共沉淀纳米粉体制备Yb:CaF2激光陶瓷及其性能研究

doi:10.15541/jim20190121

无机材料学报 ›› 2019, Vol. 34 ›› Issue (12): 1341-1348.DOI: 10.15541/jim20190121

所属专题：优秀作者论文集锦； 2019~2020年度优秀作者作品欣赏:功能材料

共沉淀纳米粉体制备Yb:CaF₂激光陶瓷及其性能研究

韦家蓓^1,²,TOCIGuido³,PIRRIAngela⁴,PATRIZIBarbara⁵,冯亚刚^1,²,VANNINIMatteo³,李江^1,²()

^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 200050
2．中国科学院大学材料科学与光电工程中心, 北京 100049
^3. 意大利国家研究委员会国立光学研究所, 佛罗伦萨 50019
^4. 意大利国家研究委员会“Carrara”应用物理研究所, 佛罗伦萨 50019;
^5. 意大利国家研究委员会国立光学研究所, 比萨 56124

收稿日期:2019-03-25 修回日期:2019-04-25 出版日期:2019-12-20 网络出版日期:2019-07-23
作者简介:WEI Jia-Bei (1993-), male, candidate of Master degree. E-mail: weijiabei@student.sic.ac.cn

Fabrication and Property of Yb:CaF₂ Laser Ceramics from Co-precipitated Nanopowders

WEI Jia-Bei^1,²,TOCI Guido³,PIRRI Angela⁴,PATRIZI Barbara⁵,FENG Ya-Gang^1,²,VANNINI Matteo³,LI Jiang^1,²()

^1. Key Laboratory of Transparent Opto-Functional Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
^2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
^3. Istituto Nazionale di Ottica, Consiglio Nazionale delle Ricerche, CNR-INO, Via Madonna del Piano 10C, 50019 Sesto Fiorentino (Fi), Italy
^4. Istituto di Fisica Applicata “Carrara”, Consiglio Nazionale delle Ricerche, CNR-IFAC, Via Madonna del Piano 10C, 50019 Sesto Fiorentino (Fi), Italy;
^5. Istituto Nazionale di Ottica, Consiglio Nazionale delle Ricerche, CNR-INO, Via G. Moruzzi, 1, 56124 Pisa (Pi), Italy

Received:2019-03-25 Revised:2019-04-25 Published:2019-12-20 Online:2019-07-23
Supported by:
Foundation item: National Natural Science Foundation of China(61575212);Key Research Project of the Frontier Science of the Chinese Academy of Sciences(QYZDB-SSW-JSC022)

摘要/Abstract

摘要：

利用共沉淀法合成的粉体, 通过真空烧结结合热压烧结后处理制备了掺镱的氟化钙透明陶瓷(Yb:CaF₂)。在600 ℃预烧1 h, 700 ℃热压烧结2 h制备的5at%Yb:CaF₂透明陶瓷在1200 nm处的直线透射率达到92.0%。对陶瓷的显微结构、光谱特性和激光性能进行了测试和讨论。研究结果表明, 陶瓷样品的显微结构均匀, 平均晶粒尺寸为360 nm。此外, 计算得到Yb:CaF₂陶瓷在977 nm处的吸收截面和1030 nm处的发射截面分别为0.39×10 ^-20和0.26×10 ^-20cm ²。最后, 对Yb:CaF₂陶瓷激光性能进行了表征, 得到最大输出功率为0.9 W, 最大斜率效率为23.6%。

关键词: Yb:CaF₂, 共沉淀法, 两步烧结, 激光陶瓷, 光学性能

Abstract:

Transparent ytterbium doped calcium fluoride ceramics (Yb:CaF₂) were successfully fabricated by vacuum sintering and hot pressing post-treatment from coprecipitated powders. In-line transmittance of 5at% Yb:CaF₂ transparent ceramics fabricated by pre-sintering at 600 ℃ for 1 h and hot pressing post-treatment at 700 ℃ for 2 h, reaches 92.0% at the wavelength of 1200 nm. Microstructure, spectroscopic characteristics and laser performance of the ceramics were measured and discussed. The sample shows a homogeneous microstructure with average grain size of 360 nm. Furthermore, the absorption cross section at 977 nm and the emission cross section at the 1030 nm of the ceramics are calculated to 0.39×10 ^-20 cm ²and 0.26×10 ^-20 cm ², respectively. Finally, the laser behavior was tested, finding a maximum output power of 0.9 W while the highest slope efficiency was 23.6%.

Key words: Yb:CaF₂, co-precipitation synthesis, two-step sintering, laser ceramics, optical property

中图分类号:

TQ174

韦家蓓, TOCIGuido, PIRRIAngela, PATRIZIBarbara, 冯亚刚, VANNINIMatteo, 李江. 共沉淀纳米粉体制备Yb:CaF₂激光陶瓷及其性能研究[J]. 无机材料学报, 2019, 34(12): 1341-1348.

WEI Jia-Bei, TOCI Guido, PIRRI Angela, PATRIZI Barbara, FENG Ya-Gang, VANNINI Matteo, LI Jiang. Fabrication and Property of Yb:CaF₂ Laser Ceramics from Co-precipitated Nanopowders[J]. Journal of Inorganic Materials, 2019, 34(12): 1341-1348.

图/表 11

Fig. 1 FT-IR spectrum of 5at% Yb:CaF2 powders

Fig. 2 XRD pattern of 5at% Yb:CaF2 powders

Fig. 3 SEM micrographs of 5at% Yb:CaF2 powders (a) and the fracture surface of 5at% Yb:CaF2 ceramics (b)

Fig. 4 The in-line transmittance and the photograph of 5at% Yb:CaF2 transparent ceramics

Fig. 5 Absorption coefficient and emission spectra of 5at% Yb:CaF2 transparent ceramics at room temperature

Fig. 6 Absorption cross section spectrum (a) and emission cross section spectrum (b) of 5at% Yb:CaF2 transparent ceramics at room temperature

Fig. 7 The calculated gain cross section of 5at% Yb:CaF2 ceramics

Fig. 8 The fluorescence decay curve of 5at% Yb:CaF2 transparent ceramics at room temperature. The time constant τ of the fitting curve is 1.974 ms

Fig. 9 Experimental set-up

Fig. 10 Laser output power vs. incident pump power for different values of the output coupler mirror transmission Toc

Table 1 Main laser emission parameters with slope efficiency being calculated with respect to the absorbed pump power

Output coupler transmission/%	Maximum power/W	Slope efficiency/%	Optical efficiency/%
2.2	0.429	9.6	8.4
5.9	0.845	18.2	15.6
7.2	0.886	21.2	17.6
12.4	0.874	23.6	19.1

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共沉淀纳米粉体制备Yb:CaF₂激光陶瓷及其性能研究

Fabrication and Property of Yb:CaF₂ Laser Ceramics from Co-precipitated Nanopowders

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