Synthesis,crystal structure and dielectric properties of C6H18N2SbCl5

The result of the X‐ray diffraction, differential scanning calorimetry and dielectric studies on a new crystal material C₆H₁₈N₂SbCl₅ is presented. The new organic–inorganic compound has been synthesized and characterized by the X‐ray diffraction method at 296(2) K. It crystallizes in the monoclinic P21/n space group. The cell dimensions are: a = 5.8617(1) Å, b = 15.7069(2) Å, c = 16.6693(2) Å, β = 97.627(1)° and Z = 4. The crystal structure consists of a discrete ionic layer of (C₆H₁₈N₂)²⁺ cations and [SbCl₅]^2? anions linked via simple and bifurcated N―H · · · Cl hydrogen bonds. DSC analysis shows that this compound undergoes a phase transition at about (384 ± 2) K. AC and DC conductivities, complex dielectric permittivity ε*(ω) and complex electrical modulus M*(ω) were respectively studied as temperature and frequency functions. The combined data support each other and confirm the existence of a structural phase transition at about 384 K. Moreover, the temperature dependence of the DC conductivity and relaxation frequency followed the Arrhenius relation. The frequency dependence of the real part of the AC conductivity in both phases follows the Jonscher's universal dynamic law: . The behavior of s(T) with temperature suggests that the hopping over barrier model (CBH) and the small polaron tunneling mechanism (SPTM) prevail in phases I and II, respectively. Copyright © 2016 John Wiley & Sons, Ltd.     

Band structure of the quasi two-dimensional purple molybdenum bronze

The molybdenum purple bronze KMo₆O₁₇ is quasi two-dimensional (2D) metallic oxide that shows a Peierls transition towards a metallic charge density wave state. Since this specific transition is directly related to the electron properties of the normal state, we have investigated the electronic structure of this bronze at room temperature. The shape of the Mo_K1s absorption edge reveals the presence of distorted MoO₆ octahedra in the crystallographic structure. Photoemission experiments evidence a large conduction band, with a bandwidth of 800 meV and confirm the metallic character of this bronze. A wide depleted zone separates the conduction band from the valence band that exhibits a fourfold structure, directly connected to the octahedral symmetry of the Mo sites. The band structure is determined by ARUPS in two main directions of the (0 0 1) Brillouin zone. It exhibits some unpredicted features but corroborates the earlier theoretical band structure and Fermi surface. It confirms the hidden one-dimensionality of KMo₆O₁₇ that has been proposed to explain the origin of the Peierls transition in this 2D compound.     

Theoretical study of relative width of photonic band gap for the 3-D dielectric structure

Calculations for the relative width (Δω/ω₀) as a function of refractive index and relative radius of the photonic band gap for the fcc closed packed 3-D dielectric microstructure are reported and comparison of experimental observations and theoretical predictions are given. This work is useful for the understanding of photonic crystals and occurrence of the photonic band gap.     

Crystal chemistry of phosphates with the eulytine structure

A crystal chemical study has allowed us to identify new phosphates with the eulytine structure and the formulae A_3-x Cd _x Bi(PO ₄)₃ and A_3-2x Na _x Bi_1+x (PO₄)₃ (A = Cd, Ca, Sr, Pb, Ba). Second harmonic generation tests carried out on powder samples have confirmed the non-centro-symmetrical character of their space group I43d. Bismuth cations were found necessary for the stability of the eulytine Cd₃Bi(PO₄)₃. The study has also confirmed that the eulytine structure is easily stabilized with large cations.     

Dielectric and ferroelectric properties of Sr_4CaSmTi_3Nb_7O_(30) with tetragonal tungsten bronze structure

Sr4CaSmTi3Nb7O30ceramics are synthesized and indexed as tetragonal tungsten bronze structure. The dielectric behavior and ferroelectric nature are investigated. Three dielectric anomalies are observed. The phase transition is a displacive phase transition with some diffusive characteristics, which indicates possible compositional variations within the materials on the microscopic scale. The weak distortion disappears in cooling process for differential scanning calorimetry measurement, and the large depression of Curie–Weiss temperature T0 indicates the difficulty in forming macroferroelectric domain. The ferroelectric nature in these filled tungsten bronze niobates originates from the off-center displacement of Bsite cations, but they are primarily dominated by A-site cation occupation. Both the radius and the valence of A1-site cations play an important role on ferroelectric properties of the filled tungsten bronze compounds. Existence of spontaneous polarization with a remanent polarization of 0.16 μC/cm2 a coercive field of Ec = 11.74 kV/cm confirms the room-temperature ferroelectric nature of Sr4CaSmTi3Nb7O30 ceramics.     

Preparation and dielectric properties of the KBiScNbO6 double perovskite

Ceramic KBiScNbO₆ compound was synthesized for the first time. X‐ray diffraction analysis revealed that at room temperature the samples consist of a mixture of the perovskite and pyrochlore phases. The dominant phase is the perovskite one. This phase can be described as distorted pseudocubic Pm3m structure with unit‐cell parameter a_c = 4.069 Å. Rhombohedral distortion leading the polar R3m phase is assumed to be one of possible structural distortions. Dielectric measurements of the compound under study demonstrated anomalies associated with relaxor ferroelectric behavior (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

In-situ formation of barium ferrite in iron-doped “tetragonal tungsten bronze”: Elaboration of room temperature multiferroic composites

Recent studies of ceramics of formula Ba₂LnFeNb₄O₁₅ (Ln=rare earth) with the “tetragonal tungsten bronze” (TTB) structure have correlated their room temperature multiferroics properties to the occurrence of barium ferrite parasitic phases. This work presents the elaboration of Ba₂LaFeNb₄O₁₅ and Ba₂EuFeNb₄O₁₅ composite samples with an excess of hematite in the TTB nominal composition. The influence of crystal-chemistry on the phase content and properties of Ba₂LnFeNb₄O₁₅ TTB composites is discussed. A particular focus on the mechanisms related to the in-situ formation of barium ferrite is given. We show that we can control the spurious ferrite phase in TTB multiferroic composites and thus modulate their magnetic response.     

Zr掺杂形式对钨电子发射材料组织性能的影响

采用中频感应加热烧结方法制备了W-1.5%La₂O₃-0.1%Y₂O₃-0.1%ZrO₂和W-1.5%La₂O₃-0.1%Y₂O₃-0.08%ZrH₂电子发射材料,烧结样品的致密度约为95.5%。热电子发射测试结果表明,添加氢化锆的热电子发射材料样品的零场发射电流密度大于添加氧化锆的样品,分析认为是添加的氢化锆在烧结时,发生分解,生成活性的Zr可以捕获钨晶界中的杂质氧,净化晶界,从而提高了电子发射;维氏显微硬度表明添加氢化锆样品的硬度高于添加氧化锆的样品,分析表明是氢化锆的添加有效改善了钨晶粒之间的结合性,提升了钨电子发射材料的硬度。利用SEM,EDS,XRD、金相显微镜等表面分析设备对样品进行了表征,样品结构显示添加氢化锆与添加氧化锆相比,不仅钨晶粒尺寸由13.63 μm降至11.63 μm,而且稀土相尺寸由1.87 μm降至1.66 μm,这种组织结构的变化有利于电子发射。     

核壳结构对弛豫铁电体介电行为的影响

介电弥散和介电隔离率的温度非线性关系是弛豫铁电体的主要特征. 通过对掺杂成分以线性梯度递减的核壳结构进行热力学函数分析, 认为核壳结构能够在低温区保持较高的介电常数, 但不能导致介电隔离率与温度的非线性关系. 通过对不同浓度掺杂的铁电体扩散相变的比较, 认为掺杂浓度会影响晶粒掺杂成分的不均匀性, 在较宽的分布条件下会导致介电隔离率与温度的非线性关系. 因而在介电常数的峰值温度区域, 顺电相与铁电相的晶粒共存. 温度变化会影响两相比例及铁电畴的变化, 从而导致弛豫铁电体的介电弥散性. 核壳结构会增大介电弥散性. 铁电陶瓷的掺杂物种类、掺杂物浓度和烧结温度均会影响核壳结构的成分不均匀性和介电弥散性.     

Synthesis and electrical characterization of tungsten oxide nanowires

Tungsten oxide nanowires of diameters ranging from 7 to 200~nm are prepared on a tungsten rod substrate by using the chemical vapour deposition (CVD) method with vapour--solid (VS) mechanism. Tin powders are used to control oxygen concentration in the furnace, thereby assisting the growth of the tungsten oxide nanowires. The grown tungsten oxide nanowires are determined to be of crystalline W₁₈O₄₉. I--V curves are measured by an \textit{in situ} transmission electron microscope (TEM) to investigate the electrical properties of the nanowires. All of the I--V curves observed are symmetric, which reveals that the tungsten oxide nanowires are semiconducting. Quantitative analyses of the experimental I--V curves by using a metal--semiconductor--metal (MSM) model give some intrinsic parameters of the tungsten oxide nanowires, such as the carrier concentration, the carrier mobility and the conductivity.     

介质阻挡放电中的局域态六边形结构

在氩气介质阻挡放电中得到了稳定的局域态六边形结构，并对其进行了时空动力学的测量.发现位于中心的放电丝的放电时刻总是领先，相邻两次放电的时间间隔表现出长短交替的周期性.利用壁电荷放电模型对上述结果进行了分析，表明微放电丝在放电过程中不仅受自身场的作用，还受到周围其他微放电丝的影响. 关键词： 介质阻挡放电 壁电荷 自组织 局域态结构     

介质阻挡放电中放电丝结构相变过程研究

在氩气和空气混合气体介质阻挡放电中,研究了放电丝结构随外加电压及气体压强的变化,并从二维体系相变的角度进行了分析.随着电压的增加,放电丝结构的演变过程为:稀疏的随机放电丝—稠密的随机放电丝—六边形结构—超六边形结构—混沌态,此过程相应于二维体系的气相—液相—简单晶体—超点阵晶体—液相的相变过程.实验还研究了相变过程中超六边形形成中晶格常数及相邻格点间距离的变化、超六边形结构中大点的形成过程以及超六边形结构的Penta-Hepta缺陷.     

Studies in molecular structure,symmetry and conformation—Part XIV. Crystal and molecular structure of L-isoleucine hydrochloride monohydrate form II

The crystal structure of a new form of L-isoleucine hydrochloride monohydrate C₆H₁₃O₂NHClH₂O (termed form II) has been determined using three-dimensional photographic data. This differs conformationally from the hydrochloride derivative (termed form I, Trommel and Bijvoet 1954) reported earlier. The crystal belongs to the orthorhombic space group P2₁2₁2₁ with cell dimensions,a=5.87±0.01,b=24.77±0.02 andc=6.85±0.01 ? and four molecules per cell,ρ _obs=1.240 g/cm³,ρ _cal=1.238 g/cm³,μ for CuKa=32.6 cm⁻¹. Contribution No. 420 from the Department of Crystallography and Biophysics, University of Madras, Madras 600025.     

不同温度下复杂介质结构内带电规律仿真分析

卫星上某些介质结构会遭遇较大范围的温度变化, 其电导率会随之出现数量级的变化, 这将显著影响内带电结果. 受限于电导率-温度模型和内带电三维仿真工具, 该温度效应远没有得到深入研究. 为此, 在真空变温(253-353 K)和强电场(MV/m量级)条件下测试了某种星用改性聚酰亚胺介质的电导率, 借鉴Arrhenius电导率-温度模型并考虑强电场下电导率的增强效应, 发现电导活化能取值为0.40 eV时, 可得到良好的拟合结果. 在此基础上, 同时考虑辐射诱导电导率, 采用地球同步轨道恶劣电子辐射能谱, 对该类介质盘环结构进行内带电三维仿真, 发现其内带电程度随温度降低而显著增加, 带电最严重的区域位于靠近辐射源的接地面边线. 温度低于250 K时, 2 mm屏蔽铝板下该区域的场强可达到10⁷ V/m量级, 发生介质击穿放电的可能性较大. 所讨论的电导率-温度模型与内带电三维建模方法对进一步评估卫星介质结构内带电程度和做好防护设计具有重要参考意义.     

Correlation of magnetic anisotropy with dielectric anisotropy in fluorinated phenyl bicyclohexane liquid crystal

Temperature dependence of magnetic anisotropy of homologous nematic fluorinated phenyl bicyclohexane liquid crystals is measured by a magneto-electric method.The result shows that the diamagnetic property is slightly influenced by the positions and the numbers of fluorine atoms substituted at the phenyl ring.By investigating the correlation of the dielectric anisotropy with the magnetic anisotropy,a novel explanation is proposed for the behaviour of the molecular dipole-dipole dimerization in the polar liquid crystal compounds.     

Factors affecting the growth of micro/nano-sized tungsten whiskers synthesised by vapour deposition

In this paper, a large number of the micro/nano-sized tungsten single-crystalline whiskers were fabricated via a vapour deposition method. The morphology and structure of the whiskers were investigated using scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The factors affecting the growth of tungsten whiskers were systematically studied, including temperature, holding time and the position of Si substrates. Results indicated that temperature, holding time and position of the Si substrates have significant effects on the growth of tungsten whiskers.     

冷动力喷涂法制备钨和钨合金涂层 及其涂层的计算模拟

采用冷动力喷涂法以纯钨和钨-镍-铁合金为原料在铜合金基体上制备了钨涂层和钨-镍-铁涂层. 研究了冷喷涂过程中钨粉粒径、喷涂距离等因素对涂层性能的影响. 用扫描电子显微镜分析了涂层的表面、断面微观结构, 并用原子力显微镜测量了涂层的粗糙度. 此外, 计算了冷喷涂过程中粉末颗粒的实际速度, 并采用有限元分析软件ANSYS/LS-DYNA模拟了冷喷涂过程中颗粒撞击基体时的变形情况.     

介质壁加速腔加速结构优化

为了在介质壁加速器中增大轴向加速电场, 提高加速梯度的同时抑制径向电场对束包络的扩张, 提出了在每个加速电极上添加金属栅网结构。采用基于粒子云网格方法的电磁粒子模拟软件对不加栅网与添加栅网的电极结构进行了数值仿真, 分析了不同结构下加速管道中的电场分布和束包络变化。通过实验对比了两种不同结构下经过相同的加速长度获得的粒子能量。结果表明：添加金属栅网结构相对于不加栅网的金属小孔式结构, 轴向加速电场强度提高20%, 同时径向电场得到有效抑制;栅网结构下, 被加速的粒子束在自由漂移空间中的径向发散基本得到抑制;在相同的加速长度下加速H3+粒子, 栅网结构得到的能量增益提高了一倍。     

掺铝3C-SiC电子结构的第一性原理计算及其微波介电性能

采用基于密度泛函理论的第一性原理平面波超软赝势法,对比研究了未掺杂和Al掺杂3C-SiC材料的电子结构和介电常数.结果表明:Al掺杂后,Fermi能级进入价带,带隙宽度略为加宽,在8.2—12.4 GHz范围内介电常数大幅度增大.利用燃烧合成法制备了Al掺杂的3C-SiC粉体吸收剂,通过矢量网络分析仪测试了样品在8.2—12.4 GHz范围内的微波介电常数,验证了理论计算结果,并讨论了微波损耗机理.     

Crystal structure of acylphosphatase from hyperthermophilic archaeon Pyrococcus horikoshii OT3

Analysis of the hyperthermophilic archaeon Pyrococcus horikoshii OT3 genome database led to the discovery and cloning of acylphosphatase (ORF PH0305a). To elucidate the first structure of archaeal acylphosphatase, we determined the crystal structure of P. horikoshii acylphosphatase at 1.72 Å resolution. The space group of the crystals was P3₂21, with unit-cell parameters a = b = 86.6 Å and c = 75.4 Å. The overall fold of P. horikoshii acylphosphatase was very similar to the structures of the eukaryotic enzymes. The conformation of putative active site was highly conserved.