Scanning Electrochemical Microscopy of Electroactive Defect Sites in the Native Oxide Film on Aluminum

Serebrennikova, Irina; White, Henry S.

doi:10.1149/1.1344278

Cited by 70 publications

(53 citation statements)

References 16 publications

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“…Scanning electrochemical microscopy has been used to demonstrate electron transfer at defect sites in the native oxide film on pure aluminum (Ͼ99.99%). 25 It is possible that the mediator facilitates electron transfer at these defect sites, perhaps making available additional sites for nucleation and subsequent polymer growth. In situ electrochemical AFM studies conducted in our laboratory ͑to be reported elsewhere͒ revealed a significant increase in the number of nucleation sites in the presence of Tiron, supporting this hypothesis.…”

Section: Resultsmentioning

confidence: 99%

Direct Electrodeposition of Polypyrrole on Aluminum and Aluminum Alloy by Electron Transfer Mediation

Tallman¹,

Vang

Wallace

et al. 2002

J. Electrochem. Soc.

133

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The direct electrodeposition of electroactive conducting polymers on active metals such as iron and aluminum is complicated by the concomitant metal oxidation that occurs at the positive potentials required for polymer formation. In the case of aluminum and its alloys, the oxide layer that forms is an insulator that blocks electron transfer and impedes polymer formation and deposition. As a result, only patchy nonuniform polymer films are obtained. Electron transfer mediation is a well-known technique for overcoming kinetic limitations of electron transfer at metal electrodes. In this work, we report the use of electron transfer mediation for the direct electrodeposition of polypyrrole onto aluminum and onto Al 2024-T3 alloy. This report focuses on the use of Tiron (4,5-dihydroxy-1,3-benzenedisulfonic acid disodium salt) as the mediator, although catechol appears to function in a similar manner. Depositions were carried out under galvanostatic conditions at current densities of 1 normalmA/cm2. The mediator reduced the deposition potential by nearly 500 mV compared to deposition performed in the absence of mediator (where Tiron was replaced by p-toluene sulfonic acid sodium salt). Polypyrrole formation and deposition appears to occur with 100% current efficiency and uniform films are obtained. Results of the characterization of these films by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, conductivity measurements, and adhesion measurements are presented. © 2002 The Electrochemical Society. All rights reserved.

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Section: Resultsmentioning

confidence: 99%

Direct Electrodeposition of Polypyrrole on Aluminum and Aluminum Alloy by Electron Transfer Mediation

Tallman¹,

Vang

Wallace

et al. 2002

J. Electrochem. Soc.

133

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“…It complements other scanning probe techniques such as the scanning reference electrode technique (SRET) [178,179], conductive scanning force microcopy (CSFM), electrochemical scanning tunneling microscopy (ECSTM), and scanning Kelvin probe techniques which are popular methods for the investigation of functional materials [180]. Basic experimental approaches include the imaging of the permeability of applied protective coatings [181][182][183][184][185][186][187][188][189][190][191][192][193], the imaging of regions with distinctly higher electron transfer rates which may be precursor sites for pitting corrosion [29,57,[194][195][196][197][198][199][200][201][202][203][204][205][206][207], the initiation of pitting corrosion by local generation of aggressive species at the UME [208,209] and the detection of active corrosion by collecting released species [55,58,60,104,[210][211][212][213][214]…”

Section: Localized Corrosionmentioning

confidence: 99%

“…Moreover, it was observed that active sites preferably start to appear at the triple points of grain boundaries and, with more negative potentials, propagate along the grain boundaries ( Figure 26) [241]. An approach to investigate defect sites on natively passivated Al in nonaqueous media was described by Serebrennikova and White [199]. Al.Al 2 O 3 electrodes were prepared inter alia from high-purity Al rods and Al foils of lower purity.…”

Section: Investigation Of Precursor Regionsmentioning

confidence: 99%

Investigation of Localized Catalytic and Electrocatalytic Processes and Corrosion Reactions with Scanning Electrochemical Microscopy (SECM)

Pust¹,

Maier²,

Wittstock³

2008

Zeitschrift Für Physikalische Chemie

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Scanning Electrochemical Microscopy (SECM) . Catalytic Electrodes .Electrochemical Energy Conversion . Fuel Cells . Oxygen Reduction Reaction . CorrosionScanning electrochemical microscopy (SECM) has developed into a very versatile tool for the investigation of solid-liquid, liquid-liquid and liquid-gas interfaces. The arrangement of an ultramicroelectrode (UME) in close proximity to the interface under study allows the application of a large variety of different experimental schemes. The most important have been named feedback mode, generation-collection mode, redox competition mode and direct mode. Quantitative descriptions are available for the UME signal, depending on different sample properties and experimental variables. Therefore, SECM has been established as an indispensible tool in many areas of fundamental electrochemical research. Currently, it also spreads as an important new method to solve more applied problems, in which inhomogeneous current distributions are typically observed on different length scales. Prominent examples include devices for electrochemical energy conversion such as fuel cells and batteries as well as localized corrosion phenomena. However, the direct local investigation of such systems is often impossible. Instead, suitable reaction schemes, sample environments, model samples and even new operation modes have to be introduced in order to obtain results that are relevant to the practical application. This review outlines and compares the theoretical basis of the different SECM working modes and reviews the application in the area of electrochemical energy conversion and localized

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“…Fe 2+ , Fe 3+ , H 2 , and O 2 ). Identification of precursor sites for pitting corrosion that often result from local damage of the oxide film has been achieved in the sample generation/tip collection (SG/TC) mode on steel [81][82][83][84][85], Ti [86][87][88][89][90], Ta [91,92], Ni [93], and Al [94,95] by use of their enhanced kinetics of heterogeneous electron transfer to dissolved components. With SECM, identification of those precursor sites in their passive state is possible because of the nondestructive character of the technique.…”

Section: Metalsmentioning

confidence: 99%

Multidimensional electrochemical imaging in materials science

2007

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In the past 20 years the characterization of electroactive surfaces and electrode reactions by scanning probe techniques has advanced significantly, benefiting from instrumental and methodological developments in the field. Electrochemical and electrical analysis instruments are attractive tools for identifying regions of different electrochemical properties and chemical reactivity and contribute to the advancement of molecular electronics. Besides their function as a surface analytical device, they have proved to be unique tools for local synthesis of polymers, metal depots, clusters, etc. This review will focus primarily on progress made by use of scanning electrochemical microscopy (SECM), conductive AFM (C-AFM), electrochemical scanning tunneling microscopy (EC-STM), and surface potential measurements, for example Kelvin probe force microscopy (KFM), for multidimensional imaging of potential-dependent processes on metals and electrified surfaces modified with polymers and self assembled monolayers.

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Scanning Electrochemical Microscopy of Electroactive Defect Sites in the Native Oxide Film on Aluminum

Cited by 70 publications

References 16 publications

Direct Electrodeposition of Polypyrrole on Aluminum and Aluminum Alloy by Electron Transfer Mediation

Direct Electrodeposition of Polypyrrole on Aluminum and Aluminum Alloy by Electron Transfer Mediation

Investigation of Localized Catalytic and Electrocatalytic Processes and Corrosion Reactions with Scanning Electrochemical Microscopy (SECM)

Multidimensional electrochemical imaging in materials science

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