Crystalline quality of lysozyme crystals grown in agarose and silica gels studied by X-ray diffraction techniques

The crystalline quality of hen egg white lysozyme (HEWL) crystals grown in agarose gels and in silica gels has been characterized by measuring resolution and mosaic spread. These crystals have been compared to solution grown ones. A quasi-plane-wave X-ray topography study has also been done on some crystals. The study concerns triclinic, monoclinic, orthorhombic and tetragonal forms of HEWL. One observes that the resolution is not really changed by gelling the growth medium, even for rather high gel contents (agarose 0.5% wt/wt). On the contrary, mosaicity, characterized through reflection profile recordings allows to differentiate crystals grown by different techniques: agarose gel grown crystals are, on average, better than solution grown ones but the best crystals are obtained in silica gel. X-ray topography confirms this result.     

Characterization of bismuth germanate crystals grown by EFG method

Bismuth germanate shaped crystals have been grown by the EFG (Stepanov) method. The correlation between growth rate, shape of crystals, their optical and scintillation parameters has been analysed. Optical and scintillation characteristics of the EFG crystals are similar to those obtained with Czochralski grown crystals, however, growth rate in EFG is by 2.5 times larger. Also we compare the photochromic effect under UV‐irradiation in EFG and Czochralski grown crystals. Material losses at fabrication of plates, pixels, and rods from EFG shaped plates may be reduced by ∼50% compared to large diameter boules.     

Growth and etching of anhydrous diglycine sulfate single crystals

Single crystals of anhydrous diglycine sulfate are grown at constant temperature by evaporation method. The crystals are grown at various temperatures and their growth rate is determined. A chemical etchant for dislocation studies is reported. The perfection of the crystals grown at various temperatures has been studied using etching technique. It is found that the crystals contained inclusions of the mother liquid. The crystals grown below 28° are almost free of inclusions and the dislocation density is also low.     

Growth of CdBr2 single crystals by zone refining

CdBr₂ has been purified using a 12-pass zone-refining technique. Single crystals grown from the starting material showed arcing in the X-ray oscillation photographs whereas this is absent in the crystals grown from zone refined material. These crystals are found to be 6R type. In order to study the effect of impurities, DC conductivity studies were made on the crystals at various stages of purification. Surface morphology of the crystals have been studied using an optical microscope.     

X-ray,optical and electrical study of melt-grown CdI2 single crystals

CdI₂ has been purified using the zone-refining technique by giving 20 passes. Single crystals grown from the starting material showed arcing in the X-ray oscillation photographs whereas it is absent in the crystals grown from the zone refined material. These crystals are found to be of the 4 H type. DC conductivity studies were made on these crystals at various stages of purification. The surface morphology of these crystals have been studied using an optical microscope.     

Growth and Morphology of Hollow Bi2Te3 Whiskers by Physical Vapour Deposition Method

Hollow crystals of bismuth telluride have been grown by the physical vapour deposition (PVD) method. Whisker crystals as long as 10 mm have been grown and were identified by X-ray analysis. The possible mechanism for the growth of hollow whiskers has also been suggested.     

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)     

Striation in Ge single crystals grown from melt under vibrations and weak heat convection

The influence of vibrations on the formation of mictohomogeneities of the properties in Ga-doped Ge single crystals grown by the method of directional crystallization with the axisymmetric upper heat supply has been studied in earth experiments. It has been established that vibrations provide the formation of inhomogeneities in the dopant distribution in the grown crystals.     

Growth and microscopic studies of yttrium aluminium garnet single crystals

A study has been made to understand the growth history and growth mechanism of flux grown yttrium aluminium garnet (YAG) single crystals. Etching has been done to reveal the growth patterns of flux grown crystals. Optical and scanning electron micrographs are presented. Optical micrographs were taken under polarised light and oblique incident light. The nature and origin of growth hillock is elucidated.     

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)     

Nucleation, growth and characterization of L-tartaric acid—nicotinamide NLO crystals

The solubility, metastable zone width and nucleation parameters of organic nonlinear optical material L-tartaric acid–nicotinamide (LTN) have been determined. The crystals of LTN are grown by the slow cooling method. The grown crystals are morphologically interpreted. The crystalline powder of the grown crystals has been examined by X-ray diffraction and thermogravimetric analysis. The different modes of vibrations present in the crystal are identified by the Fourier infrared spectroscopy analysis. The powder SHG efficiency of LTN is comparable with that of KDP.     

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)     

Microstructures of gel-grown ammonium hydrogen tartrate single crystals

Single crystals of ammonium hydrogen tartrate (AHT) have been grown in silica gels by employing the controlled reaction between ammonium chloride and tartaric acid. Transparent AHT crystals upto 24 × 4 × 3 mm³ in size have been grown at room temperature. Optical and electron-optical studies have been made on the various surface structures of {010} faces of the grown crystals. A variety of growth striations and growth hillocks have been observed. Growth layers modified by the presence of misaligned microcrystals have been illustrated. It has been suggested that two-dimensional nucleation, spreading and pilling up of growth layers is mainly responsible for the growth of these crystals and the implications are discussed.     

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.     

Effect of ammonium malate on growth rate,crystalline perfection,structural, optical,thermal, mechanical,dielectric and NLO behaviour of ammonium dihydrogen phosphate crystals

The effect of ammonium malate on the growth rate, structural, optical, thermal, mechanical, dielectric properties, crystalline perfection and second harmonic generation (SHG) efficiency of ammonium dihydrogen phosphate single crystals grown by the slow cooling method has been investigated. The lattice parameters of the grown crystals were obtained by the single-crystal X-ray diffraction analysis. Fourier transform infrared studies confirm the functional groups of the crystals. UV–vis study shows that the transparency is increased much by the dopant. Thermal analysis was performed to study the thermal stability of the grown crystals. Vickers hardness measurements reveal the higher hardness of the doped crystals. Low dielectric losses were observed from the dielectric measurements for the doped ADP crystals. The high-resolution X-ray diffraction studies show that the crystalline perfection of the crystals is good. The relative SHG efficiency measurements revealed that the dopant has enhanced the efficiency.     

Growth and characterization of cadmium magnesium tetra thiocyanate crystals

Cadmium Magnesium Tetra Thiocyanate, CdMg(SCN)₄, [CMTC] belongs to bimetallic thiocyanate complexes. CMTC crystals has been grown by solution growth technique at room temperature. The morphologies of the grown crystals are identified by single crystal analysis. Also the Powder X‐ray Diffractogram of the crystal has been recorded and the various planes of reflection are identified. The title compound crystallizes under triclinic structure with lattice parameters a = 10.0976 Å, b = 7.5015 Å, c = 5.7720 Å and β = 90.2135°. The presence of magnesium and cadmium in the grown crystals were confirmed through Atomic Absorption Spectroscopy. The grown crystals are analysed qualitatively by Fourier Transform Infrared (FTIR) and Fourier Transform Raman spectral measurements. The transmittance spectrum of the crystal in the UV‐Visible region has been recorded and analysed. The dielectric measurements for the crystals were carried out in the microwave region. The thermal stabilities of the crystals were studied by using different thermal analyses like Thermo Gravimetric Analysis (TGA), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Undoped semi-insulating GaAs crystals grown by a modified low pressure LEC method

A modified low pressure in-situ synthesis LEC method of growing undoped SI (semi-insulating) GaAs crystals has been established. The key points for controlling melt composition and As evaporation during synthesis and growth have been described. Using this novel approach, crystals are able to be grown from the nominal melt composition in the range of 0.491–0.499 As fraction with high reproducibility. Some characteristics of the undoped SI crystals grown by the present work including electrical properties, dislocation density, carbon and EL2 concentrations and thermal annealing effects have been studied.     

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)     

Synthesis, growth, thermal, optical, dielectric and mechanical properties of semi-organic NLO crystal: Potassium hydrogen malate monohydrate

Potassium hydrogen malate monohydrate (PHMM), a semi-organic nonlinear optical material, has been synthesized and single crystals were grown from aqueous solution. Single crystals of PHMM have been grown by slow evaporation of solvent at room temperature up to dimensions of 22 mm×16 mm×14 mm. Single-crystal X-ray diffraction study on grown crystals shows that they belong to monoclinic system and non-centrosymmetry spacegroup Cc. The structural perfection of the grown crystals has been analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. Fourier transform infrared (FTIR) spectroscopic study was performed for the identification of different modes of functional groups present in the compound. The UV–Vis transmission spectrum has been recorded in the range 200–1100 nm. The thermal stability of the compound has been determined by TG-DTA curves. The dielectric studies were performed. From the microhardness measurements, Vicker's hardness number (H_v), Stiffness constant (C₁₁), fracture toughness (k_c), Brittle index (B_i) and yield strength (σ_y) have been calculated. The Young's modulus was calculated using the Knoop hardness measurement. The SHG relative efficiency of PHMM crystal was found to be 1.2 times higher than that of KDP.