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双恒电位仪Bistat和旋转盘环电极RRDE最佳配置

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进行燃料电池催化剂研究的仪器配置方案,荷兰IVIUM双恒电位仪Vertex.C.EIS和旋转还盘电极装置IVI.RRDE

2

IVIUM 旋转圆盘/盘环电极 RRDE

IVIUM RDE/RRDE

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Nanoparticle–Nanorod Core–Shell LiNi0.5Mn1.5O4 Spinel Cathodes with High Energy Density for Li-Ion Batteries

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研究领域:锂离子电池电极材料 交流阻抗频率范围:500kHz - 0.01Hz Nanoparticle–nanorod core–shell LiNi0.5Mn1.5O4 spinel cathodes for Li-ion batteries were prepared using a hollow MnO2 precursor. The core and shell parts consisted of nanoparticle 100 nm and nanorod assemblies, respectively. The core–shell cathode exhibited greatly improved discharge capacities compared to nanoparticles prepared by a sol–gel method. The core–shell spinel exhibited discharge capacities of 121 and 100 mAh/g at 0.1C and 7C rates, respectively, whereas a spinel cathode prepared by a sol–gel method exhibited 99 and 80 mAh/g at those respective rates. In addition, the core–shell spinels demonstrated an energy density value that was enhanced by 52% to 1.6 Wh/cm3 compared to an analogous sample prepared by a sol–gel method, which showed a value of 0.9 Wh/cm3.

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Electrochemical Titanium Diboride TiB2 Synthesis from Fluoride Melts

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Electrochemical Titanium Diboride TiB2 Synthesis from Fluoride Melts 研究领域:熔盐电解质 测量方法:循环伏安

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Significant Improvement of LiNi0.8Co0.15Al0.05O2 Cathodes at 60°C by SiO2 Dry Coating for Li-Ion Batteries

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研究领域:锂离子电池电极材料 交流阻抗频率范围:5000Hz - 0.1Hz The cycling performance of a LiNi0.8Co0.15Al0.05O2 cathode at 60°C was substantially improved by direct SiO2 dry coating. The SiO2-coated cathode was obtained from firing of the mixture consisting of SiO2 nanoparticles and the cathode powders with a weight ratio of 99:1 at 700°C for 5 h. The first discharge capacity of the coated cathode was 172 mAh/g, whereas the uncoated one showed 182 mAh/g at 60°C. However, the coulombic efficiency of the coated sample was 95%, which was 2% higher than that of the uncoated sample. Moreover, the discharge capacities of the coated cathode at 60°C was about 2.5 times larger than those of the uncoated sample at rates of 0.5 and 1C, showing 146 and 109 mA/g, respectively. This capacity improvement at 60°C is related to the fact that the highly distributed Si element near the surface, as a type of solid solution with LiNi0.8Co0.15Al0.05O2, diminishes the side reactions of the cathode and electrolyte at 60°C.

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Air exposure effect on LiFePO4

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研究领域:锂离子电池固体电解质 交流阻抗频率范围:200kHz - 10mHz The impact of ambient air exposure on LiFePO4/C nanocomposites has been investigated. A pristine sample was prepared without any exposure to ambient air through the whole process of synthesis and characterization and compared to the exposed samples. A small amount of lithium deintercalates from the olivine structure during exposure, a majority of which can be electrochemically reintercalated. This phenomenon changes the initial surface and bulk properties and should be taken into account when diminishing the particle size of LiFePO4. Keeping nanocomposites away from oxidative moisture atmosphere could be a solution to minimize these side reactions.

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Microfluidic Push-Pull Probe for Scanning Electrochemical Microscopy

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研究领域:SECM 测量方法:循环伏安 This manuscript presents a microfluidic Push-Pull probe for scanning electrochemical microscopy (SECM) consisting of a working microelectrode, an integrated counter/reference electrode and two microchannels for pushing and pulling an electrolyte solution to and away from a substrate. With such a configuration, a droplet of a permanently renewed redox mediator solution is maintained just at the probe tip to carry out SECM measurements on initially dry substrates or in microenvironments. For SECM imaging purposes, the probe fabricated in a soft polymer material is used in a contact regime. SECM images of various gold-on-glass samples demonstrate the proof-of-concept of a Push-Pull probe for local surface activity characterization with high spatial resolution even on vertically oriented substrates. Finite element computations were performed to guide the improvement of the probe sensitivity.

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Thermal and Transport Properties of Ionic Liquids Based on Benzyl-Substituted Phosphonium Cations

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研究领域:离子液体 测量方法:交流阻抗 The physicochemical properties of two novel ionic liquids based on benzyltriethylphosphonium and benzyltributylphosphonium cations are described in this report. It was found that both benzyl-substituted phosphonium cations gave low-melting salts in combination with a bis(trifluoromethylsulfonyl)amide anion. The thermogravimetric analysis suggested that the benzyl-substituted phosphonium ionic liquids showed higher thermal stability than those of not only the alkyl-substituted phosphonium ILs but also the corresponding benzyl-substituted ammonium compounds. The benzyl-substituted phosphonium ionic liquids also exhibited relatively high conductivities when compared to those of the corresponding ammonium compounds. These results indicate an improving effect of introducing a benzyl group into the phosphonium cations on both the thermal stability and the conductivity.

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室温离子液体中纳米导电聚合物材料的制备

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研究领域:离子液体 导电聚合物是近年来的研究热点,它在电化学催化、传感、电容器等领域的成功应用引来 了越来越多关注的目光。室温离子液体作为一类新型的环境友好的绿色溶剂拥有许多优异的 物理、化学性能,它的出现为绿色化学开辟了一条崭新的道路。本论文分别采用电化学聚合 法、化学聚合法、光诱导聚合法在室温离子液体溶液以及室温离子液体与水形成的微乳液体 系中制备了具有纳米尺寸的导电聚合物材料以及导电聚合物复合材料

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Fabrication technology for silicon-based microprobe arrays used in acute and sub-chronic neural recording

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研究领域:神经生物医学 交流阻抗频率范围:1MHz - 0.1Hz This work presents a new fabrication technology for silicon-based neural probe devices and their assembly into two-dimensional (2D) as well as three-dimensional (3D) microprobe arrays for neural recording. The fabrication is based on robust double-sided deep reactive ion etching of standard silicon wafers and allows full 3D control of the probe geometry. Wafer level electroplating of gold pads was performed to improve the 3D assembly into a platform. Lithography-based probe-tracking features for quality management were introduced. Probes for two different assembly methods, namely direct bonding to a flexible micro-cable and platform-based out-of-plane interconnection, were produced. Systems for acute and sub-chronic recordings were assembled and characterized. Recordings from rats demonstrated the recording capability of these devices. (Some figures in this article are in colour only in the electronic version)

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Impedance Characterization and Modeling of Microelectrodes for Neural Recording

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研究领域:神经生物医学+微电极 交流阻抗频率范围:1MHz - 0.1Hz Electrode-electrolyte impedance is one of important characteristic for neural recording applications due to its influence on the signal/noise ratio and signal distortion. In this work a model of the electrode-electrolyte is described and validated through electrochemical impedance spectroscopy technique (EIS), using commercial platinum and platinum/iridium alloy microelectrodes used in acute neural recording. The impedance of the electrodes was measured in standard physiological saline solution (0.9% NaCl). A two electrode setup was used in which the working electrode was connected to the microelectrodes and the counter electrode was short-connected to the reference (stainless steel). The data was collected using an electrochemical analyzer (CompactStat, IviumTechnologies).In order to address the behavior of the electrode impedance an equivalent circuit of the electrode/electrolyte interface has been modeled. Since the impedance is strongly dependent on the electrode area, electrochemical characterization of the area was also performed using a standard iron ferricyanide solution – K3Fe(CN)6.

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Direct electro-oxidation of iso-octane in a solid electrolyte fuel cell

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研究领域:SOFC燃料电池 方法:IV特性和交流阻抗 范围:1MHz - 0.1Hz The present work aims to explore the activity of Cu/CeO2 composites as anodic electrodes in direct iso-octane SOFCs. When the cell was operated as a membrane reactor, the effect of temperature, Pi-C8H18 and applied anodic overpotentials on the electrocatalytic activity and products' distribution, at both open and closed circuit conditions, was examined. Additionally, in situ DRIFT spectroscopy was carried out in order to correlate the performance of Cu/CeO2 with its surface chemistry during iso-octane decomposition. Under the “fuel cell” mode of operation, the electrochemical performance and stability of Cu/CeO2 were investigated by voltage–current density–power density and AC impedance measurements. The results reveal that at high anodic polarization conditions, carbon formation can be noticeably restricted (verified also by EDAX analysis), while H2 production was enhanced due to partial oxidation, steam reforming, dehydrogenation and water gas shift reactions. Achieved power densities were found to substantially increase both with temperature and Pi-C8H18, while minor performance degradation was indicated in the step-change tests, where the overall activity of Cu–CeO2 electrodes remained essentially unaffected.

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Application as a Solid Oxide Fuel Cell Cathode

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研究领域:SOFC燃料电池 方法:IV特性和交流阻抗 范围1MHz - 0.1Hz The feasibility of using the thin film technology in utilizing lanthanum strontium manganite (LSM) for a solid oxide fuel cell (SOFC) cathode in a low-temperature regime is investigated in this study. Thin film LSM cathodes were fabricated using pulsed laser deposition (PLD) on anode-supported SOFCs with yttria-stabilized zirconia (YSZ) electrolytes. Although cells with a 1 μmthick LSM cathode showed poor low-temperature cell performance compared to that of a cell with a bulk-processed cathode due to the lack of a triple-phase boundary length, the cell with 200 nm-thick gadolinia-doped ceria (GDC) inserted between the LSM and YSZ showed enhanced performance and more stable operation characteristics in a comparison of a cell without a GDC layer. We postulate that the GDC layer likely improved the cathode adhesion, therefore contributing to the improvement of the cell performance instead of serving as an interfacial reaction buffer.

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以活性炭为燃料的固体氧化物燃料电池

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采用注浆成型法制备了管状电解质支撑的固体氧化物燃料电池(SOFC), 电解质材料为YSZ, 阳极和阴 极材料都采用银. 将活性炭不加任何气体直接用作电池的燃料. 电池的有效面积为2.5 cm2, 在800 益时给出最大 功率为16 mW, 其开路电压随温度的变化与理论结果一致. 此电池在30 mA 的恒电流下连续稳定运行了37 h, 通过电化学反应消耗了加入电池中碳燃料的42%(w), 证明了电池的工作是可以自维持的. 与使用石墨燃料的 SOFC 相比, 此电池的运行稳定性得到了明显的提高, 因为活性炭比石墨具有大得多的微孔率和表面积. 电池运 行37 h 后很快衰减, 燃料烧结和燃料量减少造成碳表面积减小可能是衰减的主要原因. 电化学阻抗谱测试结果 表明电池的极化电阻在电池的总损耗中占主导. 通过对电池反应机理进行分析, 认为发生在阳极/电解质界面的 CO 电化学氧化反应和发生在碳燃料表面的Boudouard 反应构成的循环维持了电池的运行, 因此通过添加促进上述两个反应的催化剂, 可提高电池的性能.

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Performance of cone-shaped tubular anode-supported segmented-in-series solid oxide fuel cell stack fabricated by dip coating technique

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研究领域:SOFC燃料电池 A simple and feasible technique is developed successfully to fabricate the cone-shaped tubular segmented-in-series solid oxide fuel cell (SOFC) stack. The cone-shaped tubular anode substrates and yttria-stabilized zirconia (YSZ) electrolyte films are fabricated by dip coating technique. After sintering at 1400 C for 4 h, a dense and crack-free YSZ film with a thickness of about 35.9 mm is successfully obtained. The single cell, NiO–YSZ/YSZ/LSM– YSZ, provides a maximum power density of 1.08 and 1.35Wcm2 at 800 and 850 C, respectively, using moist hydrogen (75 ml/min) as fuel and ambient air as oxidant. A two-cell-stack based on the above-mentioned cone-shaped tubular anode-supported SOFC was assembled and tested. The maximum total power at 800 C was about 3.7 W.

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Fabrication and performances of solid superacid embedded chitosan hybrid membranes for direct methanol fuel cell

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研究领域:燃料电池质子导电膜 交流阻抗频率范围:1MHz - 1Hz This study reports the fabrication and performances of hybrid proton-conducting membranes by dispersing nanosized solid superacid inorganic fillers, TiO2–SO4 2? (STiO2), into chitosan (CS) matrix. Fourier transform infrared spectra demonstrate intermolecular interactions between STiO2 and chitosan segmental chains. High resolution scanning electron microscope characterization reveals an essentially homogeneous dispersion of the solid superacid fillers within chitosan matrix. The incorporation of the superacid fillers leads to a reduced fractional free volume (FFV) of the hybrid membranes as confirmed by positron annihilation lifetime spectroscopy (PALS) analysis.

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Proton Conducting membranes obtained by doping radiation-grafted basic membrane matrices with phosphoric acid

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研究领域:燃料电池质子导电膜 交流阻抗频率范围:1MHz - 1mHz By grafting 4-vinylpyridine (4VP), N-vinylformamide (NVF), and 1-vinylimidazole (1VIm) onto electron beam irradiated ETFE and FEP films, the basic membrane matrices ETFE-graftpoly( 4VP), FEP-graft-poly(4VP), ETFE-graft-poly(1VIm), and ETFE-graft-poly(vinylamine), after subsequent hydrolysis of ETFE-graft-poly(NVF), can be obtained. These matrices are doped with phosphoric acid to produce acid–base composite materials that exhibit high proton conductivities up to 100 mScm1 at high temperatures (120 8C) and no humidification. The produced membranes are robust, flexible, and mechanically stable even at high doping levels and endure temperatures of up to 160 8C. Preliminary tests in H2/O2 fuel cells provide power densities between 75 and 150 mAcm2 at 120 8C without humidification. C. Schmidt, G. Schmidt-Naake Institut fu¨r Technische Chemie, Technische Universita¨t Clausthal, Erzstra?e 18, 38678 Clausthal-Zellerfeld, Germany Fax: (t49) 5323 72 3655; E-mail: gudrun.schmidt@tu-clausthal.de 1164 Macromol. Mater. Eng. 2007, 292, 1164–1175  2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim DOI: 10.1002/mame.200700188

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Influence of CO2 on ionic conductivity of anion exchange membrane for alkaline DMFCs

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研究领域:碱性直接甲醇燃料电池膜 交流阻抗频率范围:1MHz - 10Hz Alkaline direct methanol fuel cells (ADMFCs) have attracted considerable attention as an energy source for transport and other portable applications[1]. The anion exchange membranes (AEMs) containing positive ionic groups (typically quaternary ammonium groups : ―N+R3) are widely studied as electrolytes. Unlike conventional DMFCs using proton exchange membranes, non-platinum catalysts such as Pd or Ag can be used for ADMFCs[2, 3].

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Electricity Generation from MFCs Using Differently Grown Anode-Attached Bacteria

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研究领域:微生物燃料电池MFC 交流阻抗频率范围:100kHz - 5mHz To understand the effects of acclimation schemes on the formation of anode biofilms, different electrical performances are characterized in this study, with the roles of suspended and attached bacteria in single-chamber microbial fuel cells (MFCs). The results show that the generation of current in single-chamber MFCs is significantly affected by the development of a biofilm matrix on the anode surface containing abundant immobilized microorganisms. The long-term operation with suspended microorganisms was demonstrated to form a dense biofilm matrix that was able to reduce the activation loss in MFCs. Also, a Pt-coated anode was not favorable for the initial or long-term bacterial attachment due to its high hydrophobicity (contact angle = 124°), which promotes easy detachment of the biofilm from the anode surface.

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Electricity Generation from MFCs Using Differently Grown Anode-Attached Bacteria

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研究领域:微生物燃料电池 交流阻抗频率范围:40Hz - 0.003Hz Four non-porous materialswere compared for their suitability as bio-anode in microbial fuel cells (MFCs). These materials were flat graphite, roughened graphite, Pt-coated titanium, and uncoated titanium. The materials were placed in four identical MFCs, of which the anode compartments were hydraulically connected in series, as well as the cathode compartments. The MFCs were operated with four resistors. The anode kinetics at these electrode materialswere studied by means of dc-voltammetry and electrochemical impedance spectroscopy (EIS).

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Effective monitoring of corrosion in reinforcing steel in concrete constructions by a multifunctional sensor

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A novel multifunctional sensor is developed for in situ and non-destructive monitoring of the corrosion current and open circuit potential of reinforcing steel, as well as the pH and Cl? concentration of concrete. The pH and Cl? sensors show good responses to the pH and Cl? concentration of concrete pore solutions, respectively, and are able to monitor both the carbonization process of concrete and the ingress of Cl? in concrete. Combined with measurements of the corrosion potential and corrosion current density, as well as the EIS spectra of reinforcing steel in concrete, this study demonstrates that the pH and the Cl? concentration of concrete are two of the most crucial factors that determine the corrosion of reinforcing steel in concrete.

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Feasibility Study on Electrochemical Impedance Spectroscopy for Microbial Fuel Cells - Measurement Modes & Data Validation

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Electrochemical impedance spectroscopy (EIS) is in potential a powerful tool for the in depth analysis of microbial fuels cells (MFCs). To prevent the risk of drawing false conclusions from invalid EIS measurements we investigated the feasibility of this method on an MFC by checking: linearity, causality, stability and finiteness. EIS application under steady state conditions was partly feasible. For further application EIS on MFCs we recommend to: (1) use the constant anode or cathode potential measurement mode with a fast couple at the counter electrode; (2) record the polarization curve and measure at different amplitudes to check the linearity condition; (3) perform preliminary measurements to reveal measurement presets; (4) apply prolonged pretreatment to facilitate the stability criterion; (5) perform duplicate measurements to examine the stability; (6) use a broad frequency range to validate the finiteness criterion; (7) use a statistical based validation check based on the Kramers-Kronig transformation.

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碳钢及其与不锈钢焊件在高温LiBr溶液中腐蚀与防护的研究

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研究领域:高温热泵腐蚀 采用电化学测试技术,在常温常压下对重铬酸钾溶液钝化碳钢的行为进行了研究, 并在55%的溴化锂溶液中对其钝化效果进行了评价,结果表明,不同浓度的重铬酸钾溶 液钝化效果不同,采用浓度为15—309/L的重铬酸钾溶液钝化时钝化效果最好。而且向 15-309/L的重铬酸钾溶液中加入49/L的硝酸可以提高重铬酸钾溶液的钝化效果,但实 验表明,硝酸最佳加入量与重铬酸钾溶液的浓度有关。

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深海环境对纯镍腐蚀行为的影响

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研究领域:纯镍点蚀 测量方法:塔菲尔曲线 利用电化学测量方法测量纯镍在3.4%NaCL溶液中,静水压力为0MPa和8MPa条件下的点蚀击破电位和孕育时间,分析得到纯镍在不同静水压力下点蚀击破电位的理论精确值,利用随机分析方法分析纯镍在静水压力下的点蚀机制,实验结果表明静水压力对纯镍的点蚀过程有着重要的影响,在静水压力下纯镍的点蚀行为和机制发生了改变。

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Corrosion Resistance of Stainless Steels Analyzed by Fractal Geometry

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研究领域:不锈钢腐蚀 交流阻抗频率范围:100kHz - 1Hz Fractal property of the passivated steel surface was investigated on the basis of scaling analysis with a special focus on its relationship with corrosion resistance. For this purpose, the surface of stainless steel was intentionally oxidized under a variety of passivation conditions and its scaling property was analyzed by a triangulation method. The morphology of the passivated steel surface was satisfactorily evaluated with fractal dimension. From the chronoamperometry and impedance measurement, it proved that lower fractal dimension leads to more enhanced corrosion resistance. The higher passivity of the steel surface with lower fractal dimension was discussed in terms of active area and structural imperfection.

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A comparative H2S corrosion study of 304L and 316L stainless steels in acidic media

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研究领域:碳钢腐蚀 测量方法:塔菲尔曲线和交流阻抗 100kHz - 0.1Hz H2S corrosion of 304L and 316L in oxygen-free Na2SO4 + Na2S solution at pH 3 and temperature of 60 C were investigated by EIS, potentiodynamic polarisation, multi-component Pourbaix diagrams and microstructure characterization. At similar conditions, lower corrosion rate was observed on 316L, attributed to its denser (1.5 times) and smoother (6%) surface layer and confirmed by SEM micrograph.

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Influence of interface chemistry and network density on interfacial ion transport kinetics for styreneacrylate copolymer

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研究领域:涂层涂料腐蚀 交流阻抗频率范围:100kHz - 1Hz n-Butyl acrylate/styrene copolymer films were applied on iron and zinc surfaces. The kinetics of interfacial ion transport and cathodic delamination were tracked by in situ Scanning Kelvin Probe (SKP) measurements.A destabilisation of the interface was detected for latex network structures with an increased degree of cross-linking. In contrast, a reduction of the average macromolecular chain length resulted in films with higher resistance to interfacial ion transport.

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In-situ study of the formation process of stannate conversion coatings on AZ91D magnesium alloy using electrochemical noise

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研究领域:镁合金腐蚀 测量方法:电化学噪声 The formation process of stannate conversion coating (CC) on AZ91D alloy was in-situ investigated by electrochemical noise (EN). The wavelet transform, as well as noise resistance (Rn) and spectral noise resistance (Rsn), had been employed to analyze the EN data. It was revealed that there exist two distinguishing stages of stannate CC formation process on AZ91D alloy, including an incubation stage companying with the nucleation and nuclei dissolution process, a periodical growth stage involving hemispherical particles growth and coating dissolution process.

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The effect of H2S concentration on the corrosion behavior of carbon steel at 90 C

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研究领域:碳钢腐蚀 测量方法:塔菲尔曲线和交流阻抗 The electrochemical behavior of SAE-1020 carbon steel in 0.25 M Na2SO4 solution containing different concentrations of H2S at 90 C was investigated using the methods of weight loss, electrochemical measurements, scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results showed that the corrosion rate of carbon steel increased significantly with the increase of H2S concentration.

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纳米多孔金支持氧化钴微电极作为高性能电化学传感器

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Nature Comm-JLU-Nanoporous gold supported cobalt oxide microelectrodes as high-performance electrochemical biosensors

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混合模式方法介绍

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Ivium专为电池研究而设计的独特方法,首次也是目前唯一能够将直流方法和交流方法结合起来。 在直流充放电的同时可以监测内阻的变化。

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