Dielectric studies of metal complexes of thiourea crystals for electro‐optic modulation

In the present study three crystals of thiourea family viz. Zinc Thiourea Chloride (ZTC), Zinc Thiourea Sulfate (ZTS) and Bisthiourea Cadmium Chloride (BTCC) were grown from aqueous solution by slow evaporation technique. The grown crystals were studied by powder XRD, FT‐IR and UV‐visible. The dielectric study of grown crystals was carried out in X‐band using transmission line wave guide method. It was found that the BTCC has lowest dielectric constant among three metal complexes of thiourea crystals (ZTC, ZTS and BTCC), therefore it can be used for high speed electro‐optic modulation. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical and dielectric studies on pure and Ni2+, Co2+ doped single crystals of bis thiourea cadmium chloride

Good quality single crystals of Ni²⁺, Co²⁺ ions doped Bisthiourea Cadmium Chloride (BTCC) are some of the excellent and efficient non‐linear optical materials grown from aqueous solution by slow evaporation method. The lattice parameters of the grown crystals are determined by single crystal X‐ray analysis. UV spectral analyses on these samples reveal the improved transparency of the doped crystals ascertaining the inclusion of metal ion in the lattice. FTIR spectral analysis carried out on the materials confirm the presence of functional groups. Dielectric measurements reveal that the dielectric constant of pure and doped crystals decreases with increase of frequency. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and properties of dyed KDP crystals

Potassium dihydrogen phosphate (KDP) crystals doped with xylenol orange (XO) and methylthymol blue (MTB) are grown from aqueous solutions by the method of solvent evaporation at room temperature under the conditions of natural convection and by the method of temperature lowering. Studied is the influence of the mother solution acidity on the character of the crystal coloration. The color and coloration intensity of the grown crystals are shown to strongly depend on the solution's pH. It is revealed that the crystal habit changes in the presence of organic dyes. The optical transmission spectra and the luminescence spectra of KDP:XO solutions and of the grown crystals are measured. The effect of thermal treatment and UV‐irradiation on the coloration stability of the crystals is studied. It is found that the laser damage threshold in the prismatic impurity rich colored sectors of KDP:XO is the same as that in the prismatic sectors of pure KDP crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

Growth and characterization of dichloro tetrakis thiourea nickel single crystals

Thiourea has a large dipole moment and has an ability to form extensive network of hydrogen bonds. In the course of our studies on new semiorganic NLO materials, thiourea is selected to combine with nickel chloride. Single crystals of tetrakis thiourea nickel chloride are grown using silica gel. Green transparent crystals of NTC (nickel thiourea chloride) of dimension 8x4x3 mm³ are grown in a period of 45 days. Single crystal XRD shows that the crystal belongs to body centered tetragonal symmetry class I4. The UV‐Vis‐NIR spectrum establishes the transmission range to be 300 nm to 2500 nm, with a sharp absorption peak at the red end of the visible region, which is due to the colour of the crystal. Photoconductivity and dielectric studies are also carried out. The mechanical strength of the crystal is estimated by Vickers hardness test. The crystal starts decomposing after about 200°C. Thus, we confirm from our present investigation that NTC is a suitable candidate for NLO applications. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Exposure of high index facets in KDP crystals

A series of KDP crystals doped with WO₄^2‐ additive was grown by using rapid growth method. WO₄^2‐ additive inhibited the growth of (100) faces and made (100) faces tapering. With high additive concentration, two adjacent (100) faces twisted towards their intersecting crystal edge and (100) faces became twisting. Moreover, high index facets of (512) were exposed when the additive concentration was 500 ppm. The element analysis suggested that WO₄^2‐ was prone to being incorporated with (100) face. The growth kinetics of (100) face testified that WO₄^2‐ played an inhibited role. The AFM investigation on (100) face indicated WO₄^2‐ could impede step bunching. High concentration of WO₄^2‐ could kink the terrace of the macro‐steps and create another series of macro‐steps. The motion direction of the new creative steps was vertical to that of the original steps. When the motions of the vertical steps were both inhibited by WO₄^2‐, the steps would become tapering and (100) face would twist, which ultimately led to the exposure of (512) facets. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and electrical characterization of L‐arginine added KDP and ADP single crystals

Potassium dihydrogen orthophosphate (KDP) and ammonium dihydrogen orthophosphate (ADP) single crystals added with L‐arginine have been grown by the solution methods. DC and AC electrical measurements were carried out at various temperatures along both a‐ and c‐ directions. Results indicate an increase of the electrical parameters with the increase of temperature which can be attributed mainly to the increase of thermally generated hydrogen bond vacancies (L. defects). Also, the present study indicates that L‐arginine addition leads to reduction of electrical parameters of KDP and ADP single crystals which can be attributed mainly to the decrease of L‐defects due to creation of additional hydrogen bonds by the impurity in random directions. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of glycine doped bis thiourea cadmium chloride single crystal

Single crystal of 2 mol% glycine doped Bis Thiourea Cadmium Chloride, a semi organic nonlinear optical material has been grown by slow evaporation technique. Good quality single crystal with dimension 14 × 12 × 5 mm³ was harvested after 35 days. The influence of amino acid glycine was studied for 1, 2 and 3 mol% glycine doped Bis Thiourea Cadmium Chloride by Kurtz and Perry powder second harmonic generation test and compared with pure Bis Thiourea Cadmium Chloride which confirms the enhancement of second harmonic generation property of glycine doped Bis Thiourea Cadmium Chloride. The large enhancement was found for 2 mol% glycine doping. The grown crystal was characterized by various characterizations viz. single crystal X‐ray diffraction, energy dispersive X‐ray (EDAX), Fourier Transform Infrared Spectroscopy (FTIR) analysis, UV‐visible absorption, thermo gravimetric analysis (TGA). (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of pure and metal doped bis(thiourea) zinc chloride single crystals

Metal (Cd²⁺ and Cu²⁺) substituted single crystals of Bis(thiourea) zinc chloride (BTZC) are grown by slow solvent evaporation technique, with the vision to improve the physicochemical properties of the sample. Single crystal XRD studies of both pure and doped samples are carried out and the results are compared. Optical absorption and FTIR studies are performed to identify the UV cut‐off range and the presence of various functional groups in the grown crystals. The thermogravimetric (TG) analysis of metal doped BTZC indicates a marginal increase in the thermal stability of the crystals. The dielectric response of the samples have been studied in the frequency range 100 Hz to 5 MHz at room temperature and the results are discussed. Photoconductivity studies carried out on pure and metal doped BTZC crystals revealed the negative photoconducting nature. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of L‐alanine doped KDP crystals

Potassium Dihydrogen Phosphate (KDP) is an excellent inorganic nonlinear optical (NLO) material with different device applications. Most of amino acids possess NLO property; therefore, it is of interest to dope them in KDP crystals. In the present study, amino acid L‐alanine doped KDP crystals were grown by slow aqueous solvent evaporation technique. The doping of L‐alanine was confirmed by the paper chromatography, the CHN analysis and the FT‐IR spectroscopy. The powder XRD was carried out to assess the single phase nature of the samples. The effect of doping on thermal stability of the crystals was studied by TGA and the kinetic and thermodynamic parameters of dehydration were evaluated. As the amount of doping increased the thermal stability of crystals decreased. However, the second harmonic generation (SHG) efficiency and the UV‐Vis spectroscopy studies indicated that as the L‐alanine doping increased the SHG efficiency and optical transmission percentage increased. The dielectric behavior of the samples has been studied. The variation of dielectric constant, dielectric loss (tanδ), a.c.resistivity and a.c.conductivity with frequency of applied field in the range from 100 Hz to 100 kHz was studied. The dielectric constant and dielectric loss decreased with increase the value of frequency of applied field. The dielectric constant and the dielectric loss values of L‐alanine doped KDP crystals were lower than the pure KDP crystals. The results are discussed. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of pure and doped nonlinear optical l‐arginine acetate single crystals

Single crystals of organic nonlinear optical material of pure, Cu²⁺ and Mg²⁺ doped L‐arginine acetate (LAA) were successfully grown by slow evaporation method at room temperature. The UV‐Vis‐NIR spectra of pure and doped LAA indicate that these crystals possess a wide optical transmission window from 240‐1600 nm. Non‐linear optical studies reveal that the SHG efficiency of LAA is nearly three times that of KDP. The dielectric response of the samples was studied in the frequency region 100 Hz to 2 MHz and the influence of Cu²⁺ and Mg²⁺ substitution on the dielectric behaviour had been investigated. Photoconductivity study proves that both pure and Cu²⁺ and Mg²⁺ doped LAA crystal exhibit positive photoconductivity. It is evident from the Vickers hardness study that the hardness of the crystal decreases with increasing load both for pure and doped samples. ESR studies confirmed the incorporation of Cu²⁺ into LAA and the value of g‐factor was found to be 2.1654. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effects in B–doped KDP crystals irradiated with neutrons of large spectra energy

The results obtained for the r₆₃ electro‐optic coefficient of B‐doped and undoped KDP (KH₂PO₄) crystals irradiated with neutrons (including thermalized neutrons) produced by scattering of 30 Mev cyclotron protons on a target of Ta²⁰¹, are presented and compared to those obtained for non‐irradiated doped and undoped crystals. The B‐doped (H₃BO₃, Na₂B₄O₇ and Li₂B₄O₇) crystals were obtained by the conventional growth method by temperature decrease with 1 wt % dopant concentration in solution. The thermal neutron flux was around ϕ = 1. 10¹⁰ n/cm² s. Pulses of ∼15 μs long, in damped oscillatory mode (V= 8 kV, τ=1.95 μs) were used for the electro‐optic measurements. A Pockels cell, a photomultiplier, a He‐Ne laser (λ=632.8 nm, 5 mW, linearly polarized) and a Tk 720 A oscilloscope complete the experimental setup. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth imperfections in oriented grown KDP crystals by X‐ray topographic analysis

Potassium dihydrogen phosphate (KDP) crystals were restrained to grow in two dimensions only, using a specially designed platform. This enables us to grow the blanks of frequency conversion elements that satisfy type‐II phase matching direction out of a type‐II phase‐matched seed crystal. Synchrotron radiation topography was used to study the growth mechanism of these profiling grown KDP crystals. It is found that both dislocation growth mechanism and layer growth mechanism were involved in the growing process. Inclusions, growth striations and dislocations were the main defects that influenced the crystalline quality of these crystals. High‐resolution X‐ray diffraction was employed to study the lattice integrality of the crystal.     

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)     

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.     

Influence of lithium ions on the NLO properties of KDP single crystals

Potassium Dihydrogen Phosphate (KDP) and its isomorphous deuterated form are popular due to their applications in frequency converters and electro‐optic modulation. Different attempts have been made to dope KDP with inorganic additives, organic materials and amino acids. Since many of the metal ions possess more electro negativity which increases the non centrosymmetry, it is of interest to dope them in KDP. The influence of lithium ion (Li⁺) on NLO properties of KDP crystal has been studied in the present investigation. Single crystal of Lithium ion doped Potassium Dihydrogen Phosphate (KDP) was grown by slow evaporation technique. The enhancement in SHG efficiency after addition of ion Lithium (Li⁺) was observed by Kurtz Powder SHG test. It was found that the SHG efficiency of KDP after addition of Lithium ion is 1.33 times more than pure KDP. The crystal structure and cell parameters of grown crystal were determined by X‐ray diffraction. The Energy Dispersive X‐ray analysis (EDAX) gives the chemical composition of grown crystal. The functional groups were identified by FT‐IR spectral analysis. The presence of Lithium in the material of grown crystal was detected by Atomic absorption spectroscopy (AAS). The optical absorption and transmission studies were done by UV‐Visible spectral analysis. The grown crystal was subjected to thermogravimetric analysis (TGA) and Differential Scanning Calorimetry (DSC). (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Na+对KDP晶体生长的影响

本文利用传统的降温法和点籽晶快速生长法在不同Na+掺杂浓度的溶液中生长KDP晶体,定量研究了Na+对KDP晶体生长的影响.实验发现:Na+的存在降低了溶液的稳定性,致使KDP晶体柱面容易扩展.Na+的存在对KDP晶体的光学性能基本没有影响.     

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.     

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.     

Growth and characterization of pure and Hg2+ doped thiosemicarbazide cadmium chloride crystals

Semiorganic single crystals of thiosemicarbazide cadmium chloride (TSCCC) and mercury ions doped thiosemicarbazide cadmium chloride were synthesized by slow solvent evaporation technique. The grown crystals were subjected to powder X‐ray analysis and both the crystals were found to crystallize in the monoclinic system. EDAX analysis was carried out for chemical analysis of the grown crystals. The UV‐Vis‐NIR spectrum shows that both the materials have wide transparency window in the visible and near IR region. The dielectric studies were carried out to estimate the dielectric constant and dielectric loss with respect to frequency for both the crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)