Growth,Ferroelectric Properties,and Phonon Modes of YMnO3 Single Crystal

YMnO₃ single crystals were grown by flux method and plate‐like single crystals with the c‐axis perpendicular to the surfaces were obtained. The maximum size of these crystals was about 2 × 2 × 0.07 mm³. Ferroelectric properties were measured at various frequencies and abnormal behavior at the low frequencies were observed and discussed using non‐linear current‐voltage behavior. Raman and IR spectra were obtained, and those results were compared with previous work.     

Growth and characterization of L‐prolinium tartrate – A new organic NLO material

Single crystals of L‐Prolinium tartrate (C₅H₁₀NO₂)⁺ (C₄H₅O₆)^‐, a new organic non‐linear optical material of size: 15 × 10 × 10 mm³ were grown using submerged seed solution growth method. Characterization of the crystals was made using single crystal X‐ray diffraction and density determination. Spectroscopic, thermal, optical and mechanical studies were carried out. These studies show that the crystals are thermally stable upto 161°C, transparent for the fundamental and second harmonic generation of Nd: YAG (λ = 1064 nm) laser and possess good mechanical strength. Second harmonic generation (SHG) conversion efficiency was investigated to explore the NLO characteristics of this material using Kurtz and Perry method and it was found that the SHG conversion efficiency is about 90% of that of the standard KDP crystals. Laser damage threshold study was also carried out. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of KBi(WO4)2 single crystals

Potassium bismuth tungstate [KBi(WO₄)₂] single crystals with dimensions up to 20 mm × 15 mm × 15 mm have been successfully grown by using the top‐seeded solution growth technique and K₂W₂O₇ as solvent. Experiments show that this crystal is unstable in a strong acid or alkali environment and has a blue fluorescence emission. The density, hardness, melting point, absorption edge, transparency range, prominent Raman shift frequency are 7.57 g/cm³, 238 kg/mm², 800 °C, 380 nm, 400–5450 nm, 868 cm^–1 respectively. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The effect of cooling rate on size,quality and morphology of KTiOPO4 (KTP) crystals grown by different nucleation techniques

KTP crystals have been grown by two nucleation techniques namely spontaneous nucleation in flux medium and nucleation on Pt rod using K₆P₄O₁₃ flux.10 °C/h, 7 °C/h, 0.8 °C/h, 0.4 °C/h and 0.2 °C/h cooling rates were applied for spontaneous nucleation and crystals up to 15 × 7 × 4 mm³ in size were grown. 1 °C/h and 0.8 °C/h cooling rates were also used for nucleation on Pt rod and crystals up to 8 × 6 × 3 mm³ in size were grown. The effect of cooling rate on size, morphology and optical quality of grown crystals by both techniques were studied. For nucleation on Pt rod upper and lower rotation rates limits and an optimum rotation rate were distinguished for each cooling rate. Quality of the grown crystals by both techniques was characterized by optical transmission analysis.     

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,crystal structure and spectrum of a novel rare‐earth orthophosphate crystal: Yb:LuPO4

Yb: LuPO₄ crystals with the size up to 6×2×0.5mm³ were grown by the flux growth process using lead pyrophosphate Pb₂P₂O₇ as the high‐temperature solvent. The crystal structure of Yb: LuPO₄ crystals at room temperature was refined by using single crystal X‐ray diffraction data. Crystal structure analysis showed that Yb: LuPO₄ crystals possessed the tetragonal xenotime structure. The polarized absorption spectra of Yb: LuPO₄ were tested at room temperature. The results showed that the absorption spectral region of Yb: LuPO₄ crystal was well matched for pumping with readily available diode lasers.     

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)     

Thermal and infrared studies of calcium malate crystals grown in diffusion limited medium

Single crystals of the title compound Ca (C₄H₅O₅)₂.10H₂O are grown in silica gel using controlled chemical reaction method. Multifaceted single crystals of size up to 8 × 4 × 2 mm³ are obtained. Powder X‐ray Diffraction (XRD) pattern of the grown crystal and the Fourier Transform Infra‐Red (FTIR) spectrum in the range 400–4000 cm^–1 are recorded. The vibrational bands corresponding to different functional groups are assigned. Thermal decomposition stages observed in the Thermo‐gravimetric (TG) and Differential Thermal Analysis (DTA) studies are discussed. A six‐stage thermal decomposition scheme is proposed for the compound. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of semiorganic NLO crystals of LAHClBr

Single crystals of non‐linear optical (NLO) LAHClBr were grown by slow evaporation technique from its aqueous solution. Good optical quality crystals having dimensions up to 12 × 9 × 7 mm³ were obtained. The lattice parameters and morphology for the grown crystals were determined using single crystal XRD. The crystals were characterized by FT‐Raman, optical absorption, thermal (DTA and TGA) and dielectric studies. LAHClBr was found to be thermally stable up to 124.3°C. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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 Vanadyl Pyrophosphate Single Crystals

The present work communicates about the first successful attempt at growing of sizeable single crystals of vanadyl pyrophosphate (VO)₂P₂O₇ (VOPO) — a low dimensional antiferromagnet. The growth of VOPO is complicated by two features of this compound. The first is a strong sensitivity of the oxydation state of vanadium (and stability of VOPO) to the oxygen content in the growth atmosphere. The second is a tendency of the VOPO-melt to glass formation during the cooling due to its high viscosity. Therefore the growth has to be carried out with a very low growth rate and in an atmosphere with exactly controllable oxygen content. The best results were achieved with a combination of Czochralski and Kyropoulos techniques, i.e. pulling of crystals with simultaneous cooling of the melt. Crystals of VOPO with sizes up to 10 × 5 × 3 mm³ have been grown. The growth from the melt is accompanied by growth from gaseous phase also (sublimation). Since the VOPO phase has a homogeneity range in oxygen content, attention was paid to the composition of the grown crystals. Growth experiments combined with TGA and XRD measurements show, that the oxygen content and thus the oxidation state of vanadium in the crystals can be adjusted accurately.     

The growth,spectral and thermal properties of the coordination compound crystal‐ strontium malate

Growth of single crystals of the title compound Sr(C₄H₄O₅).3H₂O is achieved using the gel diffusion technique. Multifaceted single crystals of size up to 4x3x3 mm³ are obtained. X‐Ray Diffraction (XRD) pattern of the grown crystal and the Fourier Transform Infra‐Red (FTIR) spectrum in the range 400‐4000 cm^‐1 are recorded. The vibrational bands corresponding to different functional groups are assigned. Thermal behavior of the material is investigated using Thermo Gravimetry (TG) and Differential Thermal Analysis (DTA). Thermal studies are indicative of a five‐stage decomposition scheme. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Growth of (Er,Yb):YAl3(BO3)4 laser crystals

(Er,Yb):YAl₃(BO₃)₄ single crystals of optical quality, up to 15 × 10 × 10 mm³ in size, have been grown from a (Er_0.023Yb_0.116Y_0.862)Al₃(BO₃)₄ solution in a Y₂O₃-B₂O₃-K₂Mo₃O₁₀ melt. The initial borate concentration was 17 wt %, and the flux cooling rate increased from 0.08 to 0.12°C/h in the range 1060–1000°C. The physical properties of the single crystals grown are good enough that they can be used as laser elements in systems with diode pumping and radiation near 1.5 μm.     

Growth Kinetics of Barium Sulphate in Suspension

The growth rate of barium sulphate seed crystals from stirred solutions was studied conductometrically at 25°C by a stopped-flow technique. The supersaturation ranged from 3 × 10⁻⁷ to 3 × 10⁻⁸ mol BaSO₄/cm³. The seed crystals were grown in the system during the initial (steady-state) period of the experiment. Crystal size distributions were determined by optical microscopy. The growth rate of barium sulphate under the conditions of the experiments can be expressed by a quadratic function of supersaturation. The results, which suggest an interface rate-controlling mechanism, are discussed with respect to published data.     

Microstructures of gel-grown ammonium hydrogen tartrate single crystals

Single crystals of ammonium hydrogen tartrate (AHT) have been grown in silica gels by employing the controlled reaction between ammonium chloride and tartaric acid. Transparent AHT crystals upto 24 × 4 × 3 mm³ in size have been grown at room temperature. Optical and electron-optical studies have been made on the various surface structures of {010} faces of the grown crystals. A variety of growth striations and growth hillocks have been observed. Growth layers modified by the presence of misaligned microcrystals have been illustrated. It has been suggested that two-dimensional nucleation, spreading and pilling up of growth layers is mainly responsible for the growth of these crystals and the implications are discussed.     

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.     

Crystal growth and magnetic properties of the copper coordination polymer [Cu(µ ‐C2O4)(4‐aminopyridine)2(H2O)]n

In this paper, we consider various ways of crystal growth of the polymer [Cu(µ ‐C₂O₄)(4‐aminopyridine)₂(H₂O)]_n. Single crystals of the size of 1.5×1.5×0.2 mm³ have been grown by a slow diffusion technique from solutions of the monoammine copper complex and of the mixture of potassium oxalate and aminopyridine with the stoichiometric ratio. Magnetic susceptibility and ESR measurements have been performed on single crystals large enough for investigating anisotropic properties. The susceptibility can be well described within the model of a Heisenberg antiferromagnetic spin chain. The magnetic measurements reveal a small concentration of paramagnetic moments reflecting the high quality of the single crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth,structure, and superconducting properties of Bi2Sr2Ca2Cu3O10 and (Bi,Pb)2Sr2Ca2Cu3O10‐y crystals

Large and high‐quality single crystals of both Pb‐free and Pb‐doped high temperature superconducting compounds (Bi_1‐xPb_x)₂Sr₂Ca₂Cu₃O_10‐y (x = 0 and 0.3) were grown by means of a newly developed “Vapour‐Assisted Travelling Floating Zone” technique (VA‐TSFZ). This modified zone‐melting technique was realised in an image furnace and allowed for the first time to grow Pb‐doped crystals by compensating for the Pb losses occurring at high temperature. Crystals up to 3×2×0.1 mm³ were successfully grown. Post‐annealing under high pressure of O₂ (up to 10 MPa at T = 500°C) was undertaken to enhance T_c and improve the homogeneity of the crystals. Structural characterisation was performed by single‐crystal X‐ray diffraction (XRD) and the structure of the 3‐layer Bi‐based superconducting compound was refined for the first time. Structure refinement showed an incommensurate superlattice in the Pb‐free crystals. The space group is orthorhombic, A2aa, with cell parameters a = 27.105(4) Å, b = 5.4133(6) Å and c = 37.009(7) Å. Superconducting studies were carried out by A.C. and D.C. magnetic measurements. Very sharp superconducting transitions were obtained in both kinds of crystals (ΔT_c ≤ 1 K). In optimally doped Pb‐free crystals, critical temperatures up to 111 K were measured. Magnetic critical current densities of 2�10⁵ A/cm² were measured at T = 30 K and μ₀H = 0 T. A weak second peak in the magnetisation loops was observed in the temperature range 40‐50 K above which the vortex lattice becomes entangled. We have measured a portion of the irreversibility line (0.1‐5 Tesla) and fitted the expression for the melting of a vortex glass in a 2D fluctuation regime to the experimental data. Measurements of the lower critical field allowed to obtain the dependence of the penetration depth on temperature: the linear dependence of λ(T) for T < 30 K is consistent with d‐wave superconductivity in Bi‐2223. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of large KDP single crystals for UV spectrum range

The influence of various technological parameters of crystallization (acidity of growth solutions, crystallization temperature, growth rate, degree of solution purification) on the optical absorption of large KDP single crystals has been studied in the UV range of the spectrum. It is shown that the method of solvent recirculation with the use of the starting material with the microimpurity content not exceeding 5 × 10^?5 wt % and solution ultrafiltration under the optimum crystallization conditions (t_cr = 80°C, V_cr ～ (0.8–1.6) × 10^?6 cm/s, pH 4) enables one to grow KDP single crystals with cross sections up to 300 × 300 mm² and the transmission in the vicinity of the fundamental absorption edge λ = 200 nm) equal to 86%.     

The (NH4)H2PO4-KCl-KNO3-H2O system and growth of crystals of the [(NH4),K]H2PO4 solid solutions

On the basis of the known data on the (NH₄)H₂PO₄-KCl-KNO₃-H₂O system, 65.0 × 9.0 × 8.0-mm³-large crystals of the [K_0.75(NH₄)_0.25]H₂PO₄ solid solutions are grown on seed by the method of temperature decrease. It is shown that the 60.0 × 17.0 × 10.0 mm³-large KH₂PO₄ crystals contain impurities: 6.0 × 10⁻³ wt % Li and 0.1 wt % Na. __________ Translated from Kristallografiya, Vol. 50, No. 4, 2005, pp. 761–764. Original Russian Text Copyright ? 2005 by Soboleva.