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Research Article | Open Access

A hierarchical NiFeOOH@CeO_2−x nanosheets array boosts electrocatalytic activity and durability at high current densities for water oxidation

Wei Zhang, Liyang Xiao, Xiaorui Huang, Chunyan Han, Ying Liu, Jingtong Zhang, Haiwen Tan, Rui Zhang, Pengfei Yin, Cunku Dong, Hui Liu, Xiwen Du, Jing Yang

()

Institute of New Energy Materials, Key Laboratory of Advanced Ceramics and Machining Technology of Ministry of Education, School of Materials Science and Engineering, Tianjin University, Tianjin 300072, China

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The hierarchical NiFeOOH@CeO_2−x nanosheets array achieves superior alkalineoxygen evolution reaction performance at high current densities, due to abundant activesites, favorable interfacial electron transfer from Ni^2+/3+ to Ce^3+/4+, and improvedelectrical conductivity owning to oxygen vacancies.

Abstract

The oxygen evolution reaction (OER) reaction kinetics of nickel-iron (oxy)hydroxides (NiFeOOH) is limited by their weak adsorption of OER intermediates. Herein, a hierarchical NiFeOOH@CeO_2−x nanosheets array was in situ grown on a nickel foam by a facile laser direct writing method, which exhibits superior OER activity and durability at high current densities in alkaline electrolytes. The hierarchical nanosheets array exposes abundant catalytic active sites, which greatly promote OER reaction rate. The strong electronic interaction at the NiFeOOH/CeO_2−x interface leads to favorable electron transfer from Ni²⁺/³⁺ and Fe³⁺ to Ce³⁺/⁴⁺. The Ni sites with high valences show enhanced OH⁻ adsorption and also promote the formation of *OOH intermediate, thereby greatly improving OER intrinsic activity. The oxygen deficient CeO_2−x primary sheets guarantee good electrical conductivity. Such a well-designed catalytic electrode requires overpotentials of only 229 and 287 mV to achieve current densities of 50 and 500 mA·cm⁻², respectively, and sustains superior stability at 500 mA·cm⁻² and 1 A·cm⁻².

Keywords

hierarchical nanosheets transition metal (oxy)hydroxides oxygen evolution reaction laser direct writing water splitting

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Volume 18 Issue 3,
March 2025

Article number: 94907213

DOI: 10.26599/NR.2025.94907213

Cite this article:

Zhang W, Xiao L, Huang X, et al. A hierarchical NiFeOOH@CeO_2−x nanosheets array boosts electrocatalytic activity and durability at high current densities for water oxidation. Nano Research, 2025, 18(3): 94907213. https://doi.org/10.26599/NR.2025.94907213

Figure 1The synthetic route of hierarchical NiFeOOH@CeO_2−x nanosheets arrays.
Figure 2(a) XRD patterns of NiFeOOH@CeO_2−x/NF, CeO₂/NF and NF. (b) SEM image of NiFeOOH@CeO_2−x /NF. (c) AFM image of NiFeOOH@CeO_2−x/NF and the corresponding height profile. (d) Raman spectra of NiFeOOH@CeO_2−x /NF, CeO₂/NF and NiFeOOH/NF. (e) TEM image of NiFeOOH@CeO_2−x, the inset is SAED pattern of partial region. (f) HR-TEM image of NiFeOOH@CeO_2−x. (g) STEM image and EDS elemental mapping images of Ni, Fe, and Ce for NiFeOOH@CeO_2−x. (h) STEM image and EDS elemental mapping images of Ni, Fe, and Ce for NiFeOOH. (i) EPR spectra of NiFeOOH@CeO_2−x /NF, NiFeOOH@CeO₂/NF, NiFeOOH/NF, and CeO₂/NF.
Figure 3Ni 2p (a) and Fe 2p (b) XPS spectra of NiFeOOH@CeO_2−x/NF, NiFeOOH@CeO₂/NF and NiFeOOH/NF. Ce 3d (c) and O 1s (d) XPS spectra of NiFeOOH@CeO_2−x/NF, NiFeOOH@CeO₂/NF, NiFeOOH/NF and CeO₂/NF.
Figure 4(a) OER LSV curves with 85% iR-compensation of NiFeOOH@CeO_2−x/NF, NiFeOOH@CeO₂/NF, NiFeOOH/NF, and CeO₂/NF. (b) Comparison of the overpotentials at 50 and 500 mA·cm⁻². (c) Tafel plots. (d) EIS Nyquist plots. (e) Capacitive current plotted as a function of different scan rates. (f) Specific activities at the potential of 1.49 V vs. RHE with ECSA correction. (g) The M–S plots. (h) i–t curve of NiFeOOH@CeO_2−x/NF at 500 mA·cm⁻² for 280 h. (inset: LSV curves of NiFeOOH@CeO_2−x /NF before and after 280 h of continuous electrolysis).
Figure 5(a) Current density of NiFeOOH@CeO_2−x/NF, NiFeOOH@CeO₂/NF and NiFeOOH/NF at 1.49 V vs. RHE in electrolytes with different concentrations of KOH. The inset is the dependence of the j_KOH in different concentrations of KOH. In situ Raman patterns of (b) NiFeOOH@CeO_2−x/NF, (c) NiFeOOH@CeO₂/NF and (d) NiFeOOH/NF at potential from 1.1 to 1.6 V.
Figure 6(a) LSV polarization curves of PtNi/NF and Pt/C/NF for HER, NiFeOOH@CeO_2−x/NF and RuO₂/NF for OER at scan rate 5 mV·s⁻¹ in 1 M KOH. (b) LSV polarization curve of overall water splitting electrolyzer composed of PtNi/NF||NiFeOOH@CeO_2−x/NF and Pt/C/NF||RuO₂/NF in 1.0 M KOH. (c) Cell voltage of overall water splitting electrolyzer based on theoretical and measured values at different current densities. (d) Long-term durability of overall water splitting at a current density of 500 mA·cm⁻². Inset is an optical photograph of the water splitting electrolyzer. (e) Polarization curves of alkaline water electrolysis single cell under industrial conditions.

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