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Fabrication and characterisation of a mixed oxide-covered mesh electrode composed of NiCo2O4 and its capability of generating hydroxyl radicals during the oxygen evolution reaction in electrolyte-free water

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Abstract

A mixed oxide-covered mesh electrode composed of NiCo2O4 (MOME-NiCo2O4) was prepared on a stainless-steel substrate using thermal decomposition (slow-cooling rate method). Surface, bulk and electrochemical properties of MOME were studied using different techniques, namely scanning electron microscopy (SEM), X-ray diffraction (XRD), cyclic voltammetry (CV) with determination of the electrochemical porosity (ϕ) and morphology factor (φ) parameters, quasi-stationary polarisation curves (PC) and electrochemical impedance spectroscopy (EIS). SEM images revealed a good coverage of the metallic wires by a compact oxide layer (absence of cracks). XRD analysis confirmed the formation of the spinel NiCo2O4 with the presence of NiO. The ‘in situ’ surface parameters denoted as ϕ and φ exhibited values of 0.39 and 0.33, respectively, revealing that the electrochemically active surface area is mainly confined to the ‘outer/external’ surface regions of the oxide layer. The PC was characterised by two Tafel slopes distributed in the low (b 1 = 46 mV dec−1) and high (b 2 = 59 mV dec−1) overpotential domains. The corresponding apparent exchange current densities were j 0(1) = (3.43 ± 0.11) × 10−6 A cm−2 and j 0(2) = (6.70 ± 0.08) × 10−6 A cm−2, respectively. The EIS study accomplished in the low-overpotential domain revealed a Tafel slope (b 1) of 51 mV dec−1. According to the spin-trapping reaction using N,N-dimethyl-p-nitrosoaniline (RNO), the MOME-NiCo2O4 electrode exhibited good performance for the generation of weakly adsorbed hydroxyl radicals (HO•) during the OER in electrolyte-free water.

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Acknowledgements

L.M. Da Silva wishes to thank the “Fundação ao Amparo à Pesquisa do Estado de Minas Gerais – FAPEMIG” (Projects CEX-APQ-1181-14 and CEX-112-10), “Secretaria de Estado de Ciência, Tecnologia e Ensino Superior de Minas Gerais - SECTES/MG” (Support for the LMMA Laboratory) and “Conselho Nacional de Desenvolvimento Científico e Tecnológico – CNPq” (PQ-2 grant). This work is a collaborative research project of members of the “Rede Mineira de Química” (RQ-MG) supported by FAPEMIG (Project: CEX-RED-00010-14).

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  1. Departamento de Química, Universidade Federal dos Vales do Jequitinhonha e Mucuri, Rodovia MGT 367, km 583, 5000, Alto da Jacuba, Diamantina, MG, 39100-000, Brazil

    Emanuel R. Faria, Fernando M. Ribeiro, Débora V. Franco & Leonardo M. Da Silva

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  1. Emanuel R. Faria
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Highlights

• Mixed oxide-covered mesh electrodes containing Ni and Co (MOME-NiCo2O4) were fabricated using a stainless-steel support;

• The morphology factor (φ) and electrochemical porosity (ϕ) parameters confirmed the formation of a compact oxide layer;

• A good performance for the generation of hydroxyl radicals was verified during the oxygen evolution reaction in the electrolyte-free water;

• The MOME-NiCo2O4 electrode is a promising candidate for the electrochemical combustion of organic pollutants in the electrolyte-free water.

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Faria, E.R., Ribeiro, F.M., Franco, D.V. et al. Fabrication and characterisation of a mixed oxide-covered mesh electrode composed of NiCo2O4 and its capability of generating hydroxyl radicals during the oxygen evolution reaction in electrolyte-free water. J Solid State Electrochem 22, 1289–1302 (2018). https://doi.org/10.1007/s10008-017-3815-9

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