Journal
ANALYTICAL CHEMISTRY
Volume 80, Issue 5, Pages 1437-1447Publisher
AMER CHEMICAL SOC
DOI: 10.1021/ac701796u
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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 MOO 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 TiO2 layer to a more conductive TiOOH layer.
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