合成金刚石晶体缺陷的同步辐射形貌研究

采用同步辐射白光貌相术研究合成金刚石单晶体中的晶体缺陷,观察到晶体中存在籽晶,籽晶周围存在着大量的位错线.位错线起源于籽晶表面,终止于晶体表面.计算了位错束的空间走向和位错密度.分析了晶体的生长阶段和影响晶体缺陷的主要因素,指出通过减少籽晶表面的缺陷,保持生长条件的稳定,能够有效地降低合成金刚石晶体中缺陷的密度,提高合成金刚石晶体的完整性.     

Yb3+:KGW激光晶体生长与表征

通过对K2WO4和K2W2O7两种助溶剂的对比、分析,选择K2W2O7做助溶剂,采用顶部籽晶(TSSG)法生长YbKGW晶体.设计了合理的工艺条件转速10～15r/min;降温速率0.05℃/h;生长周期15d.通过对YbKGW晶体粉末样品的X-ray衍射谱与KGW粉末样品的X-ray衍射谱对比分析,生长晶体为β-YbKGW晶体.利用TG-DTA测定YbKGW晶体的熔点及相变温度分别是1086℃和1021℃.通过对晶体缺陷的观察分析认为,晶体裂缝及包裹物等缺陷与生长工艺条件密切相关,应尽量减少生长过程中的温度、浓度及生长速度的波动,保持晶体的稳态生长.     

坩埚下降法生长大尺寸Bi12GeO20晶体的宏观缺陷

Bi₁₂GeO₂₀晶体是一种多功能光电材料,在可见光范围内具有高速光折变响应,以及良好的压电、声光、磁光,旋光和电光等性能。目前,提拉法生长Bi₁₂GeO₂₀晶体,存在生长成本高、晶锭形状不规则、生长产率低、晶体光学质量差和有效晶体截面小等问题。本研究率先采用改进的坩埚下降法,在铂金坩埚和空气气氛中生长大尺寸Bi₁₂GeO₂₀晶体。通过各种分析测试方法研究生长获得的Bi₁₂GeO₂₀晶体中宏观缺陷的形态、分布和成分构成,探讨了晶体生长过程中主要宏观缺陷的形成过程和成因。坩埚下降法生长的Bi₁₂GeO₂₀晶体存在两种主要宏观缺陷：枝蔓状和管状包裹体。其中,枝蔓状包裹体与铂金溶蚀后的析晶相关,而管状包裹体与铂金析出、接种界面不稳定性和温度波动有关。本研究提出了消除坩埚下降法生长晶体中宏观缺陷的技术途径,通过降低生长控制温度、缩短高温熔体保持时间和优选籽晶等措施,可重复地生长...     

ZnGeP_2晶体近红外吸收特性的研究

采用布里奇曼法生长了磷化锗锌晶体,晶体毛坯尺寸达φ20mm×90mm,选取晶体尾部、晶体中部、籽晶端三个部位厚度为4.0mm的抛光晶片作为测试样品.从实验和理论上研究与分析了晶体的近红外吸收特性.实验结果显示:晶体透过率由尾部至近籽晶端逐渐增大,表明晶体近红外吸收由尾部至近籽晶端逐渐减小,这是由于晶体内缺陷密度发生了改变,且晶体内本征点缺陷分布比例不均衡,进而导致晶体的近红外吸收产生差异.理论上计算了磷化锗锌晶体施主缺陷GeZn+和受主缺陷V-Zn的吸收光谱.计算结果表明:受主缺陷V-Zn对磷化锗锌晶体吸收光谱产生的影响大于施主缺陷GeZn+.     

不同过饱和度下DKDP晶体生长和缺陷的研究

过饱和度是影响DKDP晶体生长和质量的关键因素. 本文采用“点籽晶”快速生长技术在不同的过饱和度下从氘化程度为75%的溶液中生长DKDP晶体并选取部分样品进行同步辐射X射线形貌术和粉末X射线衍射测试. 研究了不同过饱和度下DKDP晶体的生长和缺陷. 实验证明, DKDP晶体可以在的过饱和度下实现快速生长, 但晶体的缺陷随着过饱和度的增大而增加.     

不同籽晶DKDP晶体生长和光学性能研究

籽晶是影响DKDP晶体生长和光学性能的一个重要因素.通过传统降温法,分别利用Z片和[101]晶片作为籽晶,从氘化程度为85%的溶液中生长DKDP晶体并对加工样品进行了相关测试.研究了不同籽晶对DKDP晶体的生长和光学性能的影响.实验表明,[101]晶片籽晶所得DKDP晶体能有效缩短生长周期,晶体损伤阈值提高明显,但光学均匀性和透过性能有所下降.     

人工烟水晶X射线形貌

本文应用 X 射线衍射形貌术对人工烟水晶中的缺陷进行了研究。结果表明:由于掺杂,晶体中缺陷明显增多;缺陷线形态也发生了变化。Y 棒晶体 Z 生长区是缺陷主要浓集区域。籽晶平面法线与晶体 Y 轴夹角为66°的晶体,籽晶两侧缺陷线形态有显著差别。随着此夹角的增大或减小,缺陷线形态出现有规律的变化。这种变化反映了人工烟水晶三方偏方面体单形结晶习性的变化。籽晶平面法线与 Y 轴交角的变化使得该单形各组锥面显露机率不同。     

氟化钙晶体的生长与缺陷研究

采用真空坩埚下降法在石墨坩埚中生长了大尺寸CaF2晶体.通过高温氟化获得无水高纯原料,自发成核发育籽晶,以＜2mm/h的生长速率,成功生长了直径170mm的CaF2晶体.研究了晶体的顶部析晶形貌、包裹体、解理等生长缺陷.     

Yb:KGd(WO4)2激光晶体结构与振动光谱

用顶部籽晶提拉法,以K2W2O7为助溶剂,生长YbKGd(WO4)2激光晶体.经热重-差热分析,确定晶体熔点为1086℃,相变温度为1021℃.晶体结构分析确定YbKGW(WO4)2晶体由WO6八面体连接而成,WO6八面体是由(WOOW)双氧桥及(WOW)单氧桥构成.晶体粉末样品室温下的红外及拉曼光谱测试,确定WO42-、双氧桥及单氧桥的振动范围,并对其进行了归属.X射线粉末衍射测试,验证所生长的晶体为β-YbKGd(WO4)2.     

不同籽晶对KDP晶体质量的影响

采用Z片籽晶和锥头籽晶分别进行传统降温法生长KDP晶体,并对其高分辨摇摆曲线、锥光干涉图以及消光比进行测试研究。实验发现,KDP晶体在不同籽晶下均能实现较好的生长稳定性,采用锥头籽晶生长的KDP晶体具有相对更好的晶体质量。     

Magnetic coupling in La0.67Ca0.33MnO3/La0.67Sr0.33CoO3/La0.67Ca0.33MnO3 sandwiches

La_0.67Ca_0.33MnO₃ (LCMO)/La_0.67Sr_0.33CoO₃ (LSCO)/LCMO trilayer films are fabricated on single-crystal substrates NdGaO₃ (110) and the interlayer coupling are investigated. Compared with LCMO single layer, sandwiches showed the enhanced metal-insulator transition temperature of LCMO layers. The magnetoresistance is dependent on spacer thickness and the peak value dramatically decreases when LSCO layer is thick enough because of shorting by the LSCO layer. The magnetic coercivity H_C shows a nonmonotonic behavior with changing spacer layer thickness and the waist-like hysteresis indicates that there is an indirect exchange coupling between the top and bottom LCMO layers across the spacer layer.     

Varistor properties of ZnO-Pr6O11-CoO-Cr2O3-Y2O3-In2O3 ceramics

The varistor properties of the ZnO-Pr₆O₁₁-CoO-Cr₂O₃-Y₂O₃-In₂O₃ ceramics were investigated for different concentrations of In₂O₃. The increase of In₂O₃ concentration slightly increased the sintered density (5.60-5.63 g/cm³) and slightly decreased the average grain size (3.4-2.9 μm). The breakdown field increased from 6023 to 14822 V/cm with increasing concentration of In₂O₃. The nonlinear coefficient increased from 17.6 to 44.6 for up to 0.005 mol%, whereas the further doping caused it to decrease to 36.8. In₂O₃ acted as an acceptor due to the donor concentration, which decreases in the range of 1.02 × 10¹⁷ to 0.24 × 10¹⁷/cm³ with increasing concentration of In₂O₃.     

Nanocrystallization of SrBi2Nb2O9 from glasses in the system Li2B4O7---SrO---Bi2O3---Nb2O5

Transparent glasses in the system (100−x)Li₂B₄O₇–x(SrO---Bi₂O₃---Nb₂O₅) (10≤x≤60) (in molar ratio) were fabricated by a conventional melt-quenching technique. Amorphous and glassy characteristics of the as-quenched samples were established via X-ray powder diffraction (XRD) and differential thermal analyses (DTA) respectively. Glass–ceramics embedded with strontium bismuth niobate, SrBi₂Nb₂O₉ (SBN) nanocrystals were produced by heat-treating the as-quenched glasses at temperatures higher than 500 °C. Perovskite SBN phase formation through an intermediate fluorite phase in the glass matrix was confirmed by XRD and transmission electron microscopy (TEM). Infrared and Raman spectroscopic studies corroborate the observation of fluorite phase formation. The dielectric constant (_r) and the loss factor (D) for the lithium borate, Li₂B₄O₇ (LBO) glass comprising randomly oriented SBN nanocrystals were determined and compared with those predicted based on the various dielectric mixture rule formalism. The dielectric constant was found to increase with increasing SBN content in LBO glass matrix.     

PbSbBiS4-Sb2S3 and PbSbBiS4-Bi2S3 joins in the PbS-Sb2S3-Bi2S3 system

Phase equilibria along the PbSbBiS₄-Sb₂S₃ and PbSbBiS₄-Bi₂S₃ joins of the PbS-Sb₂S₃-Bi₂S₃ system have been studied for the first time using differential thermal analysis, X-ray diffraction, microstructural analysis, microhardness tests, and density measurements, and the phase diagrams of the joins have been mapped out. The joins are shown to be pseudobinary with limited series of terminal solid solutions. The solid solutions are p-type semiconductors.     

Syntheses of hollandite type Rb2Cr8O16, K2Cr2V6O16 and K2V8O16

Hollandite-type compounds, Rb₂Cr₈O₁₆, K₂Cr₂V₆O₁₆ and K₂V₈O₁₆, were synthesized under high P-T conditions up to 1200°C and 7GPa. The structural refinement using a single crystal of Rb₂Cr₈O₁₆ confirms that the structure is similar to that of K₂Cr₈O₁₆. Magnetic measurements indicate that Rb₂Cr₈O₁₆ is ferromagnetic below 295K, K₂Cr₂V₆O₁₆ paramagnetic down to 77K and K₂V₈O₁₆ has susceptibility anomaly at 175K. These compounds are all semiconductive and show discontinuities in temperature-resistivity curves at points corresponding to magnetic anomalies.     

Microstructures of YBa2Cu3O7/La0.7Ca0.3MnO3 and La0.7Ca0.3MnO3/YBa2Cu3O7 bi-layers grown on (001)LaAlO3

Epitaxial YBa₂Cu₃O₇/La_0.7Ca_0.3MnO₃ (YBCO/LCMO) bi-layers and La_0.7Ca_0.3MnO₃/YBa₂Cu₃O₇ (LCMO/YBCO) bi-layers were grown on (001)LaAlO₃ by pulsed laser deposition, and their microstructures were compared by transmission electron microscopy investigation. In the YBCO(100 nm)/LCMO(150 nm) bi-layers, the LCMO layer consists of columnar grains of ~ 17 nm in diameter and contains mixed orientation domains of [100]_c, [010]_c and [001]_c. The YBCO layer is totally c-axis oriented and the YBCO lattices are tilted − 2.5° to + 2.5° as they grew on the rough surfaces of LCMO columnar grains. For the LCMO(140 nm)/YBCO(140 nm) bi-layers, the LCMO/YBCO interface is sharp and flat. The initial 12-nm thickness of the YBCO layer is composed of c-axis oriented domains, and the upper part of YBCO layer is [100] oriented. The LCMO layer was predominantly [001]_c oriented while [100]_c-oriented domains were occasionally observed.     

Characterization of YBa2Cu3O7/PrBa2Cu3O7 superlattices

We investigated the structural and superconducting properties ofc-axis oriented (YBa₂Cu₃O₇) _nY /(PrBa₂Cu₃O₇) _npr superlattices with thicknesses of the individual layers down to one unit cell (10nY1; 18>nPr 1). By transmission electron microscopy and X-ray diffraction we find an excellent structural quality of the samples, though the quantitative analysis shows the existence of defects. In superlattices with decoupled YBa₂Cu₃O₇ layers of two unit cell thickness we find a highT _c value of 75 K. We probed the flux line structure in the superlattices by measurements of the critical current density in magnetic fields. The experiments show that the flux-line dynamics is dominated by the movement of pancake vortices.     

Vapour-liquid equilibria in the ternary mixtures N2---CH4---C2H6 and N2---C2H6---C3H8

A systematic study was performed with mixtures consisting of N₂, CH₄, C₂H₆ and C₃H₈, to investigate experimentally phase equilibria and caloric properties and to test the accuracy of thermodynamic correlations. The first part of this Paper reports results of T---p---x---y measurements on ternary systems in the range 20 < p < 120 bar and 140 < T < 220 K. The results are compared with data calculated by generalized equations of state.     

Structural study of Sr0.3Ba0.7Nb2O6 and La0.030Sr0.255Ba0.700Nb2O6 ceramic systems

Sr_0.3Ba_0.7Nb₂O₆ (SBN) and La_0.030Sr_0.255Ba_0.700Nb₂O₆ (LSBN) ceramic compounds have been prepared using the traditional ceramic method at two different calcination temperatures (900 and 1000 °C) and later sintered both at 1400 °C. A study of the effects of the calcination temperatures and La substitution on the morphological, compositional, and structural properties of SBN and LSBN is presented using scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis. From Rietveld refinement processes, the XRD patterns were interpreted to evaluate such effects in the structural parameters and the site occupation factors of the heavy metals and oxygen atoms. The effect of the incorporation of La resulted in a 0.25% cell contraction and turned out to be higher than the 0.08% dilation effect produced by the increase of calcination temperature. The La ion with similar effective ionic radius and higher electronegativity is incorporated into the structure occupying the A₁ site just like the Sr ions in the SBN compound. Differences in the site occupation factors between the SBN and LSBN samples lead to substantial changes in the physical properties such as temperature of relative dielectric constant maximum, relative dielectric constant, and dielectric loss, correlated with the distortion and the relative orientation of the oxygen octahedra.     

The effect of Bi1.5Zn0.5Nb0.5Ti1.5O7 cover layer on the dielectric and tunable properties of Ba0.6Sr0.4TiO3/Bi1.5Zn0.5Nb0.5Ti1.5O7 bilayered thin films

Bi_1.5Zn_0.5Nb_0.5Ti_1.5O₇ (BZNT) thin films with different thicknesses as cover layers were deposited on the Ba_0.6Sr_0.4TiO₃ (BST) thin films on the Pt/Ti/SiO₂/Si substrates by radio frequency magnetron sputtering method. The microstructure, surface morphology, dielectric and tunable properties of BST/BZNT heterogeneous bilayered films were investigated as a function of the thickness of BZNT films and the effect of BZNT films on the asymmetric electrical properties of BST/BZNT bilayered films was discussed. It was found that BZNT cover layer significantly improved the leakage current and the dielectric loss, and the dielectric constant and tunability of BST/BZNT bilayered thin films simultaneously decreased with the increasing thickness of BZNT films. The BST/BZNT bilayered thin film with a 50 nm BZNT cover layer gave the largest figure of merit (FOM) of 33.48 with the upper tunability of 55.38%. The asymmetric electrical behavior of BST/BZNT bilayered films is probably related to an internal electric field caused by built-in voltages at Pt/BST and BZNT/Au interfaces.