Probing the Fate of Mn Complexes in Nafion: A Combined Multifrequency EPR and XAS Study

Alexander Schnegg, Joscha Nehrkorn, Archana Singh, Irati Alonso Calafell, Shannon A. Bonke, Rosalie K. Hocking, Klaus Lips, Leone Spiccia

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Abstract

Multifrequency electron paramagnetic resonance (EPR, 9.4 and 263 GHz) and X-ray absorption spectroscopy (XAS) were employed to study structural and electrochemical changes of selected Mn complexes in contact with dried Nafion films upon electro-oxidation and after long-term illumination. It was found that when in contact with Nafion the Mn-Me3TACN complexes are reduced into Mn(II) complexes with an octahedral geometry (Me3TACN = 1,4,7-trimethyl-1,4,7-triazacyclononane). The reduction process involves an intermediate product in which Mn has been reduced from the initial +III or +IV state of the precursor Mn complex but is still coordinated to the TACN ligand. Electro-oxidation yields a MnOx mineral with a birnessite structure, in which the Mn(III) or Mn(IV) ions exhibit very strong magnetic coupling. Long-term illumination of the oxide-containing Nafion film while it is exposed to an aqueous electrolyte partially decomposes the mineral and forms a Mn(II) species with octahedral coordination.

Original languageEnglish
Pages (from-to)853-861
Number of pages9
JournalJournal of Physical Chemistry C
Volume120
Issue number2
DOIs
Publication statusPublished - 21 Jan 2016

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