Journal of Solid State Electrochemistry

, Volume 22, Issue 5, pp 1289–1302 | Cite as

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

  • Emanuel R. Faria
  • Fernando M. Ribeiro
  • Débora V. Franco
  • Leonardo M. Da Silva
Original Paper


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.


Mixed oxide-covered mesh electrodes Ni and Co oxides Morphology factor and electrochemical porosity Generation of hydroxyl radicals 



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).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


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Copyright information

© Springer-Verlag GmbH Germany 2017

Authors and Affiliations

  • Emanuel R. Faria
    • 1
  • Fernando M. Ribeiro
    • 1
  • Débora V. Franco
    • 1
  • Leonardo M. Da Silva
    • 1
  1. 1.Departamento de QuímicaUniversidade Federal dos Vales do Jequitinhonha e MucuriDiamantinaBrazil

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