Cathodic polarization of niobium specimens that have been anodized galvanostatically up to E
a=100V, and then potentiostatically at E
a=100V has been investigated in a neutral borate solution. During potetiostatic cathodic polarization below E
c=−2.36V (vs. RHE) in both aerated and deaerated solutions, the cathodic current increased rapidly initially, and then increased gradually until it reached a steady value. Hydrogen gas evolution was observed during cathodic polarization below E
c=−2.36V with no formation of blisters and pits, suggesting that H
+ reduction occurs mainly at the film surface. GD-OES spectra revealed that hydrogen species are enriched in the niobium substrate near the interface between anodic oxide films and the substrate at potentials below E
c=−2.36V, and that the trend is pronounced at lower potentials. Chemical shift was observed on Nb 3d and O 1s peaks in XPS spectra for the specimen at E
c=−3.36V, suggesting the formation of Nb
2O
3(OH)
2.
Mechanism for the reaction during cathodic polarization in a neutral solution is discussed in terms of the proton reduction at the interfaces both between oxide films / solutions and between oxide films / substrates.
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