温梯法白宝石晶体的缺陷研究

采用导向温梯法(TGT)生长出[0001]方向直径为76mm的白宝石晶体.利用扫描电子显微镜(SEM)观察晶体(0001)面的腐蚀坑形态,并对晶体内部的包裹物进行了能谱(EDS)分析.白宝石晶体中的生长缺陷主要为位错和包裹体等.Al2O3晶体(0001)面的位错腐蚀坑呈六角形,并且有台阶状结构.分析了(0001)面内的位错类型.确定了TGT法生长的白宝石内部的包裹物的主要成分为碳.     

挥发物对BBO晶体的腐蚀研究

采用顶部籽晶法,以NaF为助熔剂生长非线性光学晶体材料β-BaB2O4(简称BBO)晶体.在生长过程中发现挥发物掉落在晶体表面并严重腐蚀晶体.通过X射线粉末衍射分析,发现挥发物的主要成分是NaF,它不仅腐蚀晶体表面,而且引起晶体内部包裹物的形成.X射线衍射分析和质谱分析表明包裹物的主要成分是BaB2O4,另有少量Na+存在.探讨了由挥发物引起晶体内部形成包裹物的机理.     

CZ法生长参数对TeO2晶体质量的影响

本文主要讨论CZ法生长TeO2晶体中温度梯度、拉速、转速等工艺参数对晶体质量的影响,分析了晶体开裂、包裹物等宏观缺陷以及位错等微观缺陷的形成机理.从晶体形态、包裹体和位错密度变化等方面探讨了晶体生长参数与晶体缺陷之间的内在关系.     

γ-LiAlO2晶体的生长缺陷研究

γ-LiAlO2晶体是一种非常有前途的GaN衬底材料,本文利用化学腐蚀光学显微术和同步辐射X射线形貌术研究了LiAlO2晶体的缺陷.结果表明,提拉法生长的γ-LiAlO2晶体中的缺陷主要为位错、包裹物和亚晶界.并发现在其(100)晶片上的腐蚀形貌两面有较大差异.     

Bridgman法生长TeO2晶体的缺陷分析

采用Bridgman法生长了二氧化碲(TeO2)晶体,运用光学显微镜、电子衍射光谱、化学腐蚀等方法分析了该方法生长TeO2晶体内部的缺陷.初步讨论了散射点、微裂纹、气泡和黑点、条纹以及腐蚀坑等微缺陷的形成机理.结果表明:晶体内部的散射点来自于原料中杂质,条纹主要是由于晶体内应力引起,晶体内的气泡和黑点和晶体生长的温度密切相关,并就如何减少这些微缺陷进行了初步探讨.     

温梯法生长CaF2晶体中包裹物的研究

本文对温度梯度法生长的氟化钙(CaF2)晶体中的包裹物进行了研究,用光学显微镜和SEM观察了包裹物的形貌,对晶体中的包裹物和透明部分作了微区EDX成分分析,对包裹物所含的杂质进行了解释,提出了减小或消除包裹物的措施.分析结果表明:包裹物的主要成分是碳和氧,碳来源于石墨坩埚和石墨发热体,而杂质氧则来源于原料中的含氧化合物和生长过程气氛中氧的进入.     

激光晶体Nd:KGW晶体的表面缺陷观察

本文采用助熔剂籽晶提拉法生长出了Nd:KGW激光晶体.利用光学显微镜对晶体表面进行观察、并拍摄到晶体裂缝、生长丘、生长条纹和包裹物等缺陷的照片.分析其原因,是由于晶体生长工艺的不稳定,尤其是晶体生长过程中的温度梯度不够合适、提拉速度过快、降温速率偏快等所致.并由于生长体系粘度较大,容易形成包裹,晶体包裹物经XRD分析认为其中主要是熔体.     

高温相偏硼酸钡(α-BaB2O4)晶体的缺陷行为分析

运用同步辐射X射线白光形貌研究了α-BaB2O4晶体内部的完整性,并分析了α-BaB2O4晶体的缺陷行为及缺陷形成原因.在(001)面发现生长扇界和亚晶界,而在(100)面和(120)面分别观察到了位错、位错簇以及针状包裹体.使用双晶衍射实验发现在(001)面有生长条纹,这些生长条纹呈环形,该条纹与熔体中温度波动而导致的生长速率波动有关.运用白光形貌拍摄到高清晰的劳埃斑,表明晶体为三方结构.     

温梯法Ce:YAG闪烁晶体的宏观缺陷观察

采用温度梯度法(TGT)成功生长了直径为76mm高光学质量的Ce:YAG高温闪烁晶体,采用偏光显微镜研究了Ce:YAG闪烁晶体中的主要宏观缺陷,观察到了生长条纹、侧心、气泡、包裹物以及应力双折射等宏观缺陷.实验结果表明,晶体中的气泡、包裹物以及应力双折射等宏观缺陷主要集中在晶体边缘部分,因此温梯法可以获得高质量的Ce:YAG闪烁晶体.     

BGO晶体的缺陷与性能-(1)缺陷及其形成

下降法生长的BGO晶体中存在几种典型的宏观缺陷.用光学显微镜和电子探针对宏观缺陷内的包裹体进行研究发现:包裹体大部分为固态包裹物;不同宏观缺陷内的包裹体,其形状、大小和成份都具有典型特征.本文就包裹体的性质及其形成进行了初步的分析和讨论.     

(C2N2H10)2Mg(HP2O7)2·2H2O synthesis and crystal structure

(C₂N₂H₁₀)₂Mg(HP₂O₇)₂·2H₂O, is a new inorganic organic hybrid structure. It has been synthetized using wet chemistry. Its crystal structure consists of cis- and trans-edge sharing [MgO₄(H₂O)₂] octahedra resulting in chains, which are linked via [HP₂O₇] units to form [Mg(HP₂O₇)₂(H₂O)₂]⁴⁻ layers. The Mg²⁺ cations and the ethylendiammonium cations are located on centers of inversion. The ethylendiammonium cations are alternately located in the interlayer space. The cohesion of the crystal is well ensured by coulombic interactions between anions and cations and by several hydrogen bonds. The diphosphate anion shows an eclipsed conformation.     

Crystal structure of Rb2[GeO2(OH)2]·2H2O

Single crystals of Rb₂[GeO₂(OH)₂] · 2H₂O are studied by X-ray diffraction. The crystals belong to the orthorhombic system, sp. gr. Pna2₁, a = 13.523(6) Å, b = 8.143(4) Å, c = 13.407(6) Å, Z = 8, R ₁ = 0.0506. In [GeO₂(OH)₂]^2? anions, the Ge-O distances (1.71–1.73(1) Å) are shorter than the Ge-OH distances (1.76–1.80(1) Å). Anions are linked to each other by pairs of hydrogen bonds to form infinite chains. The chains are linked by hydrogen bonds involving water molecules to form a 3D structure. The assignment of the bands in the IR spectrum of the compound under study is performed.     

Ultraviolet Absorption of Hg2Cl2-and Hg2Br2 Single Crystals

The optical unpolarized absorption spectra of Hg₂Cl₂ and Hg₂Br₂ single crystals were measured in the spectral range 230–400 nm. A sharp exciton peak and other absorption bands of both halides were observed near the fundamental absorption edge. The absorption peaks due to the splitting of the halogen doublet were also observed. Positions of the exciton peaks are characteristic for the Frenkel (localized) type of excitons. Possible interpretations of the other observed bands are discussed.     

Elastic properties of the dithionates Na2S2O6 · 2 H2O,K2S2O6, Rb2S2O6, CaS2O6 · 4H2O and SrS2O6 · 4 H2O

Single crystals of the title compounds having optical quality and dimensions of several cm were grown from aqueous solutions. The elastic and thermoelastic constants were determined from ultrasonic resonance frequencies of thick plates. The true point symmetry of K₂S₂O₆ and Rb₂S₂O₆, which is screened by a hexagonal hypermorphy, could be clearly revealed to be trigonal (32) by the existence of the elastic constant c₁₄. In the case of CaS₂O₆ · 4H₂O and SrS₂O₆ · 4H₂O the constant c₁₄ of the specimens appeared too small to confirm the trigonal symmetry group required from electrooptic and non-linear optic effects unambiguously. The isotypy of K₂S₂O₂ and Rb₂S₂O₆ as well as that of CaS₂O₆ · 4H₂O and SrS₂O₆ · 4H₂O is confirmed by their elastic behaviour. The mean elastic stiffness of dithionates is closely related to that of the corresponding sulphates. In the vicinity of the second-order phase transition of K₂S₂O₆ near 235 K weak anomalies of the temperature derivatives of the longitudinal elastic stiffnesses are observed.     

Optical properties of the germanate melilites Sr2MgGe2O7, Sr2ZnGe2O7 and Ba2ZnGe2O7

Refractive indices and their dispersion in the wavelength range from 365 nm to 2325 nm and transmission ranges of the tetragonal melilite‐type germanates Sr₂MgGe₂O₇, Sr₂ZnGe₂O₇ and Ba₂ZnGe₂O₇ were determined. The uniaxial positive crystals Sr₂MgGe₂O₇ and Ba₂ZnGe₂O₇ both offer the possibility for phase matched second harmonic generation, a detailed analysis of phase matching conditions is given. The refractive indices of Sr₂ZnGe₂O₇ show an isoindex (isotropic) point at 467 nm. The investigation was performed on Czochralski grown large single crystals. The crystal structure of all three germanates were determined by means of X ‐ray diffraction. The results corroborate unmodulated melilite‐type structures at room temperature. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Identification of a new family of diphosphate compounds, AI2BII3(P2O7)2: Structures of Ag2Co3(P2O7)2, Ag2Mn3(P2O7)2, and Na2Cd3(P2O7)2

Syntheses and single-crystal X-ray structural results are reported for three new mixed diphosphates of the family A^I ₂B^II ₃(P₂O₇)₂; Ag₂Co₃(P₂O₇)₂ (I), Ag₂Mn₃(P₂O₇)₂ (II), and Na₂Cd₃(P₂O₇)₂ (III). All crystallize in the triclinic system, space group P1 bar: (I) a = 5.351(4), b = 6.375(4), c = 16.532(4) Å, = 80.83(6) = 81.45(4), = 72.87(5)°, V = 528.9(6) ų, Z = 2, D _calc = 4.649 mg/m³, R/Rw = 0.0428/0.0548 for 3949 obs. reflns; (II) a = 5.432(7), b = 6.619(6), c = 16.51(3) Å, = 80.78(8) = 82.43(9), = 72.82(7)°, V = 557.7(13) ų, Z = 2, D _calc = 4.338 mg/m³, R/Rw = 0.0679/0.1303 for 2100 obs. reflns and (III) a = 5.67(3), b = 7.08(4), c = 7.90(4) Å, = 77.0(2), = 82.5(2), = 67.8(2)°, V = 286(3) ų, Z = 2, D _calc = 4.249 mg/m³, R/Rw = 0.0307/0.0342 for 1945 obs. reflns. (I) and (II) are isostructural but (III) is of a different type. All three structures are characterized by layers of P₂O₇ groups alternating with layers of mixed metal atoms. Differences are seen in the conglomerate bonding patterns of B atoms and in the irregular geometry of Ag in (I) and (II) compared to the octahedral bonding seen for Na in (III). The differences in structure may be understood in terms of the ratios of the ionic radii of A and B atoms.     

Crystal structure of bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate, [C6H5CH2CHCH2CH2NH2CH2CH2]2HPO4·5H2O

The salt bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate is orthorhombic with the following unit cell dimensions: a = 11.235(2) Å, b = 27.924(6) Å, c = 9.321(4) Å space group Pca2₁ with Z = 4. The structure was solved by the Patterson method and refined to final R value of 0.049 for 1802 independent reflections. The flack parameter is 0.14 with an e.s.d. of 0.23. The structure consists of infinite parallel two-dimensional [110] planes built of mutually connected ions and water molecules by strong O—H,...,O and N—H,...,O hydrogen bonding. There are no contacts other than normal van der Waals interactions between the layers.     

Synthesis and characterization of (NH4)2CuBr2Cl2·2H2O crystals

Single crystals of a new compound, (NH₄)₂CuBr₂Cl₂.2H₂O, were grown from saturated aqueous solution at room temperature by slow evaporation method. The grown crystals were characterized through elemental, powder XRD, thermal and DSC analyses and FTIR and far IR spectra. The elemental analysis and the decomposition pattern formulated using the TG‐DTG studies confirm the stoichiometry of the compound. The crystallinity of the compound is confirmed from the powder XRD pattern. A preliminary single crystal X‐ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with a = 7.7466 Å, b = 7.783 Å and c = 8.1211 Å. The low temperature DSC shows thermal anomalies at –161.1, –156.5, –152.4, –145.2, –134, –18.5, and 1.4°C during the heating run and at –4.3, –54.8, –66.1, –90.6, –109.7 and –147.2 °C during the cooling run. The thermal hysterses indicate first order phase transitions in the title compound at these temperatures. The FTIR spectra were used to assign the characteristic vibrational frequencies due to NH₄⁺, CuX₄^2– ions and other chemical bonds. The effect of substitution of two bromine atoms on the phase transitions of a closely related crystal, diammonium tetrachloro cuprate dihydrate is also discussed. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Optical Properties of MnIn2S2Se2 Single Crystals

Optical transmittance and reflectance spectra of MnIn₂S₂Se₂ single crystals are measured in the wavelength range from 0.5 to 30 μm. The interference method is used to determine the refractive index of the compound for wavelengths between 0.8 and 12 μm. From an analysis of the absorption spectrum it follows that the fundamental edge is due to forbidden indirect transitions between parabolic bands for the polarization E ⊥ c with a gap energy of 1.50 eV at room temperature.     

Oxygen-conducting compounds with La2Mo2O9 structure in the ternary system La2Mo2O9-Sm2W2O9-Sm2Mo2O 9 + : Synthesis and properties

Polycrystalline samples in the ternary system La₂Mo₂O₉-Sm₂W₂O₉-Sm₂Mo₂O ₉ ⁺ were synthesized in air. The region of the existence of compounds with the lanthanum molybdate (La₂Mo₂O₉) structure in this system was determined. The polymorphism of the synthesized compounds was studied. Doping with samarium or with samarium and tungsten was shown to lead to the suppression of the transition between the monoclinic and cubic phases α → β and the appearance of the transition β _ms → β between two cubic phases. In samples with a high samarium content, the phase transition β _ms → β manifests itself as significant anomalies in the temperature dependences of the dielectric permeability and electric conductivity. An increase in the concentration of samarium in the samples leads to a substantial decrease in the conductivity compared with the nondoped compound La₂Mo₂O₉.