Growth of dl-malic acid-doped ammonium dihydrogen phosphate crystal and its characterization

Single crystals of dl-malic acid-doped ammonium dihydrogen phosphate have been grown using slow evaporation method and also by Sankaranarayanan–Ramasamy (SR) method with the vision to improve the properties of the ADP crystals. The characterization of grown crystals was made by single-crystal X-ray diffraction, powder X-ray diffraction, UV–vis. spectroscopy, Fourier transform infrared spectroscopy (FTIR), differential thermal analysis (DTA), Vicker's microhardness, dielectric measurements, high-resolution X-ray diffraction (HRXRD) and second-harmonic studies. Structural difference between pure and doped crystal has been studied by XRD analysis. Functional groups were identified by FTIR spectroscopy. The grown crystals were found to be transparent in the entire visible region. Decomposition temperatures of the grown crystals were measured by DTA. Vicker's hardness study carried out on (0 0 1) face at room temperature shows increased hardness of the doped crystals and SR-method-grown crystals. Dielectric measurements reveal that SR-method-grown DLM-doped ADP crystals have low dielectric loss. Crystalline perfection of the grown crystals is analyzed using HRXRD. Preliminary measurements indicate that the second harmonic generation efficiency of the doped crystals at a fundamental wavelength of 1064 nm is roughly 1.5 times greater than that of pure ADP.     

Growth of trivalent ions doped PbWO4 crystals and their scintillation properties

Undoped and series of trivalent ions(including La, Y, Gd and Tb) doped PWO crystals were grown from 5N raw materials by using Czochralski technique. Trivalent ions doping improved the transmittance, fast components of luminescence and radiation damage resistance for compensating structure defects. Corresponding, the fraction of light yield at shorter collecting time was increased. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and scintillation properties of the Eu2W3O12 crystal

The growth and scintillation properties of the Eu₂W₃O₁₂ crystal are reported. The Eu₂W₃O₁₂ single crystal has been grown by the Bridgman method. And the colored Eu₂W₃O₁₂ single crystal has been achieved. The Ultraviolet fluorescence spectra and the X-ray excited luminescence spectra show that the Eu₂W₃O₁₂ crystal has emission at the 590 nm and 612 nm. The fluorescence decay time of the Eu₂W₃O₁₂ crystal is about 520 μs. The luminosity of the Eu₂W₃O₁₂ single crystal under X-ray excitation is about 8% of the luminosity of the BGO single crystal. Those results show that the Eu₂W₃O₁₂ crystal has potential application as the X-ray intensifier.     

Growth and luminescence properties of large‐scale zinc oxide nanotetrapods

Large‐scale zinc oxide (ZnO) nanotetrapods have been grown on p‐type Si (111) substrate by oxidizing zinc pieces in air by thermal evaporation technique without the presence of any catalyst. The size and morphology of the nanostructures was found to depend on experimental parameters. The grown nanostructures were characterized by X‐ray Diffraction (XRD), Photoluminescence (PL), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), High Resolution TEM (HRTEM) and analysis of elemental composition was done by Energy Dispersive X‐ray analysis (EDX). The EDX spectrum shows that the grown product contains Zn and O only. The X‐ray diffraction pattern indicates that the microstructure of the obtained products is typical hexagonal wurtzite ZnO. The optical properties were studied using room temperature PL spectroscopy which indicates that the products are of high optical quality and the near band edge UV transition peak intensity increases with decrease in tetrapod size. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and luminescence of CsBr:Cu crystals

Special features of the incorporation of a copper impurity into CsBr crystals are studied for different types of impurities (metallic copper, CuO, and CuBr₂) and crystal-growth techniques (the Bridgman method or the method of isothermal evaporation from solution). The optical characteristics of these crystals (absorption, photoluminescence, and photostimulated-luminescence spectra) are investigated. The copper impurity is shown to enter CsBr:Cu_met crystals in the monovalent state Cu⁺ and CsBr:CuO and CsBr:CuBr₂ crystals in the divalent state Cu²⁺. It is found that the CsBr crystals doped with Cu⁺ and Cu²⁺ ions exhibit intense photostimulated luminescence and can be used as storage phosphors for visualization of X-ray images.     

Growth and optical absorption studies on potassium dihydrogen phosphate single crystals

Growth of bulk nonlinear optical (NLO) single crystals gained new significance with the advent of solid‐state laser sources for opto‐electronic applications. An optically transparent crystal of potassium dihydrogen phosphate (KDP) has been grown from aqueous solution along (001) plane with the aid of modified growth assembly of Sankaranarayanan‐Ramasamy (SR) Method. The evaporation rate was controlled and single crystals of 5 mm diameter and 60 mm length with a growth rate 5 mm per day have been grown successfully. The improved transparency of grown crystal was investigated using DRS UV transmittance spectral analysis and the presence of functional groups in the grown crystal is confirmed using FTIR analysis. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Intermediate products in solid‐state reactions of gadolinium oxide and ammonium dihydrogen phosphate

The solid‐state reactions of Gd₂O₃ with NH₄H₂PO₄ using various molar ratios (3:6, 2:8, 1:6 and 1:8) of the reactants were investigated at different temperatures (350‐1100°C) to observe the intermediate compounds. Analysis of the X‐ray powder diffraction patterns of the products obtained at 350°C; for the compositions of 2:8, 1:6 and 1:8 molar ratios revealed the formation of a new compound, NH₄GdHP₃O₁₀ which was reported previously for Nd, Ho and Er. At higher temperatures, gadolinium tripolyphosphate was obtained for all of the molar ratios. On the other hand, the IR data of the products also confirmed the proposed reaction pathways. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallographic and luminescence studies of ammonium and water adducts of anthraquinone fluorophores

Fluorescence and X-ray crystallographic results for ammonium adducts of an anthraquinone-containing polyether macrocycle, 1,8-oxybis(ethyleneoxyethyleneoxy)-anthracene-9,10-dione (1), and an open-chain fluorinated analogue are presented. The crystal structure of a pseudo-polymorph of a hydrate of compound 1 is also presented. [1 ₂·NH₄]PF₆·MeOH (2), triclinic, P-1, a=10.5948(13), b=14.903(2), c=15.918(2), α=71.260(3), β=82.063(2), γ=69.258(2), Z=2, 5250 reflections [I≥2σ(I)], R₁=0.0487, wR₂=0.1190, 173(2) K; 1 ₄ ·H₂O, Triclinic, P-1, a=12.0084(8) b=13.8050(9) c=23.8027(16), α=106.068(1), β=98.281(1), γ=90.047(1), Z=8, 8402 reflections [I≥2σ(I)], R₁=0.0488, wR₂=0.1086, 100(2) K. Different anti and gauche ring conformations are observed for macrocycles with and without guests complexed within the polyether ring.     

Preparation and some properties of thallium orthothioarsenate single crystals

Growing of large (Ø 25–30 mm, L = 50–60 mm) optically homogenous single crystals of Tl₃AsS₄ using the Bridgman-Stockbarger method is described. Tl₃AsS₄ is orthorhombic (Pnma), a = 8.85 ± 0.03, b = 10.86 ± 0.03, c = 9.18 ± 0.03 Å; z = 4; ϱ_x = 6.15 g · cm⁻³; ϱ_p = 6.15 ± 0,03 g · cm⁻³, T_m = 424 ± 3°C, Moh's hardness = 3, microhardness and ultrasonics velocity along x, y, z are 65–85 kg · mm⁻² and 2.16 – 2.37 · 10⁵ cm · sec⁻¹, respectively. The crystals possess perfect cleavage plane (010). Their transparency range is 0.6–12 microns. – Unsuccessful attempts to obtain Tl₃AsS₄ and its alloys in the vitreous state were taken. The possibilities of glass formation and boundaries of the vitreous region in the system Tl–As–S based on the characteristic features of the melt forming structural units are analyzed.     

Growth and scintillation properties of Pr doped Gd3(Ga,Al)5O12 single crystals

Pr:Gd₃(Ga,Al)₅O₁₂ single crystals were grown by the micro-pulling down (μ-PD) method. All grown crystals were greenish and transparent with 3.0 mm in diameter, 15–30 mm in length. Neither visible inclusions nor cracks were observed. Luminescence and scintillation properties were measured. The substitution at the Al³⁺ sites by Ga³⁺ in garnet structure has been studied. In these crystals, Pr³⁺ 5d–4f emission is observed with 340 nm wavelength. Pr1%:Gd₃Ga₃Al₂O₁₂ shows highest emission intensity. The light yield of Pr:Gd₃Ga₃Al₂O₁₂ sample with 3 mmφ×1 mm size was around 4500 photon/MeV. Scintillation decay time was 7.9 ns (0.5%), 46 ns (0.7%) and 214 ns (98.8%).     

Growth and characterization of undoped and thallium doped cesium iodide single crystals

Single crystals of pure and thallium (Tl) doped cesium iodide (CsI) have been grown by melt growth (Bridgman) technique. The grown crystals were subjected to powder X-ray diffraction and high-resolution XRD analysis. The cut and polished crystals were characterized for luminescence studies. UV-visible transmission studies have been carried out on the grown crystal in the wavelength range 200–650 nm. From the transmission spectrum it was found that the cut off wavelength increases with increase in Tl concentration and the transmittance is about 70%. The 0.06 mol% of Tl doped CsI crystal shows a good energy resolution of 7.6%. The hardness decreases for increasing the doping concentration. Etching studies have been carried out on doped and undoped crystals using methanol and water as etchant.     

On the preparation and electrical properties of thallium selenide monocrystals

Thallium Selenide single crystals were prepared by a special design using Bridgmantechnique constructed by the authors. An investigation was made on the influence of temperature on the electrical conductivity and Hall effect in two crystallographic directions. The anisotropic properties were checked, and the anisotropic factor was observed to increase with temperature decrease. The energy gap as well as the ionization energy was calculated. The conductivity throughout the entire temperature range was found to be of p-type. The Hall mobilities derived from these measurements at room temperature were of the order μH_⟂ = 42.66 cm²/vs and μH_∥ = 112.2 cm²/vs.     

Growth and scintillation properties of the Na2W2O7 crystal

The growth and scintillation properties of the Na₂W₂O₇ crystal are reported. The solid reaction between Na₂CO₃ and WO₃ is used to synthesise the Na₂W₂O₇ material. The Na₂W₂O₇ single crystal has been grown by the Bridgman method. And the Na₂W₂O₇ single crystal with sizes 14×7×6 mm³ has been achieved. The transmission spectra, the Ultraviolet fluorescence spectra and the X-ray excited luminescence spectra of the Na₂W₂O₇ crystal are measured. The measurement results show that the Na₂W₂O₇ crystal is a promising intrinsic scintillator.     

铌酸钾锂晶体的生长和缺陷

用电阻加热提拉法生长了一系列较大尺寸,组分离子均匀性较好的铌酸钾锂晶体.利用X射线荧光光谱法测量了不同配比的熔体中生长出的晶体组成,用同步辐射X射线测量了晶体结构,结果表明随晶体组成变化,晶体的晶格常数发生了变化.根据晶体组分离子浓度与折射率的关系研究了晶体折射率变化情况,结果表明用本方法生长的大尺寸KLN晶体,寻常折射率no在测量误差范围内没有变化,非寻常折射率ne的变化率在820nm仅为1.22×10-4/mm,在410nm仅为1.93×10-4/mm.晶体的干涉条纹证明了晶体有良好的光学均匀性.结合晶体生长实验,探讨了改进晶体组分离子浓度分布均匀性的方法,结果表明采用籽晶和坩锅向相同方向旋转可以改善晶体生长界面处组分离子浓度的波动,提高晶体组分离子均匀性.晶体的缺陷研究表明晶体结构完整性较好,位错形状与晶体结构相一致,密度为7.5×104,[001]轴是晶体的极化轴.晶体对890～960nm波长范围的cw-Ti:sapphire激光倍频结果表明晶体有良好的倍频性能.     

Growth Mechanism and Crystal Form of Potassium Dichromate

The structure of potassium dichromate (P-1, Z = 4) consists of two layers parallel to (001), between which no crystallographic symmetry relation exists. These layers are nearly coincident with each other when rotated through 90° about c*. One question remained unanswered: do the crystals grow parallel to {001} with d(002) or d(001) layers? The pseudo-fourfold axis does not run parallel to a crystallographic direction and acts only between two layers. This means that crystal growth parallel to {001} occurs in d(001) layers, which corresponds to the occurrence of one-sided intergrowths on (00-1). The layers are also nearly coincident with each other through pseudo-twofold axes parallel to [110] and [-110]. These axes do not act in the (100) or (010) projections. In the projections along the [110] and [-110] directions, the lattice directions are then extended by a factor of approximately 1.414, and the formula units in the cell of the d(002) layer are doubled. This indicates a further possible growth mechanism. The theoretical growth forms of the crystals were calculated with the Fourier transform method of morphology.     

Gd-incorporation and luminescence properties in sol-gel silica glasses

A thorough study was performed on Gd-doped sol-gel silica glasses, in the concentration range 0-8 mol% Gd. The analyses were carried out as a function of Gd content, before and after a post-densification thermal treatment. Different results concerning optical, vibrational, magnetic, and structural features were gathered in correlated experiments. The presence of Gd-rich nanoclusters was revealed. The size of nanoclusters increases by increasing the dopant concentration and by performing a rapid thermal treatment (RTT) at 1800 °C in air, which causes also a remarkable intensity increase of the ⁶P_7/2 → ⁸S_7/2 radioluminescence transition of Gd³⁺. Nanoclusters are amorphous, possibly close to a Gd₂SiO₅ stoichiometry as suggested by fast Fourier transform infrared spectroscopy (FTIR). FTIR studies revealed also the presence of Gd-dimers interacting with OH⁻ groups. Moreover, the presence of isolated Gd³⁺ ions was detected by electron paramagnetic resonance investigations. Based on the results obtained with different techniques, the Gd-incorporation in silica glass host and the resulting optical properties are discussed.     

Growth and Characterisation of Potassium Pentaborate Single Crystals

Single crystals of potassium pentaborate were grown by the solution growth method. The grown crystals were characterised by optical transmission spectrum, differential thermal analysis, and thermogravimetric analysis. The coefficient of thermal expansion was also determined and the results discussed.     

Extended study on the synthesis of amorphous titanium phosphates with tailored sorption properties

The influence of concentrations of both TiO₂ and H₂SO₄ in the syntheses of amorphous titanium phosphates (TiP) is reported. IR, XRD, TGA, BET and NMR techniques were used to characterise the isolated TiP products. The concentration of sulphuric acid in the initial synthesis plays a major role in the structural diversity and sorption properties of the final ionites. In the primary solutions, Ti(IV) is in monomeric, polymeric and colloidal forms. Upon addition of H₃PO₄ the presence of monomeric titanium ensures formation of the Ti(HPO₄)₂ phase. The polymeric Ti(IV) is responsible for formation of the titanium hydroxo-phosphate phase, Ti(OH)₂(HPO₄), whilst the colloidal form of Ti(IV) appears to have a role in coagulation of a minor Ti(OH)₄ phase in an amorphous TiP. It is found that TiP ion-exchange capacities gradually increase with an increase of both TiO₂ and H₂SO₄ concentrations and reach a maximum value of 3.8 mg-eq g^? 1 when TiO₂ is 70–100 g L^? 1 and H₂SO₄ is 480–560 g L^? 1. Analyses of compositional, structural and sorption data allowed 3D correlation diagrams to be built that can facilitate fabrication of TiP with tailored sorption properties.     

Growth and characterization of tetramethyl ammonium tetrachloro zincate II: A ferroic crystal

Ferroic crystals of tetramethyl ammonium tetrachlorozincate (TMA-ZnCl) were grown by slow evaporation technique and the morphology of the grown crystals varies with different pH values. The compound crystallizes in orthorhombic primitive system at room temperature with non-centro symmetric space group Pmna. The grown crystals were subjected to powder X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, ultraviolet–visible–near-infrared (UV–vis–NIR) spectral studies and thermal studies. Differential scanning calorimetry (DSC) measurement confirms the existence of structural phase transition and the thermogravimetric analysis (TGA) studies reveals that the crystal is thermally stable up to 330 °C. Vicker's microhardness studies expose that the material is mechanically stable up to a load of 60 g. The laser second harmonic generation (SHG) efficiency of the grown crystal was found to be 1.3 times that of potassium dihydrogen orthophosphate (KDP) crystal.