Electical,Magnetic, and Thermal Properties of Cadmium Hydrogen Phosphate Hydrate Crystals

The d.c. electrical conductivity of pelletized samples of cadmium hydrogen phosphate hydrate (CHP) crystals have been studied in the temperature range 50 °C to 250 °C. It has been observed that CHP crystals exhibit ionic conductivity at 140 °C and possess semiconducting property. At room temperature CHP has stable crystal structure. From thermal analysis it is concluded that CHP crystals possess water of crystallization and the material to be diamagnetic.     

Supramolecular Discotic Columnar Liquid Crystals Built through Single Hydrogen Bonding between Carboxylic Acid and Pyridine Moieties

New self-assembled discotic columnar liquid crystals were prepared via single hydrogen bonding between the core molecule of 1,3,5-cyclohexanetricarboxylic acid and the peripheral units of stilbazole derivatives. The hydrogen-bonded liquid crystals exhibited rectangular columnar and hexagonal columnar mesophases depending on the number of alkyl chains in three arms of the discotic mesogen through dipole-dipole interactions between carbonyl groups along the column axis. The intermolecular hydrogen bonding between carboxylic acid and pyridine moieties provides an effortless methodology to prepare the ordered columnar liquid crystals for electronic applications.     

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.     

Hydrogen passivation of residual acceptors in GaSb single crystals

Undoped GaSb single crystals were grown using the Czochralski method without encapsulant in an atmosphere of ionized hydrogen. It has been found that the resistivity increased by more than one order of magnitude (0.6–0.8 Ω cm) in comparison with the crystals grown under molecular hydrogen atmosphere only. A certain asymmetry in acceptor and donor passivation is assumated, because the Hall concentration does not change along the direction of crystal growth ((3.3–3.5) × 10¹⁷ cm^-3) and it is comparatively higher. Donors are passivated more than acceptors, which should be confirmed by increasing resistivity and decreasing mobility.     

Growth of some urinary crystals and studies on inhibitors and promoters. II. X-ray studies and inhibitory or promotery role of some substances

Best conditions were established for the gel growth of three urinary crystals viz., calcium oxalate monohydrate, calcium hydrogen phosphate dihydrate and ammonium magnesium phosphate hexahydrate. The crystals grown were characterized using single crystal X-ray diffraction techniques and density measurements. Crystal growth experiments were carried out by incorporating the extracts or juices of some natural products in the gel media. By carefully observing the changes in the growth of crystals (compared to control experiments carried out at the same conditions), results about the inhibitory or promotery role of the substance incorporated were obtained. It was found that the extracts or juices of many of the naturally occurring substances have interesting inhibitory or promotery effects. These results may have useful applications in the treatment of recurrent stone patients.     

软X射线分光晶体琥珀酸氢十四酯的合成及结晶习性研究

本文合成了软X射线分光晶体琥珀酸氢十四酯(THS).通过红外光谱、差示量热扫描等手段对所合成样品进行表征和鉴定.对THS在苯、甲苯、二甲苯、异丙醇等溶剂中的自发成核和结晶形态进行了研究,结果表明THS在苯、甲苯和二甲苯中表现出良好的结晶习性.采用平衡法测定了THS在苯、甲苯和二甲苯中的溶解度曲线.综合考虑结晶习性和溶解度情况,可选择甲苯作为晶体生长的溶剂进行单晶生长实验.     

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)     

Preparation and Properties of Single Crystals of Hydrogen Bis(Phthalocyaninato) Neodymium(III)

Single crystals of hydrogen bis(phthalo-cyaninato)neodymium(III) have been synthesized by electrochemical means. The crystals are semiconductors and follow Curie-Weiss behavior.     

Hydrogen bonded nonlinear optical γ-glycine: Crystal growth and characterization

Single crystals of γ-glycine(GG) were grown by solvent evaporation technique from a mixture of aqueous solutions of glycine and ammonium nitrate at ambient temperature. X-ray diffraction, thermogravimetric/differential thermal analysis, Fourier transform infrared spectral techniques were employed to characterize the crystal. The lattice parameters were calculated and they agree well with the reported values. GG exists as dipolar ions in which the carboxyl group is present as a carboxylate ion and the amino group as an ammonium ion. Due to this dipolar nature, glycine has a high decomposition temperature. The UV cutoff of GG is below 300 nm and has a wide transparency window, which is suitable for second harmonic generation of laser in the blue region. Nonlinear optical characteristics of GG were studied using Q switched Nd:YAG laser (). The second harmonic generation conversion efficiency of GG is 1.5 times that of potassium dihydrogen phosphate . The X-ray diffraction and Fourier transform infrared spectral studies show the presence of strong hydrogen bonds which create and stabilize the crystal structure in GG. The main contributions to the nonlinear optical properties in GG results from the presence of the hydrogen bond and from the vibrational part due to very intense infrared bands of the hydrogen bond vibrations. GG is thermally stable up to 441 K.     

马来酸氢十六酯(HHM)在过饱和溶液中的成核过程

本文研究了马来酸氢十六酯(HHM)在以甲苯为溶剂的过饱和溶液中的成核过程.测定了以诱导时间表示的成核速率.用经典的成核理论计算了固-液表面张力、成核自由能和临界成核半径.指出HHM晶体在甲苯为溶剂的过饱和溶液中的成核速率随着温度和过饱和比的提高而增大.溶剂的性质也将改变成核速率的大小.     

Observation of optical inhomogeneities in flux grown KTP crystals

Optical inhomogeneities in potassium titanyl phosphate crystals grown from different fluxes have been investigated. In the crystals grown from a flux which contains tungsten, striations parallel to the {011} faces were observed. The main reason for forming striations is the change in tungsten concentration with change in growth rate. In the case of a potassium phosphate flux, no striations were observed in the crystal which was grown at almost the same temperature and stirring conditions as for the tungstate flux. We can conclude that the phosphate flux is more suitable for the growth of optically good crystals for KTP as laser harmonic converters.     

Effect of citric acid and 1,2‐dihydroxybenzene 3,5‐disulfonic acid on crystallization of calcium sulfate dihydrate under simulated conditions of phosphoric acid production

The effect of citric acid and 1,2‐dihydroxybenzene 3,5‐disulfonic acid (DHBDSA), as additives, on the crystallization of gypsum was studied under simulated conditions of the of phosphoric acid production. Calcium hydrogen phosphate and sulfuric acid were mixed with dilute phosphoric acid at 80 °C, and the turbidity of the reaction mixture was measured at different time periods to calculate the induction time of gypsum crystals formation. Addition of citric acid increased the induction time and decreased the growth efficiency while addition of DHBDSA decreased the induction time and increased the growth efficiency compared with in absence of additives. The crystals mean and median diameters were found to decrease in the presence of citric acid and increased in the presence of DHBDSA. The surface energy decreased with citric acid and increased with DHBDSA compared to the baseline (without additives). Interestingly, the majority of the formed crystals are tabular with DHBDSA and needle‐like type with citric acid and baseline     

Resonant diffraction of synchrotron radiation: New possibilities

Resonant diffraction of synchrotron radiation (SR) is a modern method of studying the structure and properties of condensed matter that can be implemented on third-generation synchrotrons. This method allows one to investigate local properties of media (including magnetic and electronic ones) and observe thermal vibrations, defects, and orbital and charge orderings. A brief review of the advance provided by SR resonant diffraction is presented, and the capabilities of this method for analyzing phase transitions are considered in more detail by the example of potassium dihydrogen phosphate and rubidium dihydrogen phosphate crystals. It is shown that the investigation of the temperature dependence of forbidden reflections not only makes it possible to observe the transition from para- to ferroelectric phase, but also gives information about the proton distribution at hydrogen bonds.     

Hydrogen bonding patterns of 2-aminopyridinium nicotinic acetate

The crystal structure of 2-aminopyridinium nicotinic acetate (C₁₁H₁₁N₃O₂) has been determined from X-ray diffraction data using MO Kα radiation. The crystals are monoclinic, P2₁/n, with a=8.787(9) Å, b=12.176(2) Å, c=10.866(2) Å, β=110.11(1)°, and z=4. There is an intermolecular hydrogen bonding between the amino group of the 2-aminopyridine and the oxygen atoms of the nicotinic acetate. Both the six-membered rings are planar. The cations and anions are linked together in chains along the [001] direction by N–HO hydrogen bonds.     

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)     

Growth and characterization of nonlinear optical zinc hydrogen phosphate single crystal grown in silica gel

Good optical quality single crystals of zinc hydrogen phosphate (ZnHPO₄) having dimensions up to 8×2×2 mm³ have been grown with the aid of sodium meta silicate gel. Single crystal XRD studies confirm that the crystal belongs to the orthorhombic system with space group P2₁2₁2₁. The functional groups present in the crystals were confirmed using FTIR technique. Optical absorbance shows very low absorption in the entire visible region. Differential thermal and thermo gravimetric analysis confirmed that the crystal is stable up to 193°C. Photoconductivity study reveals positive photoconductivity in the presence of photo active centers formed by trap energy levels. The NLO activity of the crystal was confirmed by Kurtz powder technique. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and high frequency dielectric study of pure and thiourea doped KDP crystals

Non linear optical (NLO) materials have acquired new significance with the advent of a large number of devices utilizing solid‐state laser sources. Several NLO materials have been used for this kind of technological applications. The Potassium di‐hydrogen phosphate (KDP) one of NLO material having superior non linear optical properties has been exploited for variety of applications. In the present investigation we have grown KDP crystals from aqous solution with thiourea, an organic non linear optical material. We could enhance the SHG efficiency of thiourea doped KDP crystal. It was 1.99 times more that of pure KDP. We observed more enhancements in nonlinearity for low concentration of thiourea.The crystal structure and cell parameters of grown crystal were determined from Powder XRD.The incorporation of thiourea in the grown crystals was qualitatively analyzed from FT‐IR study. The absorption spectra of pure and thiourea doped KDP crystal reveal that thiourea doped KDP crystals would be a better nonlinear optical (NLO) material for second harmonic generation (SHG) than pure KDP. The thermal decomposition and weight loss of pure and thiourea doped KDP crystal was observed by thermogravimetric (TGA) analysis and Differential Scanning Calorimetry (DSC). The high frequency dielectric study of pure KDP crystal, thiourea doped KDP crystals and organic additive thiourea was carried out using X‐band at frequency 8GHZ and 12GHZ by transmission line wave guide method. We observed low dielectric constant of thiourea doped KDP crystal when it is doped with 2mole% of thiourea. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Properties of Doped GaSb Single Crystals Grown by the Czochralski Method

The specific electrical properties and average dislocation density of GaSb crystals are shown and discussed regarding various elements presented as dopant. The single crystals were grown by the Czochralski method without encapsulant in a flowing atmosphere of molecular hydrogen, on the one hand, and of atomic hydrogen, on the other hand. The results are summarized in the Table II.     

Hydroxyapatite synthesis from biogenic calcite single crystals into phosphate solutions at ambient conditions

Hydroxyapatite is one of the most important bone substitute biomaterials. Here, it has been successfully overgrown on biogenic seed crystals at ambient conditions. Single crystals of calcite from Atrina rigida, Paracentrotus lividus and Heterocentrotus mammillatus have been soaked in phosphate solution with different concentrations and pHs for 2 months. X-ray powder diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy have been used to characterize soaking precipitates. The results show that the conversion of calcite to hydroxyapatite occurs to an extent which depends on composition and morphology of seed crystals, and starting concentration and pH of phosphate solutions. In the same experimental conditions, synthetic calcite single crystals did not convert to hydroxyapatite. The morphological observations suggest for hydroxyapatite formation, a mechanism that involves a superficial dissolution of calcite and a subsequently overgrowth of hydroxyapatite. Moreover, the final architectural assembly of the hydroxyapatite crystals resembles the shape of the starting biogenic seed crystals.     

Hydrogen diffusion in fused silica at high temperatures

Hydrogen diffusion in a silica glass at high temperature (750–1500 °C) was investigated. The starting material was a silica glass that was melted in hydrogen atmosphere and contained a high concentration of hydroxyl and hydride. After heat treatment at various temperatures in air, the effective hydrogen diffusion coefficients were evaluated from the removal rates of hydroxyl and hydride. The obtained diffusion coefficients exhibited an unusual temperature dependence, with the lower diffusion coefficient being observed at higher temperature in the temperature range of 1000–1500 °C. This was attributed to the higher reactivity of hydrogen with the glass network at higher temperatures, effectively slowing down the hydrogen mobility. Below 1000 °C, the effective hydrogen diffusion coefficient exhibited a normal temperature dependence. This reversal of the temperature dependence of the effective hydrogen diffusion coefficient appears to be related to the reversal of the temperature dependence of the hydroxyl (or hydride) solubility in silica glass.