共沉淀纳米粉体制备Yb:Sc2O3透明陶瓷的微结构与光学性能

doi:10.15541/jim20240322

无机材料学报 ›› 2025, Vol. 40 ›› Issue (2): 215-224.DOI: 10.15541/jim20240322 CSTR: 32189.14.10.15541/jim20240322

• 研究快报 • 上一篇

共沉淀纳米粉体制备Yb:Sc₂O₃透明陶瓷的微结构与光学性能

叶君豪¹^,²(), 周真真¹^,², 胡辰¹^,², 王雁斌¹^,², 荆延秋¹^,², 李廷松¹^,², 程梓秋¹^,², 吴俊林¹^,², IVANOV Maxim³^,⁴, HRENIAK Dariusz⁵, 李江¹^,²()

1.中国科学院上海硅酸盐研究所, 透明陶瓷研究中心, 上海 201899
2.中国科学院大学材料科学与光电工程中心, 北京 100049
3.贝尔格莱德大学塞尔维亚共和国国家研究所, Vinča核科学研究所, 光电转换卓越中心, 贝尔格莱德 11001
4.俄罗斯科学院乌拉尔分院电物理研究所, 叶卡捷琳堡 620016
5.波兰科学院低温与结构研究所, 弗罗茨瓦夫 326109

收稿日期:2024-07-08 修回日期:2024-09-07 出版日期:2025-02-20 网络出版日期:2024-09-23
通讯作者: 李江, 研究员. E-mail: lijiang@mail.sic.ac.cn
作者简介:叶君豪(2000-), 男, 硕士研究生. E-mail: yejunhao22@mails.ucas.ac.cn

Yb:Sc₂O₃ Transparent Ceramics Fabricated from Co-precipitated Nano-powders: Microstructure and Optical Property

YE Junhao¹^,²(), ZHOU Zhenzhen¹^,², HU Chen¹^,², WANG Yanbin¹^,², JING Yanqiu¹^,², LI Tingsong¹^,², CHENG Ziqiu¹^,², WU Junlin¹^,², IVANOV Maxim³^,⁴, HRENIAK Dariusz⁵, LI Jiang¹^,²()

1. Transparent Ceramics Research Center, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
3. Center of Excellence for Photoconversion, Vinča Institute of Nuclear Sciences, National Institute of the Republic of Serbia, University of Belgrade, 11001 Belgrade, Serbia
4. Institute of Electrophysics Ural Branch, Russian Academy of Sciences, Ekaterinburg 620016, Russia
5. Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Wroclaw 326109, Poland

Received:2024-07-08 Revised:2024-09-07 Published:2025-02-20 Online:2024-09-23
Contact: LI Jiang, professor. E-mail: lijiang@mail.sic.ac.cn
About author:YE Junhao (2000-), male, Master candidate. E-mail: yejunhao22@mails.ucas.ac.cn
Supported by:
National Key R&D Program of China(2023YFE3812005);International Partnership Program of Chinese Academy of Sciences(121631KYSB20200039);National Center for Research and Development(WPC2/1/SCAPOL/2021);Chinese Academy of Sciences President’s International Fellowship Initiative(2024VEA0005);Chinese Academy of Sciences President’s International Fellowship Initiative(2024VEA0014)

摘要/Abstract

摘要：

Sc₂O₃作为固体激光增益材料的基质, 具有热导率高、与激活离子匹配性好等优点, 在高功率固体激光应用中有着广阔的应用前景。目前, Yb掺杂的Sc₂O₃陶瓷可以在很高的烧结温度下合成, 但陶瓷的光学质量和烧结温度还有待进一步优化。本研究采用碳酸氢铵共沉淀法制备了分散性好、平均晶粒尺寸29 nm的立方相5%Yb:Sc₂O₃(掺杂量为质量分数)纳米粉体, 并采用真空预烧结和热等静压(Hot Isostatic Pressing, HIP)后处理制备了5%Yb:Sc₂O₃透明陶瓷, 详细研究了真空预烧结温度(1500~1700 ℃)对Yb:Sc₂O₃陶瓷的致密化过程、微观结构变化及光学透过率的影响。结果表明, 所有样品均具有均匀的微观结构, 且随着烧结温度的升高, 样品的平均晶粒尺寸增大。值得注意的是, 1550 ℃预烧的Yb:Sc₂O₃陶瓷经HIP后处理后, 在1100 nm处的最佳直线透过率达到78.1%(理论值为80%)。同时, 还评估了Yb:Sc₂O₃陶瓷的光谱性能。5%Yb:Sc₂O₃陶瓷的最小粒子数反转参数β₂和发光衰减时间分别为0.041和0.49 ms。综上所述, 采用共沉淀法成功制备了Yb:Sc₂O₃纳米粉体, 通过1550 ℃真空预烧结和HIP后处理得到光学质量良好的Yb:Sc₂O₃透明陶瓷。

关键词: 纳米粉体, Yb:Sc₂O₃, 透明陶瓷, 热等静压烧结, 光学性能

Abstract:

Sc₂O₃, as a host for solid-state laser gain materials, has advantage of high thermal conductivity and easy matching with activating ions, which is promising in high-power laser applications. Currently, Yb-doped Sc₂O₃ ceramics have been fabricated at very high sintering temperatures, but their optical quality and sintering process still need further improvement. In this work, 5%Yb:Sc₂O₃ (in mass) nano-powders were obtained by co-precipitation, and then transparent ceramics were fabricated by vacuum pre-sintering and hot isostatic pressing (HIP) post-treatment. The cubic Yb:Sc₂O₃ nano-powders with good dispersity and an average crystallite of 29 nm were obtained. Influence of pre-sintering temperatures (1500-1700 ℃) on densification process, microstructure changes, and optical transmittance of Yb:Sc₂O₃ ceramics was detected. Experimental data revealed that all samples have a uniform microstructure, while the average grain sizes increase with the increase of the sintering temperatures. Impressively, the optimum in-line transmittance of Yb:Sc₂O₃ ceramics, pre-sintered at 1550 ℃ after HIP post-treatment, reaches 78.1% (theoretical value of 80%) at 1100 nm. Spectroscopic properties of the Yb:Sc₂O₃ ceramics reveal that the minimum population inversion parameter β₂ and the luminescence decay time of 5%Yb:Sc₂O₃ ceramics are 0.041 and 0.49 ms, respectively, which demonstrate that the optical quality of the Yb:Sc₂O₃ has been improved. Meanwhile, their best vacuum sintering temperature can be controlled down to a lower temperature (1550 ℃). In conclusion, Yb:Sc₂O₃ nano-powders are successfully synthesized by co-precipitation method, and good optical quality transparent ceramics are fabricated by vacuum pre-sintering at 1550 ℃and HIP post-treatment.

Key words: nano-powder, Yb:Sc₂O₃, transparent ceramic, hot isostatic pressing, optical property

中图分类号:

TQ174

叶君豪, 周真真, 胡辰, 王雁斌, 荆延秋, 李廷松, 程梓秋, 吴俊林, IVANOV Maxim, HRENIAK Dariusz, 李江. 共沉淀纳米粉体制备Yb:Sc₂O₃透明陶瓷的微结构与光学性能[J]. 无机材料学报, 2025, 40(2): 215-224.

YE Junhao, ZHOU Zhenzhen, HU Chen, WANG Yanbin, JING Yanqiu, LI Tingsong, CHENG Ziqiu, WU Junlin, IVANOV Maxim, HRENIAK Dariusz, LI Jiang. Yb:Sc₂O₃ Transparent Ceramics Fabricated from Co-precipitated Nano-powders: Microstructure and Optical Property[J]. Journal of Inorganic Materials, 2025, 40(2): 215-224.

图/表 12

Fig. 1 TG-DTG curves of the precursor

Fig. 2 XRD patterns of the precursor and the powders calcined at 1100 ℃ for 4 h

Fig. 3 FESEM micrographs of (a) the precursor and (b) the powders

Table 1 Analysis of particle size and agglomeration degree of 5%Yb:Sc2O3 nano-powders

Sample	S_BET/(m²·g^-1)	D_BET/nm	D_SEM/nm	D_XRD/nm	N₁
5%Yb:Sc₂O₃ nano-powders	25	58	43	29	6

Fig. 4 FESEM micrographs of thermally etched surfaces of the 5%Yb:Sc2O3 ceramics pre-sintered at different temperatures (a) 1500 ℃; (b) 1550 ℃; (c) 1600 ℃; (d) 1650 ℃; (e) 1700 ℃

Fig. 5 Average grain sizes and relative densities of 5%Yb:Sc2O3 ceramics with different pre-sintering temperatures

Fig. 6 FESEM micrographs of thermally etched surfaces of the synthesized 5%Yb:Sc2O3 ceramics Ceramics pre-sintered at (a) 1500, (b) 1550, (c) 1600, (d) 1650, and (e) 1700 ℃ before HIP post-treatment at 1700 ℃

Fig. 7 Average grain sizes and relative densities of 5%Yb:Sc2O3 ceramics sintered by vacuum pre-sintering and HIP post-treatment

Fig. 8 Photograph (a) and in-line transmittance (b) of the 5%Yb:Sc2O3 ceramics

Fig. 9 Absorption and emission cross-sections of the 5%Yb:Sc2O3 transparent ceramics pre-sintered at 1550 ℃ with HIP post-treatment Colorful figure is available on website

Fig. 10 Gain cross-section of the 5%Yb:Sc2O3 transparent ceramics pre-sintered at 1550 ℃ with HIP post-treatment

Fig. 11 Room temperature 2F5/2 luminescence decay of 5%Yb:Sc2O3 transparent ceramics excited by 980 nm laser and detected at 1041 nm wavelength

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共沉淀纳米粉体制备Yb:Sc₂O₃透明陶瓷的微结构与光学性能

Yb:Sc₂O₃ Transparent Ceramics Fabricated from Co-precipitated Nano-powders: Microstructure and Optical Property

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