Stoichiometric single crystal growth of AgGaS2 by iodine transport method and characterization

High quality single crystals of ternary AgGaS₂ (AGS) semiconductor with chalcopyrite structure have been grown by chemical vapor transport (CVT) technique using iodine as a transporting agent at different growth zone temperatures. The powder X‐ray diffraction and single crystal X‐ray diffraction studies indicate that the as‐grown AGS crystals belong to the tetragonal (chalcopyrite) system with (112) plane as the dominant peak. The full width at half maximum (FWHM) of the X‐ray rocking curve for the as‐grown AGS single crystal is 5 arcsec. The energy dispersive X‐ray analysis (EDAX) and optical transmission spectra of as‐grown AGS single crystals grown at different conditions show the almost same composition and band gap (2.65 eV). Photoluminescence (PL) spectra of as‐grown AGS single crystals show prominent band edge emission at 2.61 eV. The resistivity of the as‐grown AGS single crystal has been measured. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Real Structure of LiB3O5 (LBO) Crystals Grown in Li2O‐B2O3‐MoO3 System

The liquidus surface structure and field of LiB₃O₅ (LBO) primary crystallization have been revealed in Li₂O‐B₂O₃ ‐MoO₃ ternary system. The optimization of charge composition and growth conditions results in large volume optical quality LBO single crystals yielding. Crystallographic properties and real defect structure of grown LBO single crystals have been investigated by X‐ray powder diffraction method and X‐ray reflection topography. The volume of the crystals is partly free of any structural imperfections.     

Characterization of the conglomerate form of acetyl-dl-leucine by thermal analysis and solubility measurements

Starting from a mixture of enantiomers in solution, crystallization can generate different types of crystals. In order to determine which type of crystal is obtained in the case of acetyl leucine, an active pharmaceutical ingredient (API), analytical methods have been used to partially elucidate the binary and ternary phase diagrams of the system composed of the two enantiomers and water.The melting temperature phase diagram of this compound has been obtained by using differential scanning calorimetry (DSC) analyzes. The results show that it is characteristic of a conglomerate. This mode of crystallization has also been confirmed by X-ray powder diffraction analysis.Solubility measurements of enantiomerical mixtures in water enabled the determination of the ternary diagram of solubility. The empiric Meyerhoffer double solubility rule has been modified, due to the characterization of interactions between enantiomers.     

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)     

Gel growth of α and γ glycine and their characterization

The microbial free single crystals of α and γ glycine were grown from gel at room temperature in a new chemical route. These crystals showed a superior quality than the solution grown crystals. The metastable α-form and the stable γ-form of glycine were crystallized in silica gel by solubility reduction method. The form of crystallization is confirmed by single crystal and powder X-ray diffraction analyses. The crystals of α and γ glycine were found to crystallize in monoclinic and hexagonal crystal systems, respectively. For analyzing the functional group and thermal stability of α and γ glycine crystals, spectroscopic and thermal analyses have been carried out. The dielectric studies were performed to find the dielectric constant of the grown crystals and the results are discussed. Second harmonic generation efficiency of the crystal was measured by Kurtz’s powder method using Nd:YAG laser and it was found to be 2.68 times that of potassium dihydrogen phosphate crystals.     

Growth and morphology of ruby crystals with unusual chromium concentration

Single crystals of ruby have been obtained from fluxed melts based on the systems Li₂O–MoO₃, Li₂O–WO₃, Na₂O–WO₃, 2PbO–3V₂O₅, PbO–V₂O₅–WO₃, PbF₂–Bi₂O₃ and Na₃AlF₆ by both the TSSG method and spontaneous crystallization at the temperatures 1330–900 °C. Al₂O₃ solubility has been measured for the flux composition of 2Bi₂O₃–5PbF₂ in the temperature range 1200–1000 °C and dissolution enthalpy has been defined as 29.4 KJ/Mol. The composition of grown crystals was studied by electron microprobe analysis. The synthetic ruby contains from 0.51 to 6.38 at% of chromium admixture depending on the crystal growth conditions. Experimental results on growth conditions, composition and morphology of grown crystals are presented for each flux and temperature interval.     

Compositions of supersaturated solutions for enhanced growth of α-NiSO4 · 6H2O, Me 2Ni(SO4)2 · 6H2O, MeH2PO4 [Me = Li, Na, K, Rb, Cs, NH4], and K(H x D1−x )2PO4 single crystals

The possibility of determining the optimal compositions and temperatures of supersaturated solutions for enhanced growth of single crystals of congruently and incongruently dissolving solid phases from the solubility diagrams of ternary systems is shown, and this approach is justified. The NiSO₄-H₂SO₄-H₂O, Me ₂SO₄-NiSO₄-H₂O, and Me ₂O-P₂O₅-H₂O(D₂O) systems have been used to determine the optimal compositions and temperatures of supersaturated solutions for growth of α-NiSO₄ · 6H₂O, Me ₂Ni(SO₄)₂ · 6H₂O, MeH₂PO₄ [Me = Li, Na, K, Rb, Cs, NH₄], and K (H _x D_1?x )₂PO₄ (D is deuterium) single crystals.     

大尺寸电阻加热式碳化硅晶体生长热场设计与优化

大尺寸低缺陷碳化硅(SiC)单晶体是功率器件和射频(RF)器件的重要基础材料,物理气相传输(physical vapor transport, PVT)法是目前生长大尺寸SiC单晶体的主要方法。获得大尺寸高品质晶体的核心是通过调节组分、温度、压力实现气相组分在晶体生长界面均匀定向结晶,同时尽可能减小晶体的热应力。本文对电阻加热式8英寸(1英寸=2.54 cm)碳化硅大尺寸晶体生长系统展开热场设计研究。首先建立描述碳化硅原料受热分解热质输运及其多孔结构演变、系统热输运的物理和数学模型,进而使用数值模拟方法研究加热器位置、加热器功率和辐射孔径对温度分布的影响及其规律,并优化热场结构。数值模拟结果显示,通过优化散热孔形状、保温棉的结构等设计参数,电阻加热式大尺寸晶体生长系统在晶锭厚度变化、多孔介质原料消耗的情况下均能达到较低的晶体横向温度梯度和较高的纵向温度梯度。     

Specific features of the flux growth of bulk crystals of high-temperature modification of BaB2O4

High-quality single crystals of the high-temperature phase of barium metaborate (α-BaB₂O₄) up to 100–120 g in weight are grown from a flux in the ternary system BaO-B₂O₃-Na₂O. The growth temperature is below the α → β phase transition temperature. The conditions necessary for growing α-BaB₂O₄ crystals under metastable conditions are determined and the morphology and optical quality of the crystals grown are investigated.     

Optimization of the Growth Technology for Crystals with Garnet Structure Based on X-Ray Diffraction Data

High efficiency of the methods of double-crystal X-ray diffractometry (DCXRD) and topography for improving the growth technology of highly homogeneous crystals has been demonstrated on the example of gadolinium gallium garnet (GGG) single crystals. The main types of structural defects observed in Czochralski-grown GGG crystals are found to be macroscopic inhomogeneity of composition distribution, caused by the facet effect manifestation; microinhomogeneous distribution of impurity and main components of the composition in striations; dislocations; and second-phase inclusions. The relationship between the type and density of newly formed defects and the technological conditions for crystal growth are considered. Optimization of the composition of crystals and their growth technology made it possible to obtain high-quality dislocation-free crystals of GGG and complex-substituted garnets on its basis for magneto-optical and microwave devices, elements of solid-state lasers, and other applications.     

Crystallization of glass fibers of the system Zn---Fe---Mn---oxides---alumina---silica

A glass composition based on the Zn---Al---silicate ternary system was modified with the addition of Fe and Mn oxides in order to test its feasibility to be drawn as alkaline-corrosion resistant glass fibers.

Their devitrification trend was studied, under dynamic thermal conditions, in order to define after which ternary diagram the resulting phases could be best described.

A beta-quartz structured silica rich phase, alpha-willemite and magnetite have been detected both in the fibers and in the bulk mass after crystallization. However, the differential thermal analysis patterns and the microstructures of the samples revealed very noticeable differences.     

Solubility phase diagrams of Me 2SO4-NiSO4-H2O systems and the growth of Me 2Ni(SO4)2 · n H2O crystals [ Me = Na, Rb, Cs; n = 4, 6]

On the basis of the physicochemical analysis of the solubility phase diagrams for the Me ₂SO₄-NiSO₄-H₂O ternary systems (Me = Na, Rb, or Cs), the optimum concentration and temperature conditions for the crystallization of the Me ₂Ni(SO₄)₂ · nH₂O solid phases were found. Techniques for growth of single crystals of these binary salts have been developed. Such techniques allow application of mother liquors containing hydrates or anhydrous sulfates of Na, Rb, Cs, and Ni as raw materials. Na₂Ni(SO₄)₂ · 4H₂O, Rb₂Ni(SO₄)₂ · 6H₂O, and Cs₂Ni(SO₄)₂ · 6H₂O single crystals (28–34) × (8–13) × (5–10) mm³ in size have been grown from aqueous solutions in the dynamic regime. Original Russian Text ? L.V. Soboleva, 2007, published in Kristallografiya, 2007, Vol. 52, No. 6, pp. 1141–1144.     

Growth of single crystals of NaH2PO4 (NaDP), NaH2PO4 · H2O (NaDP · H2O), and NaH2PO4 · 2H2O (NaDP · 2H2O) sodium dihydrogenphosphate based on the analysis of the Na2O-P2O5-H2O phase diagram

The crystallization conditions for the NaH₂PO₄, NaH₂PO₄ · H₂O, and NaH₂PO₄ · 2H₂O solid phases have been established from the analysis of the phase diagram of solubility of the ternary Na₂O-P₂O₅-H₂O system in the temperature range from 0 to 100°C. Based on these data, the methods for growing sodium dihydrogenphosphate single crystals of the above compositions are developed. The initial components for preparing mother solutions were H₃PO₄ and NaOH solutions taken in certain weight ratios. For the first time, NaDP, NaDP · H₂O, and NaDP · 2H₂O single crystals were grown on a seed by the method of temperature decrease. The habits of the NaDP and NaDP · H₂O single crystals are determined. __________ Translated from Kristallografiya, Vol. 47, No. 5, 2002, pp. 937–944. Original Russian Text Copyright ? 2002 by Soboleva, Voloshin.     

Hybrid technique for growing homogeneous single crystals of semiconductor solid solutions from melt

A concept and fundamentals of a hybrid technique for growing homogeneous single crystals of semiconductor solid solutions (SSs) from melt are presented. The growth consists of two stages. In the first stage, a single crystal with a specified concentration of the more refractory component is grown by an innovative method of directional constitutional supercooling of a melt in the steady-state mode. In the second stage, the melt is fed with the second component. Using an example of the classical Ge-Si system, the concentration profiles of the components along the crystal axis are calculated and the SS growth dynamics ensuring single crystallinity over the entire ingot length is determined. An analysis of the results yields the optimal technological parameters and conditions for growing homogeneous single crystals of SSs of a specified composition and size.     

Investigation of the Solubility of Pleochroic Dyes in Liquid Crystals

A precise, inexpensive and relatively fast method for determining the solubility of pleochroic dyes in liquid cyrstals is described. The method has been used to investigate the solubility of two anthraquinone dyes in liquid crystals of different molecular structure. The solubility of the dye is found to be strongly dependent on the molecular structure of the dye and that of the host liquid crystal. Also the temperature dependence of the solubility in the nematic phase has been found to be different from that in the isotropic phase of the liquid crystals. At the nematic isotropic phase transition temperature a discontinuity in the solubility curve has been observed.     

Study of the temperature dependence of the electrical conductivity in strontium-barium niobate crystals with different dopants

The electrical characteristics of single crystals of strontium-barium niobate solid solutions have been studied. The temperature dependences of the electrical conductivity were obtained for different SBN compositions, nominally pure SBN:61 and SBN:75 and SBN doped with rare earth and transition-metal impurities. The influence of the chemical composition of a solid solution, thermal treatment conditions, dopant concentration, and electrode type on the specific features of the electrical conductivity of single crystals in the temperature range 20–450°C is shown.     

Symmetry and ordering of compounds with a beryl-type structure in the Mg-enriched part of the beryllium indialite-cordierite-beryl system

The boundaries of the regions of solid solutions with beryl-type structures and different symmetry and degree of order obtained by solid-phase synthesis have been refined in the beryllium indialite-cordierite-beryl system. The change in the compositions of real crystals in the course of synthesis and the character of the dependence of the melting point on the composition are taken into account.     

Crystallization of the E. coli polyamine-induced protein: a novel procedure based on the concept of ionic strength reducers

Nucleation and growth of macromolecular crystals occur in supersaturated solutions the properties of which depend on numerous parameters that influence macromolecular solubility. Detailed knowledge of the effects of those parameters is essential for crystallization. The concept of the so-called “ionic strength reducers” provides insight into the changes of solubility induced by organic solvents and hydrophilic polymers in aqueous electrolytic solutions. A simple and efficient procedure is presented which exploits the properties of ionic strength reducers in the crystallization of proteins. Using this procedure in the crystallization of the E.coli polyamine-induced protein, superior crystals compared to conventional techniques have been obtained. The procedure combines microseeding with dialysis techniques and is applicable to other proteins, particularly in cases where conditions favoring both for nucleation and growth cannot be found, or in cases where excessive nucleation leads to the growth of a large number of very small crystals.     

Electrochemical growth and properties of LaMn1−xCoxO3 (0 < x ≤ 1) single crystals

Single crystals of LaMn_1−xCo_xO₃ (0 < x < 1) with distorted perovskite structure have been obtained by the electrodeposition technique at anode from flux melt using Cs₂MoO₄‐MoO₃ binary system as solvent. An investigation of magnetic and electrical properties of the obtained crystals as well as its comparison with those for ceramic samples of the same composition were carried out. A much weaker interplay between magnetic and electrical properties and a smaller ∼8% magnetoresistance were found in the ternary oxide crystals slightly doped by Co on the verge of transition to ferromagnetic state in comparison to the data have been reported for LaMnO_3+δ single crystals. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Influence of growth conditions on microstructure and properties of GaSe crystals

GaSe crystals have been grown from melt. There are several reasons why it is difficult to meet ideal demands for nonlinear optic material, GaSe single crystal. First, these crystals have a tendency towards lamination because of great difference in a and c crystal lattice parameters and very weak Vander der Waals forces in c direction. Next, there is a great difference in saturation vapor pressure of the components, which can cause nonstoichiometry of a melt-grown crystal composition. Another obstacle in the growth of perfect GaSe crystals is dendrite formation caused by instability of the growth front. To overcome this obstacle we used Bridgman technique and have found the temperature and pressure conditions, and growth velocity which provide growth of perfect bulk single crystals of about 100 mm in length and 20 mm in diameter. Sharp Laue patterns and a rocking curve confirm perfect structure of the grown crystals. Electron-probe X-ray microanalysis shows stoichiometric composition of GaSe crystals and X-ray phase analysis reveals presence of single-phased hexagonal structure.