泡生法制备低吸收蓝宝石晶体及其性能研究

摘要/Abstract

摘要： 为保障我国相关国防重大工程对低吸收蓝宝石晶体材料的需求,本文通过自主研制的晶体生长设备,成功生长了低吸收蓝宝石晶体。该晶体在紫外、可见光、近-中红外波段展现出了良好的透过率,波长250~400 nm的透过率大于83%,波长400~4 200 nm的透过率超过85%。在晶体不同区域进行取样表征测试,得到晶体的平均位错密度为253.19 cm^-2,摇摆曲线对称且峰形尖锐,半峰全宽为14″。此外,值得注意的是,晶体在1 064 nm处的光吸收系数均在(23.3~30.4)×10^-6 cm^-1,表明晶体内部的杂质元素得到有效控制,晶体光学性能优异,可用于高能激光系统、空间相机镜头等应用场景。

关键词: 低吸收, 泡生法, 杂质元素, 光吸收系数, 透过率, 位错密度

Abstract: In order to meet the demand for low-absorption sapphire crystal materials in important national defense projects in China, a self-produced crystal growth apparatus is developed in this study and the successful growth of low-absorption sapphire crystal can be achieved. The as-obtained crystal exhibits excellent transparency in the ultraviolet, visible, and near to mid-infrared wavelength ranges. The transmittance is above 83% as the wavelength in the range of 250 nm to 400 nm, while the transmittance is above 85% as the wavelength in the range of 400 nm to 4 200 nm. On the basis of the characterization tests conducted on different regions of the crystal, the average dislocation density of crystal can be determined as 253.19 cm^-2. The rocking curve shows symmetrical and sharp peaks with a full width at half maximum of 14″. In addition, it is worth noting that the light absorption coefficient of crystal is (23.3~30.4)×10^-6 cm^-1 at the wavelength of 1 064 nm, indicating that the impurity elements inside the crystal can be effectively controlled. Accordingly, the outstanding optical properties crystal can be applied in high-energy laser systems, space camera lenses and other relevant fields.

Key words: low absorption, Kyropoulos method, impurity element, light absorption coefficient, transmittance, dislocation density

中图分类号:

O78
TQ164

赵鹏, 宋建军, 张微, 承刚, 张立生, 付春雷, 石刚, 黄存新. 泡生法制备低吸收蓝宝石晶体及其性能研究[J]. 人工晶体学报, 2023, 52(12): 2203-2209.

ZHAO Peng, SONG Jianjun, ZHANG Wei, CHENG Gang, ZHANG Lisheng, FU Chunlei, SHI Gang, HUANG Cunxin. Preparation and Properties of Low-Absorption Sapphire Crystal by Modified Kyropoulos Method[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2023, 52(12): 2203-2209.

参考文献

[1] AKSELROD M S, BRUNI F J. Modern trends in crystal growth and new applications of sapphire. Journal of Crystal Growth, 2012, 360: 134-145.
[2] 张义广, 丁明跃, 蔡超, 等. 高温高速流场条件下蓝宝石材料对红外成像影响分析[J]. 人工晶体学报, 2005, 34(2): 259-264.
ZHANG Y G, DING M Y, CAI C, et al. Analysis of the effects of Al₂O₃ on IR imaging in air flow with high-temperature and high-speed[J]. Journal of Synthetic Crystal, 2005, 34(2): 259-264 (in Chinese).
[3] 聂辉, 陆炳哲. 蓝宝石及其在军用光电设备上的应用[J]. 舰船电子工程, 2005, 25(2): 131-133+142.
NIE H, LU B Z. Sapphire window and it’s application in military electro-optical equipment[J]. Ship Electronic Engineering, 2005, 25(2): 131-133+142 (in Chinese).
[4] 王如刚, 陈振强, 胡国永. 几种LED衬底材料的特征对比与研究现状[J]. 科学技术与工程, 2006, 6(2): 121-126.
WANG R G, CHEN Z Q, HU G Y. The comparison of LED dedding materials SiC, ZnO, Al₂O₃[J]. Science Technology and Engineering, 2006, 6(2): 121-126 (in Chinese).
[5] 李鹏博, ZEIDLER SIMON, LEONARDI MATTEO, 等. KAGRA引力波探测器中蓝宝石测试镜光学性质研究[J]. 天文学报, 2021, 62(6): 41-53.
LI P B, ZEIDLER S, LEONARDI M, et al. Optical characterization of sapphire test mirror in KAGRA gravitational wave detector[J]. Acta Astronomica Sinica, 2021, 62(6): 41-53 (in Chinese).
[6] 周国清, 李红军, 乔景文, 等. LIGO计划用大尺寸蓝宝石晶体光学均匀性和弱吸收获得进展[J]. 光学学报, 2001, 21(3): 383-384.
ZHOU G Q, LI H J, QIAO J W, et al. Progress of optical homogeneity and weak-absorption of large-sized sapphire crystal used in LIGO project[J]. Acta Optica Sinica, 2001, 21(3): 383-384 (in Chinese).
[7] DEMINA S E, BYSTROVA E N, POSTOLOV V S, et al. Use of numerical simulation for growing high-quality sapphire crystals by the Kyropoulos method[J]. Journal of Crystal Growth, 2008, 310(7/8/9): 1443-1447.
[8] 张雪平. 蓝宝石晶体生长与LED应用研究[D]. 长沙: 湖南大学, 2012.
ZHANG X P. Study on sapphire crystal growth and LED application[D].Changsha: Hunan University, 2012 (in Chinese).
[9] 蔡迅. 改进热交换法生长蓝宝石晶体中的气泡研究[D]. 北京: 北京有色金属研究总院, 2013.
CAI X. Study on bubbles in sapphire crystal grown by improved heat exchange method[D]. Beijing: Dissertation of GRINM, 2013 (in Chinese).
[10] YANG X B, LI H J, XU J, et al. Growth of r-plane sapphire by edge-defined film-fed growth and temperature gradient technique[J]. Journal of the Chinese Ceramic Society, 2008, 36(5): 678-683.
[11] BUNOIU O, NICOARǍ I, DUFFAR T. Solute distribution in shaped sapphire crystals obtained by EFG method[J]. Journal of Optoelectronics and Advanced Materials, 2005, 7: 615-618.
[12] BORODIN A V, BORODIN V A, ZHDANOV A V. Simulation of the pressure distribution in the melt for sapphire ribbon growth by the Stepanov (EFG) technique[J]. Journal of Crystal Growth, 1999, 198/199: 220-226.
[13] 欧阳鹏根. 首颗700 kg级超大尺寸蓝宝石晶体生长成功[J]. 人工晶体学报, 2020, 50(1): 52.
OUYANG P G. Successful growth of the first 700 kg ultra large sapphire crystal[J]. Journal of Artificial Crystals, 2020, 50(1): 52 (in Chinese).
[14] 康森, 鲁雅荣, 石天虎, 等. 改良泡生法生长720 kg级大尺寸蓝宝石晶体[J]. 人工晶体学报, 2021, 50(8): 1397-1401.
KANG S, LU Y R, SHI T H, et al. Growth of 720 kg large-sized sapphire crystal by modified kyropoulos method[J]. Journal of Synthetic Crystals, 2021, 50(8): 1397-1401 (in Chinese).
[15] 胡克艳, 唐慧丽, 王静雅, 等. 导模法蓝宝石单晶的位错缺陷及其力学性能的研究[J]. 人工晶体学报, 2013, 42(7): 1252-1256.
HU K Y, TANG H L, WANG J Y, et al. Research on mechenical properties and dislocation defects of sapphire crystal grown by edge-defined film-fed method[J]. Journal of Synthetic Crystals, 2013, 42(7): 1252-1256 (in Chinese).
[16] 彭方, 张庆礼, 杨华军, 等. c向提拉法生长的四英寸蓝宝石单晶缺陷研究[J]. 人工晶体学报, 2012, 41(增刊): 143-147.
PENG F, ZHANG Q L, YANG H J, et al. Study on the defect of 4-inches sapphire single crystal grown along c-axis direction by czochralski method[J]. Journal of Synthetic Crystals, 2012, 41(supplyment): 143-147 (in Chinese).
[17] 柯利峰, 黎建明, 苏小平, 等. 热交换法生长蓝宝石晶体的位错研究[J]. 人工晶体学报, 2009, 38(3): 625-628+647.
KE L F, LI J M, SU X P, et al. Research of dislocations of sapphire crystals grown by heat-exchange method[J]. Journal of Synthetic Crystals, 2009, 38(3): 625-628+647 (in Chinese).
[18] 彭观良, 周国清, 庄漪, 等. r面白宝石单晶的温梯法生长及缺陷研究[J]. 人工晶体学报, 2005, 34(4): 653-656.
PENG G L, ZHOU G Q, ZHUANG Y, et al. Defect study of r-plane sapphire single crystal grown by temperature gradient technique[J]. Journal of Synthetic Crystals, 2005, 34(4): 653-656 (in Chinese).
[19] 王佳麒, 张艳, 裴广庆, 等. TSTGT蓝宝石晶体位错腐蚀形貌分析[J]. 人工晶体学报, 2015, 44(3): 627-631.
WANG J Q, ZHANG Y, PEI G Q, et al. Analysis of dislocation etched topography for sapphire single crystal grown by TSTGT method[J]. Journal of Synthetic Crystals, 2015, 44(3): 627-631 (in Chinese).