Deposition of Iron Doped Birnessite During Simultaneous Electroreduction of Permanganate and Ferrate(Vi) In Sodium Hydroxide Solution

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Abstract

The reduction of permanganate on rotating disk electrode is accompanied by inhibition of precipitating birnessite. Addition of potassium ferrate(VI) leads to an increase of inhibition. The obtaining of electrode material based on Fe-doped birnessite under alkaline conditions is demonstrated in experiment with deposition at inhibition potentials. This birnessite is single-phase and highly disordered. Fe content varies from 0 to 10 mol. % in respect to Mn with increasing ferrate(VI) content in deposition solution. Recharging potentials of birnessite are shifted which is manifested by cyclic voltammetry. Doping allows to increase the rate of oxygen evolution reaction. Specific currents are increased with the iron content in birnessite. The Tafel slope is 53 mV/dec and decreased by 2.5 times for birnessite containing 10 mol. % Fe.

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L. V. Pugolovkin

Lomonosov Moscow State University

Author for correspondence.
Email: leoff@elch.chem.msu.ru
Russian Federation, Moscow

E. E. Levin

Lomonosov Moscow State University; Crystallography and Photonics Federal Research Center of the Russian Academy of Sciences

Email: leoff@elch.chem.msu.ru
Russian Federation, Moscow; Moscow

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2. Fig. 1. Normalised voltammetry (a) recorded in KMnO4 solutions with different concentrations indicated near the corresponding curves. Voltammetryograms at 100 (b) and 2 mV/s (c) recorded in solutions of 0.3 mM K2FeO4 (1), 1 mM KMnO4 (2), 1 mM KMnO4 + 0.3 mM K2FeO4 (3) and curves (4) corresponding to the sum of curves 1 and 2. The rotation speed is 900 rpm

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3. Fig. 2. Current magnitudes as a function of the root of the slew rate in solutions of 0.3 mM K2FeO4 (1), 1 mM KMnO4 (2), and 1 mM KMnO4 + 0.3 mM K2FeO4 (3) measured at a potential of -0.3 V. The potential sweep speed is 100 mV/s

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4. Fig. 3. Diffractograms of birnessites obtained from solutions of 20 mM KMnO4 (1) and 20 mM KMnO4 + 0.3 mM K2FeO4 (2). The deposition charge is 1.05 Cl/cm2. Reflexes (3) refer to the calculated diffractogram of chemically synthesised birnessite of composition Na0.58Mn2O4×1.5H2O [30]

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5. Fig. 4. Fe and Na content in birnessite as a function of the amount of ferrate in the deposition solution, obtained from XRMS spectra, and the loading value of birnessite at a constant deposition charge of 1.05 Cl/cm2

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6. Fig. 5. Optical (a) and CR spectra (b) of birnessites obtained from solutions of 20 mM KMnO4 (1) and 20 mM KMnO4 + 0.6 mM K2FeO4 (2). The deposition charges are 0.15 Cl/cm2 (md = 47 μg/cm2) for optical spectra and 1.05 Cl/cm2 for CR spectra. The optical spectra of electrochemically deposited FeOOH with md = 5 μg/cm2 on FTO(3) and colloidal Fe(OH)3 with md = 6 μg/cm2 (4) are shown on the left and enlarged in inset (a)

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7. Fig. 6. Surface (a) and spall (b) micrographs of birnessite obtained from a solution of 20 mM KMnO4 + 0.3 mM K2FeO4. Deposition charge 1.05 Cl/cm2

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8. Fig. 7. Load-normalised voltammetry voltammetries of Birnessites in 1 M NaOH obtained from solutions of 20 mM KMnO4 with different additions of K2FeO4 at different potential intervals. The potential sweep rate was 10 mV/s and the deposition charge was 0.71 Cl/cm2. The area of maximum on the anodic branch of the voltammetry (b) is enlarged on the inset

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9. Fig. 8. Specific capacitance during cyclic recharging of birnessites obtained from solutions of 20 mM KMnO4 (1) and 20 mM KMnO4 + 0.3 mM K2FeO4 (2). The potential sweep rate was 100 mV/s and the deposition charge was 0.71 Cl/cm2. The inset shows 2 (1) and 1000 (2) cycles of birnessite deposited from a ferrate-containing solution

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10. Fig. 9. Quasi-stationary curves (a) and galvanostatic curves at a current density of 10 A/g (b) of oxygen release in 1 M NaOH on Birnessites prepared from solutions of 20 mM KMnO4 with different additions of K2FeO4. Quasi-stationary curves (a) were recorded in 10 mV increments with a staging time at each potential not exceeding 10 s. The deposition charge is 0.071 Cl/cm2 (md = 17 μg/cm2). The loss of specific capacitance calculated from cyclic curves in the potential range (-0.1 - 0.4) V after galvanostatic testing is given in the inset on the left side of the paper

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