Investigations on nucleation,thermodynamical parameters and growth of Benzimidazole crystals from low temperature solution

Metastable zonewidth and induction period measurements of Benzimidazole (BMZ) are presented. The nucleation parameters such as interfacial tension, radius of the critical nucleus and critical free energy change have been calculated for the solution grown Benzimidazole (BMZ) single crystals at different supersaturation ratios. The grown BMZ crystals were characterized by the differential scanning calorimetric studies for analysis of thermal properties. The dielectric behaviour of the crystal was studied at different temperature and frequency. The laser damage threshold studies show that BMZ crystal has higher laser damage threshold. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical and dielectric studies on pure and Ni2+, Co2+ doped single crystals of bis thiourea cadmium chloride

Good quality single crystals of Ni²⁺, Co²⁺ ions doped Bisthiourea Cadmium Chloride (BTCC) are some of the excellent and efficient non‐linear optical materials grown from aqueous solution by slow evaporation method. The lattice parameters of the grown crystals are determined by single crystal X‐ray analysis. UV spectral analyses on these samples reveal the improved transparency of the doped crystals ascertaining the inclusion of metal ion in the lattice. FTIR spectral analysis carried out on the materials confirm the presence of functional groups. Dielectric measurements reveal that the dielectric constant of pure and doped crystals decreases with increase of frequency. (© 2008 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)     

Optical and mechanical properties of a new second order nonlinear optical crystal urea l‐threonine

A new second order non‐linear optical organic crystal Urea L‐threonine has been grown by aqueous solution slow cooling technique. The grown crystal is non hygroscopic and transparent in the visible region. The solubility of the grown crystal was found. The crystal structure and perfection were determined using powder XRD and High resolution XRD. The molecular structure was confirmed by ¹H‐NMR spectrum. Thermal properties of the crystal have been studied using thermogravimetric (TG) and differential thermal analysis (DTA). The dielectric response of the crystal with varying frequencies at different temperatures was studied. UV‐Visible spectrum was recorded to study the optical transparency of the grown crystals. The second order non linear optical property was examined by Kurtz powder technique and found that the second order susceptibilities is 1.2 KDP at wavelength 1064 nm. The mechanical behaviour was studied by Vickers Microhardness test. The results are discussed in detail. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural and mechanical properties of KН2PО4 single crystals with embedded nanoparticles and organic molecules

Single crystals of KDP crystals with embedded Urea molecules and TiO₂ nanoparticles have been grown from aqueous solution by the temperature lowering method. The effect of the organic molecules and nanoparticles on the structural and mechanical properties has been studied. It has been observed that addition of Urea molecules improves laser induced damage threshold and mechanical strength of the crystal, while TiO₂ nanoparticles have the opposite effect. The structure and composition of KDP:Urea crystal are studied by three‐crystal X‐ray diffraction analysis, which reveals the existence of a correlation between the increase of the microhardness value and the change of the crystal lattice parameter. The surface features of KDP:TiO₂ crystals are analyzed by scanning electron microscopy that reveals the presence of quasi‐equidistant growth bands caused by capture of the nanoparticles. It is shown that the rise of TiO₂ nanoparticles concentration up to 10⁻⁴ wt.% and higher resulted in 3‐fold reduction of the laser damage threshold of KDP:TiO₂ relative to pure KDP in [001] and [100] crystallographic directions. It is found that microhardness and fracture toughness decrease at the nanoparticles concentration of 10⁻³ wt.% due to crack formation at crystal lattice discontinuities. The grown crystals also have been subjected to dielectric studies.     

Growth and characterization of pure and Hg2+ doped thiosemicarbazide cadmium chloride crystals

Semiorganic single crystals of thiosemicarbazide cadmium chloride (TSCCC) and mercury ions doped thiosemicarbazide cadmium chloride were synthesized by slow solvent evaporation technique. The grown crystals were subjected to powder X‐ray analysis and both the crystals were found to crystallize in the monoclinic system. EDAX analysis was carried out for chemical analysis of the grown crystals. The UV‐Vis‐NIR spectrum shows that both the materials have wide transparency window in the visible and near IR region. The dielectric studies were carried out to estimate the dielectric constant and dielectric loss with respect to frequency for both the crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Etching and dielectric studies on L‐lysine monohydrochloride dihydrate single crystal

The nonlinear optical single crystals of L‐Lysine monohydrochloride dihydrate (L‐LMHCl) have been grown and examined by High‐resolution X‐ray diffraction and etching studies for their perfection. The vibrational frequencies have been identified by the micro‐Raman studies and the dielectric behaviour has been studied and the results are presented in detail. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of pure and lithium doped L‐alanine single crystals for NLO devices

Single crystals of pure and lithium substituted L‐alanine are successfully grown by slow evaporation method at constant temperature of 32°C. The effect of lithium dopant on crystal properties has been studied. Powder and single crystal XRD analysis confirms the structure and change in lattice parameter values for the doped crystals. The crystals were characterized by solubility studies, density, melting point measurements, FTIR and UV‐Vis‐NIR techniques. Thermal and mechanical stability of crystals were tested by TGA/DTA and micro hardness analysis. NLO activity of the crystals is found to be increased in the presence of lithium ions. The dielectric constant and dielectric loss of the crystals were studied as a function of frequency. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

Physico-chemical properties of pure and x-ray irradiated single crystals of KAP

Single crystals of potassium hydrogen phthalate (KAP) have been grown by slow evaporation method from aqueous solutions. Thermal analyses indicate that KAP crystals decompose into phthalic anhydride and KOH around 520 K. Electrical properties of single crystals of KAP have been studied along with the effect of X-ray irradiation of the crystals. The electrical transport appears to be associated with tunneling of protons. The irradiated crystal exhibits lower dielectric constant and higher ac conductivity.     

Growth,spectral and thermal properties of KAP single crystals in the presence of DL‐Alanine and L‐Methionine amino acid dopants

Single crystals of potassium acid phthalate (KAP) and amino acid (DL‐Alanine, L‐Methionine) doped KAP were grown from aqueous solutions by slow cooling method. The grown crystals were characterized using powder X Ray diffraction (XRD) and Fourier Transform Infrared (FTIR) analysis. The thermal stability of KAP in the presence of dopants was analysed using Thermogravimetric and Differential Scanning caloriemetric (TGA/ DSC) studies and the maximum temperature for non linear optical application of this compound in the presence of dopants was found out. The transmittance of KAP was found to increase in the presence of dopants. Etch pits were observed for all the crystals using different etchants. Vickers microhardness tests were performed to study the mechanical stability of the crystals. The hardness of DL‐alanine doped KAP is more than that of L‐alanine doped KAP crystal. The dielectric constant and loss were determined as a function of temperature. Frequency response of the dielectric constant and dielectric loss factor have been studied over the frequency range of 50Hz – 5MHz. Second harmonic generation (SHG) was confirmed in all the crystals using the Kurtz and Perry powder technique. (© 2008 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)     

Solution growth of new ferroelectric glycine phosphite unidirectional single crystals at room temperature

Glycine phosphite [NH₃CH₂COOH₃PO₃], abbreviated as GPI is the second hydrogen bonded ferroelectric crystal combination of phosphorous acid and amino acid following βnine phosphite crystals abbreviated as BPI. Sankaranarayanan and Ramasamy‐Technique was adopted to prepare the ferroelectric glycine phosphite unidirectional single crystal. The growth orientation was imposed by the pre‐grown 〈010〉 seed. As water was the solvent, transparent, colourless crystal with cylindrical shaped ingot of sized 20mm‐diameter was grown. Powder X‐ray diffraction, HRXRD, FTIR, dielectric and mechanical studies were carried out. The results are discussed in detail. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth and characterization of Au3+ ion irradiated 2-amino-5-nitropyridinium hydrogen oxalate (2A5NPHO)

2-amino-5-nitropyridinium hydrogen oxalate (2A5NPHO) was grown using slow evaporation and bulk crystal of 2A5NPHO was harvested from Assembled Temperature Reduction (ATR) method. Cut and polished crystal was irradiated using Au³⁺ ion with various fluences. Electronic loss, nuclear energy loss and penetration depth were calculated using SRIM software. It was observed in X- ray pattern that intensity of peak was reduced. Intensity of peak decreased with increase of ion fluencies from 10¹³ ions/cm² to 10¹⁴ ions/cm². Optical properties were measured using UV-Vis spectrometer. The increase of absorption was due to excited electrons which were formed by vacancies and formation of additional defects centres. Energy band gap of irradiated crystals increased with increase of ion fluence. Energy band gap of irradiated crystals were 3.39 eV, 3.42 eV, and 3.4 eV for 10¹³ ions/cm², 5 × 10¹³ ions/cm² and 10¹⁴ ions/cm² respectively and increase of band gap was due to the increase of forbidden gap. Microhardness was calculated using Vicker's Hardness tester. Increase of microhardness in irradiation crystal was due to increase of high density lattice defects produced by Au³⁺ of 10.8 MeV. Electrical property was calculated using dielectric constant. Increase of dielectric constant was due to large polarization which caused by disorderness and rich defects in the crystalline surface. Decrease of intensity peak in fluorescence was due to transition of excited electron to intermediated energy levels from excited state which converted into vibrational energy of lattice atoms (phonon). Morphology of irradiated crystal was seen using scanning electron microscope (SEM). It was observed from the SEM image that surface of crystal was heavily damaged. It was also noticed that the thermal stability of the irradiated single crystal increased with increase of ion fluences. Impedance of irradiated crystal was measured. The bulk resistance and grain boundary resistance also were calculated.     

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)     

Optical,mechanical and thermal properties of p‐bromoacetanilide

Solubility and metastable zonewidth were estimated for p‐Bromoacetanilide. Employing slow evaporation method crystals of size 22x17x6 mm³ and 38x25x10 mm³ were grown at a constant temperature of 40°C and room temperature respectively from methanol solution. The cell dimensions were obtained by single crystal X‐ray diffraction study. The placement of protons was identified from NMR spectral analysis. UV‐Visible and fluorescence spectral analyses were carried out for the grown crystals. Vickers microhardness test was performed on the prominent (110) of the as grown crystal. Thermogravimetric and differential scanning calorimetric studies were carried out to determine the thermal properties of the grown crystal. (© 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)     

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)     

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)