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 Bis Thiourea Zinc Acetate (BTZA)

Single crystals of BTZA have been grown by low temperature solution growth method using slow cooling process at an optimized pH of 3.5. The grown crystals have been examined under an optical microscope to study its surface morphology. The morphological studies show that the growth takes place by spreading of growth layers. Formation of rectangular shaped etch pit on the as‐grown crystal has been explained in relation to the growth conditions. Single crystal X‐ray diffraction analysis has been carried out to confirm the monoclinic system. Transmission spectrum reveals that the crystal has a low UV cut off of 434.5 nm and has a transmittance of 100%. Dependence of micro hardness on load has been studied. Powder X‐ray Diffraction and FT‐IR have been carried out to characterize the grown crystals. BTZA forms metal – sulfur bond and has good optical transmission in the entire visible region, which is the essential requirement for a non‐linear crystal. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of dl-malic acid-doped ammonium dihydrogen phosphate crystal and its characterization

Single crystals of dl-malic acid-doped ammonium dihydrogen phosphate have been grown using slow evaporation method and also by Sankaranarayanan–Ramasamy (SR) method with the vision to improve the properties of the ADP crystals. The characterization of grown crystals was made by single-crystal X-ray diffraction, powder X-ray diffraction, UV–vis. spectroscopy, Fourier transform infrared spectroscopy (FTIR), differential thermal analysis (DTA), Vicker's microhardness, dielectric measurements, high-resolution X-ray diffraction (HRXRD) and second-harmonic studies. Structural difference between pure and doped crystal has been studied by XRD analysis. Functional groups were identified by FTIR spectroscopy. The grown crystals were found to be transparent in the entire visible region. Decomposition temperatures of the grown crystals were measured by DTA. Vicker's hardness study carried out on (0 0 1) face at room temperature shows increased hardness of the doped crystals and SR-method-grown crystals. Dielectric measurements reveal that SR-method-grown DLM-doped ADP crystals have low dielectric loss. Crystalline perfection of the grown crystals is analyzed using HRXRD. Preliminary measurements indicate that the second harmonic generation efficiency of the doped crystals at a fundamental wavelength of 1064 nm is roughly 1.5 times greater than that of pure ADP.     

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)     

Growth and characterization of doped hippuric acid crystals for NLO devices

Modified hippuric acid (HA) single crystals have been grown from aqueous solution of acetone by doping with NaCl and KCl using slow evaporation technique at constant temperature, with the vision to improve the physicochemical properties of the sample. The characterisation of grown crystals was made by X‐ray powder diffraction, density and melting point measurements. TGA/DTA studies indicate that doped crystals are more stable than pure crystals. The optical transmission study and Kurtz powder SHG measurement shows the suitability of doped crystals for NLO applications. Dopant concentration is identified with ICP atomic emission spectrometer system. The Vicker's hardness studies at room temperature, carried out on (111) crystallographic plane shows increased hardness of the doped crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A comparative study on pure,l-arginine and glycine doped ammonium dihydrogen orthophosphate single crystals grown by slow solvent evaporation and temperature-gradient method

Single crystals of pure, l-arginine and glycine doped ammonium dihydrogen orthophosphate (ADP) were grown by both the slow solvent evaporation method and the temperature-gradient method of Sankaranarayanan–Ramasamy (SR). The metastable zone width for different saturation temperatures of pure glycine and l-arginine added solutions were carried out. The grown crystals were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), powder X-ray diffraction (XRD), optical transmission, dielectric constant, dielectric loss, and Vickers microhardness. The DSC and TG curves of the grown crystals indicated that they were stable up to 200 °C. The XRD study confirmed the structure of the grown crystal. The optical transmission analysis revealed that the pure and doped ADP crystals had very high percentage of transmission in the entire visible region. The important optical parameters such as reflectance and extinction coefficients of the grown crystals were calculated. l-arginine and glycine were used as dopants to reduce dielectric constant of ADP. The a.c. resistivity and a.c. conductivity were calculated. Dielectric loss of the doped ADP crystals grown by the SR method is lower than the doped ADP crystals grown by the conventional method. Larger hardness value for the SR method grown crystals confirmed greater crystalline perfection.     

Ce∶GAGG与CsI(Tl)闪烁晶体性能对比研究

研究了不同反射层封装方式和与Si-PM不同耦合方式对Ce∶GAGG和CsI(Tl)闪烁晶体光输出和能量分辨率的影响,比较了Ce∶GAGG和CsI(Tl)闪烁晶体的透过率和衰减时间。实验结果表明:通过优化闪烁晶体的反射层材料和耦合方式,能大幅度提高Ce∶GAGG和CsI(Tl)闪烁晶体的光收集效率;Ce∶GAGG闪烁晶体的光输出、能量分辨率、透过率、衰减时间指标均优于CsI(Tl)闪烁晶体。Ce∶GAGG闪烁晶体使用TiO₂反射层材料封装和硅脂耦合,测试得到¹³⁷Cs放射源在662 keV最佳能量分辨率为4.89%。     

Dielectric and microhardness studies on L‐citrulline and L‐ascorbic acid admixture TGS crystals

Single crystals of amino acid doped (L–citrulline, L‐ascorbic acid) triglycine sulphate were grown by slow evaporation technique. The lattice parameters and crystalline quality were confirmed by powder X‐ray diffraction studies. The presence of functional groups in the grown crystals was confirmed by Fourier transform infrared spectrum analysis. The dielectric studies were carried out to identify the phase transition temperature and the dielectric constant was found to be less for both the doped crystals than pure triglycine sulphate crystal. Micro hardness studies were carried out using Vickers pyramidal indentation technique at room temperature showed a decrease in hardness due to doping. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Thermal and electrical properties of Tri Glycine Sulpho Phosphate (TGSP) and L‐Asparagine doped TGSP crystals

Tri Glycinsulphate with partial substitution of phosphoric acid, namely Tri Glycine Sulpho Phosphate (TGSP) has been grown by slow cooling method. Habit modifications have been observed with change in the concentration of ortho phosphoric acid (H₃PO₄). Monoclinic structure of the grown crystals has been confirmed using X‐ray diffraction analysis. TGSP crystals doped with L – Asparagine were also grown. The doping effect is qualitatively estimated using FTIR analysis. TGA, DTA studies and dielectric measurements were carried out for pure and L‐Asparagine doped TGSP crystals to investigate the thermal and electrical properties of the crystals. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Single crystal growth and properties of semiorganic nonlinear optical L‐arginine hydrochloride monohydrate crystals

L‐arginine hydrochloride monohydrate (LAHCl.H₂O) has been synthesized and single crystals have been grown from its aqueous solution by slow evaporation and slow cooling methods. The solubility of the material was measured at various temperatures and bulk crystals of size 26×13×11 mm³ have been grown by optimizing the growth parameters. The grown crystals have been subjected to single crystal XRD studies to confirm the structure and to estimate the lattice parameters. FTIR analysis indicate the mode of vibrations of different molecular groups present in LAHCl and confirm the protonation of guanidyl, amino groups and deprotonation of COO^‐ groups. UV‐Vis transmission spectrum revealed the linear optical properties of the grown crystals with a transparency of 65% over the entire visible range upto 300 nm. Thermal behavior of the grown crystal was investigated from DTA and TGA measurements. Dielectric studies have been carried out on the grown crystals. Kurtz and Perry powder SHG technique confirms the NLO property of the grown crystal. The SHG efficiency of LAHCl was found to be 0.38 with respect to KDP. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of bis-glycine sodium nitrate (BGSN), a novel semi-organic nonlinear optical crystal

Single crystals of bis-glycine sodium nitrate (BGSN), a semi-organic nonlinear optical (NLO) material, have been grown by slow cooling method. Good optical quality single crystals with dimensions up to 1.6×1.6×1.0 cm³ are obtained. Using a single-crystal diffractometer, the morphology of BGSN crystal was identified. Powder X-ray diffraction confirms the crystalline nature of BGSN. The grown crystals were characterized by optical transmission spectrum (UV) and FTIR studies. The NLO property of the crystal was confirmed by Kurtz second harmonic generation (SHG) test, and the output power generated by the crystal was compared with that of KDP. The thermal stability of the crystal was studied by thermo-gravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetry (DSC). Micro hardness study was carried out for different planes, and the anisotropy behavior of the crystal was observed.     

Growth,optical and thermal studies of nonlinear optical L‐arginine perchlorate single crystals

A potentially useful semiorganic nonlinear optical (NLO) material, L‐arginine perchlorate, has been synthesized and bulk crystals have been grown by slow cooling technique. The grown crystals were characterized by single crystal X‐ray diffraction, UV‐Vis‐NIR spectroscopy, FT‐IR, thermal analysis and SHG measurements. The grown crystals were thermally stable upto 153°C and exhibit SHG efficiency of about 0.17 with respect of Urea. The etching studies have been carried out on the grown crystal. LAPC has good optical transmission not only in the visible range, however, also in the near UV part of the spectra and hence it is a potential material for nonlinear frequency conversion. The refractive index was measured by the Brewster's angle method. (© 2008 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)     

Crystal structure,spectroscopic studies and non‐linear optical properties of 2‐amino‐3‐nitropyridinium trichloroacetate

A new quadratic nonlinear optical crystal, 2‐amino‐3‐nitropyridinium trichloroacetate (2A3NPTCA), was synthesized and the single crystals were grown by slow evaporation method at room temperature. Single crystal X‐ray diffraction and powder X‐ray diffraction experiments were carried out in order to confirm the structure and crystalline nature of 2A3NPTCA crystal. The chemical bonding and various functional groups present in the 2A3NPTCA were identified from FT‐IR spectrum. The UV–visible–NIR transmission spectrum shows that it is suitable for frequency‐converting in the wavelength region of 431–1200 nm. Thermogravimetric (TG) and differential thermal analysis (DTA) were carried out to characterize the thermal behaviors of the grown crystals. Kurtz and Perry powder method for second harmonic generation (SHG) measurements demonstrate that 2A3NPTCA is a phase matching material and its nonlinear optical efficiency is two times that of KDP. All the above results suggest that 2A3NPTCA is a potential candidate of NLO material.     

大尺寸高浓度掺杂Nd:GGG和Nd:YAG晶体的光谱性质

由于Nd3 离子半径0.112nm和Y3 离子半径0.101nm相差10.9%,使得Nd3 离子非常难于进入YAG晶体中。我们用温度梯度法生长了大尺寸高浓度(2.8 at%)的Nd:YAG晶体,同时与用提拉法Nd:GGG晶体进行了比较。分析了高浓度掺杂Nd:GGG和Nd:YAG晶体浓度猝灭问题。研究了不同浓度掺杂的猝灭效应。在同样的掺杂浓度下,我们发现它们的猝灭程度不同,其原因是两种晶体中ΔE(m is-)m和ΔE(m i s )m不同。     

Growth of thiourea-doped TGS crystals and their characterisation

Thiourea-doped Triglycine sulphate (ThTGS) crystal with three different concentrations of thiourea was grown from aqueous solution by slow cooling technique. The cell parameters were determined from powder X-ray diffraction analysis. A qualitative analysis of the presence of thiourea in doped crystals was estimated by FTIR analysis. Microhardness studies were carried out using Leitz Weitzler hardness tester at room temperature. Dielectric properties of the crystals were studied which showed a shift in the T_c when compared to pure TGS crystal. Pyroelectric studies were carried out and the pyroelectric coefficient was found. Piezoelectric studies (d₃₃ coefficient) has also been carried out.     

Growth and Optical Absorption of Photorefractive Bi12SiO20 Crystals Doped with Zn and Cd and Co-doped with P

Single crystals of Bi₁₂SiO₂₀ (BSO) Zn- and Cd-doped and co-doped with P have been grown by Czochralski technique and optimum conditions for producing optically homogeneous crystals were established. The transmission and reflection spectra have been measured in the range 0.38–0.85 μm and absorption coefficients have been determined. The Zn dopants have been found to bleach the crystals and decrease the transmission shoulder, whereas Cd dopant increases the absorption and makes the shoulder well pronounced. P-doping strongly decreases the transmission shoulder and shifts absorption to shorter wavelengths. The absorption Coefficient of BSO doped with P has been found to decrease with dopant concentration increase up to 3 mol% P and above it increases with P concentration in the whole studied range. Zn + P- and Cd + P-co-doping (P concentration in the crystal less than 3 mol%) decreases strongly the absorption coefficient and shifts the spectra to short wavelengths.     

Synthesis,growth and characterization of organic nonlinear optical bis-glycine maleate (BGM) single crystals

A new organic compound of bis-glycine maleate was synthesized in the alkaline medium of 10% ammonium hydroxide solution. The bulk single crystals of Bis-Glycine Maleate (BGM) have been grown by slow cooling method. The grown crystals were characterized by employing single crystal and powder X-ray diffraction, Fourier transform infrared, optical absorption spectral studies and thermo gravimetric analysis. The microhardness studies confirmed that the BGM has a fairly high Vicker’s hardness number value (41 kg mm⁻²) in comparison to other organic NLO crystals. Second harmonic generation efficiency of the crystal measured by Kurtz–Perry powder method using Nd:YAG laser is found to be comparable to that of potassium dihydrogen phosphate (KDP). Frequency dependent dielectric studies were carried out along the major growth axis.     

Synthesis,growth and characterization of single crystals of pure and thiourea doped L‐glutamic acid hydrochloride

L(+)Glutamic acid hydrochloride [HOOC (CH₂)₂CH(NH₂) COOH·HCl], a monoamino dicarboxylic acid salt of L‐Glutamic acid was synthesized and the synthesis was confirmed by FTIR analysis. Solubility of the material in water was determined. Pure and Thiourea doped L‐Glutamic acid hydrochloride crystals were grown by low temperature solution growth using solvent evaporation technique. XRD, UV‐Vis‐NIR analyses were carried out for both pure and thiourea doped crystals. The crystals were qualitatively analyzed by EDAX analysis and the presence of thiourea was confirmed. The cell parameters of L‐Glutamic acid hydrochloride have been determined as a = 5.151 Å, b = 11.79 Å, c = 13.35 Å by X‐ray diffraction analysis and it crystallizes in orthorhombic space group P2₁2₁2₁. UV‐Vis‐NIR spectra analysis showed good optical transmission in the entire visible region for both pure and doped crystals. Micro hardness of both pure and doped crystals has been determined using Vickers micro hardness tester. The SHG efficiencies of both pure and doped crystals were determined using Kurtz powder test and pure L‐Glutamic acid hydrochloride crystal was found to possess better efficiency than thiourea doped L‐Glutamic acid hydrochloride crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

不同X射线管电压下CsI和CsI(Tl)晶体的X射线辐照致发光

在室温(290 K)和低温(25 K)下,测量了从11～40 kV的一系列管电压下X射线激发纯CsI和CsI (Tl)晶体的辐照致发光(RL)谱.结果表明:在固定温度下,管电压变化后, 305 nm和340 nm的本征发光带和580 nm的非本征发光带的形状结构均不发生变化,只是其强度发生变化.对所测得的各发光带强度随管电压的变化关系用抛物线模型进行了拟合分析,得到了较好的结果.同时还发现纯CsI和CsI (Tl)晶体中所有本征RL发光带强度与X射线强度基本上成正比关系,而当管电压增加时,CsI (Tl)晶体中非本征发光带强度的增加速度慢于本征发光带.分析认为,290 K时这可能与样品中另一个位于400 nm左右的发光带有关;而在25 K时则可能和H心与VK心的竞争有关.