三元混合配合物Cu(C10H8N2O3)·(C5H5N)·(H2O)的合成和晶体结构

The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C₁₀H₈N₂O₃)·(C₅H₅N)·(H₂O) (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm³, Z= 2, D_c= 1.547 Mg·m^-3, μ(MoKα) = 1.417 mm^-1, F(000) = 374. The final R₁ = 0.030 6, wR₂= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C₁₀H₈N₂O₃^2- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.     

配合物Ni(C14H10N2O3)(C5H5N)的合成和晶体结构

A novel nickel(Ⅱ) complex with 2,4-dihydroxybenzalidene benzoylhydrazone and pyridine ligands, Ni(C₁₄H₁₀N₂O₃)(C₅H₅N), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pbca. The cell parameters are: a=1.580 20(19) nm, b=1.362 18(16) nm, c=1.616 50(19) nm, and V=3.479 5(7) nm³, Z=8, D_c=1.497 Mg·m^-3, μ(MoKα)=1.139 mm^-1, F(000)=1 616, R=0.032 9 and wR=0.077 0 for 2 772 observed reflections (I>2σ(I)) out of 3810 unique ones. The nickel(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone schiff base ligand and one nitrogen atom of the pyridine ligand. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 244668.     

二正丁基锡邻二茂铁基苯甲酸酯配合物的合成、表征及其体外抗癌活性

用2－Fe-C6H4CO2H和(n-Bu)2SnO反应合成了（2－Fe-C6H4CO2)2Sn(n-Su)2(A)和{[2-Fe-C6H4O2)Sn(n-Bu)2]2O}(B)(Fe=（η^5-C5H5)Fe(η^5-C5H4)两种新的二正丁基锡配合物,并用元素分析,红外光谱和核磁共振（1H,13C）谱等方法对配合物的组成和结构进行了表征,由此推测出配合物可能的分子结构,测定了配合物的体外抗癌活性,结果表明配合物对HL－60,HCT,BGC－823,KB等癌细胞均有很好的抑制能力。     

二正丁基锡双(二茂铁硫代甲酸酯)配合物的红外光谱和核磁共振谱

合成了二正丁基锡新型配合物（n-Bu)2Sn(FcCOS)2[Fe=(η-C5H5)Fe(1-5-η-C5H4)-1；研究了该配合物的红外光谱和核磁共振（1H，13C，119Sn)谱，并推测出配合物可能的分子结构。     

Nucleation mechanism and morphology evolution of MoS_2 flakes grown by chemical vapor deposition

We study the nucleation mechanism and morphology evolution of MoS_2 flakes grown by chemical vapor deposition(CVD)on SiO_2/Si substrates with using S and MoO_3 powders.The MoS_2 flake is of monolayer with triangular nucleation,which might arise from the initial MoO_3-xthat is deposited on the substrate,and then bonded with S to form MoS_2 flake.The ratio of Mo and S is higher than 1:2 at the beginning with Mo terminated triangular nucleation formed.After that,the morphology of MoS_2 flake evolves from triangle to similar hexagon,then to truncated triangle which is determined by the faster growth speed of Mo termination than that of S termination under the S rich environment.The nucleation density does not increase linearly with the increase of reactant concentration,which could be explained by the two-dimensional nucleation theory.     

聚光内球面太阳能电池

为提高阳光利用率和光电转换率,研究了聚光内球面太阳能电池的主要性能,设计了聚光内球面太阳能电池的结构.通过菲涅耳聚光镜将太阳光聚光后射入内表面制备了多晶硅光伏电池的球腔内,在内球面上实现了聚光光伏效应.利用腔内光子气体模型分析计算了内球面上的光照强度,提出硅光电池上的最佳光强概念,计算了在内球面多晶硅电池半导体层厚10 μm时最佳聚光倍数为18、层厚5 μm时最佳聚光倍数为9.应用有限元分析法讨论了聚光内球面太阳能电池系统的温度,在AM1.5,8倍聚光条件下,光伏电池最高温度353.15 K,处于正常工作范围.采用主动风冷或水冷方法提高对流换热系数可大大降低光伏电池温度,稳定工作效率.通过分析硅光电池效率制约因素,设计了内球面光伏电池的优化结构,填充因子可达0.85,阳光辐射功率为800 mW/cm2时,聚光内球面太阳能电池效率将超过33％.     

叠氮化钡的高压拉曼光谱研究

在室温条件下,利用金刚石对顶砧高压技术,对叠氮化钡进行了原位高压拉曼光谱研究,采用红宝石荧光压标测压,实验的最高压力为10 GPa。实验压力范围内拉曼光谱随压力增加发生了丰富的变化。由于多处拉曼峰的出现和消失并伴随频移有拐点,我们判断叠氮化钡在3 GPa左右时发生了第一次结构相变;随着压力继续增加,在3.5~6.5 GPa范围内拉曼光谱仍不断变化,我们判断可能是相变或者是N=N=N键角和两个键长的非对称压缩导致的;压力继续增加,在8 GPa左右,多处新峰出现和峰的劈裂表明又发生了一次结构相变,并且判断叠氮化钡向着更复杂的结构转变。通过实验可以确定,实验压力范围内N=N=N离子并未被破坏。其实验结果有待高压同步辐射实验的进一步确认。     

通用H点标准加入法解析灰色体系

通用H点标准加入法可消除未知干扰影响，测定灰色体系中待测组分含量，给出唯一解。介绍了其原理、算法，并用于定量分析中药制剂中的有效成分，以实验验证了本方法实际应用的可行性及其结果的可靠性。     

基于激光诱导击穿光谱的合金钢组分偏最小二乘法定量分析

在炼钢中合金浓度的检测和控制对产品质量影响很大,激光诱导击穿光谱(laser induced breakdown spectroscopy, LIBS)技术具有快速、非接触、无需制样等特点,非常适合应用于合金成分的在线分析。但是由于合金中的C, S, P元素的成分含量都很低,其原子发射谱线极易淹没在复杂的铁元素特征谱线之中,造成这些重要元素在线定量分析困难。以合金钢标准光谱样品为研究对象,获取激光诱导击穿光谱数据,采用定标曲线法(calibration curve, CC)和偏最小二乘法(partial least squares, PLS),对合金钢样品的主量和微量元素进行定量分析。比较两种方法的定标结果得出：对于主量元素,PLS方法的定量分析水平优于传统的CC法;更重要的是对于微量元素,由于特征谱线极弱,CC法无法得出定量结果,而PLS法仍然具有良好的定量分析能力。同时,将PLS法回归模型特征谱线处的回归系数与原始有背景干扰的光谱强度数据进行比较,阐述了LIBS数据定量分析中PLS方法的优势。结果表明,在激光诱导击穿光谱合金成分分析中,PLS方法适合用于C等微量元素的定量分析。