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)     

Growth and characterization of pure and lithium doped L‐alanine single crystals for NLO devices

Single crystals of pure and lithium substituted L‐alanine are successfully grown by slow evaporation method at constant temperature of 32°C. The effect of lithium dopant on crystal properties has been studied. Powder and single crystal XRD analysis confirms the structure and change in lattice parameter values for the doped crystals. The crystals were characterized by solubility studies, density, melting point measurements, FTIR and UV‐Vis‐NIR techniques. Thermal and mechanical stability of crystals were tested by TGA/DTA and micro hardness analysis. NLO activity of the crystals is found to be increased in the presence of lithium ions. The dielectric constant and dielectric loss of the crystals were studied as a function of frequency. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,growth and characterization of single crystals of pure and thiourea doped L‐glutamic acid hydrochloride

L(+)Glutamic acid hydrochloride [HOOC (CH₂)₂CH(NH₂) COOH·HCl], a monoamino dicarboxylic acid salt of L‐Glutamic acid was synthesized and the synthesis was confirmed by FTIR analysis. Solubility of the material in water was determined. Pure and Thiourea doped L‐Glutamic acid hydrochloride crystals were grown by low temperature solution growth using solvent evaporation technique. XRD, UV‐Vis‐NIR analyses were carried out for both pure and thiourea doped crystals. The crystals were qualitatively analyzed by EDAX analysis and the presence of thiourea was confirmed. The cell parameters of L‐Glutamic acid hydrochloride have been determined as a = 5.151 Å, b = 11.79 Å, c = 13.35 Å by X‐ray diffraction analysis and it crystallizes in orthorhombic space group P2₁2₁2₁. UV‐Vis‐NIR spectra analysis showed good optical transmission in the entire visible region for both pure and doped crystals. Micro hardness of both pure and doped crystals has been determined using Vickers micro hardness tester. The SHG efficiencies of both pure and doped crystals were determined using Kurtz powder test and pure L‐Glutamic acid hydrochloride crystal was found to possess better efficiency than thiourea doped L‐Glutamic acid hydrochloride crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of 4‐(2‐hydroxyphenylamino)‐pent‐3‐en‐2‐one single crystals

4‐(2‐hydroxyphenylamino)‐pent‐3‐en‐2‐one (HPAP) was synthesized and single crystals were grown by the solution growth technique using methanol as a solvent. The crystals having orthorhombic symmetry were characterized by single crystal XRD, FTIR spectroscopy, NMR spectroscopy, TGA, DSC and dielectric studies. Very less variation in the value of dielectric constant is found for different frequencies of applied field. The crystals were exhibiting positive photoconductivity and poor NLO responses. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation of three‐dimensional symmetric dendrites of BaWO4 microcrystals

Three‐dimensional symmetric dendrites of BaWO₄ were prepared by performing solvothermal reactions in water‐hexane bilayer solutions that contained a barium‐oleate complex in the hexane layer and sodium tungstate in the water layer. The barium‐oleate complex in hexane was obtained via a phase transfer reaction in which aqueous Ba²⁺ ions pass into the hexane phase with the assistance of sodium oleate, oleic acid, and oleylamine. Each of the BaWO₄ dendrites has a three‐dimensional structure with one trunk along the c‐axis and a series of four branches perpendicular to the trunk. As the reaction temperature or the amount of oleylamine increases, BaWO₄ dendrites with sharper branches and higher order hierarchical structures are formed. The presence of oleylamine plays an important role in the formation of the hierarchical superstructures of BaWO₄ dendrites.     

Nitrogen‐doped zirconia single crystals

The aim of this work is the preparation of nitrogen‐doped single crystals of cation‐stabilized zirconia. Thin plates of these crystals were nitrided in a graphite heated resistance furnace with nitrogen as reaction gas. Several dwell times and reaction temperatures were tested and their effect on the amount of incorporated nitrogen is investigated. During nitridation at high temperatures a rock salt‐type ‘ZrN’ layer grows on the surface, leading to the destruction of the crystal. In contrast to the fluorite‐type bulk material, which can be described as a fast anion conductor, the surface layer shows electronic conductivity. For possible applications of the bulk material (solid electrolyte) the formation of the surface layer must be avoided. Therefore, the interface between surface epilayer and bulk material was investigated in detail by electron microscopy methods. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of ultra‐high purity PbI2 single crystal: (1) Preparation of high purity PbI2

In order to prepare high purity lead iodide (PbI₂) single crystals, the starting material‐iodine (I) has been purified by the sublimation method, and the PbI₂ polycrystalline by the normal freezing method. The purification effect of these methods has been confirmed by evaluating the impurity concentration in ingot by glow discharge mass spectrometry (GDMS) analysis. By comparing the purity of three different starting materials, non‐purified iodine+6N‐Pb, purified iodine+6N‐Pb and commercial 6N‐PbI₂, PbI₂ synthesized by purified iodine in the present experiment has the highest purity. This indicates that these purification methods are suitable. The present research results are expected to prepare high‐resistivity PbI₂ used in radiation detector. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical and dielectric studies on pure and Ni2+, Co2+ doped single crystals of bis thiourea cadmium chloride

Good quality single crystals of Ni²⁺, Co²⁺ ions doped Bisthiourea Cadmium Chloride (BTCC) are some of the excellent and efficient non‐linear optical materials grown from aqueous solution by slow evaporation method. The lattice parameters of the grown crystals are determined by single crystal X‐ray analysis. UV spectral analyses on these samples reveal the improved transparency of the doped crystals ascertaining the inclusion of metal ion in the lattice. FTIR spectral analysis carried out on the materials confirm the presence of functional groups. Dielectric measurements reveal that the dielectric constant of pure and doped crystals decreases with increase of frequency. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Flux growth and characterization of Ti‐ and Ni‐doped forsterite single crystals

Forsterite monocrystals doped with Ti and Ni were grown by the flux growth technique. A suitable mixture of flux (MoO₃, V₂O₅, Li₂CO₃) and nutrient was slowly cooled down to 750 °C from 1250 °C or 1350 °C. The crystals were then characterized by powder and single‐crystal X‐ray diffraction, scanning electron microscopy and differential scanning calorimetry (DSC). Variations observed in crystal size were attributed by both the varying experimental conditions in which they had been obtained, and to the amount of Ni substituted for Mg in the structure. High abundances of doped forsterite required a cooling rate of 1.8 K h^‐1. These synthetic, well‐characterized Ti and Ni doped forsterite crystals may have potential for exploitation in industrial fields. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of pure and doped nonlinear optical l‐arginine acetate single crystals

Single crystals of organic nonlinear optical material of pure, Cu²⁺ and Mg²⁺ doped L‐arginine acetate (LAA) were successfully grown by slow evaporation method at room temperature. The UV‐Vis‐NIR spectra of pure and doped LAA indicate that these crystals possess a wide optical transmission window from 240‐1600 nm. Non‐linear optical studies reveal that the SHG efficiency of LAA is nearly three times that of KDP. The dielectric response of the samples was studied in the frequency region 100 Hz to 2 MHz and the influence of Cu²⁺ and Mg²⁺ substitution on the dielectric behaviour had been investigated. Photoconductivity study proves that both pure and Cu²⁺ and Mg²⁺ doped LAA crystal exhibit positive photoconductivity. It is evident from the Vickers hardness study that the hardness of the crystal decreases with increasing load both for pure and doped samples. ESR studies confirmed the incorporation of Cu²⁺ into LAA and the value of g‐factor was found to be 2.1654. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Capsule‐like α‐Fe2O3 nanoparticles: Synthesis,characterization, and growth mechanism

Uniform capsule‐like α‐Fe₂O₃ particles were synthesized via a simple hydrothermal method, employing FeCl₃ and CH₃COONa as the precursors and sodium dodecyl sulfate (SDS) as soft template. X‐ray powder diffraction (XRD), field emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), and high‐resolution transmission electron microscopy were used to characterize the structure of synthesized products. Some factors influencing the formation of capsule‐like α‐Fe₂O₃ particles were systematically investigated, including different kinds of surfactants, the concentration of SDS, and reaction times. The investigation on the evolution formation reveals that SDS was critical to control the morphology of final products, and a possible five‐step growth mechanism was presented by tracking the structures of the products at different reaction stages.     

Crystal growth and characterization of PbI2‐AgI binary system

The crystals of the binary system PbI₂‐AgI (PIAI) were obtained by heating the mixture of individual PbI₂ (PI) and AgI (AI) placed at 30° angle in the horizontal tubular furnace of variable temperature zone. The crystals were characterized by powder XRD, TG/DTA, FT‐IR and SEM. The 3.37% weight loss in the sample after heating at 853 K is due to the presence of water molecules absorbed (3446 cm^–1) by the crystals during sintering and cooling process. The cell parameters of the crystal were determined using the powder X‐ray data. The PbI₂‐AgI crystallizes in monoclinic system a = 10.799 (±0.009), b = 7.492 (±0.004), c = 6.929(±0.004) Å and α = 90°, β = 108.04(±0.073) γ = 90°, V = 533.18 ų. The electrical conductivity measurements of the crystals showed a sudden change in the current value at the temperature range 385–393 K. The activation energy before and after the drift was found to be 0.49 and 0.35 eV respectively. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Thermoelectric properties of Tl‐doped Bi2Se3 single crystals

The single crystals of the ternary system based on Bi_2‐xTl_xSe₃ (nominaly x = 0.0‐0.1) were prepared using the Bridgman technique. Samples with varying content of Tl were characterized by the measurement of lattice parameters, electrical conductivity σ_⊥c , Hall coefficient R_H (B∥c), and Seebeck coefficient S (ΔT ⊥c). The measurements indicate that by incorporating Tl in Bi₂Se₃ one lowers the concentration of free electrons and enhances their mobility. This effect is explained in terms of the point defects in the crystal lattice – formation of substitutional defects thallium on the site of bismuth Tl_Bi and the decrease of concentration of selenium vacancies V_Se⁺². We also discuss the temperature dependence of the power factor σS² of the samples. Upon the thallium doping we observe a significant increase of the power factor compare to the parental Bi₂Se₃. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Investigation of structural,electronic and optical properties of pure and Ag‐doped TiO2 nanofibers fabricated by electrospinning

Pure and 1, 2, and 3 wt% Ag doped TiO₂ nanofibers were prepared by electrospinning method at different applied voltages and heights at a constant flow rate of 2 mL/h. Characterization of the prepared samples was performed by x‐ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microcopy (AFM),four point probe method (FPPM), the differential scanning calorimetry/the thermal gravimetric analysis (DSC/TGA), ultraviolet/visible spectrometry (UV/VIS), and energy dispersive X‐ray spectrometer (EDX). It was found that the thermally untreated pure TiO₂ nanofibers and thermally treated (at 500 °C) samples have the crystalline phase of anatase (A), and mixed anatase and rutile (A+R) phases, respectively. It was also observed that the content of the silver does not affect the crystal structure, but plays strengthening role in the rutile structure. SEM micrographs showed that all fabricated nanofiber samples have uniform morphologies, and AFM measurements indicated that the nanofibers were formed in three‐dimensional coils. The band gap values of the nanofiber samples obtained from UV/VIS measurements revealed that band gap values of the nanofiber samples decrease while the diameter of the nanofiber increases.     

Growth and optical characterization of cerium and lead‐doped Bi12TiO20 sillenite single crystals

Bi₁₂TiO₂₀ (BTO) single crystals doped with PbO and CeO₂ were grown by the Top Seeded Solution Growth (TSSG) technique from the liquid phase with nominal compositions of 10Bi₂O₃ : (1–x)TiO₂ : x PbO and 10Bi₂O₃ : (1–x)TiO₂ : xCeO₂ with x = 0.25 and 0.10. No growth‐related difficulties were encountered other than those typical of sillenite crystals. Samples with good optical quality were obtained and were characterized by optical absorption, dark current, spectral photocurrent dependence, optical activity and electro‐optic coefficient measurements. A comparison is made of the results of the optical measurements of doped and undoped BTO crystals. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth,morphology, spectrographic characterization and thermal properties of 4,5‐bis(benzoylthio)‐1,3‐dithiole‐2‐thione

Single crystals of 4,5‐bis(benzoylthio)‐1,3‐dithiole‐2‐thione (BBDT), were grown from methylene chloride and the growth morphology was deduced by the Bravais–Friedel Donnay–Harker (BFDH) model. The grown crystals were characterized by optical absorption, infrared, Raman and X‐ray powder diffraction spectroscopy. The thermal behavior of BBDT has been investigated by means of thermogravimetric analysis and differential thermal analysis measurements in air. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Characterization of L‐ascorbic acid single crystals grown from solution with different solvents

Single crystals of L‐ascorbic acid, popularly known as vitamin‐C, were grown from solutions with different solvents and solvent combinations by low temperature solution growth methods. The suitability of different solvents and solvent combinations such as acetone, ethanol, methanol, isopropyl alcohol, water, water + acetone (1:1), water + ethanol (3:1), water + isopropyl alcohol (3:1) and isopropyl alcohol + methanol (1:1) for crystal growth of L‐ascorbic acid was found out by assessing the solubility and crystallization behaviours. Solubility of L‐ascorbic acid in selected solvents and solvent combinations in a range of temperatures was determined by gravimetric method. Solution prepared with water, water + acetone (1:1), water + ethanol (3:1) and water + isopropyl alcohol (3:1) were yielded crystals with tabular, columnar and prismatic habits and their morphologies were evaluated by goniometry. Grown single crystals were characterized with various instrumental techniques such as powder X‐ray diffraction, Fourier infrared spectroscopy, optical transmittance study, differential scanning calorimetry and second harmonic generation studies. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

硫镓银晶体(112)面蚀坑形貌研究

本文报道了一种能在室温下对硫镓银晶体(112)面进行择优腐蚀的新腐蚀液配方,采用新腐蚀液对改进的Bridgman法生长的AgGaS2晶体进行腐蚀,用扫描电镜对蚀坑进行了观察,得到了清晰的(112)面蚀坑形貌,形状为三角锥形.初步解释了蚀坑的形成原因.AgGaS2晶体低指数的{100}面的腐蚀速度较慢,在腐蚀过程中逐渐显露出来,最终使晶体(112)面呈现出三角锥形蚀坑形貌.     

碲锌镉单晶体的(110)面蚀坑形貌观察

本文报道了一种能够在室温下择优腐蚀碲锌镉(CZT)单晶体(110)晶面的腐蚀液配方,并对富Cd生长的CZT晶体蚀坑形貌进行了扫描电镜观察.结果表明晶体(110)面腐蚀坑形状为三角形,并初步对蚀坑的成因进行了分析,估算出CZT(110)面蚀坑密度约为103～105/cm2数量级.这说明富Cd原料的改进布里奇曼法可以生长出低蚀坑密度的CZT单晶体.     

Growth and properties of Ba‐doped KDP crystals

KDP crystals were rapidly grown from solution doped with different Ba²⁺ concentrations. The effects of Ba²⁺ on the growth rate, morphology and quality of KDP crystals were discussed. Significant changes in shapes and volume of the grown crystals have been observed. During the growth process, defect region expands gradually with the increasing Ba²⁺ concentration. Samples were cut from different parts of the as‐grown crystals for investigating the optical quality, including transmission spectrum, scattering centers. Through comparison, it is found that the nonuniform distribution of Ba²⁺ ions causes remarkable difference in optical quality between prismatic and pyramidal sectors. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)