醇水共沉淀法制备Yb:YAG透明陶瓷及其性能研究

doi:10.15541/jim20200231

无机材料学报 ›› 2021, Vol. 36 ›› Issue (2): 217-224.DOI: 10.15541/jim20200231

所属专题：【信息功能】透明陶瓷与光学晶体

• 研究快报 • 上一篇

醇水共沉淀法制备Yb:YAG透明陶瓷及其性能研究

黄新友¹(), 刘玉敏¹^,², 刘洋³, 李晓英²^,⁴, 冯亚刚²^,⁴, 陈肖朴²^,⁴, 陈鹏辉¹^,², 刘欣²^,⁴, 谢腾飞²^,⁴, 李江²^,⁴()

1.江苏大学材料科学与工程学院, 镇江212013
2.中国科学院上海硅酸盐研究所, 透明光功能无机材料重点实验室, 上海 201899
3.华北光电技术研究所固体激光科学与技术实验室, 北京100015
4.中国科学院大学材料与光电研究中心, 北京 100049

收稿日期:2020-04-29 修回日期:2020-06-23 出版日期:2021-02-20 网络出版日期:2020-09-09
通讯作者: 李江, 研究员. E-mail: lijiang@mail.sic.ac.cn
作者简介:黄新友(1963–), 男, 教授. E-mail: huangxy@ujs.edu.cn

Fabrication and Characterizations of Yb:YAG Transparent Ceramics Using Alcohol-water Co-precipitation Method

HUANG Xinyou¹(), LIU Yumin¹^,², LIU Yang³, LI Xiaoying²^,⁴, FENG Yagang²^,⁴, CHEN Xiaopu²^,⁴, CHEN Penghui¹^,², LIU Xin²^,⁴, XIE Tengfei²^,⁴, LI Jiang²^,⁴()

1. School of Material Science and Engineering, Jiangsu University, Zhenjiang 212013, China
2. Key Laboratory of Transparent Opto-functional Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
3. Science and Technology on Solid-State Laser Laboratory, North China Research Institute of Electro-Optics, Beijing 100015, China
4. Center of Materials Science and Optoelectronic Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2020-04-29 Revised:2020-06-23 Published:2021-02-20 Online:2020-09-09
About author:HUANG Xinyou (1963–), male, professor. E-mail: huangxy@ujs.edu.cn
Supported by:
National Key R&D Program of China(2017YFB0310500);Key Research Project of the Frontier Science of the Chinese Academy of Sciences(QYZDB-SSW-JSC022)

摘要/Abstract

摘要：

Yb:YAG透明陶瓷由于具有宽的吸收带和发射带、高增益、低的热负载、长的荧光寿命、高的量子效率等优点而成为有应用前景的高功率固体激光器用增益介质。本研究优化了粉体的性能并制备了高透明的Yb:YAG陶瓷。以碳酸氢铵为沉淀剂, 分别以纯水或乙醇/水混合物为溶剂, 采用共沉淀法合成了5at%Yb:YAG纳米粉体。在1250 ℃下煅烧4 h得到的所有粉体均为纯YAG相。与纯水溶剂制备的粉体相比, 醇水溶剂制备的粉体具有更小的平均晶粒尺寸和更低的团聚程度。以醇水溶剂制备的粉体为原料, 采用真空烧结法在不添加烧结助剂的情况下成功制备了5at%Yb:YAG透明陶瓷, 并对1500~1825 ℃烧结20 h和1800 ℃烧结10~50 h所得陶瓷的微观结构和直线透过率进行了探究。除在1825 ℃下烧结20 h所得的陶瓷外, 其余的5at%Yb:YAG陶瓷都具有均匀的微观结构。在1800 ℃下烧结50 h制备的5at%Yb:YAG陶瓷具有最高的光学质量, 在1100和400 nm处的直线透过率分别为78.6%和76.7%(样品厚度为2.2 mm)。该Yb:YAG透明陶瓷在937 nm处的吸收截面为5.03×10^-21 cm², 在1031 nm处的发射截面为13.48×10^-21cm²。

关键词: Yb:YAG透明陶瓷, 醇水共沉淀法, 真空烧结, 微观结构, 光学性能

Abstract:

Yb ³⁺ doped YAG transparent ceramics have great potential as gain medium for high-power solid-state lasers due to many advantages, such as broad absorption and emission bands, high gain, low thermal loading, long fluorescence lifetime and high quantum efficiency. So Yb:YAG transparent ceramics have gradually been paid more attention. In this work, we aimed at optimizing the properties of powders to fabricate highly transparent Yb:YAG ceramics. 5at%Yb:YAG nano-powders were synthesized via the co-precipitation method by using ammonium hydrogen carbonate as the precipitant, and pure water or alcohol-water mixture as the solvent. All powders calcined at 1250 ℃ for 4 h exhibit a pure YAG phase. Compared to the one with pure water solvent, the 5at%Yb:YAG powder synthesized with alcohol-water solvent exhibits smaller average crystallite size and lower agglomeration degree. 5at%Yb:YAG transparent ceramics were successfully fabricated by vacuum sintering without sintering additives from the obtained powder with alcohol-water solvent. The microstructure and in-line transmittance of the ceramics sintered at 1500-1825 ℃ for 20 h and 1800 ℃ for 10-50 h were investigated. All ceramic samples show a homogeneous microstructure except for that sintered at 1825 ℃ for 20 h. The sample sintered at 1800 ℃ for 50 h shows the highest in-line transmittance of 78.6% at 1100 nm and 76.7% at 400 nm (2.2 mm thickness). The calculated absorption and emission cross sections are 5.03×10^-21 cm² at 937 nm and 13.48×10^-21 cm² at 1031 nm, respectively. Therefore, Yb:YAG ceramics with high optical transparency and uniform microstructure have been fabricated from powder with alcohol-water solvent.

Key words: Yb:YAG transparent ceramic, alcohol-water co-precipitation, vacuum sintering, microstructure, optical property

中图分类号:

TQ174

黄新友, 刘玉敏, 刘洋, 李晓英, 冯亚刚, 陈肖朴, 陈鹏辉, 刘欣, 谢腾飞, 李江. 醇水共沉淀法制备Yb:YAG透明陶瓷及其性能研究[J]. 无机材料学报, 2021, 36(2): 217-224.

HUANG Xinyou, LIU Yumin, LIU Yang, LI Xiaoying, FENG Yagang, CHEN Xiaopu, CHEN Penghui, LIU Xin, XIE Tengfei, LI Jiang. Fabrication and Characterizations of Yb:YAG Transparent Ceramics Using Alcohol-water Co-precipitation Method[J]. Journal of Inorganic Materials, 2021, 36(2): 217-224.

图/表 11

Fig. 1 TG-DTA curves of the as-prepared precursors synthesized with pure water (a) and alcohol-water (b) solvents

Fig. 2 XRD patterns of the powders calcined at 1250 ℃ for 4 h synthesized with pure water and alcohol-water solvents

Fig. 3 FESEM micrographs of the as-synthesized precursors synthesized with pure water (a) and alcohol-water (b) solvents

Fig. 4 FESEM micrographs of the 5at%Yb:YAG powders synthesized with pure water (a) and alcohol-water (b) solvents calcined at 1250 ℃ for 4 h

Fig. 5 Photographs (a) and in-line transmittances (b) of 5at%Yb:YAG ceramics (2.2 mm thickness) sintered at different temperatures for 20 h

Fig. 6 FESEM micrographs of the thermally-etched surfaces of 5at%Yb:YAG ceramics sintered at various temperatures for 20 h

Fig. 7 Relative densities and average grain sizes of the 5at%Yb:YAG ceramics sintered at various temperatures for 20 h

Fig. 8 In-line transmission curves of the 5at%Yb:YAG ceramics (2.2 mm thickness) sintered at 1800 ℃ for various holding time

Fig. 9 FESEM micrographs of the thermally-etched surfaces of Yb:YAG ceramics sintered at 1800 ℃ for various holding time: (a) 10 h, (b) 20 h, (c) 50 h

Fig. 10 Absorption and emission cross sections of the 5at%Yb:YAG ceramic sintered at 1800 ℃ for 50 h

Fig. 11 Gain cross sections of the 5at%Yb:YAG ceramic sintered at 1800 ℃ for 50 h

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醇水共沉淀法制备Yb:YAG透明陶瓷及其性能研究

Fabrication and Characterizations of Yb:YAG Transparent Ceramics Using Alcohol-water Co-precipitation Method

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