Controllable synthesis of metal hydroxide and oxide nanostructures by ionic liquids assisted electrochemical corrosion method

Cu(OH)(2) nanowires have been synthesized by anodic oxidation of copper through a simple electrolysis process employing ionic liquid as an electrolyte. Controlling the electrochemical conditions can qualitatively modulate the lengths, amounts, and shapes of Cu(OH)(2) nanostructures. A rational mechanism based on coordination self-assembly and oriented attachment is proposed for the selective formation of the polycrystalline Cu(OH)(2) nanowires. In addition, the FeOOH nanoribbons, Ni(OH)(2) nanosheets, and ZnO nanospheres were also synthesized by this route, indicative of the universality of the electrochemical route presented herein. The morphologies and structures of the synthesized nanostructures have been characterized by transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), powder X-ray diffraction (XRD). Fourier transform infrared spectra (FT-IR), and thermogravimetric (TG). (C) 2007 Elsevier Masson SAS. All rights reserved

Application of electrochemical impedance spectroscopy for monitoring allergen-antibody reactions using gold nanoparticle-based biomolecular immobilization method

Gold nanoparticles were used to enhance the immobilization amount and retain the immunoactivity of recombinant dust mite allergen Der f2 immobilized on a glassy carbon electrode (GCE). The interaction between allergen and antibody was studied by electrochemical impedance spectroscopy (EIS). Self-assembled Au colloid layer (Phi = 16 nm) deposited on (3-mercaptopropyl)trimethoxysilane (MPTS)-modified GCE offered a basis to control the immobilization of allergen Der f2. The impedance measurements were based on the charge transfer kinetics of the [Fe(CN)(6)](3-/4-) redox pair, compared with bare GCE, the immobilization of allergen Der f2 and the allergen-antibody interaction that occurred on the electrode surface altered the interfacial electron transfer resistance and thereby slowed down the charge transfer kinetics by reducing the active area of the electrode or by preventing the redox species in electrolyte solution from approaching the electrode. The interactions of allergen with various concentrations of monoclonal antibody were also monitored through the change of impedance response. The results showed that the electron transfer resistance increased with increasing concentrations of monoclonal antibody.

Determination of surface pK(a) of HS(CH2)(10)COOH SAMs using an electrochemical titration method

The self-assembled monolayer(SAM) of 11-mercaptoundecanoic acid [HS(CH2)(10)COOH] was formed on a gold electrode and the effect of the charge of end group on the electrochemical response of Fe(CN)(6)(3-) at the SAM modified electrode was studied by cyclic voltammetry. At high pH, when the -COOH groups are dissociated, the current of Fe(CN)(6)(3-) is suppressed; as the solution pH is lowered, the current of Fe(CN)(6)(3-) increases. The electrochemical titration curve was obtained by correlating the currents of Fe(CN)(6)(3-) to the different pH values of electrolyte, from which the surface pK(a) was obtained to be 3. 0+/-0. 2. Furthermore, the reason of small pK(a) value was explained using SAMs of different surface coverage.

Determination of surface pK(a) of SAM using an electrochemical titration method

A self-assembled monolayer (SAM) of 3-mercaptopropionic acid (HSCH2CH2COOH) was formed on a gold electrode. The effect of the charge of the end group on the electrochemical response of Fe(CN)(6)(3-) at the SAM modified electrode was studied by using cyclic voltammetry. At high pH, when the -COOH groups are dissociated, Fe(CN)(6)(3-) current is suppressed; as the solution pH is lowered, Fe(CN)(6)(3-) current increases. The electrochemical titration curve was obtained by correlating the currents to the different electrolyte pH values, from which the surface pK(a) was obtained to be 5.2+/-0.1. Furthermore, a calculation equation was presented to simulate the electrochemical titration. As comparison, the surface pK(a) was also measured by contact angle titration as 5.6+/-0.1. The surface pK(a) values determined by the two methods in our work are consistent and accurate.

A novel potentiodynamic method of electrochemical growth for layer-by-layer film formation based on electrostatic interaction

A novel method of electrochemical growth was developed for layer-by-layer film formation and proven more advantageous than the commonly used immersion growth in obtaining more uniform multilayer assemblies, as well as being able to proceed in salt-containing solutions without competitive adsorption from the salt ions. (C) 1999 Elsevier Science S.A. All rights reserved.

A double logarithmic method for studying the adsorption effects in an irreversible electrochemical process

The adsorption of an electroinactive product greatly influences an irreversible electrochemical reaction in three ways, including self-block, self-inhibition, and self-acceleration, and changes not only the heterogeneous electron-transfer rate constant but also the modified formal potential and electron-transfer coefficient of the electrochemical reaction. In order to study these adsorption effects, a double logarithmic method was suggested to be used in processing the potential-controlled thin layer spectroelectrochemical data. The result shows three types of double logarithmic plots for three kinds of adsorption effects. These double logarithmic plots can be a diagnostic criterion of the adsorption effects and enable us to determine some thermodynamic and kinetic parameters. The combination of nonlinear regression with double logarithmic method is a convenient way to examine the suggested mechanism and to extract more information from the limited experimental data. Some examples are given to test the theoretical results. (C) 1999 The Electrochemical Society. S0013-4651(98)05-012-5. All rights reserved.

A double logarithmic method in thin-layer spectroelectrochemistry for distinction among mechanisms of an irreversible electrochemical process

A simple double logarithmic method in potential-controlled thin-layer spectroelectrochemistry for an irreversible electrochemical process has been studied by numerical analysis and examined by experimental examples. This simple algorithm has a novel function offering some important information about the mechanism of a complex electrochemical process directly from a limited amount of potential-spectrum data, and can be used to distinguish different reaction mechanisms such as E, EC, EE, as well as to determine the electron-transfer coefficient, a, and the kinetically modified E-0'. Combination of the double logarithmic method with nonlinear regression provides a powerful tool to examine the proposed mechanism and also to estimate other thermodynamic and kinetic parameters. (C) 1999 The Electrochemical Society. S0013-4651(98)06-090-X. All rights reserved.

Influence of Electrostatic Interaction on Fibrinogen Adsorption on Gold Studied by Imaging Ellipsometry Combined with Electrochemical Methods

Imaging ellipsometry was combined with electrochemical methods for studying electrostatic interactions of protein and solid surfaces. The potential of zero charge for gold-coated silicon wafer/solution interfaces wad determined by AC impedance method. The potential of the gold-coated silicon wafer was controlled at the potential of zero charge, and the adsorption of fibrinogen on the potential-controlled and non-controlled surfaces was measured in real time at the same time by imaging ellipsometry The effect of electrostatic interaction was studied by comparing the difference between the potential of controlled adsorption and the Potential of noncontrolled adsorption. It was shown that the rate of fibrinogen adsorption on the potentiostatic surface was faster than that on the nonpotentiostatic surface. The electrostatic influence on fibrinogen adsorption on the gold-coated silicon wafer was weak, so the hydrophobic interaction should be the major affinity.

Nano-polypyrrole supercapacitor arrays prepared by layer-by-layer assembling method in anodic aluminum oxide templates

A novel method for preparing nano-supercapacitor arrays, in which each nano-supercapacitor consisted of electropolymerized Polypyrrole (PPy) electrode / porous TiO2 separator / chemical polymerized PPy electrode, was developed in this paper. The nano-supercapacitors were fabricated in the nano array pores of anodic aluminum oxide template using the bottom-up, layer-by-layer synthetic method. The nano-supercapacitor diameter was 80 nm, and length 500 nm. Based on the charge/discharge behavior of nano-supercapacitor arrays, it was found that the PPy/TiO2/PPy array supercapacitor devices performed typical electrochemical supercapacitor behavior. The method introduced here may find application in manufacturing nano-sized electrochemical power storage devices in the future for their use in the area of microelectronic devices and microelectromechanical systems.

Electrochemical fabrication and electronic behavior of polypyrrole nano-fiber array devices

Electrochemically active Polypyrrole (PPy) nano-fiber array device was fabricated via electrochemical deposition method using aluminum anodic oxide (AAO) membrane as template. After alkaline treatment electrochemically active PPy nano-fiber lost electrochemical activity, and became electrochemically inactive PPy. The electronic properties of PPy nano-fiber array devices were measured by means of a simple method. It was found that for an indium-tin oxide/electrochemically inactive PPy nano-fiber device, the conductivity of nano-fiber increased with the increase of voltage applied on the two terminals of nano-fiber. The electrochemical inactive PPy nano-fiber might be used as a nano-fiber switching diode. Both Au/electrochemically active PPy and Au/electrochemically inactive PPy nano-fiber devices demonstrate rectifying behavior, and might have been used for further application as nano-rectifiers. (c) 2005 Elsevier B.V. All tights reserved.

An improved method for the extraction of low molecular weight organic acids in variable charge soils

Due to specific adsorption to variable charge soils, low molecular weight organic acids (LMWOAs) have not been sufficiently extracted, even if common extractants, such as water and 0.1 M sodium hydroxide (NaOH), were employed. In this work, the method for extracting LMWOAs in soils with 0.1 M NaOH was improved for variable charge soils; e.g. 1.0 M potassium fluoride (KF) with pH 4.0 was applied as an extractant jointed with 0.1 M NaOH based on its stronger ability to change the electrochemical properties of variable charge soils by specific adsorption. With the proposed method, the recoveries of oxalic, tartaric, malic, citric and fumaric acids were increased from 83 4, 93 1, 22 2, 63 +/- 5 and 84 +/- 3% to 98 +/- 2, 100 +/- 2, 85 +/- 2, 90 +/- 2 and 89 +/- 2%, respectively, compared with NaOH alone. Simultaneously, the LMWOAs in Agri-Udic Ferrosol with field moisture were measured with a satisfactory result.

Preparation and characterization of CdS nanotubes and nanowires by electrochemical synthesis in ion-track templates

CdS nanotubes and nanowires have been synthesized with controlled dimensions by means of template-electrodeposition method in etched ion-track membranes. The diameters of nanotubes and nanowires are between 20 and I 10 nm, and the lengths are up to tens of micrometers. X-ray diffraction (XRD) and selected area electron diffraction (SAED) pattern investigations demonstrate that CdS nanotubes and nanowires are polycrystalline in nature. The UV-vis absorption spectra of CdS nanotubes and nanowires embedded in polycarbonate (PC) membranes show that the absorption edges of PC films shift towards the shorter wavelength, with decreasing diameters of the deposited nanostructures. The results indicate that nanowires are formed from nanotubes by nanotube-stuffing-growth mechanism.

An alternative approach to ascertain the rate-determining steps of TiO2 photoelectrocatalytic reaction by electrochemical impedance spectroscopy

In an attempt to ascertain the rate-determining steps (RDS) of TiO2 photoelectrocatalytic (PEC) reaction, the PEC oxidation of sulfosalicylic acid (SSA) solution in a TiO2-coated electrode reactor system was monitored by applying the electrochemical impedance spectroscopy (EIS) method. In the meantime, an EIS mathematical model was first established to theoretically simulate the PEC reaction. Based on the EIS model, the theoretical simulation indicates three typical reactions in a PEC oxidation process, which include the charge-transfer-dominated reaction, both the charge-transfer- and adsorption-dominated reaction, and the adsorption-dominated reaction. The experimental results of EIS measurement showed that there was only one arc/semicircle on the EIS plane display when the external bias applied was below 200 mV (vs SCE) in the SSA PEC degradation whereas there were two arcs/semicircles when the externally applied bias exceeded 200 mV (vs SCE). The experimental results have a good agreement with the model simulation. The EIS method in this study provides an easier way to determine the RDS in a PEC oxidation process, which would be helpful to better control the reaction in practice.

Electrochemical surface plasmon resonance detection of enzymatic reaction in bilayer lipid

In this paper, electrochemical surface plasmon resonance (SPR) method was first used to detect enzymatic reaction in bilayer lipid membrane (BLM) based on immobilizing horseradish peroxidase (HRP) in the BLMs supported by the redox polyaniline (PAn) film. By SPR kinetic curve in situ monitoring the redox transformation of PAn film resulted from the reaction between HRP and PAn, the enzymatic reaction of HRP with H2O2, was successfully analyzed by electrochemical SPR spectroscopy.