Crystal Growth of Lead (II) Iodide from the Melt

Bulk Pbl₂ crystals up to 20 cm³ have been grown from high purity source material in a controlled way using a modified Bridgman-Stockbarger technique. The cleavage plane (0001) of crystals grown by a natural seed selection in a tipped-end ampoule is nearly parallel to its axis. On a mica substrate epitaxially grown crystals cleaved perpendicularly to the axis of a specially designed double wall ampoule.     

二苯甲酮晶体的过冷熔体生长及性能

本文采用过冷熔体法进行二苯甲酮晶体的生长实验,得到尺寸约为30mm×40mm×60mm的单晶.测定了单晶的光谱透射率、折射率及SHG系数,并与溶液法生长的结果进行比较,发现过冷熔体法生长的二苯甲酮单晶在近紫外到近红外波段具有更为优异的光学特性,适合用作YAG激光倍频晶体,也可用作黄绿波段激光调制器.     

Determination of Physical Constants of the Melt and the Parameters of the Control Object Concerning Crystal Growth from the Melt

New Techniques are presented for the determination of the capillary constant and the coefficient of thermal expansion of the melt using an electrocontact sensor (ECS). The density of the melt, the capillary constant, the coefficient of the thermal expansion of the melt, the growth angle, and the characteristic time of thermal relaxation of the thermal zone are determined for the case of growing the lithium niobate crystals by Czochalski technique.     

Mechanisms of Interaction of Molybdenum and Tungsten Polyoxide with Aluminum Oxide Melt under Reducing Conditions

The main chemical reactions between Mo and W polyoxides and Al₂O₃ melt in a controlled Ar + H₂ atmosphere (T = 2400 K, P = 1 bar) during sapphire growth by horizontal directional solidification have been investigated. Under these thermodynamic conditions, the melt and products of its dissociative evaporation may actively react with the tungsten heater and molybdenum thermal screens of the crystallization system. It is shown that the polyoxides formed during evaporation do not directly interact with the melt; this interaction occurs only with participation of reagents exhibiting pronounced reducing properties (Al, H₂, H, WO, Al₂O, AlH, AlH₂, AlH₃). It is established that most of processes occur with participation of aluminum hydrides. A particular role of Mo(W) dioxide–W(Mo) polyoxide functional pairs in the interaction with the melt is determined.

     

熔体分层对BaBiBO4晶体生长的影响

研究在用助熔剂法生长BaBiBO4晶体的过程中,熔体分层对晶体生长的影响.以Li2Mo3O10作为助熔剂,采用自发成核和顶部籽晶两种方法来生长晶体.对于这两种方法得到的晶体,用X射线粉末衍射及拉曼光谱进行了表征,结果显示,在晶体生长过程中,由于熔体分层,导致通过自发成核和顶部籽晶分别得到BaMoO4多晶和LiBaB9O15单晶两种不同的物相.     

Effect of Melt Convection on the Growth of Nd: YAG Crystal by the Czochralski Method

The effect of melt convection on the formation of constitutional supercooling defects was studied simply by changing the shape and size of the Ir crucible. The experimental results show that there is a favourable ratio of crucible diameter d to depth h, i.e. d/h is about 1, and a moderate range of the crystal rotating rate must be avoided to grow a quality Nd: YAG crystal.     

铝高温氧化过程中表面氧化物的有序转变及形貌观察

采用同步热分析(Simultaneous Thermal Analysis, STA)分析了Al在非高压空气下(压力0.2 MPa,流速20 NmL/min)的氧化过程.用X射线衍射(XRD)对铝粉颗粒表面生成的氧化物进行了物相分析并用扫描电镜(SEM)观察了表面形貌.研究结果表明,140 ℃铝开始氧化,300 ℃以上开始生成γ-Al2O3,一直持续至515 ℃左右.从666.1 ℃开始,表面生成氧化物的铝粉颗粒芯层中的铝熔融.从773 ℃开始,γ-Al2O3转变成α-Al2O3, 800 ℃,α-Al2O3开始生长,α-Al2O3的生长遵循Sigmoid(Boltzmann)模型.整个氧化过程,铝粉的氧化占主要地位,但也包括铝粉的氮化.XRD、SEM的分析结果表明,表面生成的AlN及α-Al2O3为纳米级,弥散分布于铝粉颗粒表面.     

大直径硅单晶生长过程中固/液界面形状及熔体流动的数值分析

数值模拟技术是提升大直径硅单晶质量、降低晶体制备成本的有效工具.利用切克劳斯基法生长硅单晶时,固/液界面的形变程度是衡量晶体质量的关键参数.由于单晶炉体内的高温环境导致对界面的直接观察极为困难,因此本文采用有限元法对生长16英寸直径硅单晶过程中,不同生长阶段的固/液界面形状及熔体流动情况进行计算.数值计算结果表明:在本文所用的热场及工艺参数条件下,随着晶体长度的不断增加,固/液界面的形变量增加同时晶体内部的热应力加大;通过对晶体提拉速率及晶体转速-坩埚转速的比值的调整,我们发现,降低晶体的提拉速率以及精确的控制转速比可以使晶体各个阶段都获得比较理想的界面形状.     

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.     

晶体生长时的固液相结构变化分析

晶体的溶解、熔化以及结晶成核生长时的固液相原子结构是怎样变化的,晶体生长时的生长基元是原子还是原子团.本文根据各种材料液相结构的最新研究结果,提出不饱和配位结构转换模式,并以此模式对各种常见晶体材料从溶解、熔化到结晶生长时的液态母相结构变化以及晶体成核过程进行了描述和分析,认为晶体生长时的界面结构和液相结构十分接近,溶解、熔化主要是晶体表面的不饱和配位原子(离子)转换到液相结构的过程,晶体生长主要是液相中的不饱和配位原子(离子)转换到固液生长界面的位错位置,使配位结构更饱和的过程.随着液相过饱和度的增大,液相结构单元的原子数越来越多,吸附到晶体生长界面若来不及转换回液相,就形成新的位错生长中心,形成晶体生长缺陷.     

Epitaxial Growth of Silver Bromide on Mica from the Melt

It is shown that it is possible to grow silver bromide crystals with definite crystallographic orientation by solidification of liquid silver bromide between mica and quartz plates by cooling the mica side. The orientation is (111). The maximum dimensions were 15mm × 15 mm × 1 mm. The surface is investigated by electron reflection (RHEED). The crystals have a smooth surface and can be used for optical application without surface reconstruction.     

The Growth of Some Aromatic Hydrocarbons Single Crystals from the Melt

The present work summarizes results concerning growth of anthracene, pyrene, p-terphenyl, carbazole, and phenanthrene single crystals by Bridgman method. The temperature conditions and rate of crystal growth as well as seeding conditions have been determined and discussed in the aspect of purity grade of considered materials.     

KDP晶体杂质对生长及出槽应力分布的影响

KDP晶体中的杂质易导致其开裂.本文采用有限元法分析了不同属性、尺寸、形状的晶体杂质对大尺寸KDP晶体生长及出槽应力分布的影响.结果表明,不同属性的杂质对晶体生长应力和出槽应力分布具有不同程度的影响.杂质附近的生长应力与杂质的弹性模量呈正向变化;杂质附近的出槽应力与杂质和晶体的热膨胀系数之差呈正向变化;杂质的尺寸越大,形状越尖锐,杂质附近的生长应力和出槽应力均增大.     

Crystal Growth from Silica Gels and Single Crystal Structure of Bariumchromate

Rhombic single crystals of bariumchromate were grown in silica gels up to 1.5 mm in size. The influence of the initial pH-value of the gel and the kind and concentration of reactants are studied. The crystal structure has been determined. The compound crystallizes in space group Pnma, with cell dimensions a = 9.113(4) Å, b = 5.528(3) Å, c = 7.336(4) Å and Z = 4. The structure was refined to R = 0.062 on the basis of 364 reflections. Every barium atome, centered in a distorted archimedian antiprism, is coordinated to 8 oxygen atoms each belonging to a chromate tetrahedron. Interatomic distances and bond angles were calculated.     

Crystal Growth of High‐melting Multi‐component Rare Earth‐Transition Metal Intermetallic Compounds from the Melt

The crystal growth of different classes of high melting multi‐component Rare Earth‐Transition Metal‐Compounds by vertical floating zone melting with inductive heating has been investigated. Phase diagram features of the multi‐component systems relevant for the crystallization process have been revealed. The critical zone travelling rate for RENi₂B₂C crystal growth is one order of magnitude smaller than for RE₂TMSi₃ compounds. This is attributed to different solidification modes of both classes of compounds, peritectic and congruent melting, respectively. The crystal perfection, element segregation and selected properties of the bulk crystals such as critical temperature of superconductivity were studied as function of the axis co‐ordinate. In the case of RE₂TMSi₂ plate‐like RESi or RESi₂ precipitates were detected in the single crystalline matrix. They were partially dissolved by annealing and subsequent quenching. The anisotropy of various superconducting and magnetic properties was determined at YNi₂B₂C and TbNi₂B₂C single crystalline specimens.     

固态材料形成过程中的晶体生长机理探讨

同样由熔体凝固、溶液沉淀或者气相沉积出来,为什么有的材料呈晶相,有的呈非晶相? 晶体生长是由自组装形成的还是由外界条件决定的?是哪项因素决定了晶体生长时原子的有序排列?本文根据实际现象,用晶体生长的热力学理论分析了逆向离子解离对晶体成核及生长的作用机理,并对固态材料的形成与晶体成核生长之间的关系也作了进一步的阐述和分析,由此得出结论认为,由化学键结合的材料在晶体生长时必须伴随着逆向离子解离平衡,正是固态材料形成过程中的逆向离子解离过程,如同时伴随着电离的溶解、熔化及升华过程,决定了晶体生长时原子的有序排列.     

直拉硅单晶中双空洞长大动力学的相场模拟

为了研究硅单晶直拉法生长过程中双空洞的长大动力学以及空洞间的相互作用机理,采用已建立的空洞演化的相场模型及其应用程序,模拟研究了直拉硅单晶生长过程中双空洞演化和相关因素的影响规律.结果表明:所建相场模型能够有效地模拟基体中空位扩散和双空洞长大的过程;双空洞长大趋势随着模拟时间和初始空位浓度的增强而加强;随着空洞初始中心间距的增加和初始空位浓度的减小,双空洞长大由相互融合模式转变为独立长大模式.     

On the Mechanism of Crystal Growth from Undercooled Melts

The mechanism of crystal growth from undercooled melts is studied experimentally by means of a simple capillary technique. Thymol and Na₂S₂O₃ · 5 H₂O are used as model substances. Dislocation-free crystal faces of these compounds are obtained by continuous growth in the capillary or by prolonged annealing under appropriate conditions. Two-dimensional mechanism of growth was experimentally verified on such perfect crystal planes. The conditions under which the surface nuclation mechanism operates are described accounting for the supersaturation, the influence of impurities etc. Transition from two-dimensional into spiral growth of purposedly defected crystal faces is demonstrated and investigated. The mechanism of formation of perfect crystals is discussed and further experimental evidence on the possibility of two-dimensional growth from melts is given.     

直拉单晶硅生长时空洞演化的相场模拟

为研究大直径直拉硅生长时空洞的演化规律,建立了与有限元模型所模拟的晶体生长温度场相结合的空洞演化相场模型,并应用该模型模拟研究了空洞形貌及其分布状态的变化过程以及不同初始点缺陷浓度对空洞演化的影响规律.结果表明:直拉硅单晶生长过程中,空洞的演化经历了孕育-形核-长大-稳定四个阶段,其形貌和分布状态亦由孤立的球形向偏聚的串珠形转变;与较低的点缺陷浓度相比,初始点缺陷浓度较高时,空洞的数目、平均尺寸、面积分数普遍较大,孕育阶段缩短、形核和长大阶段延长;空洞的偏聚及合并、长大的现象显著;当温度低于980 K时,大直径的空洞数目不再增加.