In situ characterization of localized corrosion of stainless steel by scanning electrochemical microscope

Scanning electrochemical microscopy (SECM) area scan measurements have been performed to investigate the localized corrosion of type 304 stainless steel in neutral chloride solution. Variations in the Faradaic current measured at selected tip potential values can be related to changes in the local concentration and electrochemical activities of electroactive species involved in corrosion reactions occurring at the substrate as a function of immersion times of the substrate and polarized currents or potentials applied on the substrate. To further verify the results acquired from cyclic voltammetric experiments, SECM measurements were employed to in situ study the compositions and electrochemical activity distribution profile of the pitting corrosion products of stainless steel. It has been demonstrated that the combination of feedback current mode with generation-collection (G-C) mode of SECM is suitable to elucidate the possible reaction mechanisms and paths involved in the localize corrosion of stainless steel in neutral chloride solution.     

Preparation and electrochemical properties of LiFePO<Subscript>4</Subscript>/graphene composites from tailoring graphene oxides

LiFePO₄/graphene composites have been prepared by using tailoring graphene oxide (GO) nanosheets as precursors. The structure and electrochemical properties of the composites were investigated by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), Raman microscopy, and a variety of electrochemical testing techniques. The decrease in graphene size reduces the contact resistance between activated materials, and enhances the lithium-ion transport in LiFePO₄/graphene composites. With low weight fractions of small-size graphene sheets, the composites show better electrochemical performance than those with large size graphene sheets.     

An L‐shaped nanoprobe for scanning electrochemical microscopy–atomic force microscopy

We present an L‐shaped nanoprobe for scanning electrochemical microscopy–atomic force microscopy (SECM–AFM) capable of imaging the surface topography and the electrochemical activity of nanostructures of interest. Owing to the geometry of the protrusive peak in the L‐shaped probe, the distance between the probe electrode and the substrate is maintained precisely at ～100 nm during surface scanning. The reduction in electrode‐to‐substrate distance significantly improves the positive feedback current on top of the electrochemically active nanomaterials. The L‐shaped nanoprobe successfully acquired simultaneous a topographical image and an electrochemical current image of individual carbon nanotubes (CNTs) in a two‐dimensional (2D) CNT network.

     

Chemical, electrical and electrochemical characterization of hybrid organic/inorganic polypyrrole/PW12O40 coating deposited on polyester fabrics

A study of the stability of conducting fabrics of polyester (PES) coated with polypyrrole/PW₁₂O₄₀³⁻ (organic/inorganic hybrid material) in different pH solutions (1, 7, 13) has been done. Washing tests were also done in views of its possible application in electronic textiles such as antistatic clothing. X-ray photoelectron spectroscopy (XPS) studies have been done to quantify the amount of counter ion that remains in the polymer matrix and determine the doping ratio (N⁺/N) after the different tests. Scanning electron microscopy (SEM) was also used to observe morphological differences after the different tests. Surface resistivity changes were measured by means of electrochemical impedance spectroscopy (EIS). Scanning electrochemical microscopy (SECM) was employed to measure changes in electroactivity after the different tests. Higher pHs caused a decrease of the doping ratio (N⁺/N), the loss of part of the counter ions and the decrease of its conducting and electrocatalytic properties. The stability in acid media and neutral media and after the washing test was good. Only at pH 13 the loss of the counter ion was widespread and there was a decrease of its conducting and catalytic properties; although the fabrics continued acting mainly as a conducting material.     

Dynamics of individual atomic kinks during crystal dissolution

The dynamics of kink motion via atom removal/deposition as a fundamental step in dissolution/crystallization of solids have become directly accessible by a novel scanning tunneling microscopy technique. Results obtained for the electrochemical dissolution of Cu(100) in HCl solution show pronounced local dissolution/redeposition fluctuations at the individual kinks even at the onset of Cu dissolution with average kink propagation and reaction rates in the range 10(3) and 10(5) atoms s(-1), respectively. These experiments allow one to directly measure the central kinetic properties of this electrochemical reaction.     

Decorating graphene sheets with Pt nanoparticles using sodium citrate as reductant

In this paper, we proposed a novel and green approach for the synthesis of graphene nanosheets (GNS) and Pt nanoparticles-graphene nanosheets (Pt/GNS) hybrid materials, employing graphene oxide (GO) as precursor and sodium citrate as environmentally friendly reducing and stabilizing agent. The microstructures of GO and Pt/GNS were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), Raman spectroscopy, atomic force microscopy (AFM), X-ray diffraction (XRD) and electrochemical measurements. The results confirmed that the uniform size distribution of Pt nanoparticles on the surface of GNS without agglomerates could be easily obtained via using sodium citrate as reductant, moreover the Pt/GNS hybrids exhibited high electrochemical activity.     

变压加载对直接甲醇燃料电池阳极性能的影响（英）

为评价直接甲醇燃料电池（DMFC）阳极的稳定性,利用扫描电化学显微镜和常规电化学技术,研究了变压加载过程中DMFC阳极性能的变化。结果表明,在探针扫描过程中,经不同电压加载后的DMFC阳极表面的扫描电流呈相似的锯齿状分布。当阳极加载2 h,随加载电位升高,扫描峰电流的数量减少,对应峰电流的数值则先增大再减小,表明阳极的催化活性处于不均匀分布状态且随加载时间延长和加载电位升高而逐渐降低。在不同加载电位下,随加载时间延长,循环伏安曲线上的正向和反向电流峰先负移再正移,但抗CO性能持续降低。DMFC阳极在0.6 V下分别加载16 h和72 h后,催化剂粒径由3.4 nm分别增大到3.6 nm和4.4 nm。在0.8 V下加载72 h后,Pt/Ru重量比由2.0增加到3.9。变压加载使催化活性的不均匀分布加剧催化剂粒径长大,Ru流失加快,从而导致阳极催化性能衰减。     

Scanning probe microscopy characterization of gold-chemisorbed poplar plastocyanin mutants

Two poplar plastocyanin mutants adsorbed onto gold electrodes have been characterized at single molecule level by scanning probe microscopy. Immobilization of the two redox metalloprotein mutants on Au(1 1 1) surface was achieved by either a disulphide bridge (PCSS) or a single thiol (PCSH), both the anchoring groups having been introduced by site-directed mutagenesis. Scanning tunneling microscopy (STM) and atomic force microscopy (AFM) analysis gives evidence of a stable and robust binding of both mutants to gold. The lateral dimensions, as estimated by STM, and the height above the gold substrate, as evaluated by AFM, of the two mutants well agree with crystallographic sizes. A narrower height distribution is observed for PCSS compared to PCSH, corresponding to a more homogeneous orientation of the former mutant adsorbed onto gold. Major differences between the mutants are observed by electrochemical STM. In particular, the image contrast of adsorbed PCSS is affected by tuning the external electrochemical potential to the redox levels of the mutant, consistent with some involvement of copper active site in the tunneling process. On the contrary, no contrast variation is observed in electrochemical STM of adsorbed PCSH. Moreover, scanning tunneling spectroscopy experiments reveal asymmetric I–V characteristics for single PCSS proteins, reminiscent of a rectifying-like behaviour, whereas an almost symmetric I–V relation is observed for PCSH.     

Preparation and physical/electrochemical characterization of carbon nanotube-chitosan modified pencil graphite electrode

In this work, preparation and characterization of single-walled carbon nanotube-chitosan (SWNT-chitosan) modified disposable pencil graphite electrode (PGE) was carried out. Firstly, commercial single-walled carbon nanotube was purified and characterized using thermal gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersive analysis of X-ray (EDX) for this purpose. Purified SWNT was mixed with chitosan polymer for preparing their composite. Then, PGE was modified with this composite. The characterization of the modified electrode was carried out using atomic force microscopy (AFM). The electrochemical behaviour of the obtained electrode was investigated and compared with the electrochemical behaviour of chitosan modified and unmodified PGEs using cyclic voltammetry (CV), differential pulse voltammetry (DPV) and alternative current (AC) impedance spectroscopy. In order to obtain more sensitive electrochemical signals, the effect of SWNT concentration was studied. This modified electrode also showed electrocatalytic effect for hydrogen evolution.     

The adsorption behavior and corrosion inhibition mechanism of anionic inhibitor on galvanic electrode in 1% NaCl solution

The adsorption behavior of dodecanoic acid and its sodium salt (DDAS) as an anionic inhibitor on the galvanic electrode has been investigated by using electrochemical methods, Fourier transform infrared spectroscopy (FT-IR), and atomic force microscopy (AFM). The galvanic electrode was prepared by coupling N80 carbon steel (CS) and S31803 stainless steel (SS), and all experiments were performed in NaCl solution at pH 4 in the presence or absence of DDAS. Electrochemical experiments reveal SS and CS carry positive and negative excess charges in NaCl solution at pH 4, and DDAS is mainly anodic type inhibitor for the galvanic corrosion. FT-IR and AFM were used to analyze the protective layer formed on the electrodes, a stronger adsorbability of the inhibitor on the anode (CS) of GE was measured. Results indicate the protective layer formed on the single CS electrode is less compact than which on the coupled CS. The adsorption regulation of anionic inhibitor on the galvanic electrode is summarized based on the results obtained from electrochemical methods, FT-IR and AFM.     

Effects of water plasma immersion ion implantation on surface electrochemical behavior of NiTi shape memory alloys in simulated body fluids

Water plasma immersion ion implantation (PIII) was conducted on orthopedic NiTi shape memory alloy to enhance the surface electrochemical characteristics. The surface composition of the NiTi alloy before and after H₂O-PIII was determined by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) was utilized to determine the roughness and morphology of the NiTi samples. Potentiodynamic polarization tests and electrochemical impedance spectroscopy (EIS) were carried out to investigate the surface electrochemical behavior of the control and H₂O-PIII NiTi samples in simulated body fluids (SBF) at 37 °C as well as the mechanism. The H₂O-PIII NiTi sample showed a higher breakdown potential (E_b) than the control sample. Based on the AFM results, two different physical models with related equivalent electrical circuits were obtained to fit the EIS data and explain the surface electrochemical behavior of NiTi in SBF. The simulation results demonstrate that the higher resistance of the oxide layer produced by H₂O-PIII is primarily responsible for the improvement in the surface corrosion resistance.     

Electrochemical deposition of cerium on porous silicon to improve photoluminescence properties

In this work, we present results for Cerium (Ce) doping effects on photoluminescence (PL) properties of porous silicon (PS). Cerium was deposited using electrochemical deposition on porous silicon prepared by electrochemical anodization of P-type (100) Si. From the photoluminescence spectroscopy, it was shown that porous silicon treated with cerium can lead to an increase of photoluminescence when they are irradiated by light compared to the porous silicon layer without cerium. In order to understand the contribution of cerium to the enhanced photoluminescence, energy dispersive X-ray (EDX) spectroscopy, Fourier transmission infrared spectroscopy (FTIR), X-ray diffraction (XRD) and atomic force microscopy (AFM) were performed, and it was shown that the improved photoluminescence may be attributed to the change of Si–H bonds into Si–O–Ce bonds and to a newly formed PS layer during electrochemical Ce coating.     

腐蚀时间对蓝宝石衬底上外延生长GaN质量的影响

使用熔融的KOH在高温下对c面蓝宝石衬底进行不同时间的腐蚀,借助扫描电镜、原子力显微镜对衬底表面进行了表征,然后利用金属有机物化学气相沉积设备在不同腐蚀时间的衬底样品上进行了GaN材料的外延生长。通过X射线衍射结果比较了两组衬底上外延材料的质量,利用原子力显微镜结果对外延层表面形貌进行了分析,最后论述了腐蚀时间的调整对蓝宝石衬底上外延生长氮化镓质量的影响机理。     

Fabrication of patterned polyaniline microstructure through microcontact printing and electrochemistry

Polyaniline (PANI) microstructures on ITO glass surface were achieved by microcontact printing of self-assembled film and electrochemical polymerization in an aqueous monoaniline solution. The patterned microstructures of PANI were easily transferred to an adhesive tape surface, which could be applied in the area of plastic circuit application. Optical microscope, atomic force microscopy (AFM), lateral force microscopy (LFM) and X-ray photoelectron spectroscopy (XPS) were used to examine the topography and properties of patterned PANI films. Optical microscope and AFM results showed that the PANI microstructure has regular pattern and clear boundary, while LFM and XPS results implied that this microstructure was completely covered by PANI. The data suggested that the interfacial properties of the surface control the rate of electrochemical polymerization, and the polymerization rate on the modified ITO surface is higher than that on the bare ITO area. In our experiments, cyclic voltammetric method, potentiostatic method and chronopotentiometry method were employed to deposited patterned PANI films on octadecyltrichorosilane modified ITO substrate.     

Monitoring the effect of sonoporation on the cells using electrochemical approach

Sonoporation is applied to enhance the permeability of the cell to bioactive materials by employing the acoustic cavitation of microbubbles. This phenomena would be helpful in molecular biology, delivery of large molecules into the cells and gene therapy. Many methods have been applied to monitor the biological effects and trace of sonoporation on the cells such as scanning/transmission electron microscopy, confocal imaging and flow cytometry. Here, we monitored the effect of sonoporation on the cells using electrochemical method with an integrated three electrode system. Electrochemical responses of stimulated cells, compared to flow cytometry and electron microscopy results, presented different patterns of sonoporation in the cells detectable by cyclic voltammetry. In addition, confocal microscopy from actin stress fibers and young’s modulus measured by AFM revealed the correlation of cell mechanics and amount of induced sonopores in the cells. This method could be applied as a new trend in cellular mechanochemical studies.     

NPB表面形貌对OLED光电特性的影响

用原子力显微镜观察了沉积在不同温度基板上NPB表面形貌,发现NPB薄膜在室温下比较平坦的点状结构变为100℃时直径为0.2μm的岛状结构。为研究NPB表面形貌对OLED器件性能的影响,设计了结构为玻璃/ITO/NPB/Alq3/Al器件,比较了不同基板温度沉积的NPB薄膜对器件性能的影响。     

Physical and electrochemical study of platinum thin films deposited by sputtering and electrochemical methods

In this work platinum thin films deposited by sputtering and electrochemical methods were characterized through physical and electrochemical analysis. The as-grown platinum thin films were characterized through X-ray diffraction (XRD), atomic force microscopy (AFM); scanning electronic microscopy (SEM) and through electrochemical impedance spectroscopy (EIS) measurements. Structural studies indicated that platinum thin films were polycrystalline. Morphological characteristics were significantly affected by the substrate type and synthesis method. Finally the EIS analysis indicated that platinum films were electrochemically stable and present both low resistance of charge transfer and low series resistance; the equivalent circuit of platinum interface has been proposed.     

Surface analysis of thermally annealed porous silicon

Quasi-monocrystalline porous silicon (QMPS) has high potential for photovoltaic application for its enhanced optical absorption compared to bulk silicon in the visible range of solar spectrum. In this study, QMPS was formed from low porosity (∼20-30%) porous silicon (PS) produced by electrochemical anodization, and thermal annealing in the temperature range 1050-1100 °C under pure hydrogen ambient for a duration of 30 min. We analyzed the material surface by grazing incidence X-ray diffraction (GIXRD), field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM) and dynamic secondary ion mass spectroscopy (SIMS) study. The crystallinity was confirmed by GIXRD while FESEM studies revealed that the surface layer is pore free with voids embedded inside the body. AFM studies indicated relatively smooth and uniform surface and the dynamic SIMS study showed the depth profiles of impurities present in the material.     

Roughness evolution of highly ordered nanoporous anodic aluminum oxide films

In this paper, we report on the surface roughness evolution of highly ordered anodic aluminum oxide (AAO) films based on an atomic force microscopy (AFM) study. Root mean square of the surface roughness was measured on AFM images taken from highly ordered AAO films produced by two-step anodization under different conditions including electrolyte type, anodization voltage, and anodization time. Surface roughness of highly ordered AAO films increases step by step through the two-step anodizing process including electropolishing, first-step anodization, dissolution, and second-step anodization. However, increase of the surface roughness is proportional to the anodization voltage and time. The surface roughness of AAO films changes as a function of length scale until it finally approaches a maximum termed the saturation roughness. The variation of roughness of the growth of AAO could be scaled with an anomalous dynamic behavior as it saturates over a critical length scale while the saturation roughness is dependent on the anodizing time and voltage.     

Cross-linked gelatin/nanoparticles composite coating on micro-arc oxidation film for corrosion and drug release

A composite coating which could control drug release and biocorrosion of magnesium alloy stent materials WE42 was prepared. This composite coating was fabricated on the surface of the micro-arc oxidation (MAO) film of the magnesium alloy, WE42, by mixing different degrees of cross-linked gelatin with well-dispersed poly(dl-lactide-co-glycolide) (PLGA) nanoparticles. The PLGA nanoparticles were prepared by emulsion solvent evaporation/extraction technique. Nano ZS laser diffraction particle size analyzer detected that the size of the nanoparticles to be 150-300 nm. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) was used to analyze the morphology of the nanoparticles and the composite coating. Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) were used to evaluate the corrosion behavior of the composite coating. Drug release was determined by ultraviolet-visible (UV-vis) spectrophotometer. The corrosion resistance of the composite coating was improved by preventing the corrosive ions from diffusing to the MAO films. The drug release rate of paclitaxel (PTX) exhibited a nearly linear sustained-release profile with no significant burst releases.