Analytical Chemistry · 2008 · 61 citations · 33 references
Natural SciencesMaterials EngineeringMaterials ScienceElectrochemistryMetallic MaterialsSurface ScienceAlloysElectrode MaterialsGrain Structure AnalysisMetalsScanning Probe MicroscopySurface CharacterizationAlloyingAlloying ElementsGrain BoundariesGrain Boundary AnalysisGrain Boundary CharacterizationReactivityScanning Electrochemical MicroscopyTitanium Alloys
Scanning electron microscopy/energy dispersive X-ray analysis (SEM/EDX) was applied to investigate the grain boundaries on ASTM grade-7 titanium (Ti-7) with a freshly polished surface, and the results showed that the alloying element, Pd, and the impurity, Fe, cosegregated to grain boundaries. Scanning electrochemical microscopy (SECM) was used to study the variations in reactivity on Ti-7 exposed to an aerated neutral solution of 0.1 M NaCl. Locations that possessed an enhanced reactivity compared to the oxide-covered (TiO(2)) surface of the grains on SECM images were proposed to be the boundaries. These areas were further activated by the application of a cathodic bias, and interconnection of the active locations allowed the construction of "grain boundary maps". Variations in surface reactivity were quantitatively analyzed by fitting probe approach curves (PACs) to curves simulated with a model based on finite element analyses using the platform of COMSOL multiphysics software. The difference in reactivity between active grain boundaries and oxide-covered grains was up to a factor of 100 on freshly polished surfaces. This difference decreased to a factor of 10-15 after longer-term exposure of the Ti-7 to the aerated solution, indicating partial passivation of the Pd/Fe-stabilized beta-phase in the grain boundaries. PAC analyses of oxide-covered grains showed that the reactivity increased logarithmically as the bias potential to the Ti-7 was decreased, consistent with reduction of the insulating TiO(2) layer to a more conductive TiOOH layer.
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Voltammetry with Microscopic Electrodes in New Domains
R. Mark Wightman · Science · 1988 · 266 citations
Norberto Casillas, S. Charlebois, William H. Smyrl et al. · Journal of The Electrochemical Society · 1994 · 200 citations
Natural Sciences, Materials Engineering, Materials Science +12