深圳大学学报理工版

研究了高径比分别为1.36和1.50的两组坩埚在炉体内的轴向、径向温度梯度和液流情况. 在两组坩埚中进行晶体生长实验,将生长出来的晶体进行掏棒和切片,并对晶棒进行应力和气泡检测,对晶片进行位错和双晶摇摆曲线检测. 对比理论计算和实验结果表明,当纵横温度变化近似一次函数,且纵横温度梯度作用下的固液面的夹角在45°～60°时,可以有效降低应力,减少开裂几率; 当熔体内部只有一个涡旋的时候,可有效减少晶体气泡; 坩埚高径比为1.36时,能有效降低位错密度,提高结晶性.

We investigate the effects of the crucible height to diameter ratio H/D on the quality of large size sapphire single crystal theoretically and experimentally. For two crucibles with H/D ratios of 1.36 and 1.50 we calculate the axial and radial temperature gradients and flow theoretically. We analyze the effects of two temperature fields on the growth of sapphire crystal in these two temperature fields. By comparing the theoretical calculation results with experimental results of these two temperature fields, the following conclusions are obtained: the stress and cracking probability are effectively reduced when the axial and radial temperature curves are close to linear function and the angle of solid surface is between 45° and 60° in the role of the axial and radial temperature gradient; the bubble inside the sapphire crystal is reduced when the melt has only one vortex; the dislocation density is reduced, and the crystallization quality is increased when the crucible H/D ratio is 1.36.

引言
1 理论计算
2 实验过程
3 模拟计算及结果分析
4 结论

图1 泡生法示意图[21]<br/>Fig.1 Sketch map of Kyropoulos[21]

图1 泡生法示意图[21]
Fig.1 Sketch map of Kyropoulos[21]

表1 四组实验理论模拟结果对比<br/>Table 1 The numerical simulation results of four experimental groups

表1 四组实验理论模拟结果对比
Table 1 The numerical simulation results of four experimental groups

图2 轴向和径向温度梯度<br/>Fig.2 Temperature gradients of the axial and radial

图2 轴向和径向温度梯度
Fig.2 Temperature gradients of the axial and radial

图3 Ⅰ号和Ⅱ号单晶炉温场轴向温度曲线<br/>Fig.3 The axial temperature curves of theⅠ andⅡ

图3 Ⅰ号和Ⅱ号单晶炉温场轴向温度曲线
Fig.3 The axial temperature curves of theⅠ andⅡ

图4 Ⅰ号和Ⅱ号单晶炉温场径向温差度曲线<br/>Fig.4 The radial temperature curves of the furnace Ⅰ and Ⅱ

图4 Ⅰ号和Ⅱ号单晶炉温场径向温差度曲线
Fig.4 The radial temperature curves of the furnace Ⅰ and Ⅱ

图5 Ⅰ号和Ⅱ号单晶炉生长出的晶体<br/>Fig.5 Crystals fabricated from the furnaceⅠandⅡ

图5 Ⅰ号和Ⅱ号单晶炉生长出的晶体
Fig.5 Crystals fabricated from the furnaceⅠandⅡ

图6 应力测试图<br/>Fig.6 The results of stress tests

图6 应力测试图
Fig.6 The results of stress tests

图7 温场理论计算熔体液流情况<br/>Fig.7 The results of molten fluid flows

图7 温场理论计算熔体液流情况
Fig.7 The results of molten fluid flows

图8 气泡检测结果<br/>Fig.8 The results of air bubble detections

图8 气泡检测结果
Fig.8 The results of air bubble detections

图9 位错腐蚀结果<br/>Fig.9 The results of dislocations by corrosion

图9 位错腐蚀结果
Fig.9 The results of dislocations by corrosion

$图10 晶片双晶X射线摇摆曲线<br/>Fig.10 The X-ray double-crystal diffractometry$

图10 晶片双晶X射线摇摆曲线
Fig.10 The X-ray double-crystal diffractometry

[1] Akselrod M S, Bruni F J. Modern trends in crystal growth and new applications of sapphire[J]. Journal of Crystal Growth, 2012, 360(1): 134-145.
[2] Scheel H J. Historical aspects of crystal growth technology[J]. Journal of Crystal Growth, 2000, 211(1): 1-12.
[3] Nassau K. Verneuil: the man and the method[J]. Journal of Crystal Growth, 1972, s13/s14(3):12-18.
[4] Akasaki I. Key inventions in the history of nitride-based blue LED and LD[J]. Journal of Crystal Growth, 2007,300(1):2-10.
[5] Komaki H, Nakamura T, Katayama R, et al. Growth of In-rich InGaN films on sapphire via GaN layer by RF-MBE[J]. Journal of Crystal Growth, 2007, s301/s302(4):473- 477.
[6] Foxon C T, Campion R P, Grant V A, et al. Use of band-gap thermometry to investigate the growth of GaN on sapphire and GaAs[J]. Journal of Crystal Growth, 2007,301(4):482- 485.
[7] 王东阳, 贺威, 李玲, 等. 光学质量大尺寸蓝宝石单晶工艺研究[J]. 深圳大学学报理工版, 2015, 32(4): 350-356.
[8] 杨琳, 左然. 泡生法蓝宝石不同生长阶段热应力的数值模拟研究[J]. 材料导报, 2012, 26(22): 134-137.
[9] Yamada M, Tao C. Microscopic observation of strain induced in heteroepitaxial layers with reflection type of infrared polariscope[J]. Journal of Crystal Growth, 2000,210(1):102-106.
[10] Khattak C P, Schmid F. Growth of the world's largest sapphire crystals[J]. Journal of Crystal Growth, 2001,225(2/3/4):572-579.
[11] Labelle H E. EFG, the invention and application to sapphire growth[J]. Journal of Crystal Growth, 1980,50(1):8-17.
[12] Budenkova O N, Vasiliev M G, Yuferev V S, et al. Simulation of global heat transfer in the Czochralski process for BGO sillenite crystals[J]. Journal of Crystal Growth, 2004,266(1/2/3):103-108.
[13] Bunoiu O M, Nicoara I, Santailler J L, et al. On the void distribution and size in shaped sapphire crystals[J]. Crystal Research & Technology, 2005,40(9):852-859.
[14] 曾贵平, 殷绍唐, 秦青海, 等. 钛宝石晶体中的位错以及退火对位错的影响[J]. 硅酸盐学报, 2001,29(2): 168-171.
[15] 徐军, 周国清, 邓佩珍, 等. 温梯法蓝宝石(Al2O3)晶体的脱碳去色退火研究[J]. 无机材料学报, 2005, 20(5): 1095-1098.
[16] 姚泰, 韩杰才, 左洪波, 等. 蓝宝石单晶的气孔形成研究[J]. 无机材料学报, 2008, 23(3): 439- 442.
[17] 姚泰, 左洪波, 韩杰才, 等. 蓝宝石单晶生长过程中应力分布的数值模拟[J]. 哈尔滨理工大学学报, 2006,11(5): 100-104.
[18] 韩杰才, 孟松鹤, 左洪波, 等. 大尺寸蓝宝石单晶的冷心放肩微量提拉制备法: 中国,CN1724722[P]. 2006- 01-25.
[19] 汪传勇, 左然, Andrey S,等. 泡生法生长蓝宝石单晶的热场改进与模拟优化[J]. 人工晶体学报, 2011,40(1): 83-87.
[20] 李金权, 苏小平. 气流湍流对泡生法生长蓝宝石单晶温场的影响[J]. 人工晶体学报, 2008,37(1): 236-247.
[21] 韩江山, 左然. 钼屏发射率对泡生法蓝宝石单晶生长影响的数值模拟研究[J]. 材料导报, 2013, 27(16): 143-150.

备注

引言

1 理论计算

2 实验过程

3 模拟计算及结果分析

4 结论

期刊信息

备注

引言

1 理论计算

2 实验过程

3 模拟计算及结果分析

4 结 论

期刊信息

4 结论