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.     

点籽晶法快速生长中等口径KDP单晶及其性能表征

本文使用德国MERCK公司生产的KDP原料和自行研制的晶体快速生长装置,采用"点籽晶"快速生长法成功生长出了150 mm级中等口径的KDP单晶,晶体生长速度达到20 mm/d.晶体生长过程中,生长溶液稳定,没有杂晶出现,生长的晶体完好且透明.X射线粉末衍射和摇摆曲线分析表明晶体有着较好的结构完整性;同时,测试了晶体的透过光谱和光损伤阈值,发现快速生长的晶体有着较好的光学性能.     

超大尺寸KDP/DKDP晶体研究进展

KDP/DKDP晶体具有生长方法简单、成本较低、光学性能良好等优点,而可生长出的超大尺寸KDP/DKDP晶体是目前唯一可用于高功率激光工程的单晶材料。但是在晶体的生长过程中存在很多影响因素,同时对晶体进行后处理也会影响晶体的性能,这都直接关系到超大尺寸KDP/DKDP晶体的实际应用。鉴于此,本文综述了近些年超大尺寸KDP/DKDP晶体的重要研究进展, 特别是针对传统生长和快速生长中存在的问题和相应的解决对策以及晶体性能相关的研究,并重点对晶体的透过率、氘化率、激光诱导损伤等进行了分析和讨论。     

优质DKDP晶体的点状籽晶生长及其表征研究

本文在研究DKDP溶液稳定性的基础上,采用Z切点状籽晶(5mm×5mm×3mm)生长了多块DKDP晶体,在250ml和1000ml生长瓶中分别获得了在[100]和[001]向生长速度可达到3mm/d和4.5 mm/d的点状籽晶生长优质DKDP晶体的生长条件.通过等离子体发射光谱(ICP)和紫外可见光谱分析发现DKDP晶体柱面的金属离子含量比锥面高,柱面的紫外可见吸收比锥面大.性能测试结果表明,点状籽晶全方位生长的DKDP晶体的激光损伤阈值约为5GW/cm2、半波电压约为4kV、动态消光比约为1600∶1,发现与传统方法生长晶体的性能没有明显的差别.     

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).     

点状籽晶法生长DKDP晶体的研究

本文研究了影响溶液稳定性的因素,主要包括溶液的纯度、饱和点和过饱和度等,并对DKDP的点状籽晶法生长进行了初步研究.同时比较了不同生长速度生长的晶体质量.结果表明:经超细过滤的高纯度溶液稳定性有很大提高,而此时生长速度对晶体质量的影响不大.最后,获得了X、Y向生长速度达3.8mm/d的点状籽晶,生长出尺寸为44mm×44mm×48mm的高质量DKDP晶体,并对晶体生长的表面进行了微观观察,分析了DKDP晶体生长的微观机制.     

过饱和度对KDP晶体生长与光学性能的影响研究

在不同过饱和度的溶液中生长了KDP晶体,对生长晶体的透过率,光散射和激光损伤阈值进行了表征.研究了不同过饱和度对KDP晶体生长及光学性能的影响.实验表明:KDP晶体可以在高过饱和度(σ＞3;)溶液中实现快速生长,生长速度可大于10 mm/d;但随着溶液过饱和度的增加,KDP晶体生长溶液的稳定性降低,晶体容易出现包藏、开裂和添晶等缺陷,晶体的光学性能也随之降低.     

大尺寸KDP/DKDP晶体热膨胀系数研究

采用Perkin Elmer公司的Diamond TMA热机械分析仪对KDP/DKDP晶体在25～100℃范围内的平均线性热膨胀系数进行了研究.得到KDP/DKDP晶体x切向、z切向、Ⅰ类切向和Ⅱ类切向的平均线性热膨胀系数,分别为:KDP(2.454×10-5/℃、4.168×10-5/℃、3.465×10-5/℃和2.884×10-5/℃),DKDP(2.602×10-5/℃、4.284×10-5/℃、3.568×10-5/℃和3.052×10-5/℃).另外,实验结果表明大尺寸KDP/DKDP晶体不同部位热膨胀系数存在不均匀性.     

KDP晶体快速生长溶液的稳定性研究

本文研究了搅拌,过滤,过热和添加剂对KDP晶体快速生长溶液的稳定性的影响并分析了其影响机理.结果表明,利用0.2μm的滤膜对溶液过滤,在饱和点以上20℃时对溶液过热20h,或在溶液中添加某些特定的添加剂均可有效提高KDP晶体快速生长溶液的稳定性.通过对生长溶液进行综合的前处理,利用“点籽晶”快速生长技术实现了KDP晶体的快速生长,生长速度达20 mm/d,生长尺寸达5 cm量级.     

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.     

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)     

Study on rapid growth of KH2PO4 and its characterization

Large size crystals of KH₂PO₄ (KDP) were grown by adopting rapid growth technique from point seeds in a 1500‐liter crystallizer which is used to grow KDP crystals by conventional method. The grown KDP crystal size can reach to 310 × 310 × 320 mm³ and the average growth rate was 8mm/day. The optic properties of the rapidly grown KDP crystals were characterized comparing with the KDP crystals grown by the traditional temperature reduction method. We found it that the optical quality of the KDP crystals we grown rapidly are not significantly different from those of KDP crystals grown by traditional 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.     

Effects of anions on rapid growth and growth habit of KDP crystals

The synthesis of KDP from its raw material has been found exist in the growth solution. In the crystal growth experiment, significant extension of specific faces was observed at low dopant concentration. At high doping concentration, the growth rate of the whole crystal decreased with no significant habit modification. The inhibiting effects of phosphite and other H-bonding anionic ions on the growth of pyramidal faces are discussed. Rapid growth rate experiments have been carried out with purified material and an averaged growth rate of 18.6mm/day was obtained.     

Growth and optical absorption studies on potassium dihydrogen phosphate single crystals

Growth of bulk nonlinear optical (NLO) single crystals gained new significance with the advent of solid‐state laser sources for opto‐electronic applications. An optically transparent crystal of potassium dihydrogen phosphate (KDP) has been grown from aqueous solution along (001) plane with the aid of modified growth assembly of Sankaranarayanan‐Ramasamy (SR) Method. The evaporation rate was controlled and single crystals of 5 mm diameter and 60 mm length with a growth rate 5 mm per day have been grown successfully. The improved transparency of grown crystal was investigated using DRS UV transmittance spectral analysis and the presence of functional groups in the grown crystal is confirmed using FTIR analysis. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

Growth and high frequency dielectric study of pure and thiourea doped KDP crystals

Non linear optical (NLO) materials have acquired new significance with the advent of a large number of devices utilizing solid‐state laser sources. Several NLO materials have been used for this kind of technological applications. The Potassium di‐hydrogen phosphate (KDP) one of NLO material having superior non linear optical properties has been exploited for variety of applications. In the present investigation we have grown KDP crystals from aqous solution with thiourea, an organic non linear optical material. We could enhance the SHG efficiency of thiourea doped KDP crystal. It was 1.99 times more that of pure KDP. We observed more enhancements in nonlinearity for low concentration of thiourea.The crystal structure and cell parameters of grown crystal were determined from Powder XRD.The incorporation of thiourea in the grown crystals was qualitatively analyzed from FT‐IR study. The absorption spectra of pure and thiourea doped KDP crystal reveal that thiourea doped KDP crystals would be a better nonlinear optical (NLO) material for second harmonic generation (SHG) than pure KDP. The thermal decomposition and weight loss of pure and thiourea doped KDP crystal was observed by thermogravimetric (TGA) analysis and Differential Scanning Calorimetry (DSC). The high frequency dielectric study of pure KDP crystal, thiourea doped KDP crystals and organic additive thiourea was carried out using X‐band at frequency 8GHZ and 12GHZ by transmission line wave guide method. We observed low dielectric constant of thiourea doped KDP crystal when it is doped with 2mole% of thiourea. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Ⅰ类高氘DKDP晶片性能研究

受到晶体尺寸以及非线性光学性能的影响,目前可供选择的非线性晶体非常有限。DKDP晶体作为传统大尺寸光电材料,在光参量啁啾脉冲放大(OPCPA)装置中得到了应用。高氘化的DKDP晶体有更好的光学性能,然而生长出高氘化DKDP晶体对生长环境等有更加严格的要求。本文通过改良的原料合成罐以及生长槽,采用点籽晶快速生长法成功生长出高氘DKDP晶体。按照Ⅰ类(θ=37.23°, φ=45°)切割方式制备样品,并对其氘含量、透过率、光学均匀性以及晶体激光损伤阈值进行测试。实验结果表明,晶体的平均氘含量达到98.49%,在可见-近红外波段下具有较宽的透过波段和较高的透过性能。R-on-1的测试结果显示,在3 ns、527 nm条件下,DKDP晶体的激光损伤阈值达到了19.92 J/cm²。晶体光学均匀性均方根达到了1.833×10^-9,表明晶体具有良好的光学均匀性。