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Electrochemical Measurements as Screening Method for Water Oxidation Catalyst

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Testing Novel Water Oxidation Catalysts for Solar Fuels Production

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Abstract

In actual water splitting devices, the WOC will be deposited on an anode surface. Therefore, whatever the results obtained with WOC particles suspended in stirrer tank reactors, it becomes necessary to study WOC performances by means of electrochemical experimental setups. The WOCs deposition on an anode will depend on their physico-chemical nature, therefore several deposition methods, including wet and dry approaches, are found in literature. This Chapter reviews the available electrochemical techniques that can be adopted to study WOCs that are deposited on an electrode. In addition, the parameters used in literature to compare the different WOC materials will be explained. At the end of the Chapter, an example of the performance of different MnOx films will be reported. The water oxidation activity of three MnOx crystalline phases prepared by two deposition techniques will be compared. The aim of the comparison is to determine whether two electrodes having the same crystalline phase behave differently or not when they are deposited by two different techniques.

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Author information

Authors and Affiliations

  1. School of Biochemical Engineering, Pontificia Universidad Católica de Valparaíso, Valparaíso, Chile

    Carminna Ottone

  2. Department of Applied Science and Technology, Politecnico di Torino, Turin, Italy

    Simelys Hernández

  3. Department of Applied Science and Technology, Politecnico di Torino, Turin, Italy

    Marco Armandi

  4. Department of Applied Science and Technology, Politecnico di Torino, Turin, Italy

    Barbara Bonelli

Authors
  1. Carminna Ottone
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  2. Simelys Hernández
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  3. Marco Armandi
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  4. Barbara Bonelli
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Corresponding author

Correspondence to Carminna Ottone .

Appendix

Appendix

5.1.1 Characterization Techniques

XRD patterns of the films were collected on an X’Pert Phillips diffractometer using Cu Kα radiation = 1.541874 Å (20–60 2θ range; step width = 0.02°; time per step = 2 s) and indexed according to the Powder Data File database (PDF 2000, International Centre of Diffraction Data, Pennsylvania). The morphology of the samples was studied by Field Emission Scanning Electron Microscopy (FE-SEM) pictures, which were collected on a high-resolution instrument (LEO 1525). Cross-section images were used to determine the average film thickness of selected samples.

5.1.2 Electrochemical Measurements

The catalytic activity of the Mn oxides films was tested at pH = 7 in 0.1 M phosphate buffer in a standard three-electrodes setup in a lab-made glass cell with Ag/AgCl (3 M KCl) electrode as reference electrode and a Pt wire as counter electrode. The measurements were recorded using a multichannel VSP potentiostat/galvanostat (BioLogic), with EC-Lab v. 10.1x software for data acquisition. Cyclic voltammetries (CV) were performed in the range of 0.6 to 2.0 V versus RHE with a sweep rate of 20 mV s−1. Tafel plots were constructed from the data obtained from quasi-stationary current density between 1.4 and 2.0 V versus RHE (with steps of 40 mV). Ohmic drop correction was performed, hence, impedance spectra were recorded at every potential/current step at 10 kHz with a modulation amplitude of 20 mV in order to determine the ohmic resistance of the solution (Rs). The overpotential (η) reported in the Tafel plot was calculated as follow: \(\eta = E_{RHE} - E_{RHE}^{0} - i R\), where \({\text{E}}_{\text{RHE}}^{0}\) is the standard potential of the water splitting reaction (~1.23 V) and i is the current density.

Evolved oxygen and hydrogen was measured by a micro-GC (Varian 490, equipped with a Molsieve column) during chrono-amperometry test (at 2.0 V vs. RHE). Previous the experiment, the cell was purged with a continuous Ar flow (25 Nml min−1) for 1 h. Argon flow was maintained during the experiment to strip the evolved O2 and H2 gases from the cell to the micro-GC.

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Ottone, C., Hernández, S., Armandi, M., Bonelli, B. (2019). Electrochemical Measurements as Screening Method for Water Oxidation Catalyst. In: Testing Novel Water Oxidation Catalysts for Solar Fuels Production. PoliTO Springer Series. Springer, Cham. https://doi.org/10.1007/978-3-030-12712-1_5

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