Czochralski法生长Lu2SiO5:e晶体的发光特性

本文使用铱坩埚感应加热Czochralski法成功地生长出了无色透明且尺寸达φ50mm×60mm 的Lu2SiO5:e晶体.XRD结构分析表明, 该晶体为单斜结构.在室温下分别以X射线和紫外光为激发源测量了该晶体的发射光谱,获得的发射波长分别为403nm和420nm,光衰减时间为41ns,光产额达32000p/MeV.发射光谱的双峰结构以及晶体的发光特性证明其发光源于Ce3+离子的5d1→5F5/2 和 5d1→5F7/2跃迁.     

Czochralski法生长Lu2SiO5：Ce晶体的发光特性

本文使用铱坩埚感应加热Czochralski法成功地生长出了无色透明且尺寸达5 0mm× 6 0mm的Lu2 SiO5:Ce晶体。XRD结构分析表明 ,该晶体为单斜结构。在室温下分别以X射线和紫外光为激发源测量了该晶体的发射光谱 ,获得的发射波长分别为 4 0 3nm和 4 2 0nm ,光衰减时间为 4 1ns,光产额达 32 0 0 0p/MeV。发射光谱的双峰结构以及晶体的发光特性证明其发光源于Ce3 离子的 5d1→5F5/ 2 和 5d1→5F7/ 2 跃迁。     

Growth and photorefractive properties of Mg:Ce:Cu:LiNbO3 crystals grown by Czochralski method

In this paper, photorefractive properties of Mg:Ce:Cu:LiNbO₃ crystals were studied. The crystals doped with different concentration of Mg ions have been grown by the Czochralski method. Mg concentrations in grown crystals were analyzed by an inductively coupled plasma optical emission spectrometry (ICP‐OE/MS). The crystal structures were analyzed by the X‐ray powder diffraction (XRD), ultraviolet‐visible (UV‐Vis) absorption spectra and infrared (IR) transmitatance spectra. The photorefractive properties of crystals were experimentally studied by using two‐beam coupling. In this experiment we determined the writing time, maximum diffraction efficiency and the erasure time of crystals samples with He‐Ne laser. The results showed that the dynamic range (M/#), sensitivity (S) and diffraction efficiency (η) were dependent on the Mg doping concentration, and the Mg(4.58mol%):Ce:Cu:LiNbO₃ crystal was the most proper holographic recording media material among the six crystals studied in the paper. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)     

Photoluminescence study of annealing effects on CuI crystals grown by evaporation method

Cuprous iodide (CuI) is the ultrafastest inorganic scintillation crystal at present. But the low intensity of its ultrafast component luminescence limits the wide application of CuI at room temperature. In this paper, the photoluminescence (PL) characteristics of different quality CuI crystals before and after annealing in various conditions have been investigated in terms of peak position and peak intensity. The origin of different emission band peaked around 426 nm, 680 nm, 718 nm and 820 nm is discussed and the excitation spectra of two mainly emission bands is obtained. Meanwhile, the relative peak intensity of the ultrafast luminescence component to slow lumiescence component of CuI crystals has been studied with respect to the defect concentration of I vacancies. Especially, the method of improving the intensity of ultrafast compentent luminescence of CuI crystals is concluded. These results can provide an important reference for optimizing the luminescence performance of CuI crystals.     

The effect of crucible bottom deformation on the quality of Nd:GGG crystals grown by Czochralski method

In this paper, we report the growth of neodymium doped Gadolinium Gallium Garnet (Nd: GGG) crystal using Czochralski (CZ) method, and study the effects of crucible bottom deformation and thermal insulator thickness on the growth process and crystal quality. Garnet structure and <111> crystallography orientation of the crystal were confirmed by the X‐Ray diffraction (XRD) analysis. Macroscopic defects, residual stresses, quality, and homogeneity of the crystals were investigated by means of parallel plane polariscope and laser fizeau interferometer respectively and the results compared together. Experimental observations show that the crucible bottom deformation from flat to convex, and decreasing the thickness of zirconia insulator under the crucible result in the formation of lateral cores and increasing the crystal inhomogeneity and tensions, leading to the decrease of the crystal quality. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of thermal annealing conditions on the microdefect formation in undoped GaAs single crystals grown by Czochralski method

The effect of thermal annealing conditions on the microdefect formation in undoped GaAs single crystals grown by the Czochralski method has been studied by X-ray diffraction and metallographic analyses. It is found that the standard heat treatments performed with the aim to relieve elastic stresses and to increase the homogeneity of wafers substantially affect microdefects formed in the crystal. Upon annealing, the micro-defects in ingots and wafers exhibit different behavior. Prolonged annealing leads to an increase in the sizes of large microdefects but does not suppress the formation of small-sized microdefects. The latter defects are formed at T< 950°C upon cooling from the annealing temperature, and their number strongly depends on the density of dislocations, which serve as sinks for intrinsic point defects.     

Properties of AgGa1‐xInxSe2 single crystals grown by Bridgman method

High‐pure and single‐phase AgGa_1‐xIn_xSe₂ (x=0.2) polycrystalline was synthesized by the mechanical and temperature oscillation method. Adopting the modified Bridgman method an integral AgGa_1‐xIn_xSe₂ single crystal with diameter of 14 mm and length of 35 mm has been obtained at the rate of 6 mm/day. It was found that there is a new cleavage face which was (101), and observed the four order X‐ray spectrum of the {101} faces. By the method of DSC analysis the melting and freezing points of the AgGa_1‐xIn_xSe₂ (x=0.2) single crystal were about 828°C and 790°C. The transmission spectra of the AgGa_1‐xIn_xSe₂ (x=0.2) sample of 5×6×2 mm³ were obtained by means of UV and IR spectrophotometer. The limiting frequency was 774.316nm and the band gap was 1.6eV. It can be found in the infrared spectrum that the infrared transmission was above 60% from 4000cm^‐1 to 600cm^‐1. The value of α in 5.3µm and 10.6µm were 0.022cm^‐1 and 0.1cm^‐1 respectively. All results showed that the crystal was of good quality. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Defect structure and light‐induced scattering of Zr‐doped near‐stoichiometric Mn:Fe:LiNbO3 crystals grown by TSSG method

Near‐stoichiometric Mn:Fe:LiNbO₃ crystals doped with various concentration of ZrO₂ were grown by top seed solution growth (TSSG) method in the air atmosphere. The Zr concentration in the crystal was determined by inductively coupled plasma optical emission spectrometer. The defect structures were analyzed by means of ultraviolet‐visible and infrared transmittance spectra. The appearance of vibration peak at 3466 cm^‐1 in infrared spectra manifested that Li/Nb ratio in crystals approached to stoichiometric proportion. The fundamental absorption edge represented continuous red‐shift which was discrepancy with congruent doped LiNbO₃ crystals showed that doping ions possessed different location mechanism. The light‐induced scattering of the doped stoichiometric LiNbO₃crystals were quantitatively scaled via incident exposure energy. The results demonstrated that Zr(2 mol%):Mn:Fe:LiNbO₃ crystal had the weakest light‐induced scattering and the mechanism related to their defect structures was discussed. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Singular ring‐shaped distribution of Nd in NdxY1‐xVO4 crystals grown by floating zone method

A singular ring‐shaped distribution of high Nd concentration was observed in Nd‐doped YVO₄ single crystals grown by the floating zone (FZ) method. The ring‐shaped distribution appeared 500‐1000 μm inside from the rim of the crystals. Results of growth experiments by the anisotropic heating floating zone (AHFZ) method showed that the Nd concentration was high at the high‐temperature side of the grown crystals. We found a small concave projection at a part of the convex solid‐liquid interface by quenching the molten zone during growth. The cause of the singular ring‐shaped distribution of the Nd‐rich area was discussed in relation with the concave projection at the interface and the convection in the molten zone. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of crystal disorder on linewidth of the Raman modes in GaS1‐xSex layered mixed crystals

The linewidths of Raman‐active intralayer compressional modes in GaS_1‐xSe_x layered mixed crystals (0 ≤ x ≤ 1) have been measured in the 10‐300 K temperature range to study the anharmonic effect as a function of compositional variation and temperature. It was found that the anharmonicity increases with an increase in substitutional disorder. The cubic (three‐phonon) processes with energy conservation is responsible for the anharmonic contribution to the broadening of the intralayer phonon lines with temperature. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Problems in the growth of Ce3+‐doped Li6Gd(BO3)3 crystals by Czochralski method

Cerium‐doped lithium gadolinium borate (Li₆Gd(BO₃)₃:Ce) single crystal has been grown by the Czochralski method. Some problems like macro defects and concave growth face were found. The macro defects are suggested to be caused by constitutional supercooling and concave growth face is caused by interface inversion. These problems can be resolved or eliminated through controlling the growth parameters strictly. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Nd(III) and Yb(III) ions incorporated in Y4Al2O9 obtained by sol‐gel method: synthesis,structure, crystals and luminescence

The nanocrystalline powders of Y₄Al₂O₉ (YAM) pure and doped by Nd, Yb and codoped by Nd and Yb were obtained via modified sol‐gel method. These powders were characterized by X‐ray diffraction method, scanning electron microscopy and high resolution scanning electron microscopy, luminescence spectroscopy and differential thermal analysis (DTA). We obtained single phase powders of crystalline structure with average size 70 nm exhibiting interesting luminescent properties. Efficient non‐radiative energy transfer between Nd and Yb was found. DTA confirmed the phase transition at about 1400 °C. From these nanocrystalline powders, the crystals YAM:Yb, YAM:Yb,Nd were grown by micro‐pulling down technique. They were cracking during cooling owing to the phase transition. Luminescent properties of YAM:Nd,Yb crystals were identical with properties of corresponding nanopowders within experimental incertitude. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Defect structure characteristics in near‐stoichiometric In:LiNbO3 single crystals grown by K2O‐flux method

With K₂O as flux, near‐stoichiometric In:LiNbO₃ (In:SLN) crystals with different indium contents were grown by the top seed solution growth (TSSG) method. Defect structure characteristics and the replacement principle of extrinsic ions were derived from X‐ray powder diffraction, differential thermal analysis (DTA), ultraviolet‐visible (UV) absorption and infrared (IR) spectrum measurement. Further analysis indicated that the threshold concentration of In₂O₃ in near‐stoichiometric LiNbO₃ crystals were about 1.1 mol%. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Determination of the Li/Nb ratio in LiNbO3 crystals grown by Czochralski method with K2O added to the melt

Off-congruent lithium niobate single crystals were grown by the Czochralski method with K₂O added to the congruent melts in a concentration varying between 2 and 10.5 wt%. The Li/Nb ratio was determined by means of indirect methods such as the fundamental absorption edge positon, the IR vibrational spectrum, lattice parameters and the variation of the refractive indices. The data presented in this work show that the Li/Nb ratio can be controlled by the amount of K₂O added to the congruent melt. Moreover, the techniques employed for characterization are good tools for the determination of the Li/Nb ratio.     

Investigation of carrier scattering mechanisms in TlInS2 single crystals by Hall effect measurements

TlInS₂ single crystals are studied through the conductivity and Hall effect measurements in the temperature regions of 100‐400 and 170‐400 K, respectively. An anomalous behavior of Hall voltage, which changes sign below 315 K, is interpreted through the existence of deep donor impurity levels that behave as acceptor levels when are empty. The hole and electron mobility are limited by the hole‐ and electron‐phonon short range interactions scattering above and below 315 K, respectively. An energy level of 35 meV and a set of donor energy levels located at 360, 280, 220 and 170/152 meV are determined from the temperature dependencies of the carrier concentration and conductivity. A hole, electron, hole‐electron pair effective masses of 0.24 m_o, 0.14 m_o and 0.09 m_o and hole‐ and electron‐phonon coupling constants of 0.50 and 0.64, respectively, are obtained from the Hall effect measurements. The theoretical fit of the Hall coefficient reveals a hole to electron mobility ratio of 0.8. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Influence of cationic substitution on lattice constants and optical characterization in solution grown mixed crystals of potassium‐ ammonium zinc chloride

Mixed crystals of potassium‐ammonium zinc chloride in different concentrations were grown from aqueous solution employing the techniques of slow cooling and controlled evaporation. Powder x‐ray diffraction studies were carried out on the grown crystals. The comparison between lattice parameters a, b and c are experimentally determined and calculated by Vegad's law. The concentration of K⁺ ions in the crystals was measured by the atomic absorption technique. The crystal morphology changed considerably by increasing K⁺ concentration. The optical absorption coefficient (α) indicated strong influence changing concentration. The optical energy gap was found to decrease with increasing K⁺ concentration. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of γ‐irradiation on spectral properties of undoped Y2SiO5 crystals

The absorption spectra of undoped Y₂SiO₅ crystals were studied before and after γ‐irradiation. After γ‐irradiation, the additional absorption peaks at 260‐270 and 320nm were observed in as‐grown and H₂‐annealed Y₂SiO₅ crystal, but it did not occur in air‐annealed Y₂SiO₅ crystal. These absorption peaks were attributed to F color centers and O^– hole centers, respectively. Owing to more oxygen vacancies and color centers in H₂‐annealed Y₂SiO₅ crystal than that in as‐grown Y₂SiO₅ crystal after γ‐irradiation, the additional absorption peaks were more intense in the former than that in the latter. With the irradiation dose increasing from 20 to 220kGy, the intensity of additional absorption peaks increased. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Spectroscopic investigation of strain induced by compositional variation in bulk InxGa1–xAs crystal grown by MCZM method

Raman scattering (RS), photoluminescence (PL) and energy dispersive X‐ray (EDX) experiments have been carried out to investigate residual strain and hence to understand breakage issue in bulk In_x Ga_1–x As crystal grown by multi component zone melting (MCZM) method. It is found from a comparison that there is a large discrepancy among the RS, PL and EDX results due to the strain induced by compositional variation in the crystal. The strain induced changes in TO_GaAs and PL peak positions are found to be 4.04 cm^–1 and 0.097 eV, respectively, for the variation of composition from 0.06 to 0.29 from the seed‐end to the tail‐end of the crystal. By assuming a simple one‐dimensional strain distribution, the strain value corresponding to 4.04 cm^–1/ 0.097 eV can be obtained of the order of 10^–2, which is large enough for understanding the breakage issue in the crystal investigated here. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of reduction/oxidation treatment on blue photorefraction in In:Fe:Cu:LiNbO3 crystals

In:Fe:Cu:LiNbO₃ crystals with reduced/oxidized treatments were prepared by the Czochralski method. The defect structure was analyzed by the UV‐Visible absorption spectra. The blue photorefractive properties, such as the refractive index change, response time, recording sensitivity, dynamic range as well as two‐wave coupling gain coefficient, were also investigated at 488 nm wavelength using the two‐wave coupling experiment. Comparing the as‐grown and oxidized In:Fe:Cu:LiNbO₃ crystals, the reduced sample has the highest recording sensitivity and largest dynamic range. Meanwhile, the high diffraction efficiency is still maintained. Experimental results definitely show that reduction treatment is an effective method to improve the blue photorefractive performance of In:Fe:Cu:LiNbO₃ crystals. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)