射频磁控溅射制备氮化锌薄膜的椭圆偏振光谱研究

在不同的衬底温度下,使用反应射频磁控溅射法,在玻璃衬底上制备了氮化锌薄膜样品.用X射线衍射仪、原子力显微镜和椭偏仪对薄膜的晶体结构、表面形貌、光学性质进行了表征分析.薄膜的晶粒尺寸会随着衬底温度的升高先增大后减小,在200?C时薄膜的结晶性最好.用椭偏仪测试样品,建立物理模型计算出氮化锌薄膜在430—850 nm范围内的折射率和消光系数等光学参数.利用Tauc公式计算出氮化锌薄膜的光学带隙在1.73—1.79 eV之间.     

θ-2θ型X射线衍射仪测定水溶液的结构

采用θ-2θ型粉末衍射仪并以NaCl溶液为研究对象,完成了该溶液不同浓度的结构测定,验证了方法在测定溶液尤其是低浓度溶液中的可行性。由衍射数据可知,随着浓度的提高,溶液的衍射曲线的特征峰由13.4°到14°发生偏移,且19°肩峰逐渐消失,表明随着浓度的增大,NaCl溶液的微观结构发生了较明显的变化。利用PDFgetX3软件对衍射数据进行了处理,得到了溶液的差值对分布函数,由差值对分布函数分析得到水分子间O-O间的峰位为0.276nm,该峰随浓度的增大,逐渐降低,当质量分数大于15%时出现了较明显的0.314nm处的Cl--O峰。     

同步辐射核共振振动能谱学(上):原理篇

核共振振动能谱学(简称核振能谱)是一种以同步辐射为实验基础的新型的振动能谱学方法。与红外、拉曼等传统的振动光谱学方法相比,核振能谱在理论上和实验上具有一系列突出的特点和优越性,从而在各学科,特别是在铁基化学和铁基生物化学的研究中有着广泛的应用。文章分为上下两篇,上篇介绍核振能谱的基本概念、基本理论、实验方法和实验条件等基础内容,并以简单的四氯化铁离子([FeCl4]-)为例,演示由原始核振能谱到振动态密度函数(PVDOS)的分析流程。在选材上,文章侧重先进性、代表性和实用性;在叙述上,考虑到非同步辐射专业研究者的阅读需要,文章突出实验科学和应用科学的内容,力求简单明了、通俗易懂。下篇将系统介绍该能谱学方法在化学与生物化学中的应用实例。     

Evolution from Diffuse Ferroelectric to Relaxor Ferroelectric in Pb1-xBax（Fe1/2Nb1/2）O3 Solid Solutions

Dielectric and ferroelectric characteristics for Pb1-xBax（Fe1/2Nh/2）O3 （x = 0,0.05,0.1,0.15, and 0.2） ceramics are determined together with their structures. X-ray diffraction （XRD） analysis confirms the solid solutions with the cubic structure. The dielectric nature changes from diffuse ferroelectric to relaxor ferroelectric with increasing x, while the phase transition temperature Tc （or Tm） decreases monotonously. The diffuse ferroelectric phase transition is observed in the solid solutions with 0≤x ≤0.05. For Pbl-xBax（Fe1/2Nb1/2）O3 with 0.1≤ x≤0.2, relaxor ferroelectric behavior is determined, and the Vogel-Fulcher equation is used to describe the relaxor behavior. The 1/ε versus T plots reveal the diffusion dielectric characteristics in both diffuse and relaxor ferroelectrics.     

Controllable synthesis,characterization,and growth mechanism of hollow Zn_x Cd_(1-x) S spheres generated by a one-step thermal evaporation method

Novel hollow ZnxCdl xS spheres that are uniform in size are synthesized through the one-step thermal evaporation of a mixture of Zn and CdS powder. From an X-ray diffraction （XRD） study, the hexagonal wurtzite phase of ZnxCdl_xS is verified, and the Zn mole fraction （x） is determined to be 0.09. According to the experimental results, we propose a mechanism for the growth of Zn0.09Cd0.91S hollow spheres. The results of the cathodoluminescence investigation indicate uniform Zn, Cd, and S distribution of alloyed Zn0.09Cd0.91S, instead of separate CdS, ZnS, or nanocrystals of a core- shell structure. To the best of our knowledge, the fabrication of ZnxCd1-xS hollow spheres of this kind by one-step thermal evaporation has never been reported. This work would present a new method of growing and applying hollow spheres on Si substrates, and the discovery of the Zn0.09Cd0.91S hollow spheres would make the investigation of ZnxCd1-xS micro/nanostructures more interesting and intriguing.     

A Novel Mixed-valence and Capped-keggin Structural Polyoxometal Complex： {[Co（dien）]4- [（PO4）MoVs（WVI0.56 noVI0.44）4033（OH）3]}.nH2O （n ≈ 1）

A novel inorganic-organic hybrid compound, {[Co（dien）]4[0aO4）MoV8（wV10.56MoV10.44）4- O33（OH）3]}＇nH20 （1, n = 1, dien = diethylenetriamine）, has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system with a = 11.927（2）, b = 13.328（3）, c = 19.306（4）A, a = 93.76（3）, β = 94.14（3）, γ = 109.99（3）°, V= 2863.2（12） A3, space group P1 and Z = 2 at 173 K. The final full-matrix least-squares refinement converged to R = 0.049 for 9621 observed reflections with 1 〉 2σ（I） and wR = 0.139 for all data （9871） and S = 1.073. Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributed e-Keggin structural polyanion capped by four Co（dien） fragments with the main group element P occupying the center site. These results were further confirmed by energy-dispersive X-ray spectroscopy （EDS）, X-ray powder diffraction （XRD）, Fourier transform infrared spectroscopy （FTIR）, Raman spectroscopy, Thermogravimetry （TG） and X-ray photoelectron spectroscopy （XPS） analyses.     

Transitional Metal Complexes with 1,2,4-Triazole Ligand： Syntheses and Crystal Structures

Four novel transitional metal complexes with 3-（4-pyridly）-4-phenyl-5-sulfhydryl- 1,2,4- triazole （HL1） and 3-（3-pyridly）-4-phenyl-5-sulfhydryl-l,2,4-triazole （HLz） were synthesized and characterized by elemental analysis, IR and X-ray diffraction. Complexes 1, 3 and 4 have two-dimensional （2-D） neutral rhombohedral grid with a （4, 4） topology. In 1, 3 and 4, all the metal ions are six-coordinated to four nitrogen atoms of four distinct ligands and two O atoms from water molecules. Complex 2 has tetranuclear CuaCI4 units which are interconnected by four desulfuri- zation ligands （L1-S） via Cu-N bonds to form a 2-D layer with （4,4） topology.     

A New Sandwiched-type Polyoxotungstate Containing {Cd4} Transition-metal Cluster： Synthesis,Structure and Luminescent Property

A new sandwiched polyoxometalate [HK11Cd4Cl2（PW9034）2]·18H2O （1）, incor- porating a unique hybrid tetranuclear cadmium cluster （abbreviated to {Cd4}） with two trivacant polyanions [B-α-PW9O34]9-, has been hydrothermally synthesized and structurally characterized by elemental analyses, IR spectroscopy, UV-vis, and single-crystal X-ray diffraction analysis. Crystal data for 1： monoclinic, space group C2/c, a = 19.2997（4）, b = 13.8014（3）, c = 31.9819（8） A, β = 102.764（2）°, V= 8308.3（3） A3, Z = 4, P2O86Cl2K11Cd4W18H37, Mr = 5735.13, Dc = 4.584 mg-mm-3, F（000） = 10084, μ = 26.579 mm-1, the final R = 0.0378 and wR = 0.0989 for 6558 observed reflections （I〉 2σ（I））. X-ray crystallographic study shows that the molecular structure of 1 contains four cadmium atoms. Two CdO6 distorted octahedra and two CdOsC1 distorted octahedra combine with each other in turn via edge-sharing, resulting in a regular rhomb-like cluster sandwiched between two {B-a-PW9034} units. Further, the sandwich-type polyoxoanions were connected by K＋ ions to form a complicated 3-D open-framework through connecting with each terminal O atom of the [Cd4C12（PW9O34）2]12- polyoxoanions. In addition, compound 1 exhibits photoluminescence property at room temperature and the band gap can be assessed at 3.25 eV.     

松花粉中16种常量和微量元素的TXRF对比分析

采用微波消解前处理,全反射X射线荧光分析法(TXRF)同时测定松花粉中16种元素,并对马尾松、云南松、油松、黑松、赤松等五种松花粉中16种元素含量进行了测定与比较。结果表明:五种松花粉中都含有这16种元素;Ca,Ti,Mn,Zn和Rb等五种元素平均含量在不同树种间均存在极显著性差异(p≤0.01);K,V,Fe,Co,Cu和Sr等六种元素平均含量在不同树种间均存在显著性差异(p≤0.05);Cr,Ni,As,Pb和Se等五种元素平均含量在不同树种间不存在显著性差异(p>0.05);研究还表明松花粉具有温性或偏寒凉性药的元素谱征。研究结果可以初步断定,松花粉中这16种元素的含量和树种有关,和生长环境、地域等密切相关。     

Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Nickle （II） Achieved from 5-Iodo-isophthalic Acid Ligand

A new coordination polymer [Ni（L）（m-bix）（H2O）]n （1, H2L = 5-iodo-isophthalic acid, m-bix=1,3-bis（imidazol-1-ylmethyl）-benzene） has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, powder XRD and single-crystal X-ray analysis. The crystal is of triclinic, space group Pī with a = 9.1638（3）, b = 10.2319（3）, c = 13.2463（4） ？, α = 80.1710（10）, β = 83.671（2）, γ = 70.3790（10）o,C22H19NiIN4O5, Mr = 605.02, V = 1150.85（6） ？3, Dc = 1.746 g/cm3, F（000） = 600, μ = 2.225 mm-1, S = 1.045 and Z = 2. The final R = 0.0388 and wR = 0.1257 for 5089 observed reflections with I 〉 2σ（I）. In the title complex, the M and P layers are arranged alternately to give a double-layer structure by the symmetry related hydrogen bonds, and these double-layers are further joined together to achieve a 2D supramolecular architecture through I···π interaction involving iodine atoms and imidazole rings. The thermal stability of the title complex was studied by thermal gravimetric （TG） and differential thermal analysis （DTA）.