The development of a bi-functional active and stable catalyst for both hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) is an important challenge in overall electrochemical water splitting. In this study, firstly, nickel nanocones (NNCs) were formed using electrochemical deposition, and then Ni–Co–Fe based mixed sulfide ultrathin nanosheets were obtained by directly depositing on the surface of the nanocones using the CV method. With a hierarchical structure of Ni–Fe–Co–S nanosheets, not only was a high active surface area created, but also the electron transfer and mass transfer were enhanced. This structure also led to the faster release of hydrogen bubbles from the surface. An overpotential value of 106 mV was required on the surface of this electrode to generate a current density of 10 mA cm−2 in the HER, whereas, for the OER, 207 mV overpotential was needed to generate a current density of 10 mA cm−2. Furthermore, this electrode required 1.54 V potential to generate a current density of 10 mA cm−2 in the total electrochemical water splitting. The resulting electrode also exhibited reasonable electrocatalytic stability, and after 10 hours of electrolysis in the overall water splitting reaction, the voltage change was negligible. This study introduces a simple, efficient, reasonable and cost-effective method of creating an effective catalyst for the overall water splitting process.

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