提拉法下Yb:YAG单晶缺陷的正电子湮没研究

doi:10.15541/jim20220364

无机材料学报 ›› 2023, Vol. 38 ›› Issue (3): 316-321.DOI: 10.15541/jim20220364 CSTR: 32189.14.10.15541/jim20220364

提拉法下Yb:YAG单晶缺陷的正电子湮没研究

石小兔¹^,²^,³(), 张庆礼¹^,³(), 孙贵花¹^,³, 罗建乔¹^,³, 窦仁勤¹^,³, 王小飞¹^,³, 高进云¹^,³, 张德明¹^,³, 刘建党⁴(), 叶邦角⁴

1.中国科学院合肥物质科学研究院, 安徽光学精密机械研究所, 光子器件与材料安徽省重点实验室, 合肥 230031
2.中国科学技术大学研究生院科学岛分院, 合肥 230026
3.先进激光技术安徽省实验室, 合肥 230037
4.中国科学技术大学核探测与核电子学国家重点实验室, 合肥 230026

收稿日期:2022-06-28 修回日期:2022-08-20 出版日期:2023-03-20 网络出版日期:2022-11-16
通讯作者: 张庆礼, 研究员. E-mail: zql@aiofm.ac.cn;
刘建党, 高级工程师. E-mail: liujd@ustc.edu.cn
作者简介:石小兔(1999-), 女, 硕士研究生. E-mail: shih1999@mail.ustc.edu.cn
基金资助:
国家自然科学基金(51802307);国家自然科学基金(11875248);安徽省实验室重点基金(AHL20220ZR04)

Positron Annihilation Study of Yb:YAG Single Crystal Defects under Czochralski Method

SHI Xiaotu¹^,²^,³(), ZHANG Qingli¹^,³(), SUN Guihua¹^,³, LUO Jianqiao¹^,³, DOU Renqin¹^,³, WANG Xiaofei¹^,³, GAO Jinyun¹^,³, ZHNAG Deming¹^,³, LIU Jiandang⁴(), YE Bangjiao⁴

1. The Key Laboratory of Photonic Devices and Materials of Anhui Province, Anhui Institute of Optics and Fine Mechanics, Hefei Institutes of Physical Science, Chinese Academy of Sciences, Hefei 230031, China
2. Science Island Branch of Graduate School, University of Science and Technology of China, Hefei 230026, China
3. Advanced Laser Technology Laboratory of Anhui Province, Hefei 230037, China
4. State Key Laboratory of Particle Detection and Electronics, University of Science and Technology of China, Hefei 230026, China

Received:2022-06-28 Revised:2022-08-20 Published:2023-03-20 Online:2022-11-16
Contact: ZHANG Qingli, professor. E-mail: zql@aiofm.ac.cn;
LIU Jiandang, senior engineer. E-mail: liujd@ustc.edu.cn
About author:SHI Xiaotu (1999-), female, Master candidate. E-mail: shih1999@mail.ustc.edu.cn
Supported by:
National Natural Science Foundation of China(51802307);National Natural Science Foundation of China(11875248);Key Laboratory Fund of Anhui Province(AHL20220ZR04)

摘要/Abstract

摘要：

为满足固体激光器的应用需求, 研究人员不断改进YAG激光晶体生长技术, 其中控制 YAG中的缺陷结构对于晶体的生长尤为重要。本工作对提拉法两种工艺制备的晶体样品进行了缺陷研究, 特别是晶体散射点的起源。正电子湮没技术是一种对材料微观结构十分灵敏且有效的核物理技术分析表征手段, 对空位缺陷、微孔等极为敏感。根据正电子湮没寿命谱与多普勒展宽谱的分析结果, 无论工艺、有无散射点, 样品的正电子寿命及多普勒展宽线性参数均存在差异。这说明晶体主要缺陷是YAG结构中的本征缺陷, 散射点可能是空位团聚引起的纳米微孔, 研究表明该技术可以灵敏地表征YAG晶体散射点。正电子湮没实验反映的晶体单晶质量差异与X射线衍射、单晶摇摆曲线、光透过率以及位错密度结果吻合。在研究晶体的物理性能和缺陷与材料微结构的关系上正电子湮没技术具有独特的技术优势, 同时正电子湮没技术可以在微观尺度上有效反映晶体质量。

关键词: 晶体缺陷, 正电子湮没, Yb:YAG晶体, 提拉法

Abstract:

In order to meet the development needs of solid-state lasers, it is necessary to continuously improve the YAG laser crystal growth technology. However, controlling the defect structure in YAG is particularly difficult for crystal development in industry and scientific research. The defects of crystal samples prepared by the two processes were studied, especially the origin of crystal scattering points. Positron annihilation technology (PAT) is a sensitive and effective nuclear technology for analysis and characterization method being used to control microstructure of materials, which is extremely sensitive to vacancy defects and micropores. According to the PAT analysis results,the positron annihilation lifetime spectrum and Doppler broadening spectrum, the positron lifetimes and line-shape parameters of Doppler broadening spectra of samples vary with different processes and with or without scattering points indicating that the main defects of the crystal are the intrinsic defects in the YAG structure.The scattering points may be nanopores caused by vacancy agglomeration, indicating that the PATis very sensitive to characterize the scattering points in the YAG crystal. The present experimental results of positron annihilation are consistent with the results of single crystal quality reflected by X-ray diffraction (XRD), single crystal rocking curve (XRC), optical transmittance, and dislocation density, indicating the uniqueness and technical advantages of positron annihilation technology in studying the relationship between physical properties and defects/microstructure of crystal materials. Meanwhile, it can be concluded that the PAT can effectively reflect the crystal quality at micro scale.

Key words: crystal defects, positron annihilation, Yb:YAG crystal, Czochralski method

中图分类号:

石小兔, 张庆礼, 孙贵花, 罗建乔, 窦仁勤, 王小飞, 高进云, 张德明, 刘建党, 叶邦角. 提拉法下Yb:YAG单晶缺陷的正电子湮没研究[J]. 无机材料学报, 2023, 38(3): 316-321.

SHI Xiaotu, ZHANG Qingli, SUN Guihua, LUO Jianqiao, DOU Renqin, WANG Xiaofei, GAO Jinyun, ZHNAG Deming, LIU Jiandang, YE Bangjiao. Positron Annihilation Study of Yb:YAG Single Crystal Defects under Czochralski Method[J]. Journal of Inorganic Materials, 2023, 38(3): 316-321.

图/表 8

图1 两组Yb:YAG晶体的X射线粉末衍射图谱与标准图谱(ICSD#20090)对比

Fig. 1 XRD patterns of two groups of Yb:YAG crystals compared to the standard pattern (ICSD#20090)

图2 两组Yb:YAG晶体样品的X射线摇摆曲线

Fig. 2 X-ray rocking curves of two groups of Yb:YAG crystals

图3 双光路透过率测量装置光路图

Fig. 3 Optical path diagram of double optical path transmittance measurement

表1 同一样品中有无散射点区域的光学透过率

Table 1 Optical transmittance of a sample syncroneously with and without scattering points

Area	Transmittance/%			Average value/%
With scattering point	83.38	83.00	83.22	83.20
Without scattering point	84.06	84.17	84.26	84.16

图4 Yb:YAG晶体(111)晶面的位错腐蚀形貌

Fig. 4 Dislocation etching pits of Yb:YAG crystal at (111) crystalline face

表2 各个样品的正电子湮没寿命特征参数

Table 2 Positron annihilation lifetime results of each sample

Sample	τ₁/ps	I₁/%	τ₂/ns	I₂/%	τ_av/ps
1-1	165.72	98.80	2.037	1.198	186.97
1-2	167.26	98.95	2.043	1.051	188.14
2-1	161.42	100.00	/	/	161.42
2-2	165.24	100.00	/	/	165.24
2-3	162.90	100.00	/	/	162.90
2-4	164.40	100.00	/	/	164.40

图5 各个样品的正电子湮没寿命图

Fig. 5 Positron annihilation lifetime diagrams of each sample

图6 不同工艺Yb:YAG晶体样品的正电子多普勒展宽线性参数S和W的变化

Fig. 6 Line-shape parameters of Doppler broadening spectra of Yb:YAG crystal samples under different processes (a) Variation of S-parameter values; (b) Plots of S-parameter vs. W-parameter

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提拉法下Yb:YAG单晶缺陷的正电子湮没研究

Positron Annihilation Study of Yb:YAG Single Crystal Defects under Czochralski Method

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