Structural and optical investigations on Mn doped Li2B4O7 crystals

Lithium tetraborate crystals have great demand due to its non‐critical phase matching at 90°. Transparent and good optical quality single crystals of undoped and Mn doped Li₂B₄O₇ were grown by Czochralski technique in air atmosphere. The crystalline phase was determined by X‐ray diffraction. Doping of Mn in the grown crystals was confirmed by energy dispersive analysis of X‐rays (EDAX) technique. Transmission spectra show that the crystal is transparent in the visible region. Birefringence interferograms were recorded to qualitatively analyse the optical homogeneity of the grown crystals and to quantify the birefringence of the samples in desired crystal direction. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of pure and Co2+‐doped Li2B4O7 single crystals

Pure and Co‐doped Li₂B₄O₇ (LBO) single crystals were grown by the Czochralski method. Starting concentrations of Co₂O₃ in the melt were: 0.5, 0.85 and 1 mol% relative to Li₂CO₃. Technological factors affecting the quality of both crystals were discussed. Optical absorption and EPR spectra were analyzed to define the oxidation states and lattice sites of cobalt ions. It was shown that Co²⁺ ions enter LBO crystal at octahedral Li⁺ site positions. Low‐temperature EPR measurements revealed that two types of Co²⁺ complexes can be distinguished in the Li₂B₄O₇:Co crystals. Additional absorption calculated for γ‐irradiated crystals showed V_k type defects suggesting the creation of cation vacancies during growth. The concentration of the defects decreases with an increase of intentional Co concentration. Introduction of cobalt ions to LBO crystal is limited probably by the formation of cobalt ion pairs or by the entrance of cobalt as Co⁺. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crack resistance and atomic structure of Li2B4O7 single crystals

The nature of destruction of single crystals of lithium tetraborate Li₂B₄O₇ under the action of a concentrated load is investigated. It is established that planes of easy crack propagation in Li₂B₄O₇ single crystals are the (100), (010), (001), and {111} planes. It is found that crack propagation occurs in each case along the atomic layers that are linked by bridge oxygen atoms between main structural units (B₄O₉) and, therefore, are most weakly bound.     

Charge transport in Li2B4O7 in single crystal and glassy states

The electrophysical properties of Li₂B₄O₇ single crystals and glasses are studied in the temperature range 290–1100 K and the frequency range 1–1000 kHz. The strong frequency dispersion of ionic conductivity at temperatures close to room temperature is explained by the low-frequency hoppings of lithium ions from the basic to the interstitial positions. The dielectric relaxation accompanying the transport of lithium ions is analyzed within the framework of the Debye-Skanavi model. The minimum hopping length of Li⁺ ions and the height of the potential barrier between their closest positions are determined. The parameters obtained are compared with the known structural data.     

Optimisation of chromium doping in LiNbO3 single crystals

Growth of undoped and Cr doped (0.1, 0.25 and 0.5 mol % Cr₂O₃) congruently‐ melting‐composition LiNbO₃ single crystals by Czochralski technique is reported. Chromium doping was optimised to get crystals with potential for an integrated, broadband, tunable laser in the 700‐1100 nm spectral range. Typical sizes of the grown crystals are 25‐30 mm in diameter and 30‐40 mm in length. Symmetrical and sharp conoscopy pictures confirm the optical homogeneity of the crystals. Optical transmission was recorded for both undoped and doped crystals. 70% transmittance was observed. The grown crystals have reasonably good laser damage threshold. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Temperature Dependence of Static Electrical Conductivity of Li2B4O7 Crystals

Crystallography Reports - The static dc electrical conductivity of one-dimensional ion conductor Li2B4O7 (sp. gr. I41cd) has been investigated in the temperature range of 293–820 K using...     

Li2B4O7晶体在SAW技术中的应用研究

采用CZ法生长了30×30mm3的Li2B4O7单晶体.对晶体的压电性能进行了研究,弹性系数的交叉分量少,数值相对较小;在(001)面内有较高的声波传播速度,其变化范围为6500～7080m/s,在[001]方向有较低的声波传播速度,大约为5160m/s;而压电性能表明在不同方向的机电耦合系数均比石英晶体相应参数大得多.对晶体谐振器和压控震荡器的性能进行了研究,发现其机电耦合系数近似石英的十倍,很适合用来制作宽频器件.晶体谐振器的频率温度特性为抛物线型,其转变温度在室温,在-10℃～55℃温度范围内频率变化为3×10-4,具有良好的频谱响应,其寄生频率高出主振180kHz,衰减大于30dB,完全能满足器件使用要求.晶体滤波器3dB带宽的相对宽为1;,而石英仅为0.4;.     

Behavior of LiOH·H2O crystals obtained by evaporation and by drowning out

In the present work, the behavior of crystals derived from two different crystallization methods applied in a concentrated aqueous lithium salt solution was studied. The LiOH·H₂O crystals obtained by a simple evaporation (Crystal I) differed in terms of morphology and solubility from those precipitated from lithium hydroxide solutions by addition of ethanol as a co‐solvent (Crystal II). Solubility of Crystal II at different temperatures (15 to 35°C) and mass ratios of ethanol to water (0 to 0.1) was determined. Polymorphic like behavior of these crystals was evidenced from X‐ray diffraction patterns. Measurement of density, refractive index, absolute viscosity and electrical conductivity of saturated solutions are reported. A thermodynamic analysis in terms of the Chen model for the calculation of activity coefficients, indicate that the polymorphic system in water and in water + ethanol (ethanol/water ratio 0.1) is enantiotropic. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A novel growth method for ZnAl2O4 single crystals

ZnAl₂O₄ is a well‐known wide band gap compound semiconductor (E_g=3.8eV), ceramic, opto‐mechanical, anti‐thermal coating in aero‐space vehicles and UV optoelectronic devices. A novel method for the growth of single crystals of a ternary oxide material was developed as a fruit of a long term work. Material to be grown as metal incorporated single crystal was taken as precursor and put into a bath containing acid as reaction speed up reagent (catalyst) as well as solvent with a metal foil as cation scavenger. Using this method, ZnAl₂O₄ crystals having hexagonal facets are prepared from a single optimized bath. Structural and compositional properties of crystals were studied using Philips, Xpert ‐ MPD: X‐ray diffractometer and Philips, ESEM‐TMP + EDAX. Thus technique was found to be a new low cost and advantageous method for growth of single crystals of ternary oxide a material. We hope that these data be helpful either as a scientific or technical basis in material processing. Dedicated to Prof. P. Ramasamy © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Nuclear57Fe relaxation in Fe2+-containing NiFe2O4 and CoFe2O4 single crystals

Spin-lattice (T ₁) and spin-spin (T ₂) relaxation times of ⁵⁷Fe nuclei in the single-crystal NiFe₂O₄ and CoFe₂O₄ ferrites containing Fe²⁺ ions have been studied in the temperature range of 4.2–100 K by a spin-echo technique. The peaks of relaxation rates T ₁ ^?1 and T ₂ ^?1 caused by the presence of Fe²⁺ ions were observed for both ferrites in the ranges 38–42 and 28–32 K, respectively. The analysis of the results obtained with invocation of the data on ferromagnetic resonance and the measurements of the temperature dependence of resistivity shows that the mechanism of nuclear relaxation responsible for “impurity” peaks and is a slow relaxation process caused by electron exchange Fe²⁺ ? Fe³⁺, characterized by a low activation energy.     

Domain structures and etching morphologies of lithium niobate crystals with different Li contents grown by TSSG and double crucible Czochralski method

Stoichiometric lithium niobate single crystals with different Li contents have been grown both by the top‐seeded solution growth (TSSG) method from potassium containing flux and by the double crucible Czochralski (DC Cz) method. Spectroscopic properties (e.g. the UV absorption edge, Raman linewidth) and the Curie temperature measurement have been used for the characterization of the crystal composition. The double crucible Czochralski method is found to be suitable for mass production of stoichiometric LiNbO₃ with Li content larger than 49.7 mol% and homogeneity of 0.03 mol%. The domain structures and etching morphologies on negative and positive c‐surface were also investigated by chemical etching method. A new domain structure of three‐fold symmetric sectors were observed in near‐stoichiometric LiNbO₃ grown by TSSG method. The straight line arrangement hillocks on negative c‐surface and the net‐like arrangement etch lines were observed and explained by stress etching mechanism. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Evolution of nanocrystalline BaBi2Nb2O9 in Li2B4O7–BaO–Bi2O3–Nb2O5 glass system

Transparent glasses and glass nano crystal composites (GNCs) of various compositions in the system (100 − x)Li₂B₄O₇–x(BaO–Bi₂O₃–Nb₂O₅) (where x = 10, 20, and 30 in molar ratio) were fabricated via splat-quenching technique. The glassy nature of the as-quenched samples was established by differential thermal analyses. X-ray powder diffraction and transmission electron microscopic (TEM) studies confirmed the formation of layered perovskite BBN via a fluorite like phase. TEM studies revealed the presence of 10 nm sized spherical crystallites of fluorite like BaBi₂Nb₂O₉ phase in the glassy matrix of Li₂B₄O₇ (LBO). The influence of composition on the dielectric and the optical properties (transmission, optical band gap) of these samples has been investigated.     

Nucleation of struvite (MgNH4PO4 · 6 H2O) single crystals and aggregates

The conditions (concentration and pH) for preparation of single crystals of struvite at 25 °C from ammoniacal solutions equimolar with respect to magnesium and phosphate ions are given. The limits are found above which crystal aggregates (twins or dendrites) precipitate as dominant morphology. The mechanisms of nucleation are discussed and the interfacial tension between crystals and solution is evaluated.     

Thermal expansion,pyroelectricity and linear optical properties of Li2SeO4·H2O and Li2SO4·H2O

Large single crystals of polar Li₂SeO₄·H₂O were grown at 343 K from aqueous solution. Temperature dependent thermal expansion coefficients of Li₂SeO₄·H₂O and Li₂SO₄·H₂O were determined within the temperature range 133 K–313 K and coefficients of the pyroelectric effect within the temperature range 183–343 K. Refractive indices between 365 nm and 1530 nm as well as unpolarized absorption spectra of Li₂SeO₄·H₂O and Li₂SO₄·H₂O were measured and phase‐matching curves for second harmonic generation were calculated. Both compounds allow type I and type II phase‐matching at wavelengths from about 650 nm to the near infrared region. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Some characteristic features of formation of composite material based on KDP single crystal with incorporated Al2O3·nH2O nanoparticles

Composite material based on KDP (KH₂PO₄) crystal matrix with incorporated aluminum oxyhydroxide Al₂O₃·nH₂O nanoparticles is obtained and peculiarities of the formation of KDP:Al₂O₃·nH₂O composite structure are studied by selective etching, optical and scanning electron microscopy. Influence of the nanoparticles on the formation of defect subsystem is analyzed. The obtained material is shown to have a zonal structure with a period independent of the concentration of nanoparticles. By means of FTIR‐spectroscopy, interaction of nanoparticles with KH₂PO₄ solution is studied. A model of the capture of nanoparticles by the {100} KDP crystal face is proposed.     

Observations of crack patterns in NaSbF4 and NaSb2F7 single crystals

Crack pattern studies on NaSbF₄ and NaSb₂F₇ single crystals have been carried out using Leitz Wetzler microhardness tester. Attempts have been made to understand the nature of the cracks developed around the microindentation impression. The fracture toughness, index of brittleness and crack resistance have also been calculated.     

Optical absorption and photoelectric properties of Ga2In4S9 single crystals

Presented in this paper are the results obtained from the investigation of absorption edge and photoconductivity of layered Ga₂In₄S₉ single crystals as well as from the investigation of the photovoltaic effect in Pt—Ga₂In₄S₉ surface-barrier structures. We determined the magnitude of the direct band gap to be E_g = 2.72 eV and the position of the sensitizing centres to be ≈︁0.15 eV above the valence band top. In the regions of the photon energies smaller than E_g the absorption band edge is described by an exponential dependence with a temperature independent slope.     

Growth of lithium triborate (LiB3O5) single crystals in the Li2O-B2O3-MoO3 system

Solubility curves are plotted and optimal solvents for growing lithium triborate (LiB₃O₅) single crystals are determined. The crystallization range of this compound in the Li₂O-B₂O₃-MoO₃ system is refined. The molybdenum content in the crystals grown is analyzed.     

Electrooptical coefficients and temperature and pressure derivatives of the elastic constants of tetragonal Li2B4O7

New values for the following properties of tetragonal Li₂B₄O₇ are reported: dielectric, electrostrictive, electrooptic, elastic, thermoelastic and piezoelastic constants, coefficients of thermal expansion and indices of refraction. These values are considered to be of superior precision compared to earlier published data. Most elastic constants possess positive temperature derivatives. This anomalous behaviour is not reflected in the pressure derivatives. The electrooptic effects are not large enough to compete with other materials used for technical applications.     

Optical properties of ZnNb2O6 single crystals prepared via the optical floating zone technology

By using an optical floating zone technology, orthorhombic columbit ZnNb₂O₆ single crystals are fabricated successfully. The as‐prepared sample are blue and transparent rods of Φ 4 to 6 mm ×L 48 mm and the biggest domain of Φ 4 mm× L 25 mm. After annealing, the sample fades to colorless. X‐ray diffractions indicates that the as‐perpared samples are ZnNb₂O₆ with orthorhombic columbite structure and grows along the a‐axis. The micropolariscopy in cross transmission arrangements analyzing give that the crystals are of low‐angle crystal boundary‐free and bubble‐free. Besides, the crystals have also been tested by Raman spectra, optical absorption and photoluminescence spectra before and after being annealed. The luminescence pattern has an emission peak located at 450 nm blue‐region.