Growth of Ni-doped MgF2 crystals in self-sealing graphite crucibles

Large Ni-doped MgF₂ single crystals of excellent optical quality have been grown in self-sealing graphite crucibles by a vertical gradient freeze technique. This relatively simple technique always yields single crystals having excellent optical quality and should be applicable to the melt growth of other crystals that are too volatile to permit the use of open systems.     

Absorption and ionic conductivity of oxygen-containing SrF2 crystals

An absorption band at 3644 cm⁻¹ is caused by isolated OH⁻ ions. O⁻ ions cause an absorption band at 213 nm the oscillator strength of which is 0.020. Charge-compensation of O⁻ ions is effected by F⁻ ion vacancies (F). As for CaF₂ crystals there occur monomers and dimers of [O⁻ – F] complexes. The mass action constants of association of F with oxygen centres are K_AD = ⅓ exp (4.28 – 0.82 eV/kT) for [O⁻ – F], K_AT = 4 exp (17.4 – 1.25 eV/kT) for [2 O⁻ – F] and K_AQ = exp (4.2 – 0.89 eV/kT) for [2 O⁻ – 2 F].     

Influence of purity of NdF3 single crystals on their ionic conductivity

Single crystals of the NdF₃ superionic conductor have been grown by the Bridgman method from a melt in a helium atmosphere using a fluorinating PbF₂ agent. Commercial NdF₃ reagents of special purity grade, reagent grade, and pure grade are used. It is found that the ionic conductivity ?? of the crystals depends considerably on the purity grade of the starting substances: at 200°C ?? = 1.4 × 10^?, 3 × 10^?4, and 8 × 10^?4 S/cm for reagents of special purity grade, reagent grade, and pure grade, respectively.     

Anisotropy of the ionic conductivity of CsCu2Cl3 single crystals

The conductivity of CsCu₂Cl₃ single crystals (orthorhombic system, sp. gr. Cmcm) has been investigated for different electric-field directions, perpendicular to the crystallographic c axis and along it, in the temperature range 390–530 K. The increase in conductivity with temperature is due to the ion-carrier transport with activation energies E _a = 0.65 and 0.80 eV for the directions perpendicular to and along the crystallographic axis, respectively. The anisotropy of the crystal ionic conductivity is found to be σ_⊥c /σ_∥c ≈ 40 at 435 K. The thermally activated contribution to the conductivity in the CsCu₂Cl₃ structure is determined by the transport of Cu⁺ ions.     

Compositional mapping of GaSb wafers from as-grown crystals and after post-growth annealing treatments

Spatial compositional analysis has been carried out on single and polycrystal wafers of GaSb grown from stoichiometric and non-stoichiometric melts. In crystals grown from stoichiometric melt, the ratio of Ga to Sb is slightly more and remains uniform throughout. At the grain boundaries in polycrystals, the Sb content is more than in the other regions of the crystal. Crystals grown from either Ga- or Sb-rich melts exhibit inclusions of the excess component. Post-growth annealing treatments in vacuum and Ga-rich atmospheres have been performed. Heat treatments in vacuum atmosphere produce very little effect on the local composition of the crystal. On the other hand, localized crystallization at grain boundaries and inclusions takes place in the presence of excess gallium. It has been shown that annealing treatments in Ga ambient can produce defect-free wafers with extremely homogeneous composition. It is concluded that the excess Sb which is liberated from the crystal during growth resides at the grain boundaries and other extended defect centers. The vacant Sb sites are then responsible for the formation of the native acceptor centers like V_Ga and Ga_Sb.     

Growth of USb2 single crystals and their structural perfection

USb₂ single crystals were grown by three methods; I — Chemical vapour transport with iodine as transporting reagent, II — Crystallization from U Sb liquid solution, III — Crystallization from U Sb Sn liquid solution. The morphology of growth and results of X-ray topography examination of crystal surface are given.     

Growth of thiourea-doped TGS crystals and their characterisation

Thiourea-doped Triglycine sulphate (ThTGS) crystal with three different concentrations of thiourea was grown from aqueous solution by slow cooling technique. The cell parameters were determined from powder X-ray diffraction analysis. A qualitative analysis of the presence of thiourea in doped crystals was estimated by FTIR analysis. Microhardness studies were carried out using Leitz Weitzler hardness tester at room temperature. Dielectric properties of the crystals were studied which showed a shift in the T_c when compared to pure TGS crystal. Pyroelectric studies were carried out and the pyroelectric coefficient was found. Piezoelectric studies (d₃₃ coefficient) has also been carried out.     

Growth of CdBr2 crystals by zone-melting and study of their growth features

A detailed surface microtopographic study has been carried out on the (0001) faces of melt-grown CdBr₂ single crystals. Mainly the growth of the crystals takes place by continuous solidification at the solid-liquid interface. Rarely, the growth occurs by two-dimensional nucleation and still more rarely by spiral mechanism. Most spirals are seen to be polygonized such that the polygonization extends right upto the centres of the spirals.     

Growth and ionic conductivity of Li3 + x P1 − x GexO4 (x = 0.34) single crystals

Li_{3 + x} P_{1 ? x} Ge_xO₄ crystals (x = 0.34) with dimensions of about 3 × 3 × 5 mm³ were grown for the first time from flux. The conductivities of the crystals measured along three directions have close values and are equal to σ ≈ 1.8 × 10^?6 and 3.7 × 10^?2 Sm/cm at the temperatures 40 and 400°C, respectively (similar to the case of pure lithium phosphate, somewhat lower values of electric conductivity were measure along the b axis). The activation energy of conductivity is equal to 0.54 eV. A considerable increase in the conductivity of the solid solution in comparison with the conductivity of pure lithium phosphate is explained by the specific features of the lithium sublattice in the crystal structure of the λ-Li₃PO₄ type.     

Superionic conductivity of Sr0.68Pr0.32F2.32 (type CaF2) and Pr0.85Sr0.15F2.85 (type LaF3) crystals,as-grown and after high-temperature annealing

The influence of high-temperature annealing (900°C, 14 days) in a fluorinating atmosphere on the superionic conductivity σ of as-grown Sr_0.68Pr_0.32F_2.32 single crystals with fluorite structure (CaF₂) and Pr_0.85Sr_0.15F_2.85 single crystals with tysonite structure (LaF₃), obtained by the directional solidification of melts in the SrF₂-PrF₃ system using the Bridgman method, is studied. The annealing that brings the defect structure of crystals to equilibrium at 900°C (which is retained by quenching) does not affect σ values. At 500 K, σ is 4 × 10^?4 and 2 × 10^?2 S/cm for Sr_0.68Pr_0.32F_2.32 and Pr_0.85Sr_0.15F_2.85, respectively. As-grown superionic conductor single crystals, which are formed in some MF₂-RF₃ systems (M = Ca, Sr, Ba; R are rare earth elements), where the mutual solubility of components in nonstoichiometric phases depends weakly on temperature, can be used in solid-state electrochemical devices operating at high temperatures and under temperature cycling conditions without the deterioration of their electrical characteristics.     

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)     

Growth of spinel crystals in vanadium slag and their characterization

Morphology of vanadium slags were investigated by scanning electron microscopy (SEM). The mineralogical phases were characterized by energy disperse X‐ray spectrometry (EDS) and powder X‐ray diffraction (XRD). The obtained results show that spinels and silicates are the major phases in the vanadium slag, and V is concentrated in Fe_xV_3‐xO₄ and Mg_x(V, Ti)_3‐xO₄. Both the spinel grain size and volume fraction in the slag with higher V₂O₃ content are much larger than that with lower V₂O₃ content. (Fe, Mn)₂SiO₄ and (Fe, Mn)SiO₃ have a higher proportion in the slag with lower V₂O₃ and higher SiO₂ content. The relation among cooling conditions and grain size and volume fraction of spinels is also discussed. It is found that low cooling rate and long holding time benefit spinel crystal growth, especially for the interval of 1200‐1250 °C. Both mean diameter and volume fraction of spinels could achieve or exceed the industry vanadium slag when holding more than 45 min. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of Yb-doped Y2O3, Sc2O3, and Lu2O3 single crystals by the micro-pulling-down technique and their optical and scintillation characterization

In this report, growth of Yb-doped sesqui-oxide crystals of Y₂O₃, Sc₂O₃, and Lu₂O₃ by the micro-pulling-down technique and their scintillation performance are discussed. Growth of these crystals is difficult mostly as a result of their extremely high melting point of around 2400 °C. Nevertheless, appropriate design of the thermal zone and careful control of the growth parameters allowed fabrication of these crystals of reasonable quality. Based on the results of measurements of emission spectra under α-ray excitation and pulse height spectra under α-ray and γ-ray excitations, scintillation characteristics of above crystals including emission wavelength and light yields under α-ray and γ-ray excitations were examined. Additionally, decay kinetics of these materials under α-ray excitation were evaluated.     

Growth and characterization of magneto‐optical YFeO3 crystals

The floating zone growth of magneto‐optical crystal YFeO₃ has been investigated. The polycrystalline feed rod was prepared by a pressure of 250MPa and sintering at about 1500°C. A crack‐ free YFeO₃ single crystal has been successfully grown. The crystal preferred to crystallize along <100> direction with about 10° deviation. The X‐ray rocking curve of the crystal has a FWHM of 24 arcsec, confirming the high crystal quality of the sample. The (100) plane was etched by hot phosphoric acid and the dislocation density was about 10⁴/cm². A thin outer layer with Y₂O₃‐rich composition was found at the periphery of as‐grown crystals, which was attributed to the Fe₂O₃ evaporation during growth. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and electrical conductivity of Pb2Ru2O6.5 crystals

Single crystals of Pb₂Ru₂O_6.5 have been grown by flux method from a mixture of lead oxides. The electrical conductivity of the crystals is of a metallic type, major current carriers being holes.     

Growth and structural, optical, and electrical properties of zincite crystals

An X-ray diffraction study of ZnO crystals grown by the hydrothermal method has revealed reflections that give grounds to assign them to the sp. gr. P3 rather than to P6₃ mc. The distribution of Zn1, Zn2, O1, and O2 over structural positions, along with vacancies and incorporated zinc atoms, explains the dissymmetrization observed in terms of the kinetic (growth) phase transition of the order-disorder type, which is caused by ordering Zn and O atoms over structural positions. The color of crystals of refined compositions (Zn_0.975□_0.025)Zn _i(0.015)(O_0.990□_0.010) (green) and (Zn_0.965□_0.035)Zn _i(0.035)O (bright green) is related to different oxygen contents, which is confirmed by the results of electron probe X-ray microanalysis and absorption spectroscopy. The degree of the structural quality of crystals, their resistivity, and activation energy are also related to oxygen vacancies.     

Preparation and electric conductivity of V2O5 single crystals

Present paper deals with the preparation of V₂O₅ single crystals, both pure and doped with Mg, Mn, and Fe respectively, by the method of zone melting. To verify the quality of crystals, measurements of electric conductivity were carried out in the direction perpendicular to cleavage plane (010). The results have shown that the prepared crystals are suitable for further investigation of physical properties.     

Doping of KDP single crystals with cerium: Growth and optical properties

The features of doping of KDP crystals with cerium ions and organocerium complexes with alizarin complexon and arsenazo III have been investigated. It is established that “direct” doping by introducing cerium salts into the initial solution cannot be implemented. The effect of organometallic complexes of cerium on the crystal growth has been studied. Organocerium complexes predominantly enter the prismatic or pyramidal growth sectors. It is shown that the complex arsenazo III + Ce blocks the growth of the prismatic sector. Cerium-doped KDP crystals exhibit a photoluminescence band peaking at the wavelength λ_max= 350 nm.