用化学镀法制备Pd/Ag膜时膜厚和组成的控制

 研究了不同 Pd2+含量的镀液在多孔陶瓷载体上的化学沉积规律, 发现当 Pd 沉积层厚度达到约 5 μm 后, 即使镀液中反应物的消耗比例很小, 膜厚增长也明显变缓, 沉积反应主要受膜层表面的催化活性位控制; 当镀液中 Pd2+含量只能沉积形成小于 4 μm 的 Pd 膜时, 在 323 K 化学镀 180 min 后, 镀液中 Pd2+的转化率高于 90%. 与之相似, 当 Ag 镀液中的 Ag+含量等于 0.5~2 μm 的 Ag 膜层所需量时, 在 333 K 化学镀 120 min 后, Ag+的转化率可达 95%. Ag+的高转化率与 Ag 颗粒的择向生长特性有关. 根据 Pd 和 Ag 的化学镀沉积规律, 通过调节镀液中金属离子的含量能够预先设计和精确控制超薄 Pd/Ag 膜的膜厚和组成.     

偏转法研究普鲁士蓝及六氰亚铁铟膜与电解质溶液间的离子效应

用现场偏转法结合循环伏安法研究了普鲁士蓝（ＰＢ）及六氰亚铁铟（ＩｎＨＣＦ）膜的电化学氧化还原过程。证实了ＰＢ膜的离子交换的机理为：且酸性条件下还原ＰＢ膜是Ｈ~＋先于Ｋ~＋进入膜内。还原态的ＩｎＨＣＦ膜氧化时，溶液中的阴阳离子同时参与了该反应，但随着阴离子的增大，Ｋ~＋成为该反应的主要参与者。     

新型不对称四硫代富瓦烯导电LB膜的研究

新型不对称四硫代富瓦烯导电ＬＢ膜的研究李洪启姚钟麒刘丹谭干祖俞贤达（中国科学院兰州化学物理研究所７３００００）Ｌａｎｇｍｕｉｒ－Ｂｌｏｄｇｅｔ（ＬＢ）技术已成为制备分子厚度的有序导电薄膜的有力工具，该领域中四硫代富瓦烯（ＴＴＦ）衍生物是导电ＬＢ膜的研...     

混合导电型陶瓷透氧膜材料的化学稳定性

考察了Sr-Co -Fe -O系列和Bi-Sr-Fe -O系列混合导电型无机透氧膜材料在氧分压小于 1.0 13Pa的气氛中 ,在 850℃和 950℃高温下加热 2 4～ 10 0h前后结构的变化。发现Bi -Sr -Fe-O系列透氧膜材料具有良好的化学稳定型 ,可以用于还原气氛下的催化反应。     

核级银铟镉合金中Ag In Cd 的连续滴定

研究了测定核级银铟镉合金中Ａｇ、Ｉｎ、Ｃｄ的连续滴定法。以电位滴定法测定Ａｇ；在ｐＨ２．５以ＥＤＴＡ滴定Ｉｎ；在ｐＨ≥５．５以ＥＤＴＡ滴定Ｃｄ，当ｎ＝１１时，其ＲＳＤ分别为：Ａｇ０．１１％、Ｉｎ０．５２％、Ｃｄ１．１％，合成试样分析回收率分别为：Ａｇ９９．８％～１００．１％、Ｉｎ９９．６％～１００．３％、Ｃｏ９７．６％～１０１．３％，测定９２个合金试样，其Ａｇ，Ｉｎ，Ｃｄ合量范围为：９９．７８％～     

导电聚合物超薄膜的制备及性能表征

采用修饰LB膜法制备了导电聚合物聚-3,4-乙烯二氧噻吩/硬脂酸(PEDOT/SA)复合超薄膜. 将硬脂酸(SA)/FeCl3 LB膜暴露于EDOT单体气氛中, EDOT 单体在多层膜中聚合, 制备了PEDOT/SA多层复合LB膜. 紫外-可见光-近红外(UV-Vis-NIR)吸收光谱和X射线光电子能谱(XPS)分析表明EDOT单体在多层膜中发生聚合并生成PEDOT导电聚合物. 扫描电子显微镜(SEM)分析显示生成的PEDOT导电聚合物颗粒分散于硬脂酸LB膜中, 被LB 膜所包裹. 二次离子质谱(SIMS)及XPS分析还发现S元素含量随LB 膜的深度变化而变化, 表明PEDOT 较好地分散于多层膜中. 采用四探针电导率仪对复合多层膜的电导率进行了测试, 结果显示60 层复合LB 膜的电导率为2.6 S·cm-1, 比普通PEDOT薄膜的电导率高一个数量级, 且表现出较好的掺杂/脱掺杂能力. 研究还发现复合膜电导率与薄膜在EDOT 单体中处理时间有关, 处理时间至120 min 后电导率达到最大值并趋于稳定, 氧化剂浓度较低可能影响EDOT在LB膜中的聚合反应速率. 对复合LB 膜的气敏特性进行了分析, 发现在较低气体浓度范围(φ<30×10^-6), PEDOT 复合LB 膜有较快的反应速率, 气敏性与气体浓度呈非线性. 在较高浓度范围(φ=(30-120)×10^-6), 气敏性与浓度呈较好的线性关系. PEDOT复合LB膜对HCl气体表现出较好的响应恢复特性. 同时对PEDOT 复合膜相关的导电机理及气体敏感机理进行了分析.     

厚体液膜拆分克伦特罗外消旋体及其动力学研究

以D-( )-二苯甲酰酒石酸(D-( )-DBTA)为流动载体,研究了克伦特罗(clenbuterol,Cle)对映体的厚体液膜法拆分,建立了手性拆分条件和动力学拆分模型。考察了D-( )-DBTA浓度、缓冲液pH值对手性拆分性能的影响,进行了动力学分析,并测定了膜-料液界面的萃取反应表观速率常数k1和膜-反萃相界面的反萃取表观速率常数k2。结果表明:在优化的实验条件下(pH为7,手性载体与Cle浓度比为1∶4),Cle外消旋体能被含有手性载体D-( )-DBTA的厚体液膜有效拆分,分离因子大于1.08;Cle单体的跨膜迁移过程可以用两个串联的准一级不可逆过程进行描述。     

导电聚合物膜修饰电极的研究Ⅲ: 杂多酸掺杂聚吡咯膜电极的电子自旋共振(ESR)特性研究

本文通过对不同条件下的Co(W_2O_7)_6~(10-)和CuW_(12)O_(40)~(6-)掺杂聚吡膜ESR谱线的分析并以相同条件下NO_3~-掺杂聚吡咯膜作为参照,表明杂聚阴离子不仅起着中和电性的作用,而且与聚吡咯分子链相作用形成某种加合物,它影响聚吡咯的电结构,这种加合物在过正或过负的电位下均不稳定.首次发现在CuW_(12)O_(40)~(6-)掺杂的干态聚吡咯膜具有Dysonian线型,表明膜中其它电结构的存在.     

导电高分子PEDOT/PSS保护银纳米颗粒的制备与表征

利用导电高分子聚(3,4-二氧乙基噻吩)/聚(对苯乙烯磺酸)(PEDOT/PSS)作保护剂,制备了银纳米颗粒,用UV-Vis和TEM对其进行了表征.结果表明,选择合适量的PEDOT/PSS保护剂可以得到大小分布较窄银纳米颗粒.     

类金刚石碳薄膜对碳膜导电性能的影响

以聚酰亚胺薄膜为原料,经炭化形成碳膜;进而在碳膜表面制备了类金刚石碳(DLC)薄膜,研究了制备条件对碳膜导电性能的影响.采用扫描电镜分析了薄膜的表面形貌和微观结构;采用X射线衍射仪分析了薄膜的晶体结构.结果表明,DLC薄膜的电阻率随着沉积时间的延长先减小后增加;当沉积时间达到3 h时,相应DLC薄膜的电阻率达到最小值5.66×10-5Ω.m.     

Highly conducting and transparent sprayed indium tin oxide

Spray pyrolysis process has been used to deposit highly transparent and conducting films of tin doped indium oxide onto glass substrates. The electrical, optical and structural properties have been investigated as a function of various deposition parameters namely dopant concentrations, temperature and nature of substrates. X-ray diffraction patterns have shown that deposited films are polycrystalline without second phases and have preferred orientation [400]. Indium tin oxide layers with small resistivity value around 7.10⁻⁵Ω.cm and transmission coefficient in the visible and near IR range of about 85–90 % have been easily obtained.     

The electroreduction of formaldehyde on tin and indium

The electrochemical behavior of formaldehyde on tin and indium cathodes has been studied over a wide range of pH (0.4–13), concentrations (1×10^?3 to 6×10^?1M) and potentials. Potentiostatic, potentiodynamic, ac impedance and photoe mission techniques were used to determine the kinetics of the reaction and to postulate a mechanism. The behavior on indium is similar to that reported on mercury cathodes. Tafel slopes are about 65 to 80 mV/decade. This value indicates that protonation of a reaction intermediate is the rate determining step of the reaction. The value of the slope depends slightly on concentration and pH because of adsorption under Temkin conditions. The reaction order with respect to formaldehyde is close to 1 in the limiting current region, but smaller in the Tafel region. The effect of formaldehyde on tin in neutral and alkaline solutions is to decrease the hydrogen overpotential by about 0.5 V, without affecting the Tafel slope. The rate of formaldehyde reduction is very slow. An explanation for this catalytic effect is postulated, based on the adsorption of formaldehyde-related species on the electrode surface. Formation of bridge-type complexes is also postulated. The exact nature of the adsorbed species is unknown. Preliminary results indicate that the behavior of formaldehyde on lead is similar to that on tin. The influence of this species on the reduction of formic acid on tin and lead is discussed.     

A plasmonic mercury sensor based on silver–gold alloy nanoparticles electrodeposited on indium tin oxide glass

We construct silver–gold alloy nanoparticles (Ag–AuNPs) as the basis of a reagentless, sensitive and simple mercury sensor. Ag–AuNPs were electrodeposited directly on transparent indium tin oxide film coated glass. Hg(II) ions in aqueous solution could be reduced by Ag atoms existing in Ag–AuNPs; the deposition/amalgamation of Hg on the nanoparticles resulted in a blue shift of the localized surface plasmon resonance peak. Therefore, Hg^2 + can be detected quantitatively by using a spectrophotometer. The sensor response is linear in the range from 0.05 to 500 ppb of Hg(II) concentration. No sample separation or preconcentration is required for detection of ultralow levels of mercury in water samples. The results shown herein have potential applications in the development of a new optical sensor for the detection of low concentrations of mercury.     

Immobilization of laccase on gold, silver and indium tin oxide by zirconium-phosphonate-carboxylate (ZPC) coordination chemistry

In this paper we present a simple method allowing for stable laccase immobilization on various conducting surfaces that retains the activity of the enzyme. The strategy for laccase immobilization presented in this paper relies on Zr(4+) ion coordination chemistry that involves -COO- terminal groups present on the protein. Using a host of techniques, including surface plasmon resonance (SPR), quartz crystal microbalance (QCM) gravimetry, atomic force microscopy (AFM), surface enhanced Raman scattering (SERS), resonance Raman scattering (RR) and electrochemical techniques, we show that laccase bound to a surface coordinatively through zirconium phosphonate/carboxylate (ZPC) functionalities forms a stable enzymatic layer with the enzyme retaining its activity to a significant extent.     

Low temperature H_2S sensor based on copper oxide/tin dioxide thick film

Nanostructured tin dioxide (SnO2) powders were prepared by a sol-gel dialytic process and and the doping of CuO on it was completed by a deposition-precipitation method.The thick film sensors were fabricated from the CuO/SnO2 polycrystalline powders.Sensing behavior of the sensor was investigated with various gases including CO,H2,NH3,hexane,acetone,ethanol,methanol and H2S in air.The as-synthesized gas sensor had much better response to H2S than to other gases.At the same time,the CuO/SnO2 sensor had enough sensitivity,together with fast response and recovery,to distinguish H2S from those gases at 160 and 210 ?C.Therefore,it might have promising applications in the future.     

Low temperature H2S sensor based on copper oxide/tin dioxide thick film

Nanostructured tin dioxide (SnO2) powders were prepared by a sol-gel dialytic process and and the doping of CuO on it was completed by a deposition-precipitation method. The thick film sensors were fabricated from the CuO/SnO2 polycrystalline powders. Sensing behavior of the sensor was investigated with various gases including CO, H2, NH3, hexane, acetone, ethanol, methanol and H2S in air. The as-synthesized gas sensor had much better response to H2S than to other gases. At the same time, the CuO/SnO2 sensor had enough sensitivity, together with fast response and recovery, to distinguish H2S from those gases at 160 and 210 ℃. Therefore, it might have promising applications in the future.     

The influence of electrode metals and its configuration on the response of tin oxide thin film CO sensor

Thin films of tin oxide were deposited by electron beam evaporation. The effects of the electrode materials (Ag, Al, Au and Pt) and different electrode configurations on the CO-sensing of tin oxide thin films were investigated. The Pt and Au electrodes with bottom electrode configuration show much higher response than Ag and Al electrodes. The sensor response and recovery times have also been measured. The films were characterized using X-ray diffraction and X-ray photoelectron spectroscopy. All the films were found to be amorphous. It was found that the CO-sensing properties depend both on the electrode materials and configuration.     

Tunneling characteristics of octadecyl derivatives on tin and indium electrodes

In this paper we report the tunneling behavior based on the capillary tunnel junctions of n-octadecylmercaptan (C18H37SH), octadecylamine (C18H37NH2), nonadecanoic acid (C17H35COOH), octadecanol (C18H370H), and n-iodooctadecane (C18H37I), sandwiched between tin and indium electrodes utilizing the naturally existing oxide surfaces, respectively. The surfaces of the electrodes were examined by X-ray diffraction (XRD), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) methods, and the self-assembled monolayers adsorbed on the electrode surfaces were inspected by contact angle measurements and XPS. The measured characteristic curves on tin electrode indicated a sequence of energy gaps associated with the specimen: deltaC17H35COOH > deltaC18H37OH > deltaC18H37SH > deltaC18H37NH2 > deltaC18lH37I. The results on the energy gaps obtained on indium electrodes displayed similar sequence behavior although with different gap values. The experimental observations indicate that the molecule-electrode contact, including both the functional groups and substrates, could contribute jointly to the overall conductance characteristics of molecular junctions.     

Multifractal analysis of drop‐casted copper (II) tetrasulfophthalocyanine film surfaces on the indium tin oxide substrates

This paper applies multifractal spectrum theory to characterize the structural complexity of 3D surface roughness of copper (II) tetrasulfophthalocyanine (CuTsPc) films on the indium tin oxide (ITO) substrate, obtained with atomic force microscopy (AFM) analysis. CuTsPc films were prepared by drop cast method on ITO substrate. CuTsPc films surface roughness was studied by AFM in tapping‐mode?, in air, on square areas of 2500 µm². A novel approach, on the basis of computational algorithms for analysis of 3D roughness surface applied for AFM data, was presented. Results revealed that the 3D surface roughness of CuTsPc films prepared by drop cast method on ITO substrate can be described using the multifractal geometry. The generalized dimensions D_q and the multifractal spectrum f(α) provided quantitative values that characterize the local scale properties of CuTsPc films surface geometry at nanometer scale. Data provide valuable information to describe the spatial arrangement of 3D surface roughness of CuTsPc films on ITO substrate, which was not taken into account by classical surface statistical parameters. Copyright © 2014 John Wiley & Sons, Ltd.     

Development of silver/gold nanocages onto indium tin oxide glass as a reagentless plasmonic mercury sensor

We demonstrate the utilization of silver/gold nanocages (Ag/Au NCs) deposited onto transparent indium tin oxide (ITO) film glass as the basis of a reagentless, simple and inexpensive mercury probe. The localized surface plasmon resonance (LSPR) peak wavelength was located at ∼800 nm. By utilizing the redox reaction between Hg²⁺ ions and Ag atoms that existed in Ag/Au NCs, the LSPR peak of Ag/Au NCs was blue-shifted. Thus, we develop an optical sensing probe for the detection of Hg²⁺ ions. The LSPR peak changes were lineally proportional to the concentration of Hg²⁺ ions over the range from 10 ppb to 0.5 ppm. The detection limit was ∼5 ppb. This plasmonic probe shows good selectivity and high sensitivity. The proposed optical probe is successfully applied to the sensing of Hg²⁺ in real samples.