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.     

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)     

Tracing of dislocations in ammonium hydrogen tartrate single crystals

Sparingly soluble ammonium hydrogen tartrate (AHT) crystals are grown by the gel method, derived from the diffusion of ammonium chloride into the set gel containing tartaric acid. Crystals up to 23 × 5 × 3 mm³ in size are grown at room temperature. AHT crystals are cleaved along (010) planes and the cleavage surfaces are studied by using multiple beam interferometry. The interferograms have revealed that the cleavages are quite flat. An attempt is made to trace the trajectory of dislocations of isolated as well as matched pairs of (010) cleavages of AHT when etched in a mixture of formic acid and methyl alcohol (2:1) and 1.0 M SrCl₂ solutions. Optical and transmission electron micrographs of dislocations show oblique, parallel and continuous line characteristics. Rows of equally spaced dislocation pits are observed and the implications of this are discussed.     

Crystal growth and dislocation structure of gallium antimonide

Single crystals of GaSb have been grown by the Czochralski method under reducing conditions. Crystals were grown in the 〈100〉, 〈111〉, and 〈112〉 directions. The 〈111〉 growth direction was found to be the most suitable for the successful and reliable crystal growth. Dislocation densities in 〈111〉 oriented crystals were examined by chemical etching. The etch pits density in these crystals didn't exceed the value of 1 × 10² cm⁻².     

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)     

Growth of Nd:Sr3Ga2Ge4O14 crystals by a modified Bridgman method

Bridgman growth of Nd:SGG (Sr₃Ga₂Ge₄O₁₄) crystals has been investigated for the first time. Pt crucible of ∅︁25mm×250mm with a seed well of ∅︁10mm×80 mm is used, and seed is SGG crystal of ∅︁10mm×50mm grown by Bridgman method in advance. The growth parameters are optimized as the furnace temperature is set to 1450∼1500°C, temperature gradient in the crystal‐melt interface is less than 25 K/cm and growth rate is less than 0.5mm/h. The Nd:SGG crystals with 25mm in diameter and 60mm in length are grown successfully from 1.5 to 8at% Nd³⁺ doped stoichiometric Sr₃Ga₂Ge₄O₁₄ melt. The distribution coefficient and concentration of Nd³⁺ in Nd:SGG crystals are obviously higher than those of Nd:YAG crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Microhardness studies of ammonium hydrogen tartrate single crystals

Single crystals of ammonium hydrogen tartrate AHT NH₄HC₄H₄O₆ have been grown employing the controlled reaction between NH₄Cl and (CHOHCOOH)₂ by slow diffusion process in silica gels. The variation in the microhardness of AHT crystals has been determined using Vicker's microhardness indentor. The effects of annealing and quenching on the mechanical properties of these crystals have been studied. It is observed that: (i) irrespective of the relative orientation of the indentor and the crystal, the median vents initiated at the sharp indentation edges, (ii) the microhardness of the crystals depends on the applied load, (iii) the microhardness of the crystal is independent on the duration of loading, and (iv) maximum plasticity is observed in quenched crystals. The implications of this behaviour are discussed.     

Single crystal growth,structural, optical,mechanical, dielectric and thermal studies of formic acid doped potassium dihydrogen phosphate crystal for NLO applications

Optically transparent formic acid (FA) doped potassium dihydrogen phosphate (KDP) crystal of dimension 21×15×9 mm³ has been grown by slow evaporation solution technique (SEST). The X‐ray diffraction (XRD) technique was used to confirm the cell parameters and the shifts in peak positions of identified reflecting planes. The incorporation of FA in KDP has been qualitatively analyzed by fourier transform infrared analysis. The UV‐visible absorption spectrum of crystals has been recorded in the range of 200 to 900 nm and the doped KDP crystal is found to have improved optical parameters than pure KDP. The color centered photoluminescence emission spectrum of grown crystal has been illustrated in visible region. The mechanical behavior of pure and doped KDP crystal has been investigated using the Vicker's microhardness analyzer and hardness parameters have been calculated. The effect of FA on thermal stability of KDP crystal was examined by means of thermogravimetric and differential thermal analysis. The temperature dependent dielectric behavior of crystals was studied.     

Crystal growth,thermal, optical and microhardness studies of tris (thiourea) zinc sulphate - a semiorganic NLO material

Tris (thiourea) zinc sulphate (ZTS), a semiorganic nonlinear optical (NLO) material has been synthesized at 30 °C. The solubility was determined in different solvents such as water, ethanol and water mixture of ethanol (1:1). Good quality single crystals with size 10 × 8 × 6 mm³ were grown by slow evaporation technique within three weeks with approximate growth rate of 0.5 mm/day. The grown crystals have been subjected to single crystal X-ray diffraction to determine the unit cell dimensions and morphology. The TGA and DTA reveal that the material has good thermal stability. The UV-Vis spectrum shows that the material has wide optical transparency in the entire visible region. The second harmonic generation was confirmed by Kurtz powder method. The birefringence of the crystal was measured in the visible region and it was found to vary with the wavelength. The microhardness test was carried out in (100) plane and the load dependent hardness was measured. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of ferroelectric magnesium hydrogen phosphate single crystals

Ferroelectric Magnesium Hydrogen Phosphate MgHPO₄ (MHP) single crystals are grown by slow diffusion of magnesium chloride in sodium metasilicate gels impregnated with orthophosphoric acid. Bright and transparent prismatic, tabular, and isometric habit MHP crystals upto 3 × 2 × 1 mm³ are obtained. Results of chemical, X-ray diffraction, EDAX, microhardness and magnetic analysis are reported. The average etch pit density is determined by chemical etching to be 7 × 10³ cm⁻². Microtopographic investigations revealed the mechanism of crystal growth.     

Growth and characterisation of Na3Sb2F9 single crystals

Optically clear single crystals of Na₃Sb₂F₉ have been grown from solution by slow evaporation technique at constant temperature. Crystals of sizes upto 30 × 8 × 8 mm have been grown in a period of three months. Vickers microhardness measurements have been carried out on these crystals. Attempts have also been made to understand the nature of the cracks developed around the microindentation. Single crystal X-ray diffraction studies have been carried out and cell parameters are determined.     

Enhancement of thermoelectric efficiency in vapor deposited Sb2Te3 and Sb1.8In0.2Te3 crystals

Pure and indium doped antimony telluride (Sb₂Te₃) crystals find applications in high performance room temperature thermoelectric devices. Owing to the meagre physical properties exhibited on the cleavage faces of melt grown samples, an attempt was made to explore the thermoelectric parameters of p‐type crystals grown by the physical vapor deposition (PVD) method. The crystal structure of the grown platelets (9 mm× 8 mm× 2 mm) was identified as rhombohedral by x‐ray powder diffraction method. The energy dispersive analysis confirmed the elemental composition of the crystals. The electron microscopic and scanning probe image studies revealed that the crystals were grown by layer growth mechanism with low surface roughness. At room temperature (300 K), the values of Seebeck coefficient S (⊥ c) and power factor were observed to be higher for Sb_1.8In_0.2Te₃ crystals (155 μVK⁻¹, 2.669 × 10⁻³ W/mK²) than those of pure ones. Upon doping, the thermal conductivity κ (⊥ c) was decreased by 37.14% and thus thermoelectric efficiency was improved. The increased figure of merit, Z = 1.23 × 10⁻³ K⁻¹ for vapour grown Sb_1.8In_0.2Te₃ platelets indicates that it could be used as a potential thermoelectric candidate.     

Growth and characterization of semi organic nonlinear optical LHPCL crystals

The growth of single crystals of L‐histidinium perchlorate (LHPCL), a semi organic nonlinear optical material with dimension upto 5 × 6 × 2.5 mm³ is reported. Good optical quality single crystals were grown from aqueous solution by slow solvent evaporation technique. The grown crystals were characterized by single crystal X‐ray diffraction (XRD), FT‐IR and optical transmission studies. Thermal studies confirm that LHPCL has a fairly high thermal stability (272°C) when compared with other members of histidine family. The scanning electron microscopy (SEM) provides information on the quality of the samples and grain distribution over the surface of the sample. The dielectric constant and dielectric loss of the compound were measured at different frequencies, and also at varying temperatures and the results of these experiments are discussed. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of α-NiSO<Subscript>4</Subscript> · 6H<Subscript>2</Subscript>O crystals at high rates

The high-rate growth of nickel sulfate hexahydrate NiSO₄ · 6H₂O (α-NSH) crystals up to 120 × 120 × 65 mm³ in size is described for the first time. The data on the distribution of related impurities in the {011} and {001} growth sectors of α-NSH crystals grown at different rates are reported. The transmission spectra of both growth sectors of these crystals are obtained. The structural quality and the optical properties of rapidly and slowly grown α-NSH crystals are compared. It is established that the {011} growth sector of crystals grown at rates exceeding 5 mm/day shows the best characteristics for application in UV filters.     

The effect of cooling rate on size,quality and morphology of KTiOPO4 (KTP) crystals grown by different nucleation techniques

KTP crystals have been grown by two nucleation techniques namely spontaneous nucleation in flux medium and nucleation on Pt rod using K₆P₄O₁₃ flux.10 °C/h, 7 °C/h, 0.8 °C/h, 0.4 °C/h and 0.2 °C/h cooling rates were applied for spontaneous nucleation and crystals up to 15 × 7 × 4 mm³ in size were grown. 1 °C/h and 0.8 °C/h cooling rates were also used for nucleation on Pt rod and crystals up to 8 × 6 × 3 mm³ in size were grown. The effect of cooling rate on size, morphology and optical quality of grown crystals by both techniques were studied. For nucleation on Pt rod upper and lower rotation rates limits and an optimum rotation rate were distinguished for each cooling rate. Quality of the grown crystals by both techniques was characterized by optical transmission analysis.     

Crystal growth and magnetic properties of the copper coordination polymer [Cu(µ ‐C2O4)(4‐aminopyridine)2(H2O)]n

In this paper, we consider various ways of crystal growth of the polymer [Cu(µ ‐C₂O₄)(4‐aminopyridine)₂(H₂O)]_n. Single crystals of the size of 1.5×1.5×0.2 mm³ have been grown by a slow diffusion technique from solutions of the monoammine copper complex and of the mixture of potassium oxalate and aminopyridine with the stoichiometric ratio. Magnetic susceptibility and ESR measurements have been performed on single crystals large enough for investigating anisotropic properties. The susceptibility can be well described within the model of a Heisenberg antiferromagnetic spin chain. The magnetic measurements reveal a small concentration of paramagnetic moments reflecting the high quality of the single crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of BPO4 single crystals from Li2Mo3O10 flux

Transparent single crystal of BPO₄ with a typical sizes of 5 × 7 × 9 mm³ have been grown by the top-seeded solution growth (TSSG) slow-cooling method using Li₂Mo₃O₁₀ as the flux. X-ray powder diffraction result shows that the as-grown crystal was well crystallized and indexed in a tetragonal system. The processing parameters and the effects of the flux on the crystal growth were investigated.     

Studies on conventional and Sankaranarayanan–Ramasamy (SR) method grown ferroelectric glycine phosphite (GPI) single crystals

Transparent single crystals of glycine phosphite were grown by Sankaranarayanan–Ramasamy (SR) method and conventional slow evaporation solution technique (SEST) which had the sizes of 100 mm in length, 30 mm diameter and 10×11×8 mm³. The conventional slow evaporation and Sankaranarayanan–Ramasamy method grown glycine phosphite single crystals were characterized using laser damage threshold, chemical etching, Vickers microhardness, UV–vis–NIR and dielectric analysis. The laser damage threshold value was higher in SR method grown GPI crystal as against conventional method grown crystal. The SR method grown GPI has higher hardness and also higher transmittance compared to conventional method grown crystal. The chemical etching and dielectric loss measurements indicate that the crystal grown by SR method has low density of defects and low value of dielectric loss compared to conventional method grown GPI crystal.     

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 and characterization of KBi(WO4)2 single crystals

Potassium bismuth tungstate [KBi(WO₄)₂] single crystals with dimensions up to 20 mm × 15 mm × 15 mm have been successfully grown by using the top‐seeded solution growth technique and K₂W₂O₇ as solvent. Experiments show that this crystal is unstable in a strong acid or alkali environment and has a blue fluorescence emission. The density, hardness, melting point, absorption edge, transparency range, prominent Raman shift frequency are 7.57 g/cm³, 238 kg/mm², 800 °C, 380 nm, 400–5450 nm, 868 cm^–1 respectively. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)