Investigation of surface structure and composition of in situ annealed Fe–Mn binary alloy samples using RHEED and electron spectroscopy

The formation of oxides at the surface of Fe–1.5%Mn and Fe–0.6%Mn binary alloys was investigated as a function of the conditions of the heat treatments. Both the influence of temperature and the atmosphere under which the experiments were performed were studied. The range of annealing temperatures was adjusted to 800°C. The atmosphere consisted of a mixture of N₂–5%H₂ and traces of water vapour, with different fixed dew points ranging from −10°C to −30°C. The state of the annealed surfaces was determined using in situ analytical devices attached to the annealing reactor in order to avoid surface contamination or the formation of native oxides after the experiments due to contact with air. The structure and composition of the surfaces were determined by reflection high-energy electron diffraction (RHEED) and electron spectroscopy (XPS, AES). Copyright © 2002 John Wiley & Sons, Ltd.     

Electrochemical studies of the oxidation mechanism of polyamide on glassy carbon electrode

Polyamides containing N-methyl pyrroles and N-methyl imidazoles are a type of small molecule that can bind and recognize the bases of DNA with high affinity and specificity. Five polyamides were studied at glassy carbon electrode in acetate buffer by cyclic and differential pulse voltammetry to clarify their redox pathways. The polyamide electrochemical responses are compared by peak currents and peak potentials. The slopes of the three anodic E_p vs. pH plots of a typical polyamide are linear and show 0.059, 0.057, 0.056 V per pH in acid media, respectively, which correspond to a mechanism involving the equal number of electrons and protons. A possible mechanism for the redox pathway of various polyamides is proposed: the oxidation product of imidazole ring is acylamide and the results of in situ UV–Vis spectroscopy at Pt web electrode support the proposed mechanism. electrospray ionization mass spectroscopy (ESI-MS) indicates that one or two oxygen atoms are added into polyamide molecule after electrochemical oxidation.     

Investigation of nucleation processes under the influence of magnetic fields

The present work demonstrates the possibilities and the limits of the in situ electrochemical scanning tunneling microscopy for investigation of nucleation processes in magnetic fields on the examples of Cu and Co electrodeposition onto Au(111) electrodes from sulfate electrolytes with pH 3. Cyclic voltammograms of Cu in the underpotential range (UPD) exhibit no significant change in the cathodic and anodic peaks recorded in magnetic fields parallel to the surface. In magnetic fields of a permanent magnet, the reconstruction of Au has been annihilated during UPD of Cu. In the overpotential range, the dissolution of Cu is inhibited. This triggers the formation of a Cu–Au surface alloy. The UPD deposition of Co onto Au(111) could be proven without magnetic field, which leads to the formation of two monolayers. The nucleation in an applied field could not be observed due to higher induced fluctuations and microconvective effects. Contribution to special issue “Magnetic field effects in Electrochemistry”.     

Hydrothermal in situ Ligand Synthesis from 1,10-Phenanthroline-5,6-dione and Characterization of 1D Coordination Polymers [Co（bpdc）（H2O）3] · H2O and [Cu（bpy）V2O6]

Hydrothermal treatment of MCl2(M=Co or Cu), NH4VO3, and 1,10-phenanthroline-5,6-dione(pdon) resulted in the formation of a duplex coordination polymer [Co(bpdc)(H2O)3]·H2O(bpdc=2,2′-bipyridine-3,3′-dicarboxylate) and a chain-like coordination polymer [Cu(bpy)V2O6](bpy=2,2′-bipyridine). X-ray single-crystal structural analysis shows that under hydrothermal conditions and in the presence of different transition metals, the organic reagent pdon was transformed in situ into bpdc and bpy, respectively. Mechanism of the in situ ligand synthesis reaction has been discussed.     

In Situ Fabrication of ZnS Semiconductor Nanoparticles in Layered Organic-inorganic Solid Template

Ordered ZnS semiconductor nanoparticles were in situ synthesized in metal halide perovskite organic/inorganic layered hybrids (CnH2n 1NH3)2ZnCl4 (n=10 and 12) by reaction of their spin-casting films with H2S gas. Transmission electron microscopy, UV-vis spectroscopy and small-angle X-ray diffraction were used to characterize the morphology and the structure of formed nanoparticles. Obtained results indicate an effective way to incorporate functional inorganic nanoparticles into structured organic matrices.     

Synthesis,Characterization and Catalysis of Ce‐MCM‐41

The cerium‐containing MCM‐41 (Ce‐MCM‐41) has been synthesized by direct hydrothermal method. The low‐angle XRD patterns revealed the typical five major peaks of MCM‐41 type hexagonal structures. The interplanar spacing d₁₀₀ = 38.4 Å was obtained that can be indexed on a hexagonal unit cell parameter with a_o = 44.3 Å which was larger than that of pure siliceous MCM‐41 (Si‐MCM‐41). Transmission electron micrograph shows the regular hexagonal array of uniform channel characteristics of MCM‐41. The BET surface area of Ce‐MCM‐41 was 840 m²/g, which is much reduced as compared to that of Si‐MCM‐41, with the pore size of 26.9 Å and mesopore volume of 0.78 cm³/g were measured by nitrogen adsorption‐desorption isotherm at 77 K. Along with the results, the synthesized Ce‐MCM‐41 exhibited a well‐ordered MCM‐41‐type mesoporous structure with the incorporation of cerium. Using Ce‐MCM‐41 as a support, the Rh (0.5 wt%) catalyst exhibited very high activity for the NO/CO reactions.     

原位合成分子筛膜毛细管色谱柱的研制

吸附型多孔层毛细管柱既耐高温又对气体及烃类异构体有选择性，同时又具有毛细管色谱快速、高效等优点，是解决难分离组分的重要柱型．常用作气一固吸附色谱固定相的有强极性的硅、中极性的氧化铝、非极性的碳质及特殊吸附作用的分子筛．其中分子筛以其独特的吸附作用，在永久性气体和烃类碳数族组成分析中有重要地位．Pruecell和Soulages[1，2]等制备了涂渍型5A和13X型分子筛的毛细管柱，对低碳烃类化合物显示了良好的分离能力，分析柱温较填充柱降低约100℃．邹乃忠等[3～5]也先后制备了分子筛层的毛细管柱用来作直馏汽油的分析．由于通…     

Future of biological aerosol detection

Biological aerosol detection in real time is an urgent civilian and military requirement. Such detection capability will be useful in environmental monitoring, for example, in gathering information in perceived hazardous areas such as housing developments downwind of sewage treatment plants. To be truly functional, the instrument has to operate continuously, 24 h a day and 7 days a week with minimal maintenance and few false alarms. A novel concept is proposed. The system employs a rapid front-end warning/alarming mechanism based on optical technologies that provides useful information for protection decision makers. This is connected to a sample collector that feeds a slower back-end liquid chemistry system that provides analytical results to the medical personnel to assist in prophylaxis and therapy decisions. Experience gained from measuring fluorescence signals of single bacterial spores under flow cytometry (FCM) using UV excitation at 340-360 nm, was applied to concept testing of a prototype instrument, built to do the same for aerosols. This machine was capable of resolving particle size as well as fluorescence intensity of each particle under laboratory and field conditions; it was called the fluorescent aerodynamic particle sizer (FLAPS). This paper describes practical aspects of measuring biological aerosols when the results must be compared to reference samplers that provide culturable or “live” data. Treatment of particle size and fluorescence information is discussed with respect to FLAPS and reference data fidelity. Along with an objective method to evaluate FLAPS data correlation to reference data, an approach for determining limit of detection in the field is discussed. In addressing the back-end detector chemistry, we have prioritized a number of important biological characteristics that must be given to a clinician to help in prophylaxis and therapy decisions. A series of biochemical measurements are proposed to define the threat of a sample and different solutions are given to implement these tests. We predict that the future for biological detection looks promising for fluorescence in situ hybridization (FISH) techniques in identifying microorganisms. A conceptual instrument based on merging FCM and microchip-based analysis is described.     

Ag-MoO3催化丙烯直接气相环氧化反应的原位红外研究

制备了对丙烯直接气相环氧化具有较好催化性能的Ag-MoO3催化剂, 采用原位FT-IR技术研究了丙烯、环氧丙烷及丙烯+氧气的混合气在Ag和Ag-MoO3催化剂表面上的吸附及反应行为. 研究表明, 丙烯在Ag和Ag-MoO3催化剂表面上吸附后, 均不发生化学反应, 而环氧丙烷吸附后在较高温度下则发生开环和聚合反应直至产生积炭. 与Ag催化剂相比, 在Ag-MoO3催化剂上, MoO3的加入在降低催化剂活性的同时, 在一定程度上抑制了产物环氧丙烷的开环及深度反应, 使环氧丙烷的选择性提高. 另外, 在较低的反应温度和较短的滞留时间下, 环氧丙烷发生深度反应的程度明显降低.     

DeNOx催化剂FeZSM-5/Raney Fe的制备

用原位晶化法合成了FeZSM-5/RFe(RFeRaney Fe)催化剂. 合成液的组成为5Na2O*100SiO2*10TPABr*7 000H2O,pH＞11.5. 合成液中不含Al,ZSM-5分子筛的骨架Al只来源于Raney Fe的表面. 此法提高了ZSM-5分子筛中骨架Al的稳定性和分子筛上Fe离子的负载量. FeZSM-5/RFe用作DeNOx催化剂时具有较高的活性和水热稳定性.