Growth of single crystals of barium iodate and strontium iodate in silica gels

Single crystals of iodates of barium and strontium grown by gel method are reported. Optimum conditions for good quality single crystals are worked out. Different habits of these crystals are reported. A brief report for characterization of these crystals by different methods is given.     

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)     

Etching of CaF2 single crystals in silica gels

Etching of {111} cleavage faces of CaF₂ crystals in aqueous solution of 50% HCl is carried out in citric acid set silica gel, and the kinetics of growth of etch pits at the sites of dislocations is investigated as a function of temperature, time of etching and height of gel column above the crystal surface. It is observed that the transient period required to initiate etch pit at the sites of a dislocation decreases (1) at particular temperature, with a decrease in gel height, and (2) for a particular gel height, with an increase in the temperature of etching. It is also observed that the morphology of dislocation etch pits remains triangular irrespective of the gel height and the temperature of etching. The results are compared with those of solution etching and discussed.     

Growth and characterization of pure and doped lead hydrogen phosphate single crystals in silica gel

Following the chemical reaction method pure and doped lead hydrogen phosphate single crystals were grown in silica gel using different gel density, various concentrations of phosphoric acid, and lead nitrate solutions. As the gel pH plays an important role in the formation of different H₃PO₄ species in the phosphoric acid system, the pH range in which HPO ions dominate, was considered which in turn in necessary for the growth of lead hydrogen phosphate crystals. Characteristics of these crystals were carried out by infrared spectral analysis and microhardness study.     

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)     

Tooth enamel proteins enamelin and amelogenin cooperate to regulate the growth morphology of octacalcium phosphate crystals

To examine the hypothetical cooperative role of enamelin and amelogenin in controlling the growth morphology of enamel crystals in the post-secretory stage, we applied a cation selective membrane system for the growth of octacalcium phosphate (OCP) in the truncated recombinant porcine amelogenin (rP148) with and without the 32kDa enamelin fragment. Enamelin alone inhibited the growth in the c-axis direction more than rP148, yielding OCP crystals with the smallest aspect ratio of all conditions tested. When enamelin was added to the amelogenin "gel-like matrix", the inhibitory action of the protein mixture on the growth of OCP in the c-axis direction was diminished, while that in the b-axis direction was increased. As a result, the length to width ratio (aspect ratio) of OCP crystal was markedly increased. Addition of enamelin to amelogenin enhanced the potential of amelogenin to stabilize the amorphous calcium phosphate (ACP) transient phase. The ratio of enamelin and amelogenin was crucial for stabilization of ACP and the growth of OCP crystals with larger aspect ratio. The cooperative regulatory action of enamelin and amelogenin was attained, presumably, through co-assembling of enamelin and amelogenin. These results have important implications in understanding the growth mechanism of enamel crystals with large aspect ratio.     

FTIR spectroscopic,thermal and growth morphological studies of calcium hydrogen phosphate dihydrate crystals

Calcium hydrogen phosphate dihydrate (CHPD or DCPD) is found quite frequently in urinary calculi (stones). The CHPD crystals were grown by the single diffusion gel growth technique in sodium metasilicate gel. The crystals were found to be having platelet and broad needle type morphologies. The crystals were analyzed by FTIR spectroscopy. The thermal properties were studied by employing the thermogravimetric analysis. Various kinetic and thermodynamic parameters for dehydration were estimated. The selected platelet was studied by SEM for the growth morphologies indicating that the crystals grew in the form of leaflets having prominent (010) faces. This was in agreement with earlier reported studies. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of calcium phosphate crystals in Silica gel

The results of a study of the crystal growth of calcium phosphates in silica gel employing double diffusion system with CaCl₂ and KH₂PO₄ aqueous solutions are reported. Liesegang rings, spherical crystalline agglomerates and brushite dendrites are formed near the CaCl₂ solution. It was found that the agglomerates consist of octacalcium phosphate and hydroxyapatite crystals with the predominance the former.     

Growth of single crystals of potassium chloride from gels

The growth of single crystals of potassium chloride (KCl) in silica gels upto 3 × 3 × 3 mm³ in size is described. To crystallize KCl incorporated in the gel, hydrochloric acid has been used to crystallize the KCl in the gel media. The crystalline perfection has been studied by the chemical etch pit technique.     

Comment on “the growth of dicalcium phosphate dihydrate on octacalcium phosphate at 25°C” by J.-C. Heughebaert, J.F. De Rooij and G.H. Nancollas

An apparent disagreement with respect to the growth kinetics of octacalcium phosphate (OCP) is shown to arise from different methods of data analysis.     

Crystalline quality of lysozyme crystals grown in agarose and silica gels studied by X-ray diffraction techniques

The crystalline quality of hen egg white lysozyme (HEWL) crystals grown in agarose gels and in silica gels has been characterized by measuring resolution and mosaic spread. These crystals have been compared to solution grown ones. A quasi-plane-wave X-ray topography study has also been done on some crystals. The study concerns triclinic, monoclinic, orthorhombic and tetragonal forms of HEWL. One observes that the resolution is not really changed by gelling the growth medium, even for rather high gel contents (agarose 0.5% wt/wt). On the contrary, mosaicity, characterized through reflection profile recordings allows to differentiate crystals grown by different techniques: agarose gel grown crystals are, on average, better than solution grown ones but the best crystals are obtained in silica gel. X-ray topography confirms this result.     

Growth of CaMoO4 and SrMoO4 crystals in silica gel media

Growth kinetics and characterization of calcium and strontium molybdate crystals grown in silica gel have been studied under a variety of parameters. The changes in nucleation characteristics, growth habit, quality of these crystals were carefully observed and are found directly related to pH of the medium. The profound influence of pH on spontaneous crystallization of CaMoO₄ crystals has been carefully investigated; and its crystallization range has been determined. The wide morphological change of SrMoO₄ with respect to pH variation has been studied. The quality of the crystals has been critically examined.     

Growth and characterization of mixed neodymium praseodymium oxalatze decahydrate crystals in silica gel

Mixed single crystals of neodymium praseodymium oxalate decahydrate were grown from silica gel by controlled reaction of rare earth nitrates with oxalic acid. The crystals were characterized using X-ray powder diffraction and optical absorption studies.     

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)     

The preparation of calcium oxalate dihydrate crystals

Two simple related methods for exclusively preparing well-developed tetragonal bipyramidal crystals of calcium oxalate dihydrate at moderate supersaturations and at ambient temperature are reported. These crystals have an average length of 5.7–7.2 μm and are easy to wash and filter. One of the methods is suitable for studies of the kinetics of spontaneous precipitation and crystal morphology of the oxalate in the presence and absence of additives. A tentative mechanism is given to account for the sole formation of this particular hydrate. At 70 °C a mixture of the monohydrate and dihydrate phase were formed with various crystal shapes and sizes. These phases were also identified in the presence of sucrose at this temperature, although some of the crystals contained tetragonal habit as obtained at ambient temperature.     

Vanadyl ion stability in silica gels

Silica gels doped with vanadium were prepared from tetra ethyl orthosilicate and an aqueous solution of NH₄VO₃, at a final sol pH of 1.5–2.5. Absorption and electron paramagnetic resonance (EPR) spectral studies establish that under ambient conditions the incorporated pentavalent vanadium is stabilized as tetravalent vanadyl ion in the gel monoliths. Dried gels were very stable under ambient conditions, however, transformation of V⁴⁺ to V⁵⁺ was noted during gel densification.     

Growth and optical absorption studies on potassium dihydrogen phosphate single crystals

Growth of bulk nonlinear optical (NLO) single crystals gained new significance with the advent of solid‐state laser sources for opto‐electronic applications. An optically transparent crystal of potassium dihydrogen phosphate (KDP) has been grown from aqueous solution along (001) plane with the aid of modified growth assembly of Sankaranarayanan‐Ramasamy (SR) Method. The evaporation rate was controlled and single crystals of 5 mm diameter and 60 mm length with a growth rate 5 mm per day have been grown successfully. The improved transparency of grown crystal was investigated using DRS UV transmittance spectral analysis and the presence of functional groups in the grown crystal is confirmed using FTIR analysis. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Drying evolution of wet silica gels

Two kinds of porosity have been found in wet gels prepared by an esterification-controlled hydrolysis: macropores and mesopores. The textural evolution during the during shows that the most dilute gel shrinks the most rapidly. The dynamical part of the Scherer model gives a good account of this observed behavior.