快速生长大尺寸KDP单晶

用传统降温法生长了大尺寸KDP单晶,生长速度一般在1～2 mm/d,周期长,风险大.本文采用"点籽晶"快速生长法多次成功生长出了200 mm级的大尺寸KDP单晶,晶体生长速度达到20 mm/d,晶体生长正常.同时,摇摆曲线表明快速生长的晶体有着很好的结构完整性.     

新添加剂下KDP晶体快速生长及其性能表征

我们使用优级纯的KH2PO4和超纯水(电阻率≥18.2MΩ·cm)为原料,采用新的添加剂KCl(氯化钾)及EDTA钾盐,使生长溶液的稳定性得到提高,在5L生长槽内生长出51mm×54mm×40mm的KDP单晶,生长速度达到15～20mm/d,并检测了快速生长晶体的重要的应用性能,发现与高质量慢速生长晶体性能相当,可以达到使用要求.     

快速生长KDP晶体的光学性质研究

本文研究了快速生长的KDP晶体光学性质,结果表明快速生长的KDP晶体的光学性质低于传统降温法生长的晶体,原料中阴离子杂质的存在是造成这一结果的主要原因,确保快速生长晶体质量的首要条件是提高原料的纯度.     

添加剂下KDP晶体的快速生长

本文在测定KDP溶解度曲线及介稳区的基础上,通过添加几种硼酸盐类添加剂,并采用Z切点籽晶实现了KDP晶体的快速生长,[001]和[100]方向的生长速度可达10～15mm/d(5L生长槽).     

KDP晶体的点状籽晶法生长及其缺陷研究

研究了溶液Ph值对KDP晶体生长形态的影响,进行了晶体生长实验和参数对比.以提高溶液Ph值为主要手段在低过饱和度下进行KDP晶体点状生长.对点状法生长的晶体进行了缺陷分析,测定了晶体不同区域的金属离子含量并进行了对比分析.实验表明溶液Ph值对晶体各向的相对生长速度有显著的影响.在Ph=5.0、低过饱和度(σ＜0.02)条件下生长出50×50×50mm3的晶体.     

KDP类晶体快速生长技术研究

概述了本课题组在KDP类晶体快速生长领域的研究及进展情况。通过集成生长设备的管道系统、升级连续过滤系统、研发晶体生长过程的实时监控系统以及高精度退火设备,实现晶体生长系统的集成化;通过数值模拟优化晶体表面流场状态、全流程量化控制实现晶体稳定生长以及精密热退火进一步提升晶体性能;针对点籽晶快速生长KDP类晶体中存在的柱锥交界面问题,相继提出了长籽晶锥区限制生长法和长籽晶自由生长法,为大尺寸高性能KDP类晶体生长提供新的技术方案。     

HPVB法生长的CdSe单晶性能研究

采用有籽晶的高压垂直布里奇曼法(HPVB)生长了直径35 mm的大尺寸CdSe单晶.使用X射线衍射仪测试了晶体的结晶质量,结果表明生长的晶体为纯六方相CdSe单晶,(002)晶面的摇摆曲线峰型尖锐且对称性好,峰值半高宽(FWHM)可达0.082°.使用辉光放电质谱法(GDMS)、霍尔效应测试、傅里叶变换红外光谱仪(FTIR)对晶体生长轴向的微量杂质含量及分布、电学性能和光学性能进行测试和分析,结果表明微量杂质在晶体轴向方向呈现出不同的分凝特性,杂质的不均匀分布影响晶体的电学性能和光学性能.晶体呈现出较高的电阻率(108Ω· cm)和优良的红外透过性能,在8~12 μm范围内平均透过率约为70;,吸收系数小于0.058 cm-1.     

溶液降温法快速生长KDP晶体的新装置

利用溶液降温法分别在锥形底生长装置和传统晶体生长装置中进行了KDP晶体点状籽晶法快速生长实验,对KDP晶体的生长条件进行了对比,分析了不同生长装置对KDP溶液稳定性的影响,利用扫描电镜观察了KDP晶体中的包裹体,测定了晶体的透过率,对比分析了锥形瓶快速生长装置的优越性.     

生长温度对KDP晶体光学性质影响的研究

用降温法在不同的温度下快速生长KDP晶体,并测量其透过光谱、光学均匀性、金属杂质含量和光散射性能.结果表明随着生长温度的提高,KDP晶体的紫外光吸收和光散射点密度明显降低,但均匀性和杂质金属离子含量并无明显变化.     

快速生长KDP晶体表面的光学显微实时观察

设计了一套溶液降温法晶体生长显微实时观察装置,对快速生长KDP晶体{101}和{100}表面形貌的演化过程进行了实时观测分析.测量了晶体表面生长层切向生长速度随溶液过饱和度的变化曲线,并利用台阶生长动力学方程计算了相关动力学参数.进行了Fe3+掺杂实验,结果表明Fe3+的存在会影响到不同晶面上生长层的动力学系数,从而改变KDP晶体表面生长层的切向生长速度.     

KDP/DKDP晶体生长的研究进展

采用传统降温法,KDP晶体的生长速度一般在1～2 mm/d,DKDP晶体的生长速度甚至更慢,并且晶体的恢复区域较大,利用率低;而采用快速生长法,晶体的生长速度可以提高到20～50 mm/d,并且晶体的恢复区域小,利用率高.本文回顾了KDP/DKDP晶体生长的研究进展.并重点评述了KDP/DKDP晶体快速生长的研究进展,报道了近年来大尺寸、高质量KDP晶体的研究动态.     

Rapid growth of KDP crystal from aqueous solutions with additives and its optical studies

Potassium Chloride (KCl) and Ethylene diamine tetraacetie acid (EDTA) as new additives were added into the KDP solutions in a small amount (5M% and 0.01M% respectively). The solubility curve and metastable zone width of KDP solution with 5M%KCl was determined and we explained the mechanism of rapid growth of KDP crystal with KCl additve. The clear transparent crystal of KDP with a dimension of 54 × 54 × 42 mm have been grown rapidly by cooling solution method in 2 days. The crystal grown from additives added solution was subjected to optical transmission and laser damage threshold studies as compared with the crystal grown by traditional growing method. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Improvement of growth habit and optical properties of rapidly grown KDP crystal by adding diethylene triamine pentacetate acid in growth solution

By altering the concentration of a new additive ‐ diethylene triamine pentacetate acid (DTPA) in the growth solution, a series of KDP crystals were obtained by the “point seed” rapid growth method. The growth rates up to about 20 mm/day. Effects of DTPA on the growth habit and optical properties of these as‐grown KDP crystals were investigated. The results reveal that, with the increase of DTPA concentration in growth solution, the contents of impurity metal ions incorporated into crystal and aspect ratio of crystal morphology were both decreased gradually, while the UV transmittance of crystal was enhanced continually. In the presence of moderate concentration of DTPA (100–200 ppm), the solution stability was increased and optical properties of crystal (including optical homogeneity, light scattering and laser damage threshold) were all improved. However excessive doping (>500 ppm) has opposite effects. The impact mechanism was also analyzed combining with the structure of KDP crystal and chemical characteristics of DTPA molecular.     

Growth and properties of Ba‐doped KDP crystals

KDP crystals were rapidly grown from solution doped with different Ba²⁺ concentrations. The effects of Ba²⁺ on the growth rate, morphology and quality of KDP crystals were discussed. Significant changes in shapes and volume of the grown crystals have been observed. During the growth process, defect region expands gradually with the increasing Ba²⁺ concentration. Samples were cut from different parts of the as‐grown crystals for investigating the optical quality, including transmission spectrum, scattering centers. Through comparison, it is found that the nonuniform distribution of Ba²⁺ ions causes remarkable difference in optical quality between prismatic and pyramidal sectors. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

红外非线性光学晶体CdSe生长与性能表征

采用垂直无籽晶气相法(VUVG)生长出尺寸达26 mm×45 mm的CdSe单晶体,对CdSe晶体的稳态气相生长速率进行了深入讨论.采用气相升华法提纯后的CdSe多晶原料的X射线粉末衍射谱与PDF卡片值(65-3436)吻合,生长出的单晶体{100}和(110)面XRD衍射峰尖锐,无杂峰,且{100}面出现3级衍射峰.晶锭密度为5.74 g/cm3,与理论计算值接近.退火处理后的晶片在1000～7000 cm-1 红外波段范围内透过率达到70;.采用VUVG法生长的CdSe单晶体,结晶性能好、结构致密、尺寸大和红外透过率高,可用于制备红外非线性光学器件.     

Rapid growth of KDP crystals in the coniform bottom device and their characterization

The coniform bottom device was designed and used in the rapid growth process of KDP crystal. A seed support rack was also designed to be used in rapid growth of KDP crystal to avoid spontaneous nucleation on the interface of seed crystal and rack. The KDP crystals were fast grown at the growth rate of up to 25 mm/day. The optical scatter centers in KDP crystals were observed and their transmissions of different parts were measured. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)