氟化钙晶体的生长与缺陷研究

采用真空坩埚下降法在石墨坩埚中生长了大尺寸CaF2晶体.通过高温氟化获得无水高纯原料,自发成核发育籽晶,以＜2mm/h的生长速率,成功生长了直径170mm的CaF2晶体.研究了晶体的顶部析晶形貌、包裹体、解理等生长缺陷.     

泡生法生长掺碳钛宝石激光晶体的研究

钛宝石激光晶体在现代高功率激光领域具有重要的应用价值, 但大尺寸、高品质的晶体生长仍是当前钛宝石应用面临的重大难题. 本文研究了泡生法技术生长大尺寸掺碳钛宝石激光晶体, 结果显示, 泡生法生长得到的直径180 mm、30 kg的钛宝石没有出现应力集中的开裂等宏观缺陷现象, 钛离子在晶体中分布均匀接近理论值, 晶体的FOM值达到200. 该研究对低红外残余吸收, 高品质因素、大尺寸钛宝石激光晶体的生长应用具有重要的现实意义.     

蓝宝石单晶的气孔形成研究

采用冷心放肩微量提拉法(SAPMAC法)生长的蓝宝石晶体, 气孔是其主要缺陷. 本文探讨了影响气孔形成的工艺因素, 从晶体生长动力学角度分析了气孔形成机理. 结果表明, 通过优化温场、选择合适的生长速度及控制微凸固/液界面形状, 可有效降低晶体中气孔的数量.     

Cd补偿垂直布里奇曼法生长Cd0.9Zn0.1Te晶体

采用传统垂直布里奇曼法和Cd补偿垂直布里奇曼法,分别生长出两根尺寸为 30mm×130mm的Ccd0.9Zn0.1Te晶锭.测试了晶体的结晶质量、成分分布、位错腐蚀坑密度(EPD)、红外透过率及电阻率.结果表明,Cd补偿垂直布里奇曼法生长的晶体结晶质量好、成分分布均匀、EPD低、红外透过性能好且电阻率高.这说明Cd补偿垂直布里奇曼法是一种生长高阻值CZT晶体的优良方法.     

大尺寸Y:PbWO4晶体的坩埚下降法生长与光学均匀性研究

报道了大尺寸Ｙ：ＰｂＷＯ_４晶体的坩埚下降法生长工艺,讨论了影响晶体生长的主要 因素．探讨了消除晶体开裂、抑制晶体组分过冷的工艺措施,成功地生长出无宏观缺陷的大尺 寸Ｙ：ＰｂＷＯ_４晶体,尺寸达５２ｍｉｎ×５２ｍｍ×２５０ｍｍ．同时,对实验样品沿晶体生长方向不同部 位的横向透过率及发射光谱进行了测试,结果表明,坩埚下降法生长的大尺寸Ｙ：ＰｂＷＯ_４晶体 具有较好的光学均匀性．     

氟化物激光晶体Cr:LiSAF的坩埚下降法生长

报道了氟化物激光晶体CrLiSAF的坩埚下降法生长工艺.采用经氟化处理的无水氟化物原料,按照LiFSrF2(AlF3+CrF3)=111的摩尔比配料,控制炉体温度于900～940℃,晶体生长速度为0.4～0.8mm/h,通过密闭条件下的坩埚下降法生长出大尺寸(φ25mm×85mm)的优质完整的CrLiSAF单晶.     

温度及温度梯度对SiC单晶生长的影响

利用升华法在高温低压下生长大直径SiC单晶.通过实验发现在相同的轴向温度梯度下,SiC晶体平均生长速率随籽晶温度的升高而变大.通过减小轴向温度梯度,降低晶体生长界面的径向过饱和度分布,可以抑制多型的生长.通过优化温场的径向温度梯度,利用φ50mm的籽晶进行生长,得到了φ57mm的SiC单晶,实现了晶体的扩径生长.     

大尺寸Y:PbWO4晶体的坩埚下降法生长与光学均匀性研究

报道了大尺寸Ｙ：ＰｂＷＯ４晶体的坩埚下降法生长工艺，讨论了影响晶体生长的主要 因素．探讨了消除晶体开裂、抑制晶体组分过冷的工艺措施，成功地生长出无宏观缺陷的大尺 寸Ｙ：ＰｂＷＯ４晶体，尺寸达５２ｍｉｎ×５２ｍｍ×２５０ｍｍ．同时，对实验样品沿晶体生长方向不同部 位的横向透过率及发射光谱进行了测试，结果表明，坩埚下降法生长的大尺寸Ｙ：ＰｂＷＯ４晶体 具有较好的光学均匀性．     

悬浮区域熔炼法制备REB6（LaB6、CeB6）单晶体及其表征

采用区域熔炼法成功制备出了高质量、高纯度、大尺寸的LaB6、CeB6单晶体。系统分析了制备过程中每个参数对晶体生长的影响,确定了晶体成长最佳工艺:(1)LaB6:转速为30r/min,生长速度为8～10mm/h,两次区熔;(2)CeB6:转速为30r/min,生长速度15～20mm/h,一次区熔。然后对晶体进行表征,主要方法有单晶衍射、断面扫描、拉曼衍射、摇摆曲线。由此可知悬浮区域熔炼法是制备高质量、高纯度、大尺寸REB6的最佳方法。     

移动加热器法晶体生长工艺的研究进展

移动加热器法被认为是一种切实可行的生长大尺寸、高质量单晶体的方法,它结合了液相外延和区熔提纯的优点.本文阐述了移动加热器法晶体生长的基本原理、优缺点,综述了相关加热方式、晶体生长过程中的质量输运和热交换,并探讨了工艺条件(如重力场、磁场、强迫对流等和晶体生长速率)对移动加热器法生长晶体过程与晶体质量的影响,最后对移动加热器法的发展趋势进行了展望.     

籽晶边长对SAPMAC法蓝宝石晶体放肩阶段生长质量的影响

温度场的控制是蓝宝石生长过程关键技术问题。采用有限元方法研究了冷心放肩微量提拉法蓝宝石单晶生长过程中籽晶的边长对晶体生长放肩阶段温度场内温度分布、流场分布和晶体的等效应力分布的影响。结果表明:当籽晶边长为24mm时,放肩阶段熔体的轴径向温度变化平缓,温度场内温度分布均匀,熔体的流动和晶体的热应力均适合晶体的生长。     

Preparation, quality characterization, service performance evaluation and its modification of sapphire crystal for optical window and dome application

Sapphire (i.e., Al₂O₃ single crystal) window and dome are important sensor components. Large-sized sapphire crystal was prepared by an improved Kyropoulos method, and its machining technique of ultrasonic vibration was also reported. The quality and structure were evaluated by illumination of a He–Ne laser transmission electron microscopy (TEM), double crystal X-ray diffraction (DCXRD) and Raman spectroscopy. For practical window and dome application, its high-temperature mechanical strength and optical transmission were both measured, and a modification measure of sputtering Mg film on sapphire surface followed by annealing and subsequent quenching was demonstrated. Large-sized sapphire crystals with high quality and different profiles were successfully grown by adjustment of pulling velocity and crucible size, design of suitable temperature field. Moreover, a series of sapphire windows and domes were fabricated for different optical application. The biaxial flexure strength of sapphire crystal decreases with increasing temperature, and the infrared transmission is also slightly degraded at high temperature. In addition, it should be noted that there is sharp strength drop in the temperature range of 400° to 600 °C which is related with twin formation in sapphire crystal. Submicron MgAl₂O₄ spinel precipitation can effectively harden sapphire crystal and do not induce large optical-scattering loss, which is a potential modification method for window and dome application of sapphire crystal.     

φ300mm的大直径直拉单晶硅勾形磁场下生长的数值模拟

直径300mm硅片的生产技术是当今硅材料生产研究的重要方向之一,而晶体生长 界面的形状、温度分布、晶体中氧的浓度和均匀性等对熔体流动状态十分敏感,采用实验的方 法来测量熔体的流动、温度场分布是很困难的,因此很难通过实验的方法获得熔体的流动是如 何影响晶体生长的质量的,而数值模拟能提供熔体流动、温度分布等详细内容,为单晶硅的生 长提供有利的指导.本文采用低雷诺数的K-ε紊流模型,对直径300mm的大直径单晶硅生 长进行了数值模拟,通过熔体在有、无勾形磁场作用时的流场、温度场的分析,阐明了勾形磁 场影响熔体流动的机理.     

Photoelastic lensing effect in Ti:sapphire crystal pumped by high-energy pulses

We have built a setup with high temporal resolution to measure the very fast photoelastic lensing effect, which is on the scale of microseconds in a Ti:sapphire crystal pumped by very strong laser pulses (up to 5 J/cm2). The experimental results measured by this method and the real multimode beam profile taken by a CCD camera are applied to a three-dimensional crystal model to calculate one of the photoelastic constants of Ti:sapphire crystal, which is found to be p31=-0.03±0.01. This value is helpful to evaluate the photoelastic lensing effect in Ti:sapphire crystal for a laser beam polarized along the c axis, commonly used for laser amplification.     

导模法生长蓝宝石单晶光纤的缺陷和光学特性研究

通过导模法(EFG)成功生长了蓝宝石单晶光纤(直径400~1000 μm, 长度500 mm)。光纤的横截面大致为圆形, 侧面无明显的小面, 直径变化小于40 μm。本研究对晶体缺陷, 例如微气泡, 包裹物和生长条纹等进行观察与分析, 得出: 大多数微气泡是球状的, 且存在于光纤的外侧缘; 在蓝宝石光纤外侧面也观察到少量的钼包裹物元素; 新模具在前几次使用中往往会产生更多的钼夹杂物, 在多次使用后降低。通过对熔体膜流体流动的实验和数值模拟, 研究蓝宝石光纤中微气泡尺寸和分布, 实验和数值模拟的结果显示出良好的一致性。微气泡的分布取决于熔体膜处的流体流动模式, 流体流动的涡流使微气泡在热毛细对流作用下移动到蓝宝石光纤外侧缘。633 nm处的吸收损耗为9 dB/m, 包裹物和表面不规则性会增加散射损耗。     

Determination of butanol distribution on salol-butanol crystals using Micro Raman Spectroscopy

We carried out several analytical studies in order to determine the butanol distribution on a salol-butanol crystal. This work is required for a research using microgravity condition focused upon the in-situ observation with an interferometer of the temperature and concentration field for the organic transparent crystal (salol-butanol). In order to evaluate the concentration field for the liquid phase with an interferometer in case of crystal growth from solution in space, it is significant to determine the distribution of solute (butanol) on starting crystal before sample launching using a non-destructive analytical method. The Micro Raman Spectroscopy (MRS) was choice as the most appropriate analytical method among several analytical methods. We prepared a salol-butanol crystal enclosed into the 1mm thick quartz glass ampoule in order to verify the propriety for MRS. Obtained Raman spectrums for salol, butanol and salolbutanol crystal show that the butanol 2D-distribution on salolbutanol crystal can be determined by MRS. These results also demonstrate that there are no influences of thick glass cell upon measurements and that 3D-measurement is possible. In conclusion, we argue that MRS is the most appropriate method for determination of the 2D- and/or 3D- distribution of solute on the crystal among several non-destructive analytical methods.     

Room temperature measurement of the anisotropic loss tangent of sapphire using the whispering gallery mode technique

The anisotropic loss tangent has been determined in monocrystalline sapphire for components parallel and perpendicular to the crystal axis, using the whispering gallery (WG) mode method. The Q-factors of quasi-TE and quasi-TM modes were measured precisely in four cylindrical sapphire resonators at room temperature, from which was determined a maximum attainable Q-factor of (2.1 +/- 0.2) x 10(5) at 9 GHz in a quasi-TM mode. Sapphire dielectric material from three different manufacturers was compared over the 270-345 K temperature range and the 5-16 GHz frequency range.     

一种垂直递变流速氢化物气相外延(HVPE)反应腔流场分析及大尺寸材料生长

以氮化镓(GaN)为代表的第三代半导体材料,是我国重要战略发展方向之一,而氢化物气相外延(HVPE)作为一种重要材料生长技术,是有效制备单晶材料的工艺手段,本文提出了一种分层次递变流速下HVPE流场与温度场,在垂直腔结构条件下,模拟从腔体中间区域到边缘区域不同流速层次条件下,腔内材料生长区域反应前驱物分布,得出结论:在边缘喷射区域流速为中心区域流速三倍时,反应前驱物可以有效分布在衬底托盘表面。最后,在蓝宝石衬底GaN籽晶表面进行HVPE材料生长,获得平均厚度为20.1μm,均匀性起伏6.9%的GaN单晶,证明理论优化设计下生长出良好的单晶薄膜材料。