硅酸盐学报

直径6英寸YSZ：Er晶体生长与光谱

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陈宇轩 ¹ , 蒋新 ²^,³ , 申慧 ¹ , 田甜 ¹ , 蒋泽锋 ²^,³ , 徐家跃 ¹

硅酸盐学报 | 大尺寸高品质人工晶体制备与应用专题—研究论文 2025,53(12): 3476-3483

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硅酸盐学报 |大尺寸高品质人工晶体制备与应用专题—研究论文 2025 , 53 (12) : 3476 -3483

直径6英寸YSZ：Er晶体生长与光谱

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陈宇轩¹, 蒋新²^,³, 申慧¹, 田甜¹, 蒋泽锋²^,³, 徐家跃¹

作者信息

^1．上海应用技术大学材料科学与工程学院，上海 201418

^2．广西桂林佳兴宝石晶体有限公司，桂林 542501

^3．四川成都新兴宝石晶体有限公司，成都 610000

通讯作者:

徐家跃（1965—），男，博士，教授。

作者简介:

陈宇轩（2001—），男，硕士研究生。

Growth and Spectra of 6-inch YSZ:Er Crystals

Yuxuan CHEN¹, Xin JIANG²^,³, Hui SHEN¹, Tian TIAN¹, Zefeng JIANG²^,³, Jiayue XU¹

Affiliations

^1.School of Materials Science and Engineering, Shanghai Institute of Technology, Shanghai 201418, China

^2.Guangxi Guilin Jiaxing Crystal Gem Co., Ltd, Guilin 542501, China

^3.Sicuan Chengdu Xinxing Crystal Gemstone Co., Ltd, Chengdu 610000, China

Corresponding Author:

XU Jiayue (1965-), male, Ph.D., Professor. E-mail: xujiayue@sit.edu.cn

CHEN Yuxuan (2001-), male, Master candidate. E-mail: 236081203@mail.sit.edu.cn

出版时间: 2025-12-20 doi: 10.14062/j.issn.0454-5648.20250442

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摘要

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1.5~1.7 μm人眼安全波段激光在激光测距、激光雷达和光通信等领域具有重要应用。然而，现有的Er：YAG、Er：LuYO₃等激光晶体受限于较小的发射截面或晶体尺寸，难以满足高功率、大型化激光器的需求。因此，开发兼具大尺寸和高发射截面的新型激光晶体已成为当前研究的热点。本工作采用冷坩埚法生长了稀土掺杂钇稳定氧化锆（YSZ）晶体，晶体呈<111>择优生长取向，单体直径和长度都超过150 mm（6英寸），是目前所知最大的YSZ单晶。研究了Er掺杂YSZ晶体的吸收、发射光谱。结果表明，在971 nm波长激发下，YSZ：Er晶体在1530 nm处表现出强发射峰，对应⁴I_13/2→⁴F_15/2跃迁；发射截面随Er³⁺含量变化，Er³⁺含量为1.60%（摩尔分数，下同）时为4.811×10^-20 cm²；荧光寿命随着Er³⁺含量增加逐渐减小，Er³⁺含量为1.60%时荧光寿命为1.149 ms。通过掺杂离子和掺杂浓度的优化，YSZ：Er晶体有望成为一种潜在的激光晶体材料。

关键词

钇稳定立方氧化锆 / 冷坩埚法 / 晶体生长 / 激光晶体

Abstract

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Introduction

Lasers operating within a spectral range of 1.5-1.7 μm are essential for eye-safe applications like laser ranging, lidar, and optical communications, etc.. Nevertheless, conventional laser crystals such as Er:YAG and Er:LuYO₃ have limitations in emission cross-sections or attainable crystal dimensions, thereby constraining their utilization in high-power, large-scale laser systems. To address these challenges, the development of novel laser crystals with substantial crystal sizes and high emission cross-sections is thus imperative. Yttria-stabilized zirconia (YSZ) doped with rare-earth ions emerges as a promising candidate due to its disordered crystalline structure that enables a broader wavelength tunability and a reduced thermal loading under resonant pumping conditions. Specifically, erbium (Er³⁺) doped YSZ crystals have a significant potential due to its intense emission at 1.5 μm (⁴I_13/2→⁴F_15/2 transition) for eye-safe laser. This study was to investigate the growth of large-scale Er³⁺-doped YSZ crystals by a skull melting technique, and the optical and spectral properties were systematically investigated to explore a novel laser gain medium in the infra-red region.

Methods

Pure YSZ and Er³⁺-doped YSZ crystals (i.e., 0.36%, 1.60% and 2.54% in mole) were grown by a skull melting method (or a cold crucible technique), and a radio frequency (RF) generator was used to heat up the charges. A large-scale furnace with a diameter of approximately 150 cm was employed to accommodate the spontaneous nucleation. Graphite electrodes were used for initial arcing due to the poor conductivity of ZrO₂ at < 1200 ℃. At >1200 ℃, raw materials became an electric conductor to form the melting pool. The lowering mechanism started to work at a lowering rate of 2 mm/h, and the melt crystallized from the bottom to the top. After the growth, annealing process was performed to release the internal stresses. The phase and crystal structures of as-grown crystals were characterized by X-ray diffraction (XRD). The transmittance and absorption properties were analyzed by UV-Vis-NIR spectroscopy. The luminescence and decay curve were also systematically evaluated.

Results and Discussion

The results show that Large-sized YSZ and Er-doped YSZ crystals with the diameters and lengths of exceeding 150 mm (6 inches) are grown, representing the largest YSZ single crystals reported. The XRD patterns indicate the cubic structure with a preferred <111> preferred orientation. The lattice parameters increase slightly with Er³⁺ concentration, indicating the effective incorporation of Er³⁺ into the YSZ lattice. The transmission of exceeding 74% in the range of 400-1650 nm occurs for pure YSZ crystals, confirming relatively high crystalline qualities. The absorption spectra for Er-doped crystals show some characteristic peaks at 378, 408, 451, 489, 518, 546, 654, 971, 1460 nm and 1530 nm, corresponding to Er³⁺ transitions from the ground state ⁴F_15/2 to excited states such as ⁴G_11/2 and ⁴F_11/2. The most intense absorption band occurs at 971 nm, which is attributed to the ⁴F_15/2→⁴F_11/2 transition. Under 971 nm excitation, the emission spectra exhibit a dominant peak at 1530 nm for the ⁴I_13/2→⁴F_15/2 transition, which is ideal for eye-safe lasers. The great emission intensity appears at an Er³⁺ mole concentration of 1.60%, with an emission cross-section of 4.811×10^-20 cm², which is significantly higher than that of Er:YAG (i.e., 0.6×10^-20 cm²) and Er:LuYO₃ (i.e., 0.261×10^-20 cm²). Correspondingly, the decay time of YSZ: 0.36, YSZ: 1.60and YSZ: 2.54 crystals is 1.836 ms, 1.149 ms and 0.797 ms, respectively.

Conclusions

This study demonstrated the effective growth of large-scale (6-inch) YSZ and Er-doped YSZ crystals by a skull melting method. YSZ: Er crystals exhibited an intense emission at 1530 nm under 971 nm excitation. In particular, a high emission cross-section of 4.811×10^-20 cm² and suitable fluorescence lifetime of 1.149 ms appeared for Er³⁺ of 1.60% in mole. YSZ:Er crystals could be used as a highly promising gain medium for high-power, eye-safe lasers at 1.5 μm due to the ultra-large crystal size and relatively large emission cross-section.

Key words

yttria-stabilized zirconia / skull melting method / crystal growth / laser crystal

引用本文

陈宇轩, 蒋新, 申慧, 田甜, 蒋泽锋, 徐家跃. 直径6英寸YSZ：Er晶体生长与光谱. 硅酸盐学报, 2025 , 53 (12) : 3476 -3483 . DOI: 10.14062/j.issn.0454-5648.20250442

Yuxuan CHEN, Xin JIANG, Hui SHEN, Tian TIAN, Zefeng JIANG, Jiayue XU. Growth and Spectra of 6-inch YSZ:Er Crystals[J]. Journal of the Chinese Ceramic Society, 2025 , 53 (12) : 3476 -3483 . DOI: 10.14062/j.issn.0454-5648.20250442

基金

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国家自然科学基金(51572175)

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2025年第53卷第12期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250442

接收时间：2025-06-06
首发时间：2026-10-21
出版时间：2025-12-20

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收稿日期：2025-06-06
修回日期：2025-07-12

基金

国家自然科学基金(51572175)

作者信息

^1．上海应用技术大学材料科学与工程学院，上海 201418

^2．广西桂林佳兴宝石晶体有限公司，桂林 542501

^3．四川成都新兴宝石晶体有限公司，成都 610000

通讯作者:

徐家跃（1965—），男，博士，教授。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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