固体激光用Nd:Lu2O3透明陶瓷的制备和光学性能研究

doi:10.15541/jim20200143

无机材料学报 ›› 2021, Vol. 36 ›› Issue (2): 210-216.DOI: 10.15541/jim20200143 CSTR: 32189.14.10.15541/jim20200143

固体激光用Nd:Lu₂O₃透明陶瓷的制备和光学性能研究

刘子玉¹^,²(), TOCI Guido³, PIRRI Angela⁴, PATRIZI Barbara³, 冯亚刚¹^,², 陈肖朴¹^,², 胡殿君¹^,², 田丰¹^,², 吴乐翔¹, 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 201899
2.中国科学院大学, 材料与光电研究中心, 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

收稿日期:2020-03-23 修回日期:2020-04-28 出版日期:2021-02-20 网络出版日期:2020-06-15
通讯作者: 李江, 研究员. E-mail: lijiang@mail.sic.ac.cn
作者简介:刘子玉(1991–), 女, 博士研究生. E-mail: liuziyu@student.sic.ac.cn

Fabrication and Optical Property of Nd:Lu₂O₃ Transparent Ceramics for Solid-state Laser Applications

LIU Ziyu¹^,²(), TOCI Guido³, PIRRI Angela⁴, PATRIZI Barbara³, FENG Yagang¹^,², CHEN Xiaopu¹^,², HU Dianjun¹^,², TIAN Feng¹^,², WU Lexiang¹, VANNINI Matteo³, LI Jiang¹^,²()

1. Key Laboratory of Transparent Opto-functional Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
2. Center of Materials Science and Optoelectronic 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

Received:2020-03-23 Revised:2020-04-28 Published:2021-02-20 Online:2020-06-15
About author:LIU Ziyu (1991–), female, PhD candidate. E-mail: liuziyu@student.sic.ac.cn
Supported by:
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：

Nd:Lu₂O₃材料由于具有高热导率、低声子能量和优异的光学特性而成为非常有前景的高功率固体激光器用的增益介质。但Lu₂O₃单晶的熔点超过2400 ℃, 难以生长, 而Lu₂O₃陶瓷既能在低温下制备, 又具有与晶体相当的光学性质和激光性能从而备受关注。本研究制备了高透明的Nd:Lu₂O₃陶瓷并对其光学性质和激光性能进行探究。以共沉淀法制备的纳米粉体为原料, 采用真空烧结结合热等静压(HIP)两步烧结法制备了1.0at%Nd:Lu₂O₃透明陶瓷。对制备的粉体、素坯和陶瓷的微结构进行了表征: HIP后处理的陶瓷平均晶粒尺寸是724.2 nm。厚度为1.0 mm的1.0at%Nd:Lu₂O₃透明陶瓷在1100 nm处的直线透过率是82.4%, 样品在806 nm处的吸收截面为1.50′10^-20 cm², 而根据荧光光谱计算得到的发射截面为6.5′10^-20 cm²。分别在878.8 和895.6 nm波长激发下, 1.0at%Nd:Lu₂O₃透明陶瓷⁴F_3/2·⁴I_11/2跃迁的平均荧光寿命均为169 ms。当输出耦合镜的透过率T_OC=2.0%时, 退火后的1.0at% Nd:Lu₂O₃透明陶瓷获得了最大输出功率为0.47 W的准连续(QCW)激光输出, 斜率效率为8.7%。本研究成功制备了显微结构均匀、高透明度的1.0at%Nd:Lu₂O₃陶瓷, 并展示了其在固体激光增益介质领域的广阔应用潜力。

关键词: Nd:Lu₂O₃透明陶瓷, 共沉淀法, 两步烧结, 光学性能, 激光性能

Abstract:

Nd ³⁺ doped Lu₂O₃ crystal has been suggested to be potential gain medium for high-power solid-state lasers due to the high thermal conductivity, low phonon energy and excellent optical properties. Because of the extremely high melting point of above 2400 ℃, great attention has been paid to the Lu₂O₃-based transparent ceramics considering the comparable optical properties and laser performance with single crystal. In this work, we aimed at fabricating highly transparent Nd:Lu₂O₃ ceramics and investigating the optical properties and laser performance. 1.0at%Nd:Lu₂O₃ ceramics were fabricated by two-step sintering, namely vacuum sintering along with hot isostatic pressing (HIP) method, from coprecipitated nano-powders. The microstructures of the as-prepared powder, green body and ceramics were studied. The average grain size of the HIPed ceramics is 724.2 nm. The final ceramic sample has the in-line transmittance of 82.4% at 1100 nm (1.0 mm thickness). The absorption cross-section of 1.0at%Nd:Lu₂O₃ ceramics at 806 nm is 1.50′10^-20 cm² and the calculated emission cross-section from fluorescence spectrum at 1080 nm is about 6.5′10^-20 cm². The mean fluorescence lifetime, 169 ms, of the⁴F_3/2·⁴I_11/2 was measured at the two excitation wavelengths of 878.8 and 895.6 nm, respectively. Laser performance of the annealed ceramic sample was investigated in quasi-continuous wave (QCW) condition. A maximum laser output power of 0.47 W with a slope efficiency of 8.7% is obtained by using an output coupler with a transmission of T_OC=2.0%. Briefly, laser level Nd:Lu₂O₃ transparent ceramics with high optical transparency and uniform microstructure have been fabricated, which are promising gain media for solid-state lasers.

Key words: Nd:Lu₂O₃ transparent ceramics, co-precipitation, two-step sintering, optical property, laser performance

中图分类号:

TQ174

刘子玉, TOCI Guido, PIRRI Angela, PATRIZI Barbara, 冯亚刚, 陈肖朴, 胡殿君, 田丰, 吴乐翔, VANNINIMatteo, 李江. 固体激光用Nd:Lu₂O₃透明陶瓷的制备和光学性能研究[J]. 无机材料学报, 2021, 36(2): 210-216.

LIU Ziyu, TOCI Guido, PIRRI Angela, PATRIZI Barbara, FENG Yagang, CHEN Xiaopu, HU Dianjun, TIAN Feng, WU Lexiang, VANNINI Matteo, LI Jiang. Fabrication and Optical Property of Nd:Lu₂O₃ Transparent Ceramics for Solid-state Laser Applications[J]. Journal of Inorganic Materials, 2021, 36(2): 210-216.

图/表 10

Fig. 1 XRD patterns of the as-synthesized precursor and 1.0at%Nd:Lu2O3 powder calcined at 1100 ℃ for 4 h

Fig. 2 FESEM micrographs of (a) precursor, (b) 1.0at%Nd:Lu2O3 powder and (c) green body formed from the nano-powder

Fig. 3 FESEM micrographs of the thermally etched (1300 ℃ for 3 h) surfaces of 1.0at%Nd:Lu2O3 ceramics

Fig. 4 In-line transmittance and the photograph of the double-side polished 1.0at%Nd:Lu2O3 transparent ceramics

Fig. 5 Room-temperature absorption cross-section spectrum of the 1.0at%Nd:Lu2O3 ceramics annealed at 900 ℃ for 30 h

Fig. 6 (a) Room-temperature fluorescence spectrum and (b) emission cross-section of the 1.0at%Nd:Lu2O3 ceramics annealed at 900 ℃ for 30 h

Fig. 7 Fluorescence decay of the 1.0at%Nd:Lu2O3 ceramics excited at two different wavelengths

Fig. 8 Schematic of the laser cavity layout employed for the laser tests

Fig. 9 Laser output power vs incident pump power (a) and emission spectra for different transmission values of the OC (b)

Table 1 Main laser emission parameters

Output coupler transmission/ %	Maximum power/ W	Slope efficiency/ %	Optical efficiency*/ %	Laser threshold/ W
2.0	0.460	8.7	7.8	0.57
5.2	0.372	8.9	6.3	0.81
7.0	0.325	8.3	5.7	1.20
19.0	0.029	1.9	0.5	4.42

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固体激光用Nd:Lu₂O₃透明陶瓷的制备和光学性能研究

Fabrication and Optical Property of Nd:Lu₂O₃ Transparent Ceramics for Solid-state Laser Applications

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