导模法生长微孔蓝宝石晶体工艺及性能研究

doi:10.15541/jim20190085

无机材料学报 ›› 2019, Vol. 34 ›› Issue (12): 1290-1294.DOI: 10.15541/jim20190085

导模法生长微孔蓝宝石晶体工艺及性能研究

王东海¹,薛艳艳¹,李纳¹,周仕明¹,徐晓东²,李东振²,徐军¹(),王庆国¹()

^1. 同济大学物理科学与工程学院, 高等研究院, 上海200092
^2. 江苏师范大学物理与电子工程学院, 徐州221116

收稿日期:2019-02-23 修回日期:2019-04-29 出版日期:2019-12-20 网络出版日期:2019-06-17
作者简介:王东海(1982-), 男, 博士研究生. E-mail: <email>yingxiong3258@sina.com</email>
基金资助:
国家自然科学基金(61605069);国家自然科学基金(61805177);国家重点研发计划(2016YFB1102202)

Micro-tube Sapphire Crystal Grown by the Edge-defined-film Fed Method

WANG Dong-Hai¹,XUE Yan-Yan¹,LI Na¹,ZHOU Shi-Ming¹,XU Xiao-Dong²,LI Dong-Zhen²,XU Jun¹(),WANG Qing-Guo¹()

^1. Institute for Advanced Study, School of Physics Science and Engineering, Tongji University, Shanghai 200092, China
^2. School of Physics and Electronic Engineering, Jiangsu Normal University, Xuzhou 221116, China

Received:2019-02-23 Revised:2019-04-29 Published:2019-12-20 Online:2019-06-17
Supported by:
National Natural Science Foundation of China(61605069);National Natural Science Foundation of China(61805177);National Key R&D Program of China(2016YFB1102202)

摘要/Abstract

摘要：

采用导模法生长了内孔径470 μm的蓝宝石晶棒和内孔径160 μm板形蓝宝石晶体。基于求解拉普拉斯方程的数值解, 得到生长界面处微孔的熔体膜轮廓曲线, 采用插入钼丝的方法设计了生长模具以形成和维持晶体内的微孔尺寸, 同时解决了微孔蓝宝石长晶生长过程中的两个难点: (1)获得高质量的蓝宝石晶体; (2)在蓝宝石晶体中形成并维持所需的内孔尺寸。所生长的晶体透明完整、无开裂、双晶摇摆曲线测定显示其衍射半峰宽为3.8°, 具有良好的结晶质量

关键词: 微孔蓝宝石晶体, 导模法, 晶体生长

Abstract:

Sapphire rod with micro-tube (inner diameter: 470 μm) and sapphire plate with micro-tube (inner diameter: 160 μm) were grown by the edge-defined-film fed method (EFG). Profile curves of the small liquid menisci were investigated on the base of numerical solution of the Young-Laplace equation. By inserting Mo wires, new type of die was designed to form and sustain size of micro-tube in the volume of the crystal. Two problems were solved at the same time: 1) obtaining high quality sapphire crystal; 2) forming and sustaining necessary micro-tube sizes in the volume of the crystal. The crystal were transparent, colorless, no cracking and good XRC value of 3.8 arcmin, demonstrating the high quality of the as-grown crystal.

Key words: micro-tube sapphire crystal, edge-defined-film fed growth method, crystal growth

中图分类号:

O782

王东海, 薛艳艳, 李纳, 周仕明, 徐晓东, 李东振, 徐军, 王庆国. 导模法生长微孔蓝宝石晶体工艺及性能研究[J]. 无机材料学报, 2019, 34(12): 1290-1294.

WANG Dong-Hai, XUE Yan-Yan, LI Na, ZHOU Shi-Ming, XU Xiao-Dong, LI Dong-Zhen, XU Jun, WANG Qing-Guo. Micro-tube Sapphire Crystal Grown by the Edge-defined-film Fed Method[J]. Journal of Inorganic Materials, 2019, 34(12): 1290-1294.

图/表 10

图1 蓝宝石管生长示意图

Fig. 1 Schematic diagram of tube forming by a hollow in the die surface

表1 各机构导模法生长微孔蓝宝石最小管内径参数

Table 1 Minimal inner sizes of sapphire tube grown by different companies with EFG method

Company	Minimal tube ID size/mm	Nation
Tydex	0.80	Russia
Rostox-N	0.50	Russia
Namiki	2.00	Japan
Kyocera	1.30	Japan
Saint-gobain	0.58	France
Crytur	0.60	Australia

图2 蓝宝石微孔生长示意图

Fig. 2 Schematic diagram of micro-tube forming

图3 蓝宝石管生长计算模型

Fig. 3 Calculation model of sapphire tube growth

图4 圆管内部的熔体膜轮廓曲线

Fig. 4 Profile curves of small internal menisci at different crystal radii

图5 生长外直径5.98 mm、内孔径0.47 mm蓝宝石管熔体膜轮廓曲线

Fig. 5 Profile curve of sapphire tube with outer diameter of 5.98 mm and inner diameter of 0.47 mm

图6 熔体膜高度高于钼丝, 生长出蓝宝石晶体棒

Fig. 6 A raise meniscus level and rod formation

图7 内孔径为0.47 mm的微孔蓝宝石晶体照片(a)、显微镜测量结果(b)及SEM观察照片(c)

Fig. 7 (a) Photo of as-grown micro-tube sapphire with the inner diameter of 0.47 mm; (b) Microscopic photo of the as-grown micro-tube sapphire; (c) SEM image of the as-grown micro-tube sapphire

图8 (a) 内孔径为0.16 mm的微孔蓝宝石晶体照片; (b)显微镜测量内孔径测试结果

Fig. 8 (a) Photo of as-grown micro-tube sapphire with the inner diameter of 0.16 mm; (b) Microscopic photo of the as-grown micro-tube sapphire

图9 生长的微孔蓝宝石晶体的X射线双晶摇摆曲线

Fig. 9 X-ray rocking curve of the as-grown micro-tube sapphire crystal

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导模法生长微孔蓝宝石晶体工艺及性能研究

Micro-tube Sapphire Crystal Grown by the Edge-defined-film Fed Method

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