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Title
Downstream analytics quantification of ion release during high voltage anodisation of niobium
AuthorMardare, Andrei Ionut ; Kollender, Jan Philipp ; Mardare, Cezarina Cela ; Hassel, Achim Walter In der Gemeinsamen Normdatei der DNB nachschlagen
Published in
Journal of Solid State Electrochemistry, 2018, Vol. 22, Issue 8, page 2457-2464
PublishedSpringer Berlin Heidelberg, 2018
LanguageEnglish
Document typeJournal Article
Keywords (EN)High-field regime / Anodisation / Valve metals / Inductively coupled plasma mass spectrometry
ISSN1433-0768
URNurn:nbn:at:at-ubl:3-776 Persistent Identifier (URN)
DOI10.1007/s10008-018-3957-4 
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 The work is publicly available
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Downstream analytics quantification of ion release during high voltage anodisation of niobium [1.29 mb]
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Abstract (English)

In operando quantification of field-assisted ion release during high-voltage anodisation (up to 100 V SHE) of Nb in 0.1 M sulphuric acid was performed. Electrochemical high-field oxide formation under both potential and current control was studied separately. The quantification of in situ ion release via ICP-MS revealed an increase of the oxide dissolution factor (from 337 to 422 fm V1) when decreasing the potential scan rate from 200 to 100 mV s1. Dissolution rates measured during galvanostatic oxide formation allowed measuring oxide dissolution factors of 719 and 837 fm V1 for current densities of 1.0 and 0.5 mA cm2, respectively. As compared to the potentiodynamic case, higher dissolution rates and oxide dissolution factors were measured for galvanostatic anodisation. The overall fraction of the charge used for generation of soluble Nb species was below 0.4% for all oxide growth regimes. Cross-sectional SEM imaging proofs an oxide formation factor of 2.1 nm V1. The surface of anodised films was extremely smooth and featureless without any cracks or voids. Based on X-ray diffraction, the films were found to be amorphous, indicating that no field crystallisation is occurring under the applied oxide growth conditions even at higher voltages.

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