1.5 μm被动调Q可饱和吸收体用Co:MgAl 2O4透明陶瓷的制备

doi:10.15541/jim20200679

无机材料学报 ›› 2021, Vol. 36 ›› Issue (8): 877-882.DOI: 10.15541/jim20200679

所属专题：【信息功能】透明陶瓷与光学晶体

1.5 μm被动调Q可饱和吸收体用Co:MgAl ₂O₄透明陶瓷的制备

荆延秋¹^,²(), 刘强², 苏莎¹^,², 李晓英¹, 刘子玉¹, 王静雅¹, 李江¹^,³()

1.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
2.江苏大学材料科学与工程学院, 镇江 212013

收稿日期:2020-11-30 修回日期:2020-12-19 出版日期:2021-08-20 网络出版日期:2021-03-12
通讯作者: 李江, 研究员. E-mail: lijiang@mail.sic.ac.cn
作者简介:荆延秋(1995-), 男, 硕士研究生. E-mail: jingyanqiu@qq.com

Fabrication of Highly Transparent Co:MgAl₂O₄ Ceramic Saturable Absorber for Passive Q-switching in 1.5 μm

JING Yanqiu¹^,²(), LIU Qiang², SU Sha¹^,², LI Xiaoying¹, LIU Ziyu¹, WANG Jingya¹, LI Jiang¹^,³()

1. Key Laboratory of Transparent Opto-Functional Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
2. School of Material Science and Engineering, Jiangsu University, Zhenjiang 212013, China; Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2020-11-30 Revised:2020-12-19 Published:2021-08-20 Online:2021-03-12
Contact: LI Jiang, professor. E-mail: lijiang@mail.sic.ac.cn
About author:JING Yanqiu (1995-), male, Master candidate. E-mail: jingyanqiu@qq.com
Supported by:
Foundation item: National Key R&D Program of China(2016YFB0402101);Foundation item: 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：

钴掺杂的镁铝尖晶石透明陶瓷是用于近红外区域工作的无源调Q固态激光器的有效材料。为制备具有高吸收截面和高透过率的Co:MgAl₂O₄透明陶瓷, 采用共沉淀法合成钴掺杂的纯相镁铝尖晶石纳米粉体, 并通过真空烧结结合热等静压烧结(Hot Isostatic Pressing, HIP), 制备得到了高质量的0.05at% Co:MgAl₂O₄透明陶瓷, 同时系统研究了预烧结温度对Co:MgAl₂O₄陶瓷微观结构和光学性能的影响。当预烧结温度从1500 ℃升高至1650 ℃, Co:MgAl₂O₄陶瓷的相对密度从95.2%增大到98.5%, 而当预烧温度升高至1700 ℃, Co:MgAl₂O₄陶瓷的相对密度降低至97.7％。真空预烧后Co:MgAl₂O₄陶瓷的相对密度较低, 因此预烧后的Co:MgAl₂O₄陶瓷均为不透明的。当预烧温度从1500 ℃升高到1700 ℃, Co:MgAl₂O₄陶瓷的平均晶粒尺寸从2.3 μm增大到11.3 μm。经过HIP后处理后, 在1550~1700 ℃×5 h真空预烧条件下的Co:MgAl ₂O₄陶瓷都是透明的, 而经过1650 ℃×5 h真空预烧结合1800 ℃×3 h HIP后处理的Co:MgAl₂O₄透明陶瓷表现出最佳的光学质量, 在400和900 nm处的直线透过率分别为81.4%和85.9%, 平均晶粒尺寸为16.8 μm。在500~700 nm和1200~1600 nm波长范围内的宽吸收带表明Co ²⁺已掺入尖晶石晶格中。此外, 经计算, 最佳光学质量的样品在1540 nm处的基态吸收截面为6.18×10^-19 cm², 表明Co:MgAl₂O₄已经成为固态激光器中被动调Q可饱和吸收体的最有潜力的材料之一。

关键词: Co:MgAl₂O₄, 透明陶瓷, 可饱和吸收体, 热等静压烧结

Abstract:

The cobalt doped magnesium aluminum spinel is an efficient material for the passive Q-switching solid state lasers operating at the near infrared region. In order to prepare Co:MgAl₂O₄ transparent ceramics with high absorption cross section and high in-line transmittance, the cobalt doped magnesium aluminum spinel nanopowders with pure phase were synthesized via the co-precipitation method. And after vacuum sintering and hot isostatic pressing (HIP), highly transparent 0.05at% Co:MgAl₂O₄ ceramics were obtained. The influences of pre-sintering temperature on morphology and optical property of the Co:MgAl₂O₄ ceramics were studied. With the pre-sintering temperature increasing from 1500-1650 ℃, the relative density increased from 95.2% to 98.5%, while the relative density decreased to 97.7% with the pre-sintering temperature increasing to 1700 ℃. Because of the relative low density, the Co:MgAl₂O₄ ceramics were all opaque after vacuum pre-sintering. In the sintering temperature range of 1500-1700 ℃, the average grain size increased from 2.3 to 11.3 μm. After HIP post-treatment, the Co:MgAl₂O₄ ceramics pre-sintered from 1550 to 1700 ℃ were all transparent, the Co:MgAl₂O₄ ceramics pre-sintered at 1650 ℃ for 5 h and HIP post-treated at 1800 ℃ for 3 h showed the best optical quality, which were 81.4% at 400 nm and 85.9% at 900 nm, and the average grain size was 16.8 μm. The broad absorption bands in the wavelength range of 500-700 nm and 1200-1600 nm indicated that Co ²⁺ had incorporated into the spinel lattice. Moreover, the ground state absorption cross section of the best specimen is calculated with a value of 6.18×10^-19 cm² at 1540 nm, meaning that it’s a promising candidate for passive Q-switching in solid-state lasers.

Key words: Co:MgAl₂O₄, transparent ceramics, saturable absorbers, hot isostatic pressing

中图分类号:

TQ174

荆延秋, 刘强, 苏莎, 李晓英, 刘子玉, 王静雅, 李江. 1.5 μm被动调Q可饱和吸收体用Co:MgAl ₂O₄透明陶瓷的制备[J]. 无机材料学报, 2021, 36(8): 877-882.

JING Yanqiu, LIU Qiang, SU Sha, LI Xiaoying, LIU Ziyu, WANG Jingya, LI Jiang. Fabrication of Highly Transparent Co:MgAl₂O₄ Ceramic Saturable Absorber for Passive Q-switching in 1.5 μm[J]. Journal of Inorganic Materials, 2021, 36(8): 877-882.

图/表 7

Fig. 1 FESEM image of Co:MgAl2O4 powders

Fig. 2 FESEM images of Co:MgAl2O4 ceramics vacuum-sintered at different temperatures for 5 h (a) 1500 ℃; (b) 1550 ℃; (c) 1600 ℃; (d) 1650 ℃; (e) 1700 ℃

Fig. 3 Relative density and average grain size of 0.05at% Co:MgAl2O4 ceramics pre-sintered at different temperatures for 5 h

Fig. 4 FESEM microstructures of Co:MgAl2O4 ceramics vacuum-sintered at different temperatures for 5 h and then HIP post-treated at 1800 ℃ for 3 h (a) 1500 ℃; (b) 1550 ℃; (c) 1600 ℃; (d) 1650 ℃; (e) 1700 ℃

Fig. 5 Average grain sizes of 0.05at% Co:MgAl2O4 ceramics pre-sintered at different temperatures for 5 h and then HIP post-treated

Fig. 6 Photo (a) and in-line transmission spectra (b) of the Co:MgAl2O4 ceramics pre-sintered at 1500-1700 ℃ for 5 h and HIP post-treated at 1800 ℃ for 3 h Colorful figure are available on website

Fig. 7 Absorption coefficient spectrum of 0.05at% Co:MgAl2O4 ceramic pre-sintered at 1650 ℃ for 5 h and HIP post-treated at 1800 ℃ for 3 h

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1.5 μm被动调Q可饱和吸收体用Co:MgAl ₂O₄透明陶瓷的制备

Fabrication of Highly Transparent Co:MgAl₂O₄ Ceramic Saturable Absorber for Passive Q-switching in 1.5 μm

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