Centrifugal separation of primary silicon crystal in solvent refining of silicon using Al‐30% Si alloy

This study describes the formation of a primary silicon network during separation of an Al‐30% Si melt and the process conditions to make bigger primary silicon crystals. As the crucible rotates in the centrifugal separation, the unfrozen aluminum‐rich phase and small silicon particles are pushed outside through the openings in the silicon network. As a result, primary silicon crystals are separated in the form of a foam after centrifugation. The recovery of the silicon ranged from 13 to 18% depending on the location in the crucible. The size of the primary silicon achieved by changing the cooling rate and quenching temperature during solidification is also measured using a quenching furnace. Primary silicon particles exhibit a coarse, plate‐like morphology, although small star‐like silicon particles are also found in the aluminum‐rich matrix. The fraction of plate silicon decreases, while the fraction of small globular silicon increases with an increasing cooling rate. The thickness of the primary silicon plate also decreases with an increasing cooling rate in the samples quenched at various temperatures during solidification.     

Cooler for obtaining crystals

A modular air‐cooled tube, with a series of movable Tamman test tubes or plugs (modular unilateral and bilateral “crystallization comb”), installed in a laboratory tube furnace is presented. The setup allows easy regulation and simultaneous crystallization tests of a series of different crystallization parameters in crucible columns, enabling rapid acquisition of crystals. The relationship between the crystallization parameters has been given and numerically analyzed. This method can also be applied in crucible and chamber furnaces. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization rate control for alkali halide crystal growth by the VGF technique with a skull layer

This study describes the ability to use the melt‐level control for stabilization of the crystallization rate during NaI crystal growth by the VGF technique with a skull layer. It is shown that a conventional linear decrease of the heater temperature leads to a nonuniform crystallization rate and deterioration of crystal quality. A method and algorithm of temperature control for the stabilization of the crystallization rate during crystal growth is proposed. The series of growth experiments with NaI(Tl) crystals proved the efficiency of this approach and ability to obtain scintillators with high registration efficiency, about 6.3% energy resolution for a ¹³⁷Cs (662 keV) source.     

System of Mathematical Models for the Analysis of Industrial FZ-Si-Crystal Growth Processes

A system of coupled mathematical models and the corresponding program package is developed to study the interface shape, heat transfer, thermal stresses, fluid flow as well as the transient dopant segregation in the floating zone (FZ) growth of large silicon crystals (diameter more than 100mm) grown by the needle-eye technique. The floating zone method with needle-eye technique is used to produce high-purity silicon single crystals for semiconductor devices to overcome the problems resulting from the use of crucibles. The high frequency electric current induced by the pancake induction coil, the temperature gradients and the feed/crystal rotation determine the free surface shape of the molten zone and cause the fluid motion. The quality of the growing crystal depends on the shape of the growth interface, the temperature gradients and corresponding thermal stresses in the single crystal, the fluid flow, and especially on the dopant segregation near the growth interface. From the calculated transient dopant concentration fields in the molten zone the macroscopic and microscopic resistivity distribution in the single crystal is derived. The numerical results of the resistivity distributions are compared with the resistivity distributions measured in the grown crystal.     

Capsule‐like α‐Fe2O3 nanoparticles: Synthesis,characterization, and growth mechanism

Uniform capsule‐like α‐Fe₂O₃ particles were synthesized via a simple hydrothermal method, employing FeCl₃ and CH₃COONa as the precursors and sodium dodecyl sulfate (SDS) as soft template. X‐ray powder diffraction (XRD), field emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), and high‐resolution transmission electron microscopy were used to characterize the structure of synthesized products. Some factors influencing the formation of capsule‐like α‐Fe₂O₃ particles were systematically investigated, including different kinds of surfactants, the concentration of SDS, and reaction times. The investigation on the evolution formation reveals that SDS was critical to control the morphology of final products, and a possible five‐step growth mechanism was presented by tracking the structures of the products at different reaction stages.     

Addition to the theory of LPE growth: Crystallization mechanisms

Different possible mechanisms of crystal growth for the used in the practice LPE techniques are considered in the present paper. The time dependences of the super saturation for the cases of normal growth mechanism and screw dislocations growth mechanism are presented. The values of the stationary super saturation, of the stationary growth rate and of the time constant for the transient growth process are obtained. The effect of the initial super saturation on the growth rate is considered. Relation between the stationary value of the super saturation, the time constant of the transient process, the cooling rate and the liquidus surface slope has been ascertained. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

半导体单晶生长过程中的位错研究

阐述了现有的半导体单晶位错模型,即临界切应力模型和粘塑性模型的基本理论及应用状况.分析了熔体法单晶生长过程中影响位错产生、增殖的各种因素,以及抑制位错增殖的措施.与熔体不润湿、与晶体热膨胀系数相近的坩埚材料,低位错密度的籽晶可有效地抑制生长晶体的位错密度;固液界面的形状及晶体内的温度梯度是降低位错密度的关键控制因素,而两因素又受到炉膛温度梯度、长晶速率、气体和熔体对流等晶体生长工艺参数的影响.最后,对熔体单晶生长过程的位错研究进行了展望.     

Controllable fabrication and growth mechanism of hematite cubes

Monodispersed and single‐crystalline hematite (α‐Fe₂O₃) cubes have been successfully prepared by a template‐free hydrothermal synthetic route with FeCl₃ and CH₃COONH₄. The influences of the reactant concentration, reaction temperature, and reaction time on the crystal growth were systematically investigated. The results show that the monodisperse hematite cubes with high crystalline and narrow size distribution could be fabricated at the hydrothermal temperature of 160 °C for 24 h while the concentrations of FeCl₃ and CH₃COONH₄ were in the range of 0.03‐0.5 M and 0.05‐0.1 M, respectively. In addition, the formation mechanism of hematite cube is also proposed, where the CH₃COONH₄ plays a role of shape controller in the formation of cube hematite structure. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A method to model the transient performance of high frequency vibration in crystal growth

A general method to quantitatively study the transient fluctuation related to the high frequency vibration in crystal growth is developed. An example during the Czochralski crystal growth has been simulated, and the simulation coincides with the experimental date. On basis of the model, the influence of vibration frequency on the transient fluctuations for temperature and velocity are elucidated. Then an available approach to control the vibration effect is proposed.     

药物结晶中的经典与非经典结晶路径

晶体的结晶路径分为经典结晶路径和非经典结晶路径。经典结晶路径往往涉及一些简单的化学结构,晶体的成核、生长是通过单体的依次添加实现的,经过长期研究,目前研究人员已对其有了较为深刻的理解并形成了一套相对完善的理论体系;但对于非经典的结晶路径,由于涉及复杂中间态粒子的形成和多步结晶过程,尚未获得全面、统一的理论支持。在药物结晶领域,有机分子构象自由度的引入增加了体系的复杂性,分子间弱的相互作用使得固态药物分子存在多晶型现象。由于药物的理化性质及生物利用度与其晶型息息相关,同时,药物结晶过程中出现的一些复杂中间态粒子往往会改变最终得到的药物晶型,因此迫切需要加强对药物晶体成核和生长路径的研究,以期发展能实现对药物晶体成核和生长过程主动控制的方法。本文简要综述了目前药物在溶液或熔体中结晶的经典与非经典结晶路径,包括奥斯特瓦尔德阶段定律、独立成核、交叉成核。从溶液化学的角度看,分子在浓溶液中会通过自组装形成结构合成子,成核与溶液中的生长单元、结构合成子密切相关。从分子水平上探索溶液中有关分子运动的信息、分析各体系下晶核与结构合成子之间的关系是区分两种结晶路径的关键所在,非经典结晶在药物结晶领域是机遇也是挑战。     

Crystallization and optical properties of CaWO4 and SrWO4

Single crystals of calcium tungstate and strontium tungstate have been grown by double decomposition flux reaction technique using lithium chloride as flux. Growth conditions are optimized to synthesize well faceted crystals. Effect of primary and secondary flux density in the growth charge has been studied. Thermogravimetric study reveals that the grown crystals are highly stable in the temperature range 25 – 1000°C. Analysis of optical absorption normal to the ab‐plane in the spectral range of 200 – 800 nm reveals the true absorption edge, the nature of transition being the allowed indirect one at 4.60 eV and 4.56 eV respectively for CaWO₄ and SrWO₄. The crystals have been characterized by determining useful pertinent optical and dielectric parameters. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of 4‐(2‐hydroxyphenylamino)‐pent‐3‐en‐2‐one single crystals

4‐(2‐hydroxyphenylamino)‐pent‐3‐en‐2‐one (HPAP) was synthesized and single crystals were grown by the solution growth technique using methanol as a solvent. The crystals having orthorhombic symmetry were characterized by single crystal XRD, FTIR spectroscopy, NMR spectroscopy, TGA, DSC and dielectric studies. Very less variation in the value of dielectric constant is found for different frequencies of applied field. The crystals were exhibiting positive photoconductivity and poor NLO responses. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization kinetics of the borax decahydrate

The growth and dissolution rates of borax decahydrate have been measured as a function of supersaturation for various particle sizes at different temperature ranges of 13 and 50 °C in a laboratory-scale fluidized bed crystallizer. The values of mass transfer coefficient, K, reaction rate constant, k_r and reaction rate order, r were determined. The relative importances of diffusion and integration resistance were described by new terms named integration and diffusion concentration fraction. It was found that the overall growth rate of borax decahydrate is mainly controlled by integration (reaction) steps. It was also estimated that the dissolution region of borax decahydrate, apart from other materials, is controlled by diffusion and surface reaction. Increasing the temperature and particle size cause an increase in the values of kinetic parameters (K_g, k_r and K). The activation energies of overall, reaction and mass transfer steps were determined as 18.07, 18.79 and 8.26 kJmol⁻¹, respectively.     

基于水合碳酸镁结晶过程的化学键分析

基于晶体学结构,将化学键理论定量地应用到水合碳酸镁Mg5(CO3)4(OH)2·4H2O和MgOgO3·3H2O的结晶行为研究中,以此指导和控制实际晶体的生长行为.根据所选晶面的化学键数目和强度,可以计算出该晶面的垂直生长速率,从而方便地预测出Mg5(CO3)4(OH)2·4H2O和MMgO3·3H2O晶体的理想形貌.Mg5(CO3)4(OH)2·4H2O晶体表现出六方片状的结晶习性,MgCO3·3H2O则具有六方柱的理想形貌.在实验中,六方片状的Mg5(CO3)4(OH)2-114心O和MgO3·3H2O六方柱可以通过简单的液相反应获得,证明我们的理论计算与实验结果完全相符.目前研究结果表明,单晶生长可以通过热力学意义上调整组成原子或离子的成键方式获得本质上的改进,这一过程为我们从动力学角度优化实验策略提供了更广阔的空间.     

Crystal growth of barium aluminum (gallium) borates

Crystals listed in the JCPDS card in the BaO‐B₂O₃‐Al₂O₃ and BaO‐B₂O₃‐Ga₂O₃ systems are of interest from a viewpoint of the Second Harmonic Generation (SHG). Ba₅Al₄B₁₂O₂₉ and Ba₅Ga₄B₁₂O₂₉ are promising new crystals with SHG activity and with congruent melting mode. These crystals can be grown by the Czochralski method with a size of 3 × 3 × 0.1‐1mm. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

BGO熔体急冷自发结晶形貌

本文研究了BGO熔体在急冷的条件下自发结晶的显露形貌.在急冷的条件下,组成BGO的各个面族自由发育.{321}面族、{211}面族和{111}面族都是按[GeO4]4-四面体以顶角相连的化学键链生长发育的,生长速度快,优先显露,在熔体急冷时保留下来.表面形貌显露不完整的{100}面族是[GeO4]4-四面体以棱相连所对应的面族,生长速度较慢,尚未显露完全熔体就已冷却.从生长速度考虑,在实际生长晶体时以[321]、[211]、[111]方向生长可以获得较快的速度.     

Effect of the seed crystallographic orientation on AlN bulk crystal growth by PVT method

The growth of AlN crystals by PVT method was investigated using TaC crucible in the temperature range of 2250‐2350 °C. AlN boules with 30 mm in diameter were successfully grown on the crucible lid by self‐seeded growth. The AlN boules consist of the spontaneously nucleated AlN single crystal grains with the {1010} natural crystalline face. The fast growth rate of more than 1 mm/h was achieved. AlN crystals grown on (11 0)‐, (10 0)‐, and (0001)‐face AlN seeds were investigated. Different experimental phenomena have been observed under particular condition. The crystal grown on (11 0)‐face seed has different natural crystalline face from the seed. For the crystal grown on (10 0) or (0001) seed, the crystal natural crystalline face is same as the crystallographic orientation of the seed. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

熔体法生长大尺寸有机晶体

大尺寸有机晶体在太赫兹波产生、中子探测、微波激射等多个关系国计民生、涉及国家安全的领域具有重要应用前景.但大尺寸有机单晶生长一直是国际公认的难题,无论是在生长理论、生长方法还是生长设备方面都远远落后,在整个人工晶体领域相对小众;而且有机晶体硬度低、脆性高、易解理等本征特性为加工和后期应用带来了很多困难,制约了相关领域的...     

溶液法生长氘化磷酸二氢铵(DADP)晶体及其性能研究

使用优级纯的NH4H2PO4(含量＞99.5;)和重水(纯度＞99.5;)为原料,在重水中经过三次氘化重结晶,获得含氘量＞95;的结晶原料.上述DADP晶体作为原料配成1000ml的饱和溶液,用降温转动法生长出22mm×23mm×78mm尺寸的透明大晶体,并且测定其晶体结构、透过光谱和激光损伤阈值.从数据分析来看在最重要的光谱应用波段(1.06μm附近)DADP晶体综合性能是很优越的,这使得DADP有利于作为电光晶体材料和制作高频高灵敏度的电光器件.     

核辐射探测单晶生长方法研究进展

核辐射探测是指用各种核辐射探测器来得到核辐射信息的过程,在军用、民用和科研等领域具有广泛的应用。作为核辐射探测核心的核辐射探测器,主要分为气体探测器、闪烁体探测器和半导体探测器。相比于气体探测器,闪烁体探测器和半导体探测器都需要晶体作为核心材料,晶体质量的品质在很大程度上决定了探测器性能的上限。为了获得性能更好的探测器,人们对探测器用单晶材料的生长方法进行了大量的研究。本文综述了近几年核辐射探测单晶生长方法研究的最新进展,总结了目前主流的晶体生长方法,包括溶液法、熔体法、气相法等,并对不同晶体的主要生长方法进行了归纳。