Electrochemical preparation, characterization and application of electrodes modified with nickel–cobalt hexacyanoferrate/graphene oxide–carbon nanotubes

• A nanohybrid of graphene oxide and multiwalled carbon nanotubes (GO-CNTs) was synthesized.
• The nickel–cobalt hexacyanoferrate decorated GO-CNTs were prepared by electrodeposition.
• The resulted hybrid exhibited greatly improved electrocatalysis to hydroxylamine.

A nanohybrid of graphene oxide and multiwalled carbon nanotubes (GO-CNTs) was synthesized through π–π interaction. The nickel–cobalt hybrid hexacyanoferrate decorated GO-CNTs (NiCoHCF/GO-CNTs) was prepared by electrodeposition of NiCoHCF in different ratios of Co2 + to Ni2 + solution on GO-CNTs. The characterization was performed by UV–vis, FT-IR, Raman spectroscopy, and SEM. The electrochemistry behavior of NiCoHCF/GO-CNTs was studied by cyclic voltammetry. The NiCoHCF/GO-CNT modified GCE (NiCoHCF/GO-CNT/GCE) exhibited greatly improved electrocatalytic activity towards electrooxidation of hydroxylamine. The modified electrode exhibited a wide linear range from 0.2 μM to 150 μM and a low detection limit (LOD) of 0.08 μM.