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)     

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)     

Vibrational Studies of Gel Grown Ferroelectric RbHC4H4O6 and SrC4H4O6 4H2O Crystals

Single crystals of Rubidium Hydrogen Tartrate (RbHT) and Strontium Tartrate Tetrahydrate (SrTT) have been grown by a gel technique using a chemical reaction method. A controlled reaction has been employed between tartaric acid and feed solution (RbCl for RbHT and Sr(NO₃)₂) at room temperature. The laser Raman and FT-IR spectra of these crystals are recorded in the frequency range 100 - 4000 cm^-1. The presence of tartrate ion, monohydrogen tartrate ion, water molecules and external mode vibrational frequencies are identified and discused. The doublet and broad nature of tartrate ion vibrational frequencies have also been observed and analysed.     

Dendritic structures in gel grown Gypsum

Sparingly water soluble Calcium Sulphate dihydrate (Gypsum) single crystals are grown by gel method, derived from the highly soluble reactants, Calcium Chloride and ammonium sulphate. By the diffusion of 1M Calcium Chloride solution into Sodium metasilicate gel (Sp.gr: 1.06 gm Cm_–3, pH ∼ 7.5), imbedded before setting, with varied amounts of weak acid (acetic acid) and 20 ml of 1M ammonium sulphate solution, dendritic structures are commonly observed in the gel at the interface, at a particular concentration of the acid. The needle shaped tabular crystals are also observed to grow at the greater depths in the gel. Dendrites are studied by optical, X-ray diffraction and Infra-red studies. It has been established that the dendrites are Calcium Sulphate dihydrate crystals formed probably due to the influence of soluble impurities (like calcium acetate, in the present case), when the rate of diffusion is fairly high and the twinning mechanism favoured. The implications are discussed.     

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 properties of ferroelectric potassium ferrocyanide trihydrate single crystals

Single crystals of potassium ferrocyanide trihydrate, K₄[Fe(CN)₆·3H₂O (KFCT), a ferroelectric material with Curie temperature 251K were grown in silica gel at room temperature for the first time by the solubility reduction method. Resorcinol and ethyl alcohol were used for the purpose of gel setting and supernatant liquid respectively. Optical and mechanical properties were studied for the grown crystal. The structure of the grown crystal was confirmed by X‐ray diffraction analysis. Fourier Transform Infrared (FTIR) and FT Raman spectral analysis of the crystalline samples reveal that the crystalline sample consist consists of all functional groups. Thermal analysis of the crystalline sample was performed by TGA and DTA methods. The Vicker's micro hardness value was measured for KFCT crystals. The square etch pits with a hopper‐like structure is an indicative of 2D nucleation mechanism. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural and microhardness studies of pure and thiourea doped glycine phosphite single crystal

Ferroelectric Glycine Phosphite (GPI) crystal have been grown from aqueous solution employing the slow cooling technique. As the crystal solubility in water depends on temperature, single crystals were grown. Transparent, colourless crystals with habit morphology weighing about 8g were obtained with in a month. The same procedure was used to grow single crystals of 10 wt% of Thiourea doped GPI (TUGPI). Formation of a new crystal was confirmed by Powder X‐ray diffraction studies as well as FTIR studies. Crystalline quality were found using rocking curve for both the crystals. Due to the presence of Thiourea in TUGPI, it improves the crystalline perfection and also enhances the growth rate. The variation of hardness on (010) faces of monoclinic GPI and TUGPI crystals, with load were studied.Vickers hardness numbers, H_v were found to decrease with the increase in load. The value of Mayer's index, ‘n ’ was found to be greater than 1.6 for GPI and TUGPI showing soft‐material category. The results are discussed in detail. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

An electrolytic method to grow copper dendrites and single crystals in gels

A new electrolytic method for the growth of any metallic crystal in gel by using gel as a medium for controlled growth, is reported. Different types of large dendrites and single crystals of copper were grown by electrolytic method in the gel medium. It is found that pH of the gel medium, the concentration of the supernatant solution, the current density and the electrode material used, have considerable influence on the habits of the dendrites and the single crystals thus grown. The surface features and morphology of crystals and dendrites were studied by optical and scanning electron microscopy. Compared to other conventional electrolytic growth techniques, the present method has a number of additional parameters that can be varied, and hence a more effective controlled growth of crystals is possible.     

Growth and morphology of the single crystals of thermoelectric oxide material NaxCoO2

We have grown single crystals of recently discovered thermoelectric oxide material Na_xCoO₂ using NaCl flux. Crystals of sizes upto 1.5 x 1.5 x 1.5 mm³ having different morphological habits were reproducibly grown. The atomic force microscopic studies show that along c‐axis crystals grow via 2D layer‐by‐layer mechanism. The X‐ray diffraction analyses show that grown crystals are rich in Na content as compared to the starting charge indicating that NaCl flux also acts as a source of Na. The resistivity of the crystals exhibited a linear temperature dependence in the region between 30 and 300 K. © 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Growth and characterization of gel grown calcium pyrophosphate tetrahydrate crystals

Formation of calcium pyrophosphate dihydrate (CPPD) crystals in soft tissues such as cartilage, meniscus and synovial tissues lead afflictions. The appearance of these crystals in the synovial fluid give rise to acute arthritis attack, which is known as pseudo‐gout. The growth of calcium pyrophosphate crystals in gel medium can mimic the growth in a body. In the present study, calcium pyrophosphate tetrahydrate (CPPT) crystals are grown by a single diffusion gel growth technique and characterized by powder XRD, FT‐IR spectroscopy, TGA, kinetic and thermodynamic studies of dehydration and dielectric studies. Monoclinic crystals structure, presence of P‐O bonds and four water molecules are confirmed from powder XRD, FT‐IR and TGA studies, respectively. The dielectric investigation suggests the reduction in dielectric constant with increase in frequency. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of different habits of lead bromide crystals in silica gel by the new gel technique

Lead bromide crystals of high optical perfection and of different habits have been grown in silica gel by new gel technique starting from colloidal lead tartrate and KBr solution. pH is found to be not a factor for habit modification. Certain habits of the grown crystals exhibit interesting surface features. The growth conditions have been optimized and the various aspects of the growth process have been widely investigated.     

Growth kinetics,habit modifications and surface designs of lead iodide grown by the new gel technique

Lead iodide crystals have been grown in silica gel by the new gel technique by the inter action between colloidal lead tartrate and KI solution. The crystals are found to exhibit interesting surface designs. Growth kinetics and habit modifications of the crystal have been investigated. Two dimensional surface nucleation and screw dislocation are found to partake in the growth process of the crystals.     

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 habits of hippuric acid in gel

Hippuric acid [C₆H₅CONHCH₂COOH], also called as N‐benzoylglycine, an organic chemical constituent of urinary stone was crystallized in silica gel in our laboratory earlier. Presently, two different habits of hippuric acid are noted during crystallization in gel. The two habits of gel grown hippuric acid crystals were characterized using single crystal X‐ray diffraction and density values. Scanning electron microscopic (SEM) studies were also made. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterisation of gadolinium samarium oxalate single crystals

Single crystals of Gadolinium Samarium Oxalate (GSO) are grown by gel method. The crystals are pale yellowish in colour. Morphology and size of the crystals are found to depend on pH of the medium, gel density, concentration of the reactants and acidity of the feed solution. The crystallinity of the grown sample was confirmed by X‐ray diffraction studies and the lattice parameters were determined. X‐ray diffractogram shows well defined peaks. IR spectrum confirms the presence of water molecules and carboxylic group. EDAX analysis confirms the presence of Gd and Sm in the sample. The thermal decomposition behaviour of the crystal was analysed using TGA and DTA studies. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Photoacoustic studies on two new organic NLO materials: L‐threonine and L‐prolinium tartrate

Photoacoustic spectroscopy (PAS) is a non‐destructive testing (NDT) tool and used here for analyzing the physical properties such as thermal diffusivity, thermal diffusion length, thermal conductivity and thermal effusivity of L‐Threonine and L‐Prolinium tartrate. These two crystals belong to a group of recently developed NLO materials, in our laboratory. The single crystals of the two compounds were grown by using submerged seed solution growth method. Characterization of the crystals was made by using single crystal X‐ray diffraction. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of strontium tartrate pentahydrate crystals

Silica gel impregnated with L‐tartaric acid and using strontium nitrate as the second reactant leads to the growth of well faceted strontium tartrate pentahydrate single crystals.The morphological developmen and internal cell dimensions are observed to be different from the ones reported in the literature for strontium tartrate trihydrate crystals. The crystals are characterized using XRD, CH analysis, SEM, FTIR spectroscopy and thermoanalytical techniques. The crystals are observed to be thermally stable upto about 105°C but thereafter start decomposing and ejecting water of hydration at various stages, finally reducing to strontium oxide. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growing CuI crystals with decomplexation method modified by concentration programming

An attempt to grow CuI single crystal with decomplexation method modified by concentration programming in silica gel was performed. The results show that decreasing the concentration of feeding solution gradually can yield pure regular single crystals with larger size compared with those of increasing concentration. Replenishing feeding solution every 24 h produces crystals with higher quality than those of every 48 h. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)