Poly(vinylidene fluoride-hexafluoropropylene)/organo-montmorillonite clays nanocomposite lithium polymer electrolytes

Polymer-clay nanocomposite (PCN) materials were prepared by intercalation of an alkyl-ammonium ion spacing/coupling agent and a polymer between the planar layers of a swellable-layered material, such as montmorillonite (MMT). The nanocomposite lithium polymer electrolytes comprising such PCN materials and/or a dielectric solution (propylene carbonate) were prepared and discussed. The chemical composition of the nanocomposite materials was determined with X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy, which revealed that the alkyl-ammonium ion successfully intercalated the layer of MMT clay, and thus copolymer poly(vinylidene fluoride-hexafluoropropylene) entered the galleries of montmorillonite clay. Cyclic voltammetry and electrochemical impedance spectroscopy (EIS) were used to investigate the electrochemical properties of the lithium polymer electrolyte. Equivalent circuits were proposed to fit the EIS data successfully, and the significant contribution from MMT was thus identified. The resulting polymer electrolytes show high ionic conductivity up to 10(-3) S cm(-1) after felling with propylene carbonate.

Study on charge transfer reactions at multilayers of polyoxometalates clusters and poly(allylamine hydrochloride) (Grotthuss-018)

Multilayers of anionic phosphotungstic acid (PTA) clusters and positively charged protonated poly(allylamine hydrochloride) (PAH) were assembled by layer-by-layer self-assembled method on Au electrode modified by 3-mercaptopropionic acid (3-MPA). The effect of the charge of the surface of the multilayer assembly on the kinetics of the charge transfer reaction was studied by using the redox probes [Fe(CN)(6)](3-)/(4-) [Ru(NH3)(6)](2+/3+). The cyclic voltammetry experiments showed that the peak currents and peak-to-peak potential differences changed after assembling different layers on the electrode surface indicating that the charge of the surface has a significant effect on the kinetics of the studied charge transfer reactions. These reactions were studied in more detail by electrochemical impedance spectroscopy. When [Fe(CN)(6)](3-/-) was used as the redox label, multilayers that terminated with negatively charged PTA showed a high charge transfer resistance but multilayers that terminated with positively charged PAH showed lower charge transfer resistance. With [Ru(NH3)(6)](2+/3+) as the redox label, the charge transfer resistance at multilayers that terminated with positively charged PAH was much higher than at the multilayer terminated by the negatively charged PTA.

Preparation and layer-by-layer self-assembly of positively charged multiwall carbon nanotubes

The report described a method of more stably dispersing oxidized carbon nanotubes (CNTs) by forming complex with polycation and the layer-by-layer self-assembly behavior of the complex with polyanion was studied. The properties of the self-assembled multilayer film containing carbon nanotubes were studied. Cyclic voltammetry, UV-vis-NIR spectroscopy, electrochemical impedance spectroscopy and scanning electron microscopy were used for characterization of film assembly. UV-vis-NIR spectroscopy and cyclic voltammetry study indicated the uniform growth of the film. Electrochemical impedance spectroscopy results showed that incorporating of carbon nanotubes in the polyelectrolyte multilayers; decreased in the electron-transfer resistance R, indicating more favorable electrochemical reaction interface. The electrocatalytic property of the multilayer modified electrode to NADH was investigated mainly with different numbers of the bilayers; and the results showed that along with the increase of the assembled bilayers the overpotential of NADH oxidation decreased. The detection lit-nit Could reach 6 mu M at a detection potential of 0.4 V.

Copper hexacyanoferrate multilayer films on glassy carbon electrode modified with 4-aminobenzoic acid in aqueous solution

4-Aminobenzoic acid (4-ABA) was covalently grafted on a glassy carbon electrode (GCE) by amine cation radical formation during the electrooxidation process in 0.1 M KCl aqueous Solution. X-ray photoelectron spectroscopy (XPS) measurement proves the presence of 4-carboxylphenylamine on the GCE. Electron transfer processes of Fe(CN)(6)(3-) in solutions of various pHs at the modified electrode are studied by both cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Changing the solution pH would result in the variation of the terminal group's charge state, based on which the surface pK(a) values were estimated. The copper hexacyanoferrate (CuHCF) multilayer films were formed on 4-ABA/GCE prepared in aqueous solution, and which exhibit good electrochemical behavior with high stability.

Layer-by-layer assembly of multilayer films composed of avidin and biotin-labeled antibody for immunosensing

Protein multilayers composed of avidin and biotin-labeled antibody (bio-Ab) were prepared on gold surface by layer-by-layer assembly technology using the high specific binding constant (K-a: approximate to 10(15) M-1) between avidin and biotin. The assembly process of the multilayer films was monitored by using real-time BIA technique based on surface plasmon resonance (SPR). The multilayer films were also characterized by electrochemical impedance spectroscopy (EIS) and reflection absorption Fourier transform infrared spectroscopy (FTIR). The results indicate that the growth of the multilayer is uniform. From response of SPR for each layer, the stoichiometry S for the interaction between avidin and bio-Ab is calculated to be 0.37 in the multilayer whereas 0.82 in the first layer. The protein mass concentration for each layer was also obtained. The schematic figure for the multilayer assembly was proposed according to the layer mass, concentration and S value. The utility of the mutilayer films for immunosensing has been investigated via their subsequent interaction with hIgG. The binding ability of the multilayer increased for one to three layers of antibody, and then reach saturation after the fourth layer. These layer-by-layer constructed antibody multilayers enhance the binding ability than covalently immobilized monolayer antibody. This technology can be also used for construction of other thin films for immunosensing and biosensor.

Chitosan mediated assembly of gold nanoparticles multilayer

We initiate a systematic exploration of a natural polymer, chitosan, as a structural material for designing functional layers on electrode surfaces in this work. Au colloid films are organized on chitosan layer by adsorption. We have successfully constructed a multilayer An nanoparticle assembly through electrostatic interactions on chitosan functionalized quartz substrates by the alternate treatment of the substrate with solution of citrate-stabilized gold nanoparticles (negatively charged) and chitosan solution (positively charged). The resulting substrates were characterized by UV-Vis spectrometry, atomic force microscopy (AFM), and electrochemical impedance spectroscopy (EIS) measurements. These assemblies of colloid An multilayer are highly stable, and can be kept for a long time in distilled water, only being removed by scratching or extreme electrochemical conditions.

Assembly of alternating polycation and DNA multilayer films by electrostatic layer-by-layer adsorption

The assembly of alternating DNA and positively charged poly(dimethyldiallylammonium chloride) (PDDA) multilayer films by electrostatic layer-by-layer adsorption has been studied. The real-time surface plasmon resonance (BIAcore) technique was used to characterize and monitor the formation of multilayer films in solution in real time continuously. Electrochemical impedance spectroscopy (EIS) and UV-vis absorbance measurements were also used to study the film assembly, and linear film growth was observed. All the results indicate that the uniform multilayer can be obtained on the poly(ethylenimine)- (PEI-) coated substrate surface. The kinetics of the adsorption of DNA on PDDA surface was also studied by the real-time BIAcore technique; the observed rate constant was calculated using a Langmuir model (k(obs) = (1.28 +/- 0.08) x 10(-2) s(-1).

Studies on the room temperature conductivity of PEO-LiClO4-Al2O3 composite polymer electrolyte

A composite polymer electrolyte of Polyethylene oxide (PEO)-LiClO4 containing fine Al2O3 particles was studied by using differential scanning calorimetry, infrared spectroscopy and electrochemical impedance spectroscopy. Compared with the polymer electrolyte without Al2O3 particles, the glass transition temperature and the degree of crystallinity were decreased, and the room temperature conductivity of PEO-LiClO4-Al2O3 composite polymer electrolyte was considerably enhanced. Moreover, the equivalent circuits and the effect of dc potential on impedance spectroscopy were discussed.

Formation and characterization of heteropolyacid/polycation multilayer films on gold electrode

Ultrathin multilayer films of a polybasic lanthanide heteropoly tungstate-molybdate complex and a cationic polymer of quaternized poly(4-vinylpyridine) partially complexed with osmium bis(2,2'-bipyridine) have been fabricated on a gold electrode precoated with a cysteamine self-assembled monolayer. The multilayer films have been characterized by optical spectroscopy, small-angle X-ray diffraction, and electrochemical methods (cyclic voltammetry and electrochemical impedance). Especially, the electrochemical impedance spectroscopy is developed to monitor the layer deposition processes. It provides important information such as double-layer capacitance and charge-transfer resistance. All obtained results reveal regular film growth with each layer adsorption. (C) 2001 The Electrochemical Society.

Formation of self-assembled monolayers on gold electrodes with inclusion complexes of cyclodextrins and viologens

A novel kind of electroactive self-assembled monolayer (SAM) has been successfully prepared through the following procedure: (1) formation of inclusion complexes (denoted as CD/C8VC10SH) between N-(n-octyl)-N'-(10-mercaptodecyl)-4,4'-bipyridinium dibromide (C8VC10SH) and alpha-, beta-cyclodextrin (CD) under a mild condition; (2) spontaneous formation of SAM of CD/C8VC10SH on gold electrodes at room temperature. High-resolution H-1-NMR spectrum was used to confirm the formation of CD/C8VC10SH. Cyclic voltammetry was used to characterize the redox behavior of the resulting monolayers and chronoamperometry and electrochemical impedance spectroscopy to characterize their electron transfer kinetics. It was found that the redox sites in SAM of CD/C8VC10SH are effectively diluted, with a larger electron transfer rate constant than that of SAM of C8VC10SH.

Monitoring microbial populations of sulfate-reducing bacteria using an impedimetric immunosensor based on agglutination assay

An impedimetric immunosensor was fabricated for rapid and non-labeled detection of sulfate-reducing bacteria, Desulforibrio caledoiensis (SRB) by immobilizing lectin-Concanavalin A using an agglutination assay. The immobilization of lectin was conducted using amine coupling on the surface of a gold (Au) electrode assembled with 11-Mercaptounclecanoic acid. Electrochemical impedance spectroscopy (EIS) was used to verify the stepwise assembly of the sensor system. The work conditions of the impedimetric immunosensor, such as pH of the buffer solutions and the incubation time of lectin, were optimized. Faradic impedance spectra for charge transfer for the redox probe Fe(CN)(6)(3-/4-) were measured to determine SRB concentrations. The diameter of the Nyquist diagram that is equal to the charge-transfer resistance (RI) increased with increasing SRB concentration. A linear relationship between R-ct and SRB concentration was obtained in SRB concentration range of 1.8 to 1.8 x 10(7) cfu/ml. The variation of the SRB population during the growth process was also monitored using the impedimetric immunosensor. This approach has great potential for simple, low-cost. and time-saving monitoring of microbial populations. (C) 2009 Elsevier B.V. All rights reserved.

Characteristics of anodic coatings oxidized to different voltage on AZ91D Mg alloy by micro-arc oxidization technique

With increasing applied voltage, three types of anodic coatings, passive film, micro-spark ceramic coating and spark ceramic coating were made by micro-arc oxidization (MAO) technique on AZ91D magnesium alloy in alkali-silicate solution. The structure, composition characteristics and the electrochemical properties of coatings were also studied with SEM, XRD and EIS (electrochemical impedance spectroscopy) technique, respectively. It is found that the electrochemical properties are closely related to the structure and composition characteristics of the anodic coatings. At the same time, the characteristics of the three types of anodic coatings differ significantly, among them, the micro-spark ceramic coating, prepared in the voltage range of 170similar to220V exhibits compact, homogeneous structure and highest corrosion-resistance.

The inhibition of mild steel corrosion in 1 M hydrochloric acid solutions by triazole derivative

The title compound 1-(4,5-dihydro-3-phenylpyridine-1-yl)-2-(1H-1,2,4-triazole-1-yl)ethyl ketone (DTE) was synthesized and its inhibiting action on the corrosion of mild steel in 1 M hydrochloric acid solutions was investigated by means of weight loss, potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) and scanning electronic microscope (SEM). Results obtained revealed that DIE performed excellently as a corrosion inhibitor for mild steel in 1 M hydrochloric acid media and its efficiency attains more than 90.9% at 1.0 x 10(-3) M at 298 K. Polarization curves indicated that the inhibitor behave mainly as mixed-type inhibitor. EIS showed that the charge transfer controls the corrosion process in the uninhibited and inhibited solutions. Adsorption of the inhibitor on the mild steel surface followed Langmuir adsorption isotherm. And the values of the free energy of adsorption Delta G(ads) indicated that the adsorption of DTE molecule was a spontaneous process and was typical of chemisorption. (c) 2008 Elsevier B.V. All rights reserved.

Some new triazole derivatives as inhibitors for mild steel corrosion in acidic medium

Two triazole derivatives, 3,4-dichloro-acetophenone-O-1'-(1',3',4'-triazolyl)-methaneoxime (4-DTM) and 2,5-dichloro-acetophenone-O-1'-(1',3',4'-triazolyl)-methaneoxime (5-DTM) were synthesized, and the inhibition effects for mild steel in 1 M HCl solutions were investigated by weight loss measurements, electrochemical tests and scanning electronic microscopy (SEM). The weight loss measurements showed that these compounds have excellent inhibiting effect at a concentration of 1.0 x 10(-3) M. The potentiodynamic polarization experiment revealed that the triazole derivatives are inhibitors of mixed-type and electrochemical impedance spectroscopy (EIS) confirmed that changes in the impedance parameters (R-ct and C-dl) are due to surface adsorption. The inhibition efficiencies obtained from weight loss measurements and electrochemical tests were in good agreement. Adsorption followed the Langmuir isotherm with negative values of the free energy of adsorption Delta G(ads)(o). The thermodynamic parameters of adsorption were determined and are discussed. Results show that both 4-DTM and 5-DTM are good inhibitors for mild steel in acid media.

Effect of nano-TiO(2)on MP-25 resin

MP-25 resin is a chlorine-containing polymer widely used in coatings. The effects of two types of nano-TiO2 (P-25 and RM301 LP) on MP-25 were studied with saline immersion, UV irradiation, and electrochemical impedance spectroscopy. UV irradiation was evaluated in terms of gloss change and X-ray photoelectron spectroscopy (XPS). The results indicate that, compared to pigment R-930 TiO2, P-25 reduced the immersion resistance and accelerated UV aging of the MP-25 coating, whereas RM301 LP showed the opposite effects. XPS analysis showed that MP-25 resin degraded under UV irradiation via dechlorination and C-C bond breakage, similarly to poly(vinyl chloride), but RM301 LP could inhibit the aging of MP-25 to a certain extent. A skin effect of oxygen and chlorine was identified in MP-25 resin by XPS. RM301 LP could improve the impedance of the MP-25 coating because of its excellent fill capacity. Hence, rutile nano-TiO2 RM301 LP represents an excellent additive for MP-25 resin. (c) 2007 Wiley Periodicals, Inc.