Electrochemical preparation of microelectrodes modified with non-stoichiometric mixed-valent molybdenum oxides

A compact non-stoichiometric molybdenum (VI, V) oxide of blue film was grown on carbon fiber (CF) microelectrode surface be cycling the potential between + 0.2V and - 0.70V in a freshly prepared Na2MoO4 solution containing 5 x 10(-3) mol/L H2SO4. The quantity-of the oxide is controlled by the charge passing the electrode. The electrochemical pretreatment of CF microelectrode not only mises the deposition velocity of molybdenum oxide on CF surface, but also improves greatly the cyclic voltammetric behavior of the molybdenum oxide film prior to the electrodeposition. The cathodic processes are believed to yield the hydrogen molybdenum oxide bronzes HxMoO3(0 < x < 2), or substoichiometric lower molybdenum oxides with the formula MoO3-y(0 < y < 1). The anodic response results from the reversible oxidation of molybdenum bronze/Mo(V) centers [or perhaps Mo(IV) in more reduced coatings], to Mo(VI). Further information was gained about the chemical composition and valent state of Mo from XPS and SEM.

PREPARATION OF MODIFIED ELECTRODE WITH MOLYBDOPHOSPHATE ANION AND ITS ELECTROCATALYSIS FOR BROMATE REDUCTION

A molybdophosphate anion modified electrode has been prepared in 2 M sulfuric acid solution containing PMo12O403- by electrochemical cycling scan or simple adsorption on a glassy carbon electrode anodized before modification. The film electrode obtained is very stable upon potential cycling in acid solution. The catalytic effect of the film for reduction of bromate was investigated in detail.

ELECTROACTIVE COATINGS OF DICYANO-BIS(1,10-PHENANTHROLINE)IRON(II) ATTACHED TO NAFION POLYMER FILM-MODIFIED ELECTRODES VIA ADSORPTION

A dicyano-bis(1,10-phenanthroline)iron(II) modified elecrode was prepared. The voltammetric and the spectroelectrochemical behavior of this electrode were investigated. The influence of pH and the amount of Nafion and dicyano-bis(1,10-phenanthroline) iron(II) (DBPI) used in the electrode preparation on the electrochemical behavior is presented.

ELECTROCHEMICAL PREPARATION OF MICROELECTRODES MODIFIED WITH NONSTOICHIOMETRIC MIXED-VALENT MOLYBDENUM OXIDES

A blue, conductive, compact, mixed-valent Mo(VI, V) oxide film was grown on carbon fiber (CF) microelectrode surface by cycling the potential between +0.20 and -0.70 V vs. SCE in a fresh prepared Na2MoO4 solution (pH = 2, H2SO4). The thickness of the oxid

FLOW-INJECTION AMPEROMETRIC DETECTION OF HYDRAZINE BY ELECTROCATALYTIC OXIDATION AT A PRUSSIAN BLUE FILM-MODIFIED ELECTRODE

A Prussian Blue-modified glassy carbon electrode prepared by simple adsorption exhibited excellent electrocatalytic activity in the oxidation of hydrazine in acidic media. A film of the perfluorosulphonic acid polymer Nafion coated on top of the Prussian Blue-modified glassy carbon electrode can improve the mechanical stability of the Prussian Blue layer in the flow stream. Hydrazine was detected by flow-injection analysis at the modified electrode with high sensitivity. The limit of detection was 0.6 ng.

ELECTROCHEMICAL STUDY OF ISOPOLYOXOMETALLATES AND HETEROPOLYOXOMETALLATES FILM MODIFIED MICROELECTRODES .1. PRETREATMENT AND MODIFICATION OF THE MO80-26(4-) MODIFIED CARBON-FIBER MICROELECTRODE

In this paper the preparation of isopoly- and heteropolyoxometallates (IPA and HPA) thin film modified carbon fiber (CF) microelectrodes and the factor that influences the modification of IPA and HPA films are described. IPA and HPA film modified CF microelectrodes can all be prepared by cyclic potential scan and simple dip coating. The modified electrodes prepared are very stable and reversible in acidic solution with monolayer characteristics. The electrochemical pretreatment of CF microelectrodes plays an important role in the modification of IPA and HPA film. The absorption of IPA and HPA film on electrode surfaces has been discussed on the basis of surface conditions of the CF microelectrode and the structure of IPA and HPA.

LIQUID-CHROMATOGRAPHY WITH ELECTROCATALYTIC DETECTION OF CYSTEINE, N-ACETYLCYSTEINE AND GLUTATHIONE BY A PRUSSIAN BLUE FILM-MODIFIED ELECTRODE

Chemically modified electrodes prepared by adsorbing prussian blue on a glassy carbon electrode are shown to catalyse the electro-oxidation of cysteine, N-acetylcysteine and glutathione in acidic media. The catalytic response is evaluated with respect to the potential scan rate, the solution pH, the concentration dependence, and other variables. Covering the electrode with Nafion(R) film improved the stability and reproducibility in liquid chromatography with electrochemical detection to the extent that repetitive sample injections produced relative standard deviations of less than 5% over several hours of operation. The limit of detection was 4 pmol for cysteine, 33 pmol for glutathione and 61 pmol for N-acetylcysteine.

ELECTROCATALYTIC OXIDATION OF ASCORBIC-ACID AT A PRUSSIAN BLUE FILM MODIFIED MICRODISK ELECTRODE

The preparation and the behaviour of a Prussian Blue (PB) film on a platinum microdisk electrode has been described. Electrocatalytic oxidation of ascorbic acid has occurred at the PB film modified microelectrode. This shows a typical example of a modified microelectrode in electrocatalysis following our previous theoretical studies (J. Electroanal. Chem., 309 (1991) 103) and the related catalytic reaction rate constant was determined.

ELECTRODEPOSITION OF PLATINUM PARTICLES ON GLASSY-CARBON MODIFIED WITH COBALT PORPHYRIN AND NAFION FILM AND THEIR ELECTROCATALYTIC REDUCTION OF DIOXYGEN

In this paper, five types of chemically modified electrode (CMEs) prepared with the deposition of platinum particles on various surfaces of glassy carbon (GC) modified with cobalt porphyrin and Nafion(R) solution are characterized using the electron scanning microscope (SEM). Their activities in the four-electron reduction of dioxygen to water on the basis of their electrochemical data from cyclic voltammetric and rotating ring-disk electrode (RRDE) experiments are examined and compared. Platinum particles dispersed on the GC surface adsorbed with the cobalt porphyrin exhibit the highest activity for the electrocatalytic reduction of dioxygen. However it is interesting that the cobalt ion is lost from the center of the porphyrin ring during the preparation of the cobalt porphyrin + Nafion mixture solution, while the porphyrin ring still remains in the Nafion film, as shown by EDX analysis. The incorporation of the porphyrin may change the structure of the Nafion film into a looser form, since the platinum particles dispersed in the film are more readily exposed, resulting in more favourable mass transfer and higher activity for the electrocatalytic reduction of dioxygen.

Preparation and characterization of palladium-based composite membranes by electroless plating and magnetron sputtering

Pd and Pd-Ag (24 wt.%) alloy composite membrane were prepared by electroless plating and magnetron sputtering, respectively. The membranes were characterized by scanning electron microscopy (SEM) and H-2 permeation measurement. Commercial microfiltration ceramic membrane were coated with gamma-Al2O3-based layer by the sol-gel method and used as substrate of Pd and Pd-Ag alloy film. Both the as-prepared membranes were shown: to be He gas-tight at room temperature with a thickness of <1 mu m. Permeation results showed that H-2 permeation through these composite membranes is mainly dominated by the surface chemistry of H-2 on or/and in the membranes. The membranes exhibited a high permeation rate of H-2 and a H-2/N-2 permselectivity of higher than 60 in the optimized operation conditions. (C) 2000 Elsevier Science B.V. All rights reserved.

Preparation and characteristic of a new class of silica/polyimide nanocomposites

A new class of silica/polyimide nanocomposites was successfully prepared by the sol-gel reaction, tetraethoxysilane, (TEOS), was hydrolyzed by the water released from imidization at low and high temperature. Silica particles with diameter of around 30-50 nm were observed in the hybrid films by scanning electron microscopy. The flame retardance, decomposition temperature and glass transition temperature of the film increased with increasing silica content. The tensile strength increased slightly while the elongation at break of the films decreased with increasing silica content. (C) 2002 Kluwer Academic Publishers.

Preparation and characterization of Pd-Ag alloy composite membrane with magnetron sputtering

A Pd-Ag (24 wt%) alloy composite membrane was prepared by the magnetron sputtering. A gamma-Al2O3 membrane was synthesized by the sol-gel method and used as substrate of the Pd-Ag alloy film. The process parameters of the magnetron sputtering were optimized as a function of the compactness of the Pd-Ag alloy film. The best membrane with a thickness of 1 mu m was produced with a sputtering pressure of 2.7 Pa and a substrate temperature of 400 degrees C. The membrane had an H-2/N-2 permselectivity of 51.5-1000 and an H-2 permeation rate of 0.036-1.17 x 10(-5)cm(3)/cm(2).s. Pa, depending on operating conditions.

Net-like Ferromagnetic Mnsb Film Deposited on Porous Silicon Substrates

MnSb films were deposited on porous silicon substrates by physical vapor deposition (PVD) technique. Modulation effects due to the substrate on microstructure and magnetic properties of the MnSb film's were studied by scanning electron microscope (SEM), X-ray diffraction (XRD) and measurements of hysteresis loops. SEM images of the MnSb films indicate that net-like structures were obtained because of the special morphology of the substrates. The net-like MnSb films exhibit some novel magnetic properties different from the unpatterned referenced samples. For example, in the case of net-like morphology, the coercive field is as low as 60 Oe.

Magnetron Sputtering Growth of InAs0.3Sb0.7 Films on (100) GaAs Substrates: Strong Effect of Growth Conditions on Film Structure

The growth of highly lattice-mismatched InAs0.3Sb0.7 films on (100) GaAs Substrates by magnetron Sputtering has been investigated and even epitaxial lnAs(0.3)Sb(0.7) films have been successfully obtained. A strong effect of the growth conditions on the film structure was observed, revealing that there was a growth mechanism transition from three-dimensional nucleation growth to epitaxial layer-by-layer growth mode when increasing the substrate temperature. A qualitative explanation for that transition was proposed and the critical conditions for the epitaxial layer-by-layer growth mode were also discussed.

The Displacement and Strain Field of Three-Dimensional Rheologic Model of Earthquake Preparation

Based on the three-dimensional elastic inclusion model proposed by Dobrovolskii, we developed a rheological inclusion model to study earthquake preparation processes. By using the Corresponding Principle in the theory of rheologic mechanics, we derived the analytic expressions of viscoelastic displacement U(r, t) , V(r, t) and W(r, t), normal strains epsilon(xx) (r, t), epsilon(yy) (r, t) and epsilon(zz) (r, t) and the bulk strain theta (r, t) at an arbitrary point (x, y, z) in three directions of X axis, Y axis and Z axis produced by a three-dimensional inclusion in the semi-infinite rheologic medium defined by the standard linear rheologic model. Subsequent to the spatial-temporal variation of bulk strain being computed on the ground produced by such a spherical rheologic inclusion, interesting results are obtained, suggesting that the bulk strain produced by a hard inclusion change with time according to three stages (alpha, beta, gamma) with different characteristics, similar to that of geodetic deformation observations, but different with the results of a soft inclusion. These theoretical results can be used to explain the characteristics of spatial-temporal evolution, patterns, quadrant-distribution of earthquake precursors, the changeability, spontaneity and complexity of short-term and imminent-term precursors. It offers a theoretical base to build physical models for earthquake precursors and to predict the earthquakes.