Growth and characterization of L‐lysine monohydrochloride dihydrate (L‐LMHCl) single crystal

A nonlinear optical crystal of L‐lysine monohydrochloride dihydrate (L‐LMHCl) was grown by slow evaporation solution growth technique using deionised water and mixed solvents of deionised water and ethanol. The functional groups and vibrational frequencies were identified using FTIR and FT‐RAMAN spectra analyses. Also, the presence of hydrogen and carbon atoms in the grown sample was confirmed using proton and carbon NMR spectra analyses. Using TG‐DTA analyses, the decomposition temperature was obtained. Transmittance of the grown crystals was analysed using UV‐visible spectrum. The mechanical strength of the grown crystals was found using Vicker's microhardness tester. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth,spectral and thermal studies of ibuprofen crystals

RS ‐Ibuprofen was crystallized for the first time in silica gel under suitable pH conditions by reduction of solubility method. The grown crystals were characterized by single crystal X‐ray diffraction and density measurement. The functional groups present in the crystal were identified using Fourier transform infrared spectroscopy. Optical bandgap energy of ibuprofen was estimated as 3.19(3) eV from UV‐Vis spectrum. Thermogravimetric analysis revealed that ibuprofen is thermally stable upto 102.9 °C and the initial loss of mass was due to evaporation only. Morphological study showed that the growth is prominent along b‐axis and the prominent face is {100}. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

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 a new semi organic NLO material: L‐tyrosine hydrochloride

Single crystals of L‐Tyrosine hydrochloride were grown by using the submerged seed solution method. The grown crystals were characterized by using single crystal X‐ray diffraction. Functional groups and the modes of vibrations were identified by FTIR spectroscopy. The TGA/DTA studies showed that the crystal is stable up to 232°C. Microhardness study revealed that the crystal is a hard material. It is transparent in the entire visible region. The SHG efficiency was determined by the Kurtz and Perry method. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth,structural, thermal and optical studies on L‐glutamic acid hydrobromide – A new semiorganic NLO material

A new semiorganic crystal, L‐glutamic acid hydrobromide, C₅H₁₀NO₄Br (GHB) has been grown from aqueous solution. The single crystal X‐ray analysis of the crystal showed that it belongs to the non‐centrosymmetric P2₁2₁2₁ space group with protonated glutamic acid as cation and bromine as anion. The back‐bone conformations of the amino acid are in cis and trans form. The side‐chain conformations are observed to be in gauche I / trans / cis / trans forms. The characteristic ‘head‐to‐tail’ hydrogen bonding interaction is observed through a chain C(5) motif. Further, the crystal structure is stabilized by an intricate three‐dimensional hydrogen bonding network. TGA/DTA showed that the grown crystals are thermally stable upto 219 °C without any phase transition. The functional groups responsible for the various modes of vibrations were identified by using FTIR spectroscopy. UV‐Vis‐NIR spectra showed that the crystals have excellent transparency in the visible and infrared regions. The second harmonic generation (SHG) conversion efficiency was investigated to explore the NLO characteristics of the material. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of large La1‐xPbxMnO3+δ (x=0.32–0.35) crystals

Large crystals of La_0.63Pb_0.37Mn O_3+δ with small La(Pb)‐ deficiency of about 0.005‐0.01 at.% were grown by high temperature solution growth method. The structure of the grown crystals was determined as rhombohedral with R‐3 space group by single‐crystal X‐ray diffractometry. The surface morphology of the crystals and the exact chemical composition was examined by scanning electron microscopy and energy dispersive X‐ray analysis methods, respectively. The IR‐transmission spectrum reveals the presence of Mn³⁺O₆‐ and Mn⁴⁺O₆‐ octahedra in the lattice of La_0.63Pb_0.37Mn O_3+δ crystals. (© 2009 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)     

Growth of tetrakis thiourea potassium iodide as new second order optical material

A novel organometallic nonlinear optical (NLO) crystal, namely thiourea complex of tetrakis thiourea potassium iodide (TTPI), has been grown by slow evaporation solution growth technique. The harvested crystal is large in size. To our knowledge there is no report is available for the bulk size single crystal of TTPI. This material has a positive temperature coefficient and has been grown by slow evaporation solution growth technique. The grown crystal have been characterized by employing several techniques such as single crystal and powder X‐ray diffraction, FTIR, UV‐Vis‐NIR spectra, thermo gravimetric analyses respectively. Etching studies have also been carried out in order to know the surface defects on the as grown specimen of TTPI. The relative second harmonic generation efficiency have been tested by using Nd:YAG laser as source. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of CuInS2 single crystals from Sb2S3 and Bi2S3 solutions

The phase diagrams of the CuInS₂‐Sb₂S₃ and CuInS₂‐Bi₂S₃ systems were investigated using X‐ray powder diffraction and differential thermal analysis. Based on these results, the compositions for the growth of the CuInS₂ single crystals from CuInS₂‐Sb₂S₃ and CuInS₂‐Bi₂S₃ melts were selected and Bridgman crystal growth process was performed. The investigation of the obtained single crystals using X‐ray powder diffraction and optical absorption spectra indicates that the incorporation of the solvent atoms into the crystal lattice is absent. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of dihydroxylammonium tetrachlorocuprate dihydrate crystals

A new hydroxylammonium compound, [(NH₃OH)₂CuCl₄], was synthesized and its crystals were grown at room temperature by slow evaporation of aqueous solutions. The crystals were characterized through powder XRD, thermogravimetry (TG), differential thermal analysis (DTA), low temperature differential scanning calorimetric (DSC) and FTIR spectra. The X‐ray powder diffraction confirms the crystallinity of the compound. A fitting decomposition pattern of the compound was formulated based on the TG and thereby confirming the formation of the compound in the stoichiometric ratio. The thermal anomalies occurring in the low temperature DSC indicate successive phase transitions. The low temperature phase transitions are attributed to the ordering of [NH₃OH]⁺ ions. While most of the phase transitions are of first order type, the one occurring at –126 °C is of second order. Two glass transitions occur when the compound was cooled between –157.9 and –136.9 °C. The characteristic vibration bands due to [NH₃OH]⁺ and CuClequation/tex2gif-stack-1.gif ions are observed in the IR spectra. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Low temperature photoluminescence studies on semiorganic tris thiourea copper (I) chloride single crystal

Semiorganic tris thiourea copper (I) chloride (TTCC) single crystals have been synthesized from copper (II) chloride via slow evaporation technique. The stoichiometry of the grown anhydrous complex crystal has been confirmed by elemental CHNS (C, H, N and S) and atomic absorption spectrophotometric (AAS) analysis. The crystal structure with space group has been confirmed by single crystal and powder X‐ray diffraction (XRD) studies. The FTIR study assigned the presence of functional groups and confirmed the co‐ordination of metal ions with thiourea. It also confirmed the transition from Cu²⁺ to Cu⁺ when thiourea combined with Copper (II) chloride. The optical transparency of the crystal has been studied by UV‐Vis spectrum and deduced the energy gap. The room temperature Photoluminescence (PL) spectrum reported maximum emission line at 410.92 nm and Stokes shift has been determined as 75 nm or 16.5 eV. Low temperature luminescence study from 300 K to 77 K exhibited three blue emission peaks and one green emission peak. The green emission band has been assigned to recombination of an electron in a shallow trap and Cu²⁺. Blue emission has been attributed to S^2‐ vacancies. The interesting hysteresis loop has been exhibited by the variation of energy gap with low temperature. (© 2012 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)     

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 4‐Aminopyridinium‐4‐nitro phenolate single crystals

Organic optical material 4‐Aminopyridinium‐4‐nitro phenolate (4AP4NP) has been synthesized, and single crystals of size 20 x 14 x 6 mm³ have been grown from acetone solvent at room temperature by solvent evaporation technique. The grown crystals have been characterized by X‐ray diffraction to determine the cell parameters, and by FT‐IR technique to confirm the formation of the expected compound. The crystal belongs to monoclinic crystal system with space group P2₁/a.The structural perfection of the grown crystals has been analyzed by high‐resolution X‐ray diffraction (HRXRD) rocking curve measurements. The thermal stability of the compound has been determined by TG‐DTA curves. The transmittance of 4AP4NP has been used to determine the refractive index n; the extinction coefficient K and both the real ε_r and imaginary ε_i components of the dielectric constant as functions of photon energy. The optical band gap of 4AP4NP is 2.4 eV. The dielectric and mechanical behavior of the specimen was also studied. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,growth, morphology and characterization of ferroelectric glycine phosphite single crystals

Glycine phosphite (NH₃CH₂COO.H₃PO₃), a potential ferroelectric material, was grown as single crystals from aqueous solutions by slow evaporation and slow cooling methods. Laboratory synthesized title compound was purified by recrystallization method and confirmed by Fourier transform infrared and Laser Raman studies. Temperature dependent solubility in double distilled water in the range between 288 and 328 K was determined by gravimetric method. Morphological importance of various growth faces were studied by optical goniometry. Powder x‐ray diffraction study performed on the grown crystals confirms the crystal system and lattice parameters of the unit cell. Optical transparency of the grown crystals in the ultraviolet–visible ‐near infrared region was studied by spectroscopic method. Thermal stability of the grown crystals in the temperature region above ambient until melting was studied using differential scanning calorimetry. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,growth and characterization of S‐benzyl isothiouronium chloride single crystals

S‐Benzyl isothiouronium chloride single crystals were grown at room temperature by slow evaporation solution growth technique. Single crystal X‐ray diffraction study has been carried out to find the crystal system and unit cell parameters. Various functional groups present in the grown material have been identified using FTIR spectra. The transparency of crystal was tested using UV‐visible spectra. The grown crystal exhibits second harmonic generation (SHG). TGA/DTA analysis also carried out. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth and structure of KBi(WO4)2 single crystals

Potassium bismuth tungstate [KBi(WO₄)₂] single crystals have been grown by the top‐seeded solution growth technique. Bulk crystal with dimensions up to several centimeters is obtained for the first time. Several self‐flux systems have been used for the growth from the solution and the experiments using K₂W₂O₇ as a solvent are detailed. Powder and single crystal X‐ray diffraction of this crystal are reported. The structure refinement shows that KBi(WO₄)₂ crystallizes in the monoclinic space group C2/c, with a=10.837(3), b=10.586(3), c=7.622(2)Å, β=130.860(3)°, V=661.4(3)ų, and Z=4. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of strontium chloride on the optical and mechanical properties of γ–glycine crystals

Single crystals of γ‐glycine have been grown from aqueous solution in the presence of small amount of strontium chloride. Single crystal X‐Ray diffraction analysis was used to measure the unit cell parameters and to confirm the crystal structure. The grown crystals have also been subjected to powder X‐Ray diffraction study to identify the crystalline nature. The presence of all the functional groups of the γ‐glycine has been confirmed by Fourier Transform Infrared (FTIR) spectral analysis. The presence of hydrogen and carbon in the glycine molecules was confirmed by using proton and carbon nuclear magnetic resonance (NMR) spectral analyses. Optical behavior of the crystal was studied using UV – Visible absorbance spectroscopy and second harmonic generation (SHG) studies. The SHG efficiency of γ‐glycine is greater than that of standard potassium dihydrogen phosphate (KDP). Mechanical strength of the γ‐glycine crystal has been determined by microhardness studies. Thermal stability of the grown crystal is probed using thermo gravimetric analysis and differential thermal analysis. Laser damage threshold value has been determined using Q‐switched Nd:YAG laser operating at 1064 nm and with 13 ns pulse width in single shot mode. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of YCOB single crystals by flux technique and their characterization

Nonlinear optical single crystals of YCOB with good optical quality were grown by the flux technique for the first time. Polycrystalline YCOB samples were synthesized by solid state reaction method. The thermal analysis of the sample was performed with lithium carbonate flux in different weight proportions and the growth temperature was optimised. Single crystals of YCOB with dimensions 3 × 3 × 5 mm³ were obtained by the method of ‘slow‐cooling’. The grown crystals were characterized by XRD, UV‐VIS‐NIR, EDAX, FTIR and etching studies. The powder XRD pattern revealed the formation of YCOB compound. The lattice parameters were identified through single crystal XRD studies. The UV‐VIS‐NIR results showed that the crystal has a sharp cutoff at 220 nm and is nearly 55% transparent over a wide wavelength range enabling applications in the UV region. The EDAX measurement revealed the ‘flux‐free’ crystal formation. The presence of the functional groups belonging to the YCOB crystals was identified by the FTIR results. ‘Hillock‐like’ patterns are observed in the etching studies. The primary emphasis in this study is laid to describe ‘flux technique’ as an alternative method to grow YCOB crystals. The results are presented and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)