聚乙二醇掺杂对氧化镍-氧化钛薄膜电致变色行为的影响

以醋酸镍、钛酸正丁酯为前驱物,聚乙二醇(PEG)为掺杂剂,制备了氧化镍-氧化钛(Ni O-Ti O2)的溶胶、干凝胶和薄膜,研究了掺杂分子量分别为200、400、1000、2000的PEG对Ni O-Ti O2薄膜电化学和光学性能的影响。对溶胶进行粒径和粘度测定,考察了干凝胶的热力学行为。溶胶在基底上浸渍提拉成膜,300℃煅烧后,采用双电位阶跃计时电流法测定Ni O-Ti O2薄膜电化学性能,分光光度计测定薄膜的透过率。其中掺杂PEG200的薄膜性能最好:其双层膜的注入电量是未掺杂单层膜的2.2倍,薄膜在550nm处着色态和无色态的透过率差值最大为54%,变色效率达到37.4cm2·C-1;掺杂PEG200可延长薄膜的循环寿命至2000圈以上。     

SnO2掺杂对TiO2/Si纳米复合材料性能的影响

采用溶胶-凝胶法在p-型单晶硅的表面镀上一层TiO2-SnO2纳米复合薄膜,并在一定的温度下煅烧得到TiO2-SnO2/Si复合材料.实验研究发现,在TiO2中掺杂一定量的SnO2会使TiO2/Si复合材料的光电压增强,且SnO2的掺杂会抑制TiO2的晶相转变,使复合材料的高温稳定性增强.另外,SnO2的掺杂量和煅烧温度对复合材料的光电压都有影响.当SnO2掺杂量约为20%,煅烧温度为600℃时复合材料的光电压最强.     

溶胶-凝胶法制备α-Fe_2O_3纳米晶

研究了在硝酸铁 -乙二醇甲醚体系中用溶胶 -凝胶法制备氧化铁纳米晶 .利用 TEM、XRD和 TG- DTA手段对产物进行了表征。结果表明 ,体系中加入十二烷基磺酸钠有助于纯相α- Fe2 O3纳米晶的生成 ,而加入钛酸四丁酯则显著缩短凝胶时间 ,所得粉体的原始晶粒尺寸为 30 nm左右 .若加入硅酸乙酯替代钛酸四丁酯 ,则最终产物为 γ氧化铁和 α氧化铁的混晶相 ( γ- Fe2 O3为主晶相 ) ,晶粒尺寸约 10 nm .     

多孔TiO2薄膜的表面微结构对甲基橙光催化脱色的影响

 从含聚乙二醇的钛醇盐溶胶前驱体出发,通过浸渍提拉法在玻璃表面制备了锐钛矿型多孔TiO2薄膜．随着前驱物中聚乙二醇加入量及分子量的增加,聚乙二醇热分解后在薄膜中产生气孔的数量增多,孔径增大,TiO2薄膜表面的羟基含量也增加．TiO2薄膜中引入适当大小的微孔可明显提高薄膜的光催化活性;当孔径接近400nm时,光的散射增强,透光率下降,薄膜的光催化活性降低．     

纳米TiO2薄膜光阳极的制备及性能

本文以钛酸正丁酯为前驱物、乙醇作为分散剂、二乙醇胺作为螯合剂、聚乙二醇作为表面活性剂,采用溶胶-凝胶法制备得到一种TiO2溶胶,并通过乙酸或氨水作用后制得另外两种溶胶,分别在室温于ITO导电玻璃上涂制,得到5种单一粒径范围纳米TiO2薄膜和具有两种粒径范围膜层的6种纳米TiO2薄膜;XRD和SEM等测试结果表明,纳米TiO2薄膜为锐钛矿相或锐钛矿与金红石相的混合相,其粒径分布范围在15～30nm,30～50 nm,40～80 nm区间。采用浸渍法将所制备的膜进行染料的敏化,得到染料敏化纳米TiO2薄膜半导体光阳极,测试结果表明,在所制备的纳米TiO2薄膜中,具有两种粒径范围膜层的纳米TiO2薄膜的光电性能相对较好。     

SnO2-TiO2薄膜载体对Au-Pt纳米颗粒电化学性能的影响

采用真空镀膜法在玻碳(GC)电极表面修饰SnO2-TiO2薄膜, 在SnO2-TiO2/GC复合电极表面组装Au-Pt双金属纳米颗粒, 制得Au-Pt/SnO2-TiO2/GC复合电极. 通过循环伏安法(CV)研究了SnO2-TiO2薄膜载体对Au-Pt双金属纳米颗粒电化学性能的影响; 采用扫描电镜(SEM)及X射线光电子能谱(XPS)对Au-Pt在SnO2-TiO2薄膜沉积的形貌及结构进行了表征. 研究结果表明, 10 nm的Au-Pt双金属纳米颗粒均匀地组装于SnO2-TiO2薄膜表面; SnO2-TiO2薄膜载体改善了复合电极抗CO中毒能力; Au-Pt双金属合金的形成提高了Pt 对甲醇氧化的电催化能力, SnO2-TiO2薄膜载体又使Pt纳米粒子d空轨道增多, 提高了Au-Pt双金属纳米颗粒的稳定性和催化性能.     

沉积温度对Cu_2O薄膜生长过程及光电性能的影响(英文)

以硫酸铜为铜源,采用一步化学浴沉积法制备出了晶粒尺寸可调的纳米晶Cu2O薄膜。通过X射线衍射、扫描电镜和紫外可见分光光度法研究了沉积温度对薄膜晶体结构、成核密度、晶粒尺寸、薄膜厚度和光电性能的影响。结果表明,当在60~90℃范围内调节温度时,能够很好地控制晶粒尺寸、薄膜厚度,并将禁带宽度控制在33~51 nm、392~556 nm和2.47~2.61 eV范围内;随着晶粒尺寸的减小,紫外可见光谱的吸收边有明显的蓝移。此外还对薄膜的生长过程,成核密度和颗粒尺寸变化的机理进行了讨论。     

TiO2-SiO2二维大孔薄膜的制备及其光催化活性研究

本文采用改进的溶胶-凝胶法制备了具有锐钛矿晶型结构和较小晶粒尺寸的TiO₂-SiO₂溶胶,并以聚苯乙烯(PS)小球为模板,采用旋涂法制备了新型大孔TiO₂-SiO₂复合薄膜,探究了煅烧温度、不同硅钛比以及溶胶添加量对所制备的大孔薄膜形貌及光催化活性的影响,并考察了该薄膜真空活化前后(Ti³⁺掺杂后)在紫外及模拟太阳光下光催化降解有机污染物罗丹明B的活性。通过Raman、DRS、SEM、EPR等方法对薄膜进行表征,发现制备的复合薄膜具有高透明度、良好附着力及优异的光催化活性。     

镝对Dy_x(Fe_(47.5)Pd_(52.5))_(100-x)薄膜结构与磁性能的影响

采用直流磁控溅射法制备Dyx(Fe47.5Pd52.5)100-x(x=0,2.2,3.2,4.4,5.6)薄膜,X射线衍射实验结果表明:添加稀土元素Dy可以大幅缩短从无序的fcc相转变为有序的fct相的退火时间和退火温度,增加相转变的驱动力;此外适当添加Dy元素还具有细化晶粒的作用,晶粒尺寸可达到12~31 nm,适当的晶粒尺寸有利于晶粒之间的交换耦合作用。薄膜的磁滞回线表明:矫顽力Hc与剩磁比Mr/Ms随Dy含量的增加而先急剧增加后减小,当稀土含量x=3.2时,矫顽力的最大值为3.27 k Oe。随着退火温度的增加,矫顽力的变化也是先增加后下降,并且在Ta=550℃时达到最大。     

N掺杂TiO2纳米膜吸附胆红素分子的石英晶体微天平研究

以柠檬酸催化溶胶-凝胶法合成了晶粒尺寸为16.9 nm的锐钛矿型N掺杂TiO2(N-TiO2)纳米颗粒,并用旋转涂膜法制备了N-TiO2纳米薄膜.采用石英晶体微天平(QCM)技术研究了胆红素在纳米N-TiO2膜表面的吸附动力学行为,考察了缓冲溶液pH、硅烷亲脂试剂三甲基氯硅烷及金属离子修饰纳米N-TiO2膜对胆红素吸附...     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。