碘化钾单晶的非真空密闭坩埚下降法生长

本文报道了KI单晶在非真空密闭条件下的坩埚下降法生长.以经充分干燥的高纯KI多晶为原料,将KI多晶料密封于套层铂坩埚中,添加少量活性碳粉末,可避免碘化物熔体的氧化与挥发,从而在非真空条件下实现KI单晶的坩埚下降法生长.在晶体生长过程中,炉体温度调节于750～770 ℃,固液界面温度梯度为30～40 ℃/cm,坩埚下降速率控制为1～2 mm/h,成功生长出尺寸为φ25 mm×50 mm的透明完整KI单晶.采用XRD、DTA-TG、透射光谱、荧光光谱对所获KI单晶进行了测试表征,结果表明该单晶具有良好的光学均匀性,在450～2500 nm波长范围的光学透过率达70;以上,其光学吸收边位于280 nm左右;在266 nm脉冲光激发下,该单晶具有397 nm峰值波长的荧光发射.     

Effect of axial vibration on Bi12SiO20 crystal growth by vertical Bridgman technique

Bi₁₂SiO₂₀ single crystals have been grown successfully by vertical Bridgman technique. During the crystal growth process, different axial vibration amplitudes of 50 μm, 70 μm and 100 μm were applied with the same vibration frequency of 50 Hz. The effect of different axial vibration amplitudes on quality of the as‐grown Bi₁₂SiO₂₀ single crystals was discussed. The crystals have been characterized by X‐ray rocking curve optical and absorption spectrum. The experimental results reveal that the axial vibration amplitude has a pronounced effect on quality of the as‐grown Bi₁₂SiO₂₀ single crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Cr3+‐doped LiNbO3 crystals grown by the Bridgman method

The growth of LiNbO₃ crystals doped with Cr³⁺ ions in 0.1, 0.2, and 0.5 mol % concentrations by Bridgman method were reported. The Cr³⁺ ion concentrations in crystals were measured by inductively coupled plasma spectrometry. Electron paramagnetic resonance had been used to investigate the sites occupied by the Cr³⁺ ions. Two Cr³⁺ ion centers located at Li⁺ and Nb⁵⁺ sites (Cr_Li³⁺ and Cr_Nb³⁺ centers, respectively) were observed. Optical absorption and temperature‐dependence emission spectra of the Cr³⁺ ions were reported. The crystal‐field parameters and Racah parameters of the Cr³⁺ ion defect sites were reported and compared with those grown by Czochralski technique. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

助熔剂坩埚下降法生长近化学计量比Co:LiNbO3晶体

以K2O为助熔剂,在较大的温度梯度(90～100℃/cm)条件下进行引种和晶体生长,应用坩埚下降法成功地生长出了初始CO2+掺杂浓度为0.5mol;的近化学计量比的铌酸锂晶体.测定了该晶体的红外光谱与吸收光谱,与同成份的LiNbO3晶体相比,其紫外吸收边向短波方向移动,OH-红外吸收峰的位置发生变化.观测到520,549,612nm三个分裂的尖吸收峰以及1400nm左右为发光中心的吸收带.从吸收特性可以判断,Co离子在铌酸锂晶体中呈现+2价.比较上部与下部晶体的吸收强度,可以推测出沿着晶体生长方向Co2+离子浓度逐渐降低,Co2+离子在晶体中有效的分凝系数大于1.     

Vertical Bridgman Growth and Scintillation Properties of Doped Bi4Si3O12 Crystals

Pure BSO and Ce, Nd, Eu, Cr and Fe doped BSO crystals of high optical quality with 20x20x100mm³ have been grown by the vertical Bridgman method. After measuring their transmission spectra, light outputs, FWHM energy resolutions and excitation-emission spectra, we summarized and explained the laws of doped effects on the scintillation characteristics. we can expect that Eu may be the most promising dopant candidate of the doped elements for improving the scintillation characteristics of BSO crystal.     

Three-dimensional thermocapillary and buoyancy convections and interface shape in horizontal Bridgman crystal growth

Computer simulation is conducted to study three-dimensional (3D) thermocapillary and buoyancy convections and their effects on the growth interface for horizontal Bridgman crystal growth. The free-boundary model is based on a finite volume approximation of continuity, momentum, and energy equations on a collocated grid. Crystal growth of GaAs is used as an example. From calculated results, it is observed that the effect of buoyancy convection on the growth interface is significant. With the thermocapillary effect, the 3D flow structures are not changed much, but its effect on the growth interface is not trivial. Due to the convections, the growth interface is always concave, and its deflection is affected significantly by the growth rate and thermal environment. A simple strategy of interface control is illustrated. Furthermore, slight crucible tilting can also affect the 3D flows leading to an asymmetric growth interface.     

LiNbO3晶体的坩埚下降法生长

通过选择合适的原料配比(Li2O 48.6mol;,Nb2O5 51.4mol;),控制固液界面处的温度梯度为20～40℃/cm,晶体生长速度为0.6～1.5mm/h,采用密闭条件下的坩埚下降法工艺成功地生长出了具有良好光学均匀性的完整LiNbO3单晶.用X射线粉末衍射表征获得的LiNbO3晶相,讨论了若干工艺条件对晶体组分与质量的影响.测定了未密闭条件下生长的LiNbO3晶体不同部位样品的紫外可见光谱,发现其吸收边沿生长方向发生红移,并讨论了产生此现象的原因.     

Bridgman法晶体生长的瞬态数值模拟

采用变形有限元法对坩埚下降法晶体生长过程进行了瞬态数值模拟.对随下降距离生长位置、生长速度、界面位置处的法线方向温度梯度和凹度的变化进行了分析说明,将生长过程划分为三个阶段.结果表明在整个生长过程中,晶体生长条件一直处于变化之中,因而晶体的质量也在整块晶体中呈现一定的波动性.     

Bridgman growth and properties of potassium lithium niobate single crystals

Transparent KLN crystals 10mm in diameter and 25 to 45mm in length have been grown by the modified vertical Bridgman technique from different melts in the range of 3035mol% K₂O, 1723mol% Li₂O and 4350mol% Nb₂O₅. The growth conditions are a growth rate of less than 0.25 mm/hr, temperature gradient in solid-liquid interface of 23 °C/mm and growth direction of <110>. As-grown KLN crystals have tetragonal tungsten bronze structure. Most of the as-grown crystals do not crack when cooling through the paraelectric/ferroelectric phase transition. 180° domain structures are observed after the KLN crystal was etched in boiling 2HNO₃:Hf. Dielectric properties and transmission spectrum of the as-grown KLN crystals are measured.     

Bridgman法生长TeO2晶体的缺陷分析

采用Bridgman法生长了二氧化碲(TeO2)晶体,运用光学显微镜、电子衍射光谱、化学腐蚀等方法分析了该方法生长TeO2晶体内部的缺陷.初步讨论了散射点、微裂纹、气泡和黑点、条纹以及腐蚀坑等微缺陷的形成机理.结果表明:晶体内部的散射点来自于原料中杂质,条纹主要是由于晶体内应力引起,晶体内的气泡和黑点和晶体生长的温度密切相关,并就如何减少这些微缺陷进行了初步探讨.     

Bridgman法晶体生长的热物性各向同性坩埚的选择

本文对不同坩埚热物性组合时计算得到的结果进行了比较.对各向同性坩埚而言,应该优先选择具有与晶体和熔体的导热系数相当导热系数的材料,也可选择导热系数较大的材料.在强度允许的情况下,减小坩埚壁厚对晶体生长有利.     

Optical properties of Sr3TaGa3Si2O14 single crystal

The specific rotation ρ of strontium tantalum gallium silicate Sr₃TaGa₃Si₂O₁₄ (STGS) piezoelectric single crystal was determined from 350 to 850 nm by measuring the optical transmission between parallel polarisers in Z direction. It is shown that Sr₃TaGa₃Si₂O₁₄ has quite large a value of ρ which is a little smaller than that of strontium niobium gallium silicate Sr₃NbGa₃Si₂O₁₄ (SNGS). The crystal with ordered structure which is isostructural to calcium gallium germanate Ca₃Ga₂Ge₄O₁₄ (CGG) was grown by Czochraiski technique. And its birefringence was also determined. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Study on phase diagram of Bi2O3---SiO2 system for Bridgman growth of Bi4Si3O12 single crystal

Phase relation of Bi₂O₃---SiO₂ system was evaluated experimentally from DTA and XRD measurements and its stable and metastable phase diagrams were proposed. Although BSO melts near-congruently at 1025°C in the stable phase equilibrium, its melt crystallizes to form metastable phase Bi₂SiO₅ in accordance with the metastable phase diagram while cooling. Therefore, BSO couldn't nucleate and crystallize spontaneously without crystal seed and only Bi₂SiO₅ crystallized at about 850°C with significant supercooling during Bridgman growth. BSO single crystal with 20×20×100mm³ was grown in a vertical Bridgman furnace with a BSO seed according to its phase diagram. The measuring results of scintillation properties of BSO specimen show that its decay constant is 91 ns (about 1/3 of BGO) and light output is 23% of BGO.     

Growth and characterization of organic material 4-nitrobenzaldehyde single crystal using modified vertical Bridgman technique

The organic material 4-nitrobenzaldehyde single crystal has been grown using the single wall ampoule with nano-translation by modified vertical Bridgman technique. The grown crystal was confirmed by single and powder X-ray diffraction (XRD). Fourier transform infrared (FTIR) analysis was used to identify the functional groups present in the grown crystal. The optical property of the grown crystal was analyzed by UV–vis–NIR and photoluminescence (PL) spectral measurements. The thermal characteristics of the grown crystal were analyzed by thermogravimetric (TG) and differential thermal analyses (DTA). The dielectric measurements were carried out with four different frequencies and the results indicate an increase in dielectric and conductivity parameters with the increase of temperature at all frequencies. The microhardness measurements were used to analyze the mechanical property of the grown crystal.     

Growth and characterization of near stoichiometric LiNbO3 single crystal

A near stoichiometric LiNbO₃ single crystal has been grown by the Czochralski method from a 58.5% Li melt hold in a large platinum crucible. High resolution X‐ray rocking curves of 30 0 and 0006 reflections indicated that the near stoichiometric LiNbO₃ crystal possesses the high structural quality. Compared with the congruent LiNbO₃, the near stoichiometric LiNbO₃ possesses shorter ultraviolet absorption edge, thus higher Li concentration. The OH^– infrared absorption band analyses showed that the Li concentration in the near stoichiometric LiNbO₃ crystal is higher than that in the congruent LiNbO₃ crystal. This result is in good agreement with that of the ultraviolet absorption edge. The electro‐optic (EO) coefficient γ₂₂ of the near stoichiometric LiNbO₃ crystal was measured to be 6.75 pm/V higher than that of congruent LiNbO₃ crystal. It also proves the near stoichiometric LiNbO₃ electro‐optic Q‐switched requires a low driving voltage and it is advantageous for the device performance. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

KMgF3晶体的生长研究

本文采用Bridgman方法生长了KMgF3单晶.晶体生长参数:在1130℃、1.5×105Pa Ar气氛条件下,以4.5mm/h的速度下降,下降结束后,以1.5℃/min的降温速度降温到室温,获得了直径10mm,长40mm 的单晶,测定了所获单晶的X射线粉末衍射图谱,讨论了真空条件与惰性气氛条件以及氧含量的控制对晶体生长的影响.     

垂直布里奇曼法生长铜单晶体的研究

Cu单晶在中子和X射线单色器及激光核聚变靶材等领域有重要应用前景.本文采用自制的硅钼棒单晶生长炉和特制的镀碳石英生长坩埚,采用垂直布里奇曼法在30 ℃/cm的温度梯度下,以10 mm/d的下降速度生长出较高质量的铜单晶体.生长的晶体经多次研磨抛光腐蚀处理后进行X射线衍射分析和金相分析,显示出(200)晶面尖锐的X射线衍射峰和规则的方形蚀坑,表明生长的晶体结构完整.     

Bridgman growth of langasite‐type piezoelectric crystals

Three langasite family crystals of Sr₃Ga₂Ge₄O₁₄ (SGG), Ca₃NbGa₃Si₂O₁₄ (CNGS), and Sr₃NbGa₃Si₂O₁₄ (SNGS) were successfully grown by the modified Bridgman method. Among them, SGG crystals up to 2 inches were obtained with the multi‐crucible industrial Bridgman furnace; SNGS crystal grown in any orientation direction other than along a‐axis was realized. Commercially availability SGG boules and the advantage in SNGS crystal indicated that the modified Bridgman technique is a prospective method to realize the mass‐production of the langasite‐type crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

四方晶系晶体的Bridgman法生长的稳态数值模拟

本文对四方晶系晶体的Bridgman法生长进行了稳态数值模拟.当熔体的导热系数位于晶体横向导热系数和纵向导热系数中间的一小段时,将产生"W"形固液界面.通过比较,指出不同导热系数组合时晶体生长的难易.当熔体的导热系数位于晶体横向导热系数和纵向导热系数中间的一小段时,界面平坦,容易长出较好质量的晶体.对中、低级晶系的生长,晶体横向导热系数应大于纵向导热系数.     

VB法生长低位错GaAs单晶

用于激光二极管(LD)和发光二极管(LED)的GaAs晶片,要求其具有低的位错密度(EPD).为了获得低位错密度的GaAs晶片,必须先得到低位错密度的体单晶.我们采用垂直布里奇曼(VB)法分别得到了2英寸和3英寸的GaAs单晶,单晶长度可达10cm,平均位错密度5000cm-2.通过改变加热器结构,改善轴向和径向的温度梯度,优化了生长时的固液界面,得到的单晶长度达20cm,平均位错密度为500cm-2,最大位错密度小于5000cm-2.