基于动态纹理分析的蓝宝石熔体状态识别方法

应用泡生法生产蓝宝石晶体时,引晶必须在熔体温度梯度变化相对较小的条件下进行.针对化料后熔体界面随温度变化波动较大、难以寻找理想的引晶状态这一问题,提出了一种基于熔体界面动态纹理分析的状态识别方法.通过对经典Canny算子边缘检测技术的优化,来增强对晶体生长熔体纹理提取的鲁棒性;利用反映熔体状态的重要特征参数,实现对熔体状态的自动识别.仿真实验验证了该方法的有效性,为实现蓝宝石晶体的智能化制造提供了新途径.     

热交换法生长蓝宝石晶体的位错研究

本文用热交换法生长出a向,尺寸为φ150 mm×160 mm,重10 kg的低位错蓝宝石晶体,并采用化学腐蚀-金相显微镜法观测了(0001)晶面的位错形貌.结果显示:(0001)晶面的位错腐蚀坑呈三角形,分布较均匀和分散,图像清晰,平均位错密度较低,为2.1×103 Pits/cm2;热交换系统保温效果好,能独立控制熔体和晶体的温度梯度,温场起伏小,具有良好的稳定性和可控性,适合用来生长大直径低位错的蓝宝石晶体.     

旋转对Cz法硅晶生长过程中热输运和熔体流动影响的数值模拟

建立了一个120 kg单晶炉的二维轴对称全局模型,分别对无旋转、加入晶体旋转、加入坩埚旋转、同时加入晶体旋转和坩埚旋转的四种工况展开了数值模拟研究.得到了晶体旋转及坩埚旋转对晶体生长过程的拉晶功率、炉内温度分布和熔体流动的影响;得到了不同晶体长度下拉晶炉内的温度分布以及熔体流动的变化规律.结果显示,加入晶体旋转对晶体生长过程的拉晶功率、温度分布和熔体流动的影响小于坩埚旋转的影响;随着晶体长度的增加,晶体旋转及坩埚旋转对温度分布和熔体流动的影响不断减小.因此在单晶炉设计和优化过程中应考虑整个晶体生长过程.     

导模法蓝宝石单晶的位错缺陷及其力学性能的研究

采用导模法生长了a向,尺寸为60 mm ×5 mm ×300 mm的蓝宝石单晶片,采用化学腐蚀-金相显微镜法观测了其(0001)晶面的位错特征,并且采用INSTRON-1195万能试验机测试了抛光样品的弯曲强度.结果显示:当晶体中位错缺陷分布均匀时,在外部弯曲应力下,蓝宝石晶体发生特定晶面的高强解理断裂,位错密度的升高对蓝宝石弯曲强度没有明显损害作用.然而当晶体中出现位错密排结构时,蓝宝石单晶常温弯曲强度迅速下降.     

热交换法蓝宝石晶体生长的数值模拟研究

针对热交换法蓝宝石晶体各生长阶段的温场、流场和热应力进行数值模拟研究,并讨论了上部保温层结构、热交换器内管高度对晶体生长的影响.结果表明:长晶初期,固液界面呈椭球形;等径阶段,固液界面平坦,晶体与坩埚壁不接触;长晶后期,中心轴向晶体生长速率增加,晶体中心首先冒出熔体液面.随晶体高度增加,熔体对流由初期的两个涡胞变为等径阶段的一个涡胞,最大对流速度量级为10-3 m/s.晶体中最大热应力分布在晶体底部,热应力分布呈W型.增加炉体上部保温层,长晶后期固液界面变得平坦;降低热交换器内管高度,有利于降低晶体底部热应力.     

蓝宝石晶体热性能的各向异性对SAPMAC法晶体生长的影响

采用有限元法对冷心放肩微量提拉法蓝宝石晶体生长过程中晶体内的温度、应力分布进行了模拟计算,结合实验结果讨论了蓝宝石晶体热性能的各向异性对晶体生长的影响.研究结果表明,对于冷心放肩微量提拉蓝宝石晶体生长系统,较大的轴向热导率有利于提高晶体的生长速率和界面稳定性,而稍大的径向热导率则有利于保持微凸的生长界面.晶体内的热应力受径向热膨胀系数的影响显著,随着径向热膨胀系数的增大而增大,最大热应力总是出现在籽晶与新生晶体的界面区域.在实验中选α轴为结晶取向,成功生长出了直径达230mm、高质量蓝宝石晶体.     

μ-PD法蓝宝石纤维晶体生长中传热传质的数值模拟

在μ-PD法纤维蓝宝石单晶生长中,利用Comsol软件数值分析了陶瓷管开裂现象、熔体对流和磁场分布.结果表明,试验中陶瓷管保温层总是在距底部0.03 m处断裂,数值模拟发现该处为温度和Von Mises应力最高点位置,验证了数值模拟的准确性;适当增大陶瓷管保温层厚度有利于降低陶瓷管温度,从而降低其开裂概率;熔体对流中Marangoni对流占主导,浮力对流可忽略;磁场分布能够满足μ-PD法蓝宝石晶体生长需求,“趋肤效应”使最高温度位于铱坩埚最上端.     

冷心放肩微量提拉法大尺寸蓝宝石单晶生长过程的模拟分析

利用数值模拟方法计算了冷心放肩微量提拉法(SAPMAC)蓝宝石晶体生长过程.结合晶体直径变化、裂纹出现位置与延续方向、晶体透明性等实验现象,通过与提拉法、温梯法、坩埚移动法等相对比,分析了冷心放肩微量提拉法晶体生长各阶段的工艺特点,并根据模拟计算结果对晶体生长系统和晶体生长控制工艺进行了改进.分别利用增大热交换器的散热参数、降低加热温度、改进降温曲线、调节外加轴向和径向温度梯度的方式来实现对晶体生长的引晶、放肩、等径和收尾控制.通过实验比较证明了改进后的晶体生长系统和晶体生长控制工艺能够生长出性能较好的大尺寸蓝宝石晶体.     

四硼酸铅晶体生长及特性研究

本文采用熔体法生长出四硼酸铅透明大单晶,最大尺寸为54mm×46mm×10mm.对它的结晶学特性进行了研究,晶体形态为沿a-c晶面延伸的厚板状;晶体的质量与生长时引晶方向有关,当(010)晶面平行于液面时,晶体生长均匀,缺陷减少.该晶体的莫氏硬度为8～8.5,化学性能稳定.晶体生长时无挥发物产生,因而减少其对环境的污染.本文测试了PbB4O7晶体的熔点、透光性、热扩散物理性质,并首次定性测试了它的非线性光学性能,其倍频信号强度与KDP相当.     

ø300 mm直拉硅单晶生长过程中的变晶现象及其影响因素

直拉法生长直径300 mm硅单晶过程中,直径均匀是获得高品质硅单晶的关键。在生产实践中发现,当硅晶体进入等径生长阶段,过高的提拉速度会引起晶体发生扭晶现象,导致晶线断裂随即变晶,对等径生长不利。本文采用数值模拟和理论相结合的方法分析了ø300 mm硅单晶生长过程中扭晶现象的成因,建立了不同提拉速度下晶体直径与熔体温度分布的关系,分析了晶体发生扭晶的影响因素。结果表明,随着提拉速度的增加,熔体自由表面产生过冷区且该过冷区随提拉速度的增加不断扩大,过冷区的产生是导致晶体发生扭晶的主要原因。提出了一种基于有限元热场数值模拟的最大稳定提拉速度的判别方法,并给出了通过改变晶体旋转速度来改善熔体自由表面温度分布的工艺措施建议,从而避免晶体扭晶现象的发生。研究结果对设计大尺寸硅单晶生长热场具有一定的指导作用。     

Morphological stability of sapphire crystallization front

The main factors and specificity of growth conditions for sapphire and Ti:sapphire crystals, which affect the morphological stability of the crystal–melt interface, have been investigated with allowance for the concentration and radiative melt supercooling. It is shown that the critical sapphire growth rate is determined to a great extent by the optical transparency of the melt and the mixing conditions near the crystallization front.     

Numerical optimization of czochralski sapphire single crystal growth using orthogonal design method

Crystal quality during Czochralski (Cz) growth is influenced significantly by the convexity of solid/liquid (S/L) interface, which is related to operating conditions, such as Radio‐Frequency (RF) coil position, crystal rotation and crucible rotation. Generally, a flat interface shape is preferred for high‐quality crystal growth. It is difficult to achieve the optimized conditions even from numerical modeling due to the large computational load from examining all of the affecting factors. Orthogonal design/test method, fortunately, provides an efficient way to organize the study of multiple factors with the minimization of computational load. In the paper, this method is adopted to investigate the affecting factors of Cz‐sapphire single crystal growth based on the coupled calculation of thermal field and melt flows. The orthogonal analysis clearly reveals the optimized growth conditions to achieve a relative flat S/L interface under the current ranges of the parameters.     

加热功率波动对SAPMAC法生长蓝宝石晶体的影响

本文根据温度波在熔体介质中的传播理论,结合SAPMAC法蓝宝石晶体生长工艺特点,研究了由加热功率波动引起的温度波动对晶体生长的影响.研究表明由于氧化铝高温熔体具有较大的热扩散系数,温度波较容易传到固液界面引起界面温度起伏;界面的温度起伏会使晶体内产生气泡、空腔等缺陷.根据温度波的频率、幅值对氧化铝熔体的传递深度、衰减规律的关系,提出了提高系统热惯性、增加界面熔体包裹层厚度等抑制措施.     

Numerical investigation of heat transport and fluid flow during the seeding process of oxide Czochralski crystal growth Part 1: non‐rotating seed

For the seeding process of oxide Czochralski crystal growth, the flow and temperature field of the system as well as the seed‐melt interface shape have been studied numerically using the finite element method. The configuration usually used initially in a real Czochralski crystal growth process consists of a crucible, active afterheater, induction coil with two parts, insulation, melt, gas and non‐rotating seed crystal. At first the volumetric distribution of heat inside the metal crucible and afterheater inducted by the RF coil was calculated. Using this heat source the fluid flow and temperature field were determined in the whole system. We have considered two cases with respect to the seed position: (1) before and (2) after seed touch with the melt. It was observed that in the case of no seed rotation (ω_seed = 0), the flow pattern in the bulk melt consists of a single circulation of a slow moving fluid. In the gas domain, there are different types of flow motion related to different positions of the seed crystal. In the case of touched seed, the seed‐melt interface has a deep conic shape towards the melt. It was shown that an active afterheater and its location with respect to the crucible, influences markedly the temperature and flow field of the gas phase in the system and partly in the melt. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

双折射YVO4晶体原料的合成及最佳制备工艺的探讨

本文介绍了液相法合成用于双折射单晶生长的钒酸钇原料的工艺。着重讨论了制备条件对原料纯度的影响,确定了最佳合成方案。为了适应工业化生产的需要,探讨了原料合成的规范化(以保证保纯性,均匀性,重复性),合成出的原料已成功生长出φ42×42mm的大尺寸优质钒酸钇单晶,且剩料可重复使用10次左右。     

Simulation of temperature and flow fields in an inductively heated melt growth system

The goal of the research presented here is to apply a global analysis of an inductively heated Czochralski furnace for a real sapphire crystal growth system and predict the characteristics of the temperature and flow fields in the system. To do it, for the beginning stage of a sapphire growth process, influence of melt and gas convection combined with radiative heat transfer on the temperature field of the system and the crystal‐melt interface have been studied numerically using the steady state two‐dimensional finite element method. For radiative heat transfer, internal radiation through the grown crystal and surface to surface radiation for the exposed surfaces have been taken into account. The numerical results demonstrate that there are a powerful vortex which arises from the natural convection in the melt and a strong and large vortex that flows upwards along the afterheater side wall and downwards along the seed and crystal sides in the gas part. In addition, a wavy shape has been observed for the crystal‐melt interface with a deflection towards the melt. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

有机分光晶体季戊四醇的生长研究

本文采用多次重结晶的方法提纯季戊四醇(PET)原料,用高效液相色谱进行分析研究.通过目测法和吊籽晶法,测定了PET生长的亚稳区宽度.研究了溶液的pH值、过热时间和过热温度等因素对溶液亚稳区和诱导期的影响.采用紫外-可见光谱、红外光谱研究了长时间高温下溶液被氧化的特性.用溶液降温法在2L的生长槽中生长出30 nm×30 mm× 30 mm的PET单晶体.     

泡生法生长大尺寸蓝宝石单晶的等径控制方法

在泡生法生长大尺寸蓝宝石单晶的过程中,为了获得高质量的晶体,精确等径控制至关重要.本文根据晶体的重量变化率来控制热场,实现晶体等径生长.设计了应用在线整定多项式权值的广义最小方差(OAPW_GMV)控制方法,并建立了系统模型.该方法的主要思想是根据在线估计的被控对象参数及OAPW_GMV的输出,调整多项式的权值,实现炉内的热场控制.仿真和实验结果表明该控制方法实现了蓝宝石单晶的精确等径控制,有效地提高了蓝宝石单晶的质量.     

The role of inner and internal radiation on the melt growth of sapphire crystal

In this paper, for an inductively heated Czochralski furnace used to grow sapphire single crystal, influence of the inner (wall‐to‐wall) and crystal internal (bulk) radiation on the characteristics of the growth process such as temperature and flow fields, structure of heat transfer and crystal‐melt interface has been studied numerically using the 2D quasi‐steady state finite element method. The obtained results of global analysis demonstrate a strong dependence of thermal field, heat transport structure and crystal‐melt interface on both types of radiative heat transfer within the growth furnace.     

Influence of the crucible bottom shape on the heat transport and fluid flow during the seeding process of oxide Czochralski crystal growth

For the seeding process of oxide Czochralski crystal growth, influence of the crucible bottom shape on the heat generation, temperature and flow field of the system and the seed‐melt interface shape have been studied numerically using the finite element method. The configuration usually used in a real Czochralski crystal growth process consists of a crucible, active afterheater, induction coil with two parts, insulation, melt, gas and seed crystal. At first, the volumetric distribution of heat inside the metal crucible and afterheater inducted by the RF‐coil was calculated. Using this heat generation in the crucible wall as a source the fluid flow and temperature field of the entire system as well as the seed‐melt interface shape were determined. We have considered two cases, flat and rounded crucible bottom shape. It was observed that using a crucible with a rounded bottom has several advantages such as: (i) The position of the heat generation maximum at the crucible side wall moves upwards, compared to the flat bottom shape. (ii) The location of the temperature maximum at the crucible side wall rises and as a result the temperature gradient along the melt surface increases. (iii) The streamlines of the melt flow are parallel to the crucible bottom and have a curved shape which is similar to the rounded bottom shape. These important features lead to increasing thermal convection in the system and influence the velocity field in the melt and gas domain which help preventing some serious growth problems such as spiral growth. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)