY R . Theoretical and experimental studies of doping effects on thermodynamic properties of (Dy, Y)-ZrO₂[J]. Acta Materialia, 2016, 114, 7- 14. doi: 10.1016/j.actamat.2016.04.007
20	曹学强. 热障涂层新材料和新结构[M]. 北京: 科学出版社, 2016.
20	CAO X Q . New materials and new structures of thermal barrier coatings[M]. Beijing: Science Press, 2016.
21	向星. Y₃Al₅O₁₂: Eu³⁺红色荧光粉的化学共沉淀法合成与表征[D]. 重庆: 重庆大学, 2009.
21	XIANG X. Synthesis and characterization of Y₃Al₅O₁₂: Eu³⁺ red phosphor by coprecipitation method[D]. Chongqing: Chongqing University, 2009.
22	谭强强, 唐子龙, 张中太. 纳米四方多晶氧化锆粉体的低温制备及反应机理研究[J]. 材料工程, 2004, (11): 57- 60. doi: 10.3969/j.issn.1001-4381.2004.11.014
22	TAN Q Q , TANG Z L , ZHANG Z T . Preparation and microstructure of nanometer tetragonal polycrystal zirconia powder at low temperature condition[J]. Journal of Materials Engineering, 2004, (11): 57- 60. doi: 10.3969/j.issn.1001-4381.2004.11.014
23	CHEN H , GAO Y , LIU Y , et al. Coprecipitation synthesis and thermal conductivity of La₂Zr₂O₇[J]. Journal of Alloys and Compounds, 2009, 480 (2): 843- 848. doi: 10.1016/j.jallcom.2009.02.081
24	CHUAH G K , JAENICKE S , CHEONG S A , et al. The influence of preparation conditions on the surface area of zirconia[J]. Applied Catalysis A, 1996, 145, 267- 284. doi: 10.1016/0926-860X(96)00152-4
25	沈志坚, 方中华, 李廷凯, 等. 化学共沉淀过程pH值对Y₂O₃(MgO)-PSZ相组成的影响[J]. 硅酸盐学报, 1991, 19 (5): 403- 408.
25	SHEN Z J , FANG Z H , LI T K , et al. Effect of pH value in coprecipitation on crystal phase of calcined Y₂O₃ (MgO)-PSZ[J]. Journal of the Chinese Ceramic Society, 1991, 19 (5): 403- 408.
26	苏小莉, 李晓乐, 蔡天聪, 等. 钇稳定氧化锆的反向共沉淀制备及固溶体晶型研究[J]. 中国陶瓷, 2017, 53 (1): 41- 45.
26	SU X L , LI X L , CAI T C , et al. Study on preparation process and solid solution crystal type of yttria stabilized zirconia by reverse coprecipitation method[J]. China Ceramics, 2017, 53 (1): 41- 45.
27	LI A X , WANG Y L , XIONG X , et al. Microstructure and synthesis mechanism of dysprosia-stabilized zirconia nanocrystals via chemical coprecipitation[J]. Ceramics International, 2020, 46 (9): 13331- 13341. doi: 10.1016/j.ceramint.2020.02.112
28	WU N N , WANG Y L , LIU R T , et al. Preparation and synthesis mechanism of ytterbium monosilicate nano-powders by a cocurrent coprecipitation method[J]. Ceramics International, 2020, 46 (10): 15003- 15012. doi: 10.1016/j.ceramint.2020.03.030
29	BAHAMIRIAN M , HADAVI S M M , RAHIMIPOUR M R , et al. Synthesis and characterization of yttria-stabilized zirconia nanoparticles doped with ytterbium and gadolinium: ZrO₂9.5Y₂O₃5.6Yb₂O₃5.2Gd₂O₃[J]. Metallurgical and Materials Transactions A, 2018, 49 (6): 2523- 2532. doi: 10.1007/s11661-018-4555-x
30	ATKINS E . Elements of X-ray diffraction[J]. Physics Today, 1978, 10 (3): 50.
31	DIAZ-TORRES L A , ROSA E D L , SALAS P , et al. Efficient photoluminescence of Dy³⁺ at low concentrations in nanocrystalline ZrO₂[J]. Journal of Solid State Chemistry, 2008, 181 (1): 75- 80. doi: 10.1016/j.jssc.2007.09.033
32	RAZA M , CORNIL D , CORNIL J , et al. Oxygen vacancy stabilized zirconia: a joint experimental and theoretical study[J]. Scripta Materialia, 2016, 124, 26- 29. doi: 10.1016/j.scriptamat.2016.06.025
33	AZZOPARDI A , MÉVREL R , SAINT-RAMOND B , et al. Influence of aging on structure and thermal conductivity of Y-PSZ and Y-FSZ EB-PVD coatings[J]. Surface and Coatings Technology, 2004, 177/178, 131- 139. doi: 10.1016/j.surfcoat.2003.08.073
34	刘怀菲, 李松林, 李其连. 热障涂层用La₂O₃、Y₂O₃共掺杂稳定ZrO₂的制备及其相稳定性[J]. 无机材料学报, 2009, 24 (6): 1226- 1230.
34	LIU H F , LI S L , LI Q L . Preparation and phase stability of La₂O₃, Y₂O₃ co-doped ZrO₂ ceramic powder application for thermal barrier coating[J]. Journal of Inorganic Materials, 2009, 24 (6): 1226- 1230.
35	JIANG K , LIU S , WANG X . Low-thermal-conductivity and high-toughness CeO₂-Gd₂O₃ co-stabilized zirconia ceramic for potential thermal barrier coating applications[J]. Journal of the European Ceramic Society, 2018, 38 (11): 3986- 3993. doi: 10.1016/j.jeurceramsoc.2018.04.065
36	徐刚, 李海舰, 杨琳琳, 等. 锆液浓度、焙烧温度对氨基共沉淀法合成Y-PSZ相组成影响的研究[C]//第十一届全国高技术陶瓷学术年会论文集. 重庆: 材料导报社, 2000: 45-46.
36	XU G, LI H J, YANG L L, et al. Effect of zirconium solution concentration and calcination temperature on phase composition of Y-PSZ synthesis by amino coprecipitation[C]//Proceedings of the Eleventh National Annual Conference on High Tech Ceramics. Chongqing: Materials Reports Press, 2000: 45-46.
37	陈士冰, 王世峰, 李亮. 反向共沉淀法制备3YSZ超细粉体[J]. 陶瓷学报, 2010, 31 (2): 262- 265. doi: 10.3969/j.issn.1000-2278.2010.02.020
37	CHEN S B , WANG S F , LI L . Preparation of 3Y-TZP ultrafine powder by reverse coprecipitation[J]. Journal of Ceramics, 2010, 31 (2): 262- 265. doi: 10.3969/j.issn.1000-2278.2010.02.020
38	陆佩文. 无机材料科学基础[M]. 武汉: 武汉工业大学出版社, 1996.
38	LU P W . Fundamentals of inorganic materials science[M]. Wuhan: Wuhan University of Technology Press, 1996.

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