Underpotential Deposition Study and Determination of Bismuth on Gold Electrode by Using Voltammetry

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Preparation of Silicalite-1 Within Macroporous Silica Glass

Microcrystalline silicalite-1 was formed on the inner surface of macroporus silica glasses prepared by the sol-gel process. By heating a homogeneous precursor solution at 100°C under a hydrothermal condition, 2–5 m of plate-like particles of silicalite-1 were deposited. With an increase of mixing time of the precursor solution, the number of silicalite-1 particles increased, accompanied by the relative decrease of the particle size. Depending on the temperature and the duration of the heat-treatment of the macroporous silica, the amount of deposited silicalite-1 varied. Below 1000°C, the amount increased with the heat-treatment temperature, as a result of the competition between the precipitation of silicalite-1 and the dissolution of silica from the macroporous silica glass under a strongly basic condition. On the other hand, above 1000°C the amount of deposited silicalite-1 decreased in accordance with the decrease of the macropore diameter by the heat-treatment, because of the limited transport of the dissolved silicate species through the smaller macropores.     

Fabrication of mesoporous ZnO nanosheets from precursor templates grown in aqueous solutions

Mesoporous ZnO nanosheets were successfully prepared by pyrolytic transformation of zinc carbonate hydroxide hydrate, Zn₄CO₃(OH)₆·H₂O. The nanosheets were initially formed as assemblies on glass substrates during chemical bath deposition (CBD) in aqueous solutions of urea and zinc acetate dihydrate, zinc chloride, zinc nitrate hexahydrate, or zinc sulfate heptahydrate at 80°C. It was key to induce heterogeneous nucleation of Zn₄CO₃(OH)₆·H₂O by promoting a gradual hydrolysis reaction of urea and controlling the degree of supersaturation of zinc hydroxide species. Morphology of Zn₄CO₃(OH)₆·H₂O was largely influenced by the anions present in the CBD solutions. The Zn₄CO₃(OH)₆·H₂O nanosheets were transformed into wurtzite ZnO by heating at 300°C in air without losing the microstructural feature.     

Partially concurrent eluent evaporation with an early vapor exit; detection of food irradiation through coupled LC-GC analysis of the fat

This paper reports two subjects. It describes LC-GC transfer by partially concurrent eluent evaporation at a greatly accelerated rate, as required for optimal compatibility with 2–3 mm i.d. LC columns and LC flow rates up to some 500 μl/min. Evaporation rates around 200 μl/min were obtained using a 0.53 mm. i.d. uncoated pre-column and an early vapor exit. A stationary-phasecoated “retaining” pre-column was used for preventing escape of volatile solutes through the vapor exit. The technique was used for the detection of food irradiation by analyzing selected radiolysis products of triglycerides, namely alkanes/alkanes and aldehydes. Extracted fat of chicken, hazel-nuts, and soup mixes was injected in LO and the relevant fractions were transferred on-line to GC. For chicken and nuts, detection of irradiation was possible down to doses below 0.5 kGy. Detection limits were higher for soup mixes due to interfering peaks.     

Nanostructured ZrO2 and Zr‐C‐N Coatings from Chemical Vapor Deposition of Metal‐Organic Precursors

Nanocrystalline zirconium carbonitride (Zr‐C‐N) and zirconium oxide (ZrO₂) films were deposited by chemical vapor deposition (CVD) of zirconium‐tetrakis‐diethylamide (Zr(NEt₂)₄) and ‐tert‐butyloxide (Zr(OBu^t)₄), respectively. The films were deposited on iron substrates and characterized by scanning electron microscopy (SEM), X‐ray diffraction (XRD) and X‐ray photoelectron spectroscopy (XPS). The Zr‐C‐N films show blue, golden brown or bronze colours, with colour stability depending upon the precursor composition (pure metal amide or mixed with Et₂NH). The deposition temperature showed no pronounced effect on the granular morphology of the Zr‐C‐N films. The XRD data of the films correspond to the formation of carbonitride phase whereas the XPS analyses revealed a strong surface oxidation and incorporation of oxygen in the film. The films deposited using a mixture of Zr(NEt₂)₄ and Et₂NH showed higher N content, better adhesion and scratch resistance when compared to films obtained from the CVD of pure Zr(NEt₂)₄. Subject to the precursor composition and deposition temperature (550‐750 °C), the microhardness values of Zr‐C‐N films were found to be in the range 2.11‐5.65 GPa. For ZrO₂ films, morphology and phase composition strongly depend on the deposition temperature. The CVD deposits obtained at 350 °C show tetragonal ZrO₂ to be the only crystalline phase. Upon increasing the deposition temperature to 450 °C, a mixture of tetragonal and monoclinic modifications was formed with morphology made up of interwoven elongated grains. At higher temperatures (550 and 650 °C), pure monoclinic phase was obtained with facetted grains and developed texture.     

Lead underpotential deposition on Au(110)

The electrochemical underpotential deposition (UPD) of lead on Au(110) was investigated by XPS using a custom‐built ultrahigh vacuum apparatus containing a chamber for electrochemical studies. A two‐step deposition process for lead UPD was confirmed. A large increase in the surface concentration of oxygen was found in solutions containing lead. The presence of lead was detected on the gold surface at all potentials within the range investigated (?500 mV to 1500 mV vs. Ag/AgCl). Degradation of chlorine by x‐rays was observed. The change in surface components with potential was investigated and linked to models of UPD and oxidation. The initial random deposition of lead from solution led to surface disordering. Copyright © 2003 John Wiley & Sons, Ltd.     

Optimization of the electrophoretic deposition of YBa2Cu3O7−x superconducting large area coatings

Large area coatings (>10cm²) of the high temperature superconductor YBa₂Cu₃O_7–x (x = 0.1 – 0.2) (YBCO) have been prepared by scale up an electrophoretic deposition technique using silver sheets and Si-wafers coated with Ag or Au as substrates. Several parameters, like the kind of the solvent, the applied voltage, the distance between the electrodes, the initial concentration of the suspension and the temperature during the electrophoresis were investigated in order to attain high deposition rates, as well as uniform YBCO coatings with the proper stoichiometry. To obtain a strongly adherent and dense coating a subsequent appropriate sintering and annealing procedure has been developed. The coatings obtained were characterized for their stoichiometry and superconducting properties by X-ray diffraction (XRD), Raman spectroscopy and magnetic measurements. The homogeneity and thickness of the films and the average grain size of the deposited particles have been investigated by optical and scanning electron microscopy (SEM).     

Preparation of VPS and PVD coatings for metallographic and TEM investigations

The aim of the first part of the paper is to give some advice for the faultless metallographic preparation of vacuum plasma sprayed coatings. Several coating/substrate combinations using metals, alloys and ceramics were investigated to derive some general rules. The second part deals with a preparation technique for cross-sections- of physical vapour deposition coatings. This technique was optimized for TiN and Ti(C, N) coatings on hardmetals which were examined in an analytical transmission electron microscope.     

一步法合成吲哚用Ag／SiO2催化剂的失活及其抑制

 用简单浸渍法制备了Ag／SiO2催化剂．该催化剂对苯胺和乙二醇一步合成吲哚表现出很高的催化活性，但同时存在明显的失活．TG，XRD和TEM表征结果表明，催化剂失活的主要原因是反应过程中催化剂表面的积碳和银粒子的烧结．向反应体系中通入氢和水蒸气能够减少催化 剂表面的积碳；向催化剂体系加入ZnO助剂能较大程度地提高银的分散度，并能有效抑制反应过程中银粒子的烧结．     

化学气相沉积法制备氧化锡自组装纳米结构

采用化学气相沉积法在镀有5-10 nm厚金膜的SiO2衬底上, 通过控制生长条件, 实现了二氧化锡纳米结构的自组装生长, 成功制备出了莲花状和菊花状的二氧化锡自组装纳米结构. 利用扫描电子显微镜、X射线衍射等表征分析手段对样品的表面形貌、结构及成份进行表征和研究. 并在此基础上, 讨论了两种自组装纳米结构的生长机制.