943 resultados para Electrochemical impedance spectroscopy techniques


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TiO2 sol-gels with various Ag/TiO2 molar ratios from 0 to 0.9% were used to fabricate silver-modified nano-structured TiO2 thin films using a layer-by-layer dip-coating (LLDC) technique. This technique allows obtaining TiO2 nano-structured thin films with a silver hierarchical configuration. The coating of pure TiO2 sol-gel and Ag-modified sol-gel was marked as T and A, respectively. According to the coating order and the nature of the TiO2 sol-gel, four types of the TiO2 thin films were constructed, and marked as AT (bottom layer was Ag modified, surface layer was pure TiO,), TA (bottom layer was pure TiO,, surface layer was Ag modified), TT (pure TiO, thin film) and AA (TiO, thin film was uniformly Ag modified). These thin films were characterized by means of linear sweep voltammetry (LSV), X-ray diffraction (XRD), scanning electron microscopy (SEM), electrochemical impedance spectroscopy and transient photocurrent (I-ph). LSV confirmed the existence of Ago state in the TiO, thin film. SEM and XRD experiments indicated that the sizes of the TiO,, nanoparticles of the resulting films were in the order of TT > AT > TA > AA, suggesting the gradient Ag distribution in the films. The SEM and XRD results also confirmed that Ag had an inhibition effect on the size growth of anatase nanoparticles. Photocatalytic activities of the resulting thin films were also evaluated in the photocatalytic degradation process of methyl orange. The preliminary results demonstrated the sequence of the photocatalytic activity of the resulting films was AT > TA > AA > TT. This suggested that the silver hierarchical configuration can be used to improve the photocatalytic activity of TiO2 thin film.

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Palladium nanoparticle-loaded carbon nanofibers (Pd/CNFs) were synthesized by the combination of electrospinning and thermal treatment processes. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images show that spherical Pd nanoparticles (NPs) are well-dispersed on the surfaces of CNFs or embedded in CNFs. X-ray diffraction (XRD) pattern indicates that cubic phase of Pd was formed during the reduction and carbonization processes, and the presence of Pd NPs promoted the graphitization of CNFs. This nanocomposite material exhibited high electric conductivity and accelerated the electron transfer, as verified by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV).

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A novel electrochemiluminescence (ECL) aptasensor was proposed for sensitive and cost-effective detection of the target thrombin adopted an aptamer-based sandwich format. To detect thrombin, capture aptamers; labeled with gold nanoparticles (AuNPs) were first immobilized onto the thio-silanized ITO electrode surface through strong Au-S bonds. After catching the target thrombin, signal aptamers; tagged with ECL labels were attached to the assembled electrode surface. As a result, an AuNPs-capture-aptamer/thrombin/ECL-tagged signal-aptamer sandwich type was formed.

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A facile phospholipid/room-temperature ionic liquid (RTIL) composite material based on dimyristoylphosphatidylcholine (DMPC) and 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim]PF6) was exploited as a new matrix for immobilizing protein. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were adopted to characterize this composite film. Hemoglobin (Hb) was chosen as a model protein to investigate the composite system. UV-vis absorbance spectra showed that Hb still maintained its heme crevice integrity in this composite film.

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Horseradish peroxidase (HRP) was incorporated into multiwalled carbon nanotube/thionine/Au (MTAu) composite film by electrostatic interactions between positively charged HRP and negatively charged MTAu composite. The results of electrochemical impedance spectroscopy (EIS) confirmed adsorption of HRP on the surface of MTAu modified GC electrode.

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A label-free and highly sensitive impedimetric aptasensor based on a polyamidoamine dendrimer modified gold electrode was developed for the determination of thrombin. Amino-terminated polyamidoamine dendrimer was firstly covalently attached to the cysteine functionalized gold electrode through glutaraldehyde coupling. Subsequently, the dendrimer was activated with glutaraldehyde, and amino-modified thrombin aptamer probe was immobilized onto the activated dendrimer monolayer film. The layer-by-layer assembly process was traced by surface plasmon resonance and electrochemical impedance spectroscopy.

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A novel [Ru(bpy)(2) (dcbpy)NHS] labeling/aptamer-based biosensor combined with gold nanoparticle amplification for the determination of lysozyme with an electrochemiluminescence (ECL) method is presented. In this work, an aptamer, an ECL probe, gold nanoparticle amplification, and competition assay are the main protocols employed in ECL detection. With all the protocols used, an original biosensor coupled with an aptamer and [Ru(bpy)(2)(dcbpy)NHS] has been prepared. Its high selectivity and sensitivity are the main advantages over other traditional [Ru(bpy)(3)](2+) biosensors. The electrochemical impedance spectroscopy (EIS) and atomic force microscopy (AFM) characterization illustrate that this biosensor is fabricated successfully. Finally, the biosensor was applied to a displacement assay in different concentrations of lysozyme solution, and an ultrasensitive ECL signal was obtained. The ECL intensity decreased proportionally to the lysozyme concentration over the range 1.0 x 10-(13)-1.0 x 10(-8) mol L-1 with a detection limit of 1.0 x 10(-13) mol L-1.

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Ce6-xDyxMoO15-delta (0.0 <= x <= 1.8) were synthesized by modified sol-gel method. Structural and electrical properties were investigated by means of X-ray diffraction (XRD), Raman, X-ray photoelectron spectroscopy (XPS) and electrochemical impedance spectroscopy (EIS). The XRD patterns showed that the materials were single phase with a cubic fluorite structure. Impedance spectroscopy measurement in the temperature range between 350 degrees C and 800 degrees C indicated a sharp increase in conductivity for the system containing small amount of Dy2O3. The Ce5.6Dy0.4MoO15-delta detected to be the best conducting phase with the highest conductivity (sigma(t) = 8.93 x 10(-3) S cm(-1)) is higher than that of Ce5.6Sm0.4MoO15-delta (sigma(t) = 2.93 x 10(-3) S cm(-1)) at 800 degrees C, and the corresponding activation energy of Ce5.6Dy0.4MoO15-delta (0.994 eV) is lower than that of Ce5.6Sm0.4MoO15-delta (1.002 eV).

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The composite film based on Nafion and hydrophobic room-temperature ionic liquid (RTIL) 1-butyl-3-methyl-imidazolium hexafluorophosphate ([bmim] PF6) was explored. Here, Nafion was used as a binder to form Nafion-ionic liquids composite film and help [bmim] PF6 effectively adhered on glassy carbon (GC) electrode. X-ray photoelectron spectroscopy (XPS), cyclic voltammtery (CV) and electrochemical impedance spectroscopy (EIS) were used to characterize this composite film, showing that the composite film can effectively adhere on the GC electrode surface through Nafion interacting with [bmim] PF6 and GC electrode. Meanwhile, doping [bmim] PF6 in Nafion can also effectively reduce the electron transfer resistance of Nafion. The composite film can be readily used as an immobilization matrix to entrap horseradish peroxidase (HRP). A pair of well-defined redox peaks of HRP was obtained at the HRP/Nafion[bmim] PF6 composite film-modified GC electrode through direct electron transfer between the protein and the underlying electrode. HRP can still retain its biological activity and enhance electrochemical reduction towards O-2 and H2O2. It is expected that this composite film may find more potential applications in biosensors and biocatalysis.

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A more stably dispersing of multi-wall carbon nanotube composite (noted as PDDA-MWNT), which was obtained by wrapping the MWNT with poly (diallydimethylammonium) chloride (PDDA), was used for the immobilization of glucose oxidase (GOD) and its bioelectrochemical studies. The morphologies and structures of the PDDA-MWNT composite were characterized by environment-canning electron microscopy (ESEM) and X-ray photoelectron spectroscopy (XPS). Electrochemical impedance spectroscopy (EIS) and cyclic voltammetry were used to feature the GOD adsorbed onto the electrode modified by PDDA-MWNT composite. The immobilized GOD at the PDDA-MWNT films exhibited a pair of well-defined nearly reversible redox peaks and a fast heterogeneous electron transfer rate with the rate constant (k(s)) of 2.76 s(-1). In addition, GOD immobilized in this way retained its bioelectrocatalytic activity for the oxidation of glucose. The method of immobilizing GOD without any additional cross-linking agents presented here is easy and facile, which provides a model for other redox enzymes and proteins.

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A method for preparing nanoelectrode ensembles based on semi-interpenetrating network (SIN) of multi-walled carbon nanotubes (MWNTs) on gold electrode through phase-separation method is initially proposed. Individual nanoelectrode owns irregular three-dimensional MWNTs networks, which is denoted as SIN-MWNTs. On the as-prepared SIN-MWNTs nanoelectrode ensembles, the assembled MWNTs clusters in nanoscale serve as individual nanoelectrode and the electroinactive lipid networks located on the top of alkanethiol monolayer are used as a shielding layer. Cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), tapping-mode atomic force microscopy (TM-AFM) and scanning electron microscopy (SEM) were used to characterize the as-prepared SIN-MWNT nanoelectrode ensembles. Experimental results indicate that the well-defined nanoelectrode ensembles were prepared through self-assembly technology. Meantime, sigmoid curves in a wide scanning range can be obtained in CV experiments. This study may pave the way for the construction of truly nanoscopic nanoelectrode arrays by bottom-up strategy.

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Anticorrosion performances of polyaniline emeraldine base/epoxy resin (EB/ER) coating on mild steel in 3.5% NaCl solutions of various pH values were investigated by electrochemical impedance spectroscopy (EIS) for 150 days. In neutral solution (pH 6.1), EB/ER coating offered very efficient corrosion protection with respect to pure ER coating, especially when EB content was 5-10%. The impedance at 0.1 Hz of the coating increased in the first 1-40 immersion days and then remained constant above 10(9) Omega cm(2) until 150 days, which in combination with the observation of a Fe2O3/Fe3O4 passive film formed on steel confirmed that the protection of EB was mainly anodic. In acidic or basic solution (pH 1 or 13), EB/ER coating also performed much better than pure ER coating. However, these media weakened the corrosion resistance due to breakdown of the passive film or deterioration of the ER binder.

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Polyaniline emeraldine base/epoxy resin (EB/ER) coating was investigated for corrosion protection of mild steel coupled with copper in 3.5% NaCl solution. EB/ER coating with 5-10 wt% EB had long-term corrosion resistance on both uncoupled steel and copper due to the passivation effect of EB on the metal surfaces. During the 150 immersion days, the impedance at 0.1 Hz for the coating increased in the first 1-40 days and subsequently remained constant above 10(9) Omega cm(2), whereas that for pure ER coating fell below 10(6) Omega cm(2) after only 30 or 40 days. Immersion tests on coated steel-copper galvanic couple showed that EB/ER coating offered 100 times more protection than ER coating against steel dissolution and coating delamination on copper, which was mainly attributed to the passive metal oxide films formed by EB blocking both the anodic and cathodic reactions. Salt spray tests showed that 100 mu m EB/ER coating protected steel-copper couple for at least 2000 h.

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Solid solutions of Ce1-xNdxO2-x/2 (0.05 <= x <= 0.2) and (Ce1-xNdx)(0.95)MO0.05O2-delta (0.05 <= x <= 0.2) have been synthesized by a modified sol-gel method. Both materials have very low content of SiO2 (similar to 27 ppm). Their structures and ionic conductivities were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and electrochemical impedance spectroscopy (M). The XRD patterns indicate that these materials are single phases with a cubic fluorite structure. The powders calcined at 300 degrees C with a crystal size of 5.7 nm have good sinterability, and the relative density could reach above 96% after being sintered at 1450 degrees C. With the addition Of MoO3, the sintering temperature could be decreased to 1250 degrees C. Impedance spectroscopy measurement in the temperature range of 250-800 degrees C indicates that a sharp increase of conductivity is observed when a small amount of Nd2O3 is added into ceria, of which Ce0.85Nd0.15O1.925 (15NDC) shows the highest conductivity. With the addition of a small amount Of MoO3, the grain boundary conductivity of 15NDC at 600 degrees C increases from 2.56 S m(-1) to 5.62 S m(-1).

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In an attempt to increase the interface stability of carbon used in Li-ion batteries, a thin conducting polyaniline (PANI) film was fabricated on the surface of carbon by in situ chemical polymerization. The chemical and electrochemical properties of the composite material were characterized using X-ray diffraction, Raman spectroscopy, scanning electron microscope, cyclic voltammetry, and electrochemical impedance spectroscopy. It was confirmed that the PANI film has an obvious effect on the morphology and the electrochemical performance of carbon. The results could be attributed to the electronic and electrochemical activity of the conducting PANI films.