1-脱氢松香酰基-3-取代硫脲以及5-(脱羧脱氢松香-4-基)-3-芳氨基- 1H-1,2,4-三唑化合物的合成与生物活性

以广西的优势资源松香为原料, 脱氢松香酸与亚硫酰氯、硫氰化钾分别在回流条件下反应6 h和1.5 h, 得到脱氢松香酰异硫氰酸酯, 产率52%; 然后与胺在加热回流条件下反应1.5 h, 得到11种1-脱氢松香酰基-3-取代硫脲4, 产率63%～94%; 4a～4f 分别与水合肼在搅拌下回流反应3～6 h, 得到6种5-(脱羧脱氢松香-4-基)-3-芳氨基-1H-1,2,4-三唑化合物5, 产率70%～94%; 所有化合物的结构均经IR, 1H NMR, 13C NMR和元素分析确认. 初步生物活性测试表明, 4e, 4f, 4j, 5b对枯草杆菌抑菌率较高, 特别是4j在浓度为50 mg/L时就达到较好效果; 4b, 4h, 4i, 5e在100 mg/L时对大肠杆菌的抑菌效果较好.     

Enhanced optical nonlinear absorption of graded Au--TiO2 composite films

This paper reports that single-layer and graded Au-TiO2 granular composite films with Au atom content 15%- 66% were prepared by using reactive co-sputtering technique. The third-order optical nonlinearity of single-layer and graded composite films was investigated by using s- and p-polarized Z-scans in femtosecond time scale. The nonlinear absorption coefficient βeff of single-layer Au-TiO2 films is measured to be -2.3×10^3-0.76×10^3 cm/GW with Au atom content 15%-66%. The βeff value of the 10-layer Au-TiO2 graded film is enhanced to be -2.1×10^4cm/GW calculated from p-polarized Z-scans, which is about ten times the maximum βeff of single-layer films. Broadened response in the wavelength region 730-860 nm of the enhanced optical nonlinearity of graded Au-TiO2 composite films was also investigated.     

钴(Ⅱ)-2-(5′-溴-2′-吡啶偶氮)-5-二乙氨基苯酚体系的吸附伏安法

本文研究了钴(Ⅱ)-5-Br-PADAP体系的吸附伏安法。方法的线性范围为1×10~(-9)～5×10~(-7)mol/L。,检测下限为4×10~(-10)mol/L。并将此法应用于人发中痕量钴的测定。     

NH3/NH4Cl中镍(Ⅱ)-丁二肟体系在悬汞电极上电化学还原机理的研究

The behaviour of the Nickel(Ⅱ) ion in the presence of dimethyl-glyoxime (DMG) on the hanging mercury drop electrode in NH_3/NH_4Cl media was investigated with different electrochemical techniques. It was found that: (1) the reactant was Ni(Ⅱ) complex with DMG, Ni(Ⅱ)A_2, adsorbed on the electrode surface; (2) the intermediate was Ni(Ⅰ)A_2 and (3) the product was metal amalgam Ni(0)(Hg). Two electrons were transferred in the overall reaction and the transfer coefficient was 1.8 which was measured experimentally. From experimental results, it was obvious that the reaction orders with respect to Ni(Ⅱ), DMG and H~+ were 1,2, and 1, respectively. A new compound, X, was detected. The reaction scheme could be written as followsNi(Ⅱ)A_2+Hg<=>Ni(Ⅱ)A_2(ads)(Hg)Ni(Ⅱ)A_2(ads)(Hg)+e~-<=>Ni(Ⅰ)A_2(ads)(Hg)Ni(Ⅰ)A_2(ads)(Hg)+H~++e~-→Ni(0)(Hg)+HA(des)+A~-(des)→X+Hg     

悬汞电极阳极溶出伏安法测定人发中的铜、铅、镉、锌

从人发中了解重金属对于人的危害有其重要的作用。阳极溶出伏安法对于测定重金属来说其价格/收益比例是最好的。Chittleborough等用悬汞电极上的微分脉冲阳极溶出伏安法测定了人发中的铜、铅、镉、锌。但所用仪器较昂贵,我们实验了用悬汞电极的线性扫描阳极溶出伏安法测定人发中的这四种元素,结果是满意的。     

简易高斯灰度扩散模型的误差分析及适用性研究

为了验证简易高斯灰度扩散模型的适用性,与传统高斯灰度扩散模型进行了对比分析。将两种高斯模型做归一化处理,设定检验像素,分析检验像元灰度的归一化值的相对误差;进行星图模拟,得到4个不同高斯半径(σ)下灰度赋值相对误差与像点映射位置偏离值的关系曲线,整体上误差随σ的增大而减小;对星图模拟得到的系列星像点采用灰度重心法提取质心,质心误差随σ增大而减小,传统模型模拟像点的质心提取精度比简易模型高约2个数量级。无噪声条件下σ=0.671时,简易模型模拟像点最大质心误差仅为0.033pixel。仿真结果表明:单就像点外形仿真而言,当σ较小时,简易模型不再适用;但针对像点的质心定位及后续算法,简易模型带来质心误差量级可以忽略,运算量更小,适于应用。     

热丝化学气相沉积微晶硅薄膜结构及性质研究

采用热丝化学气相沉积(HWCVD)技术,以钨丝作为热丝,在不同热丝温度和氢稀释度下,分别在玻璃和单晶硅片衬底上沉积微晶硅(μc-Si∶H)薄膜材料.对所制备的微晶硅薄膜材料使用XRD、傅里叶变换红外吸收光谱、透射谱等进行结构与性能的表征分析.结果表明,随着热丝温度升高,氢稀释度变大,薄膜呈现明显的(220)择优生长取向,晶粒尺寸逐渐增大,光学吸收边出现红移,光学带隙逐渐变小.通过优化沉积参数,在热丝温度为1577℃、氢稀释浓度为95.2;、衬底温度为350℃,沉积速率为0.6 nm/s和沉积气压8 Pa条件下,制备的微晶硅薄膜呈现出了(220)方向的高度择优生长取向,平均晶粒尺寸为146 nm,光学带隙约为1.5 eV,光电导率σ.为3.2×10-6Ω-1·cm-1,暗电导率σrd为8.6×10-7 Ω-1·cm-1,表明制备的材料是优质微晶硅薄膜材料.     

热处理和掺铝量对溶胶-凝胶法制备AZO薄膜光电性能的影响

以(CH3COO)2Zn·2H2O和AlCl3·6H2O为前驱物,以普通玻璃为基底利用溶胶-凝胶旋转涂膜法制备AZO薄膜.采用X射线衍射仪、扫描电子显微镜、紫外-可见分光光度计、四探针电阻测试仪等对AZO薄膜的物相组分、表面形貌、透射率和方块电阻进行测量与表征,并研究了热处理温度和掺铝量对AZO薄膜的结构和光电性能的影响.结果表明:AZO薄膜的结构和光电性能与不同的热处理温度和掺铝量有关,实验得到了最佳的工艺条件为热处理温度为500℃,热处理时间为60 min,掺Al溶度为1mol;,镀膜层数为8层.     

以两种季铵碱为模板剂合成A形体富集Beta沸石及其晶化过程

以三甲基环己基氢氧化铵和二甲基乙基环己基氢氧化铵为模板剂或结构导向剂(SDA), 采用超浓水热方法合成了A形体富集的Beta沸石, 用粉末X射线衍射(XRD)、 扫描电子显微镜(SEM)、 ²⁹Si固体魔角自旋核磁共振(²⁹Si MAS NMR)以及氮气吸附等表征手段对其进行了详细表征, 探索了最优合成条件, 研究了其晶化过程. 结果表明, 在晶化初期产物中己出现A形体过量特征, 随着晶化的进行, A形体的过量程度无显著变化.