Oxygen-deficient MoOx/Ni3S2 heterostructure grown on nickel foam as efficient and durable self-supported electrocatalysts for hydrogen evolution reaction

doi:10.1007/s11705-022-2228-1

Front. Chem. Sci. Eng.

2023, Vol. 17

Issue (4) : 437-448 https://doi.org/10.1007/s11705-022-2228-1

RESEARCH ARTICLE

Oxygen-deficient MoO_x/Ni₃S₂ heterostructure grown on nickel foam as efficient and durable self-supported electrocatalysts for hydrogen evolution reaction

Zihuan Yu¹, Haiqing Yan¹, Chaonan Wang¹, Zheng Wang¹, Huiqin Yao²(

), Rong Liu³(

), Cheng Li⁴(

), Shulan Ma¹(

)

¹. Beijing Key Laboratory of Energy Conversion and Storage Materials, College of Chemistry, Beijing Normal University, Beijing 100875, China
². School of Basic Medical Sciences, Ningxia Medical University, Yinchuan 750004, China
³. Analytical and Testing Center, Beijing Normal University, Beijing 100875, China
⁴. Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China

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Abstract

High-performance and ultra-durable electrocatalysts are vital for hydrogen evolution reaction (HER) during water splitting. Herein, by one-pot solvothermal method, MoO_x/Ni₃S₂ spheres comprising Ni₃S₂ nanoparticles inside and oxygen-deficient amorphous MoO_x outside in situ grow on Ni foam (NF), to assembly the heterostructure composites of MoO_x/Ni₃S₂/NF. By adjusting volume ratio of the solvents of ethanol to water, the optimized MoO_x/Ni₃S₂/NF-11 exhibits the best HER performance, requiring an extremely low overpotential of 76 mV to achieve the current density of 10 mA∙cm^‒2 (η₁₀ = 76 mV) and an ultra-small Tafel slope of 46 mV∙dec^‒1 in 0.5 mol∙L^‒1 H₂SO₄. More importantly, the catalyst shows prominent high catalytic stability for HER (> 100 h). The acid-resistant MoO_x wraps the inside Ni₃S₂/NF to ensure the high stability of the catalyst under acidic conditions. Density functional theory calculations confirm that the existing oxygen vacancy and MoO_x/Ni₃S₂ heterostructure are both beneficial to the reduced Gibbs free energy of hydrogen adsorption (|∆G_H*|) over Mo sites, which act as main active sites. The heterostructure effectively decreases the formation energy of O vacancy, leading to surface reconstruction of the catalyst, further improving HER performance. The MoO_x/Ni₃S₂/NF is promising to serve as a highly effective and durable electrocatalyst toward HER.

Keywords molybdenum oxides oxygen vacancies heterostructure electrocatalysts hydrogen evolution reaction

Corresponding Author(s): Huiqin Yao,Rong Liu,Cheng Li,Shulan Ma

Online First Date: 17 January 2023 Issue Date: 24 March 2023

Cite this article:

Zihuan Yu,Haiqing Yan,Chaonan Wang, et al. Oxygen-deficient MoO_x/Ni₃S₂ heterostructure grown on nickel foam as efficient and durable self-supported electrocatalysts for hydrogen evolution reaction[J]. Front. Chem. Sci. Eng., 2023, 17(4): 437-448.

URL:

https://academic.hep.com.cn/fcse/EN/10.1007/s11705-022-2228-1
https://academic.hep.com.cn/fcse/EN/Y2023/V17/I4/437

Scheme1 Schematic illustration of formation of oxygen-deficient MoO_x/Ni₃S₂/NF composites.

Fig.1 XRD patterns of (a) MoO_x/Ni₃S₂/NF-01, (b) MoO_x/Ni₃S₂/NF-11 and (c) MoO_x/Ni₃S₂/NF-21.

Fig.2 SEM images of (a, a′) MoO_x/Ni₃S₂/NF-01, (b, b′) MoO_x/Ni₃S₂/NF-11 and (c, c′) MoO_x/Ni₃S₂/NF-21.

Fig.3 (a, b) TEM images of MoO_x/Ni₃S₂-11, (c, d, e) HR-TEM images of MoO_x/Ni₃S₂-11, and the visible lattice fringes images obtained from the blue and yellow square regions; (f) SAED pattern of MoO_x/Ni₃S₂-11; (g) HAADF-STEM and energy dispersive spectroscopy elemental mappings of Mo, O and Ni of MoO_x/Ni₃S₂-11; (h) electron paramagnetic resonance (EPR) spectrum of MoO_x/Ni₃S₂/NF-11 before and after 60 h I–t test, and the control sample of com-MoO₃.

Fig.4 X-ray photoelectron spectra with deconvolution of (a) Mo 3d, (b) O 1s for MoO_x/Ni₃S₂/NF-11 and com-MoO₃, (c) Ni 2p, and (d) S 2p for MoO_x/Ni₃S₂/NF-11.

Tab.1 HER performance of MoO_x/Ni₃S₂/NF-11 and some reported electrocatalysts in 0.5 mol·L^?1 H₂SO₄

Fig.5 (a) Polarization curves of MoO_x/Ni₃S₂/NF-11, com-MoO₃/NF, Ni₃S₂/NF and Pt–C/NF; (b) Tafel slopes of MoO_x/Ni₃S₂/NF-11, com-MoO₃/NF and Pt–C/NF derived from polarization curves; (c) Nyquist plots of MoO_x/Ni₃S₂/NF-11, com-MoO₃/NF and Pt–C/NF at ?200 mV versus RHE measured from electrochemical impedance spectroscopy (EIS) in the frequency range from 10⁵ to 0.01 Hz; (d) plots of current density as a function of scan rates for MoO_x/Ni₃S₂/NF-11, com-MoO₃/NF and Pt–C/NF; (e) chronoamperometric curve of MoO_x/Ni₃S₂/NF-11 at a constant applied potential of ?180 mV versus RHE; (f) polarization curves of before and after 100 h I–t test of MoO_x/Ni₃S₂/NF-11. All the measurements were performed in a 0.5 mol·L^?1 H₂SO₄ electrolyte.

Fig.6 (A) Optimized structures of (a) MoO₃, (b) O_v-MoO₃, (c) MoO₃/Ni₃S₂, (d) O_v-MoO₃/Ni₃S₂ with H^* on O site and (e) O_v-MoO₃/Ni₃S₂ with H^* on Mo site and the corresponding H adsorption free energy (ΔG_H*) at a potential U = 0 V relative to standard hydrogen electrode at pH = 0; (B) differential charge density distribution of O_v-MoO₃/Ni₃S₂; (C) vacancy formation energy of O_v-MoO₃/Ni₃S₂ and O_v-MoO₃ and corresponding models. Symbols for atoms: Mo is cyan in A and C while purple in B, S is yellow, Ni is blue in A and C while grey in B, O is red and H^* is white. The dotted box shows the position of oxygen vacancy.

Fig.7 XPS spectra of (a) Ni 2p, (b) O 1s, and (c) S 2p for MoO_x/Ni₃S₂/NF-11 before and after HER testing, and (d) Mo 3d for MoO_x/Ni₃S₂/NF-11 after HER testing.

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