Growth and characterization of Struvite‐K crystals

Struvite‐K is the natural potassium equivalent to Struvite. Struvite‐K crystals were grown by single diffusion gel growth technique in silica hydro gel medium. Struvite‐K crystals with different morphologies having transparent to translucent diaphaneity were grown with different growth parameters. The phenomenon of Liesegang rings was also observed with some particular growth parameters. The crystals were characterized by powder XRD, FT‐IR, TGA and dielectric study. The powder XRD results of Struvite‐K confirmed the orthorhombic crystal structure. The FT‐IR spectrum proved the presence of water of hydration, metal – oxygen bond and P – O bond. The TGA, DSC and DTA were carried out simultaneously. It was found that crystals started dehydrating and decomposing from 75 °C and finally at 600 °C temperature it became 64.14% of the original weight and remained almost constant up to the end of analysis. From the thermo‐gravimetry, the numbers of the water molecules associated with the crystal were calculated and found to be 5. The kinetic and thermodynamic parameters of dehydration / decomposition process were calculated. The variation of dielectric constant with frequency of applied field was studied in the range from 400 Hz to 100 kHz, which exhibited the decreasing nature of the dielectric constant as frequency increased. The dielectric study showed that a.c. conductivity increased and consequently the a.c. resistivity decreased with the increase in frequency. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of barium oxalate crystals in agar–agar gel and their characterization

Single crystals of barium oxalate have been grown by gel method using agar‐agar gel as media of growth at ambient temperature. The optimum conditions were established by varying various parameters such as concentration of gel, concentration of reactant, gel setting time etc. Prismatic platy shaped transparent crystals were obtained. The grown crystals were characterized through powder X‐ray diffraction (XRD), Fourier transform infrared (FT‐IR) studies, Thermogravimetric (TGA) and Differential thermal analysis (DTA). The compound crystallizes under monoclinic structure with lattice parameters a = 6.6562 Å, b = 8.0464 Å, c = 2.8090 Å, β= 96.832°, and V = 149.38 ų. The FT‐IR spectrum indicates OH and carbonyl group along with the presence of metal‐oxygen bond. The TGA indicates 17.75% weight loss at 550°C from which the decomposition pattern is formulated. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Characterization of gel grown iron‐manganese‐cobalt ternary levo‐tartrate crystals

In the present investigation, iron–manganese–cobalt ternary levo‐tartrate crystals of different compositions have been grown by single‐diffusion gel growth technique in silica hydrogel medium. The metallic composition in the crystals was estimated by EDAX. The coloration of the crystals changed with composition of metallic content. The powder XRD study suggested the crystalline nature and indicated the presence of some extra phases. The grown crystals were characterized by FT‐IR spectroscopy, TGA, dielectric and Vibrating Sample Magnetometer (VSM) studies. The FT‐IR study suggested the presence of O‐H, C=O, C‐O and metal‐oxygen bonds. The effect of composition of metallic content was observed in certain absorption regions in FT‐IR spectra. The thermal stability of the crystals was studied by thermogravimetry and the kinetic and thermodynamic parameters of dehydration were calculated. The effect of composition of ternary levo‐tartrate was observed in dielectric study. The dielectric study was carried out in the frequency range of applied field from 500 Hz to 1 MHz. The variations in dielectric constant, dielectric loss, a.c. resistivity and a.c. conductivity with frequency of applied field were studied. VSM study suggested that all crystals were of paramagnetic nature. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of tris allylthiourea mercuric chloride crystals

Single crystals of tris allylthiourea mercury chloride (ATMC), a semi‐organic nonlinear optical material, have been grown from a low‐temperature solution growth technique by slow cooling method. In the present work, we have grown ATMC crystal which is a new nonlinear optical material (NLO) having high optical quality and its second harmonic generation (SHG) efficiency is thrice that of Urea. The grown crystals have also been subjected to various characterization studies like X‐ray diffraction, UV‐VIS, FT‐IR and TGA‐DTA. X‐ray powder diffraction study confirmed the crystal structure of ATMC, UV‐VIS /FT‐IR spectral analysis showed the crystal has good optical transmission in the entire visible region and TGA‐DTA studies showed the thermal properties and complex degradation of ATMC crystal. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of Mn2+ doped calcium l‐tartrate crystals

Single crystals of Mn²⁺ doped calcium levo‐ tartrate tetrahydrate (CLTT) were grown by single diffusion gel growth technique in silica hydro‐gel media. The doping of Mn²⁺ was varied by mixing 0.001M, 0.005M, 0.01M, 0.05M, and 0.1M solutions of MnCl₂ with 1M CaCl₂ solution in equal volumes in the supernatant solutions. The actual amount of Mn²⁺ doping in CLTT crystals was estimated by ICP (Inductively Coupled Plasma) technique. The powder XRD of the samples suggested no significant change in the unit cell dimensions and the presence of any extra phase. The FT‐IR spectra indicated the presence of water molecule, O‐H bond, C‐O bond and carbonyl C=O bond. The EPR spectra confirmed the presence of Mn²⁺ ions in the crystals. The variation of the dielectric constant with temperature confirmed the earlier results of pure calcium tartrate crystals and indicated the ferroelectric nature of the doped crystals. As the amount of doping of Mn²⁺ increased the value of dielectric constant increased. The results are discussed. (© 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 calcium hydrogen phosphate dihydrate crystals from single diffusion gel technique

Calcium hydrogen phosphate dihydrate (CaHPO₄·2H₂O, CHPD) a dissolved mineral in urine is known to cause renal or bladder stones in both human and animals. Growth of CHPD or brushite using sodium metasilicate gel techniques followed by light and polarizing microscopic studies revealed its structural and morphological details. Crystal identity by powder x‐ray diffraction confirmed the FT‐IR and FT‐Raman spectroscopic techniques as alternate methods for fast analysis of brushite crystals which could form as one type of renal stones. P‐O‐P asymmetric stretchings in both FT‐IR (987.2, 874.1 and 792 cm^‐1) and FT‐Raman (986.3 cm^‐1, 1057.6 cm^‐1 and 875.2 cm^‐1) were found as characteristics of brushite crystals. Differential Scanning Calorimetry (DSC) analysis revealed brushite crystallization purity using gel method by studying their endothermic peaks. This study incorporated a multidisciplinary approach in characterizing CHPD crystals grown in vitro to help formulate prevention or dissolution strategy in controlling urinary stone growth. Initial studies with 0.2 M citric acid ions as controlling agent in the nucleation of brushite crystals further support the presented approach. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

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)     

Influence of calcium binding proteins on the precipitation of calcium carbonate: A kinetic and morphologic study

In our experiments, the thermodynamic effect of calcium binding proteins (CBP) on the growth of calcium carbonate (CaCO₃) was studied in vitro. The CaCO₃ crystals obtained in systems with and without CBP were characterized by scanning electron microscope (SEM), Fourier Transform Infrared spectrograph (FT‐IR) and powder X‐ray diffractometer (XRD). The kinetic process was studied by monitoring the conductivity and pH value, which revealed the obvious inducement effect of CBP on the CaCO₃ crystals growth, and the possible formation mechanism of CaCO₃ in CBP solution was discussed. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth,optical, mechanical and electrical properties of organic NLO material γ‐glycine

Single crystals of organic non‐linear optical material, γ‐glycine have been grown by gel method for the first time. The γ‐phase is confirmed by single crystal XRD. The presence of various functional groups of γ‐glycine are confirmed by FTIR. The UV‐Vis‐NIR spectrum reveals the high percentage of transmission of the sample in the entire visible region. The SHG of γ‐glycine is confirmed by Kurtz powder technique. TGA‐DTA studies indicate that the crystal is structurally stable upto 170 °C. Microhardness investigations are conducted on the grown crystals. The dielectric constant measurements are carried out and the nature of variation of dielectric constant ε′ and dielectric loss D in the frequency range of 50 Hz to 5 MHz is studied and reported. Photoconductivity studies of γ‐glycine crystals revealed the negative photoconducting nature. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of semiorganic NLO crystals of LAHClBr

Single crystals of non‐linear optical (NLO) LAHClBr were grown by slow evaporation technique from its aqueous solution. Good optical quality crystals having dimensions up to 12 × 9 × 7 mm³ were obtained. The lattice parameters and morphology for the grown crystals were determined using single crystal XRD. The crystals were characterized by FT‐Raman, optical absorption, thermal (DTA and TGA) and dielectric studies. LAHClBr was found to be thermally stable up to 124.3°C. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Aspergillums Niger assisted crystal growth of calcium tartrate: an alternative method to grow crystals

A novel method of growing calcium tartrate single crystals was developed in which the crystals were hanging freely in solution assisted by fine filaments of fungi (Aspergillums niger). Spores of A. niger were inoculated and allowed to grow in the supernatant solution of calcium chloride and tartaric acid (1:1) on the silica hydro‐gel impregnated with orthophosphoric acid. Transparent, prismatic, calcium tartrate crystals were grown hanging in the filamentous network of the fungi after 10 days in the supernatant solution. This network of the mycelium facilitated and mimicked the gel. The grown crystals were identified as calcium tartrate trihydrate and characterized by powder XRD, FTIR and TGA. This technique provides an alternate and a novel technique to grow crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

FT‐IR spectroscopic and thermal studies on pure and impurity added calcium tartrate tetrahydrate crystals

Pure and impurity (strontium) added calcium tartrate tetrahydrate single crystals were grown by the gel method. The FT‐IR spectra of these crystals were recorded in the wavenumber range 400–4000 cm^–1. The thermograms of the grown crystals were recorded in the temperature range 50–900 °C. FT‐IR spectra reveals the presence of water molecules, O‐H bond, C‐O and carbonyl C=O bonds. The thermograms show that these crystals are thermally unstable and decompose into its oxide through many stages. DTA curve of the pure crystal shows three endothermic and one exothermic peaks. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of ytterbium tartrate trihydrate crystals in silica and agar‐agar gels and their characterization

Single crystals of ytterbium tartrate trihydrate have been grown by gel method using silica and agar‐agar gels as media of growth. The medium of growth influences the morphology of grown crystals, silica gel yielding single and polycrystalline in the form of spherulites whereas agar‐agar gel leading to growth of single and twinned crystals. Materials grown as single crystals have been characterized by using optical and scanning electron microscopy (SEM), EDAX, XRD, FT‐IR, CHN and thermogravimetric techniques. The stoichiometry of the grown single crystals is suggested to be Yb(C₄H₄O₆) (C₄H₅O₆).3H₂O. The FT‐IR spectrum shows the presence of singly as well as doubly ionized tartrate ligands. Results of thermal analysis indicate that the material is thermally stable up to a temperature of 200 °C. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical and microhardness studies of semiorganic nonlinear optical material: L‐ histidine tetrafluoroborate

L‐histidine tetrafluoroborate (L‐HFB) a semiorganic nonlinear optical material has been synthesized in aqueous solution at 50°C and characterized by FT‐IR and FT‐Raman spectroscopy studies. The solubility was determined in different solvents such as water, methanol and water mixture of methanol. The single crystals with dimensions 15x12x3 mm³ were grown by slow evaporation method within four weeks with approximate growth rate of 0.25 mm/day. The grown crystals have been subjected to single crystal X‐ray diffraction studies to determine the unit cell dimensions and morphology. The Kurtz powder second harmonic generation test shows that the compound is a potential candidate for frequency conversion. The refractive index has been measured using He‐Ne laser. The microhardness test was carried out and the load dependence hardness was observed. The material has a wide transparency in the entire visible region. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural,thermal and optical characterizations of a NLO material: L‐alaninium oxalate

An organic electro‐optic and nonlinear optical (NLO) material, L‐alaninium oxalate, was synthesized by the standard method. The synthesized material was purified by repeated recrystallization. Single crystals were grown by the slow evaporation technique. The grown crystals were transparent and had optimum dimensions (20 × 3 × 2 mm³) and were characterized by single crystal XRD, FT‐NMR, FT‐IR, TGA‐DTA and UV‐Vis‐NIR techniques. The second harmonic generation (SHG) from the material was confirmed using Nd:YAG laser. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of 4‐(2‐hydroxyphenylamino)‐pent‐3‐en‐2‐one single crystals

4‐(2‐hydroxyphenylamino)‐pent‐3‐en‐2‐one (HPAP) was synthesized and single crystals were grown by the solution growth technique using methanol as a solvent. The crystals having orthorhombic symmetry were characterized by single crystal XRD, FTIR spectroscopy, NMR spectroscopy, TGA, DSC and dielectric studies. Very less variation in the value of dielectric constant is found for different frequencies of applied field. The crystals were exhibiting positive photoconductivity and poor NLO responses. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Calcium oxalate crystallization in the presence of amino acids,proteins and carboxylic acids

Reactive crystallization of calcium oxalate was investigated in the presence of amino acids, proteins and carboxylic acids at different pH and temperatures. Average particle size, filtration rates of calcium oxalate crystals obtained in the absence and presence of additives were determined. The influence of pH, temperatures and additives on crystal morphology of calcium oxalate were also investigated and discussed by SEM analysis. TG‐DTA, FT/IR and XRD analysis were carried out for all investigated conditions. Average particle size of calcium oxalate was affected significantly by the additive type and concentration. Variation of crystal morphology depending on type and concentration of the additives affected the filtration characteristics. Majority of calcium oxalate crystals occurred in the form of calcium oxalate monohydrate except those in the presence of tartaric acid. TG‐DTA, FT/IR and XRD analysis proved that calcium oxalate monohydrate and calcium oxalate dihydrate mixtures are formed in the presence of tartaric acid. The effect of all additives on scale formation was also investigated. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of the nonlinear optical crystal: L‐arginine trifluoroacetate

Single crystal growth of the organic nonlinear optical crystal, L‐arginine trifluoroacetate (L‐Arg·CF₃COOH, abbreviated as LATF) is reported. Low temperature solution growth method is employed for the growth of bulk single crystals. The cell parameters are verified by single crystal diffraction. Fourier transform infrared (FT‐IR) and Fourier transform Raman analysis are used to confirm the presence of various functional groups in the grown crystal. The thermal properties of the grown crystals are studied by thermogravimetric analysis and differential scanning calorinetry analysis (TGA/DSC). Second harmonic generation (SHG) measurement confirms the NLO properties of the grown crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)