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Article

Coupling Interface Construction of Ni(OH)2/MoS2 Composite Electrode for Efficient Alkaline Oxygen Evolution Reaction

by
Ge Liu
1,
Xuezhi Ouyang
1,
Xue-Ling Wei
2,*,
Wei-Wei Bao
2,
Xiao-Hua Feng
1 and
Jun-Jun Zhang
1,3,*
1
School of Materials Science and Chemical Engineering, Xi’an Technological University, Xi’an 710021, China
2
National & Local Joint Engineering Laboratory for Slag Comprehensive Utilization and Environmental Technology, School of Material Science and Engineering, Shaanxi University of Technology, Hanzhong 723000, China
3
State Key Laboratory of High-Efficiency Utilization of Coal and Green Chemical Engineering, College of Chemistry & Chemical Engineering, Ningxia University, Yinchuan 750021, China
*
Authors to whom correspondence should be addressed.
Catalysts 2022, 12(9), 966; https://doi.org/10.3390/catal12090966
Submission received: 5 August 2022 / Revised: 25 August 2022 / Accepted: 26 August 2022 / Published: 29 August 2022
(This article belongs to the Special Issue Advanced Catalysts for Achieving Hydrogen Economy from Liquids)
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Abstract

:
The transition metal-based catalysts have excellent electrochemical oxygen evolution reaction catalytic activity in alkaline electrolytes, attracting a significant number of researchers’ attention. Herein, we used two-step hydrothermal and solvothermal methods to prepare a Ni(OH)2/MoS2/NF electrocatalyst. The electrocatalyst displayed outstanding OER activity in 1.0 M KOH electrolyte with lower overpotential (296 mV at 50 mA·cm−2) and remarkable durability. Comprehensive analysis shows that reinforcement of the catalytic function is due to the synergistic effect between Ni(OH)2 and MoS2, which can provide more highly active sites for the catalyst. This also provides a reliable strategy for the application of heterogeneous interface engineering in energy catalysis.

Graphical Abstract

1. Introduction

The increasing use of energy consumption and serious environmental pollution have forced us to look for renewable energy [1,2]. Hydrogen is considered a promising energy source because of its low cost, sustainability and high energy density [3,4]. Currently, hydrogen production by electrolysis of water is considered to be the most efficient method [5,6]. The water splitting process can be divided into two reactions: oxygen evolution reaction (OER) and hydrogen evolution reaction [7,8]. However, the OER involves four electron and proton transfer processes, more energy needs to be expended than HER [9,10]. In general, catalysts can effectively lower the energy barrier required for the reaction [11]. For example, Pt-based catalysts, Ir-based catalysts and other noble metal catalysts have excellent catalytic activity. Nevertheless, noble metal catalysts are expensive due to their limited reserves on the Earth, which restrict their large-scale commercial applications [12,13]. Therefore, there is a need to develop highly active, inexpensive, durable and stable metal-based catalysts [14,15].
Transition metal hydroxides have the advantages of simple synthesis, low production cost and excellent electrochemical performance [16,17]. Nickel hydroxides are considered to be a good catalyst for water electrolysis [18]. However, the poor electronic conductivity and slow ion transfer rate of single transition metal hydroxides hinder further performance optimization [19,20]. Transition metal dihalide (MX2, M stands for transition metal, X stands for chalcogenides S, Te or Se) have attracted enormous attention due to their high electrochemical performance [21]. MoS2 is deemed to a promising non-noble metal catalyst [22,23]. MoS2 possess a lamellar configuration with feeble interlayer van der Waals forces [24]. At present, MoS2 is widely used as an electrocatalyst for hydrogen production because of its excellent HER performance [25]. Theoretical calculation shows that the MoS2 active sites for HER are at the edge [26]. A large number of unsaturated sulfur atoms at the edge can easily adsorb H, generating hydrogen on the surface of MoS2 [21,27]. Similarly, the OER active center of MoS2 is also located at the edge [28]. It has been reported that MoS2 can be used to enhance the OER activity through heteroatom-doping, changing the electronic structure, and constructing a hetero-cooperative interface [6,29,30,31]. Moreover, the intrinsic conductivity and surface electronic structure of electrocatalysts determine the level of electrochemical activity [32]. In general, the heterostructures formed can adjust their electronic configuration and thus improve electrical conductivity [19,20,21,22,23,33,34].
Based on the above understandings, in this paper, a Ni(OH)2/MoS2/NF composite electrode was constructed using the two-step hydrothermal and solvothermal methods for OER. The 50 and 100 mA·cm−2 current density correspond to the 296 and 314 mV overpotential. The prominent electrochemical function comes from the self-supporting effect of NF and the synergistic effect of the formed heterostructures. It provides an idea for the subsequent preparation of non-noble metal catalysts with heterostructures structures for OER.

2. Results

Here, the Ni(OH)2/MoS2/NF composite electrode was fabricated using the two-step hydrothermal/solvothermal method, as shown in Figure 1. Ni(OH)2 three dimensional arrays were anchored on NF by simple hydrothermal method. Further, the MoS2 substance was grown on Ni(OH)2 nanosheets through the secondary solvothermal process. The specific experimental process can be seen in the Supplementary Materials. The Ni(OH)2 nanosheets were grown directly on the NF, avoiding use of binders and providing more active area. Additionally, the Ni(OH)2 nanosheets are overlapped, providing more load position for the granular MoS2 [35]. The heterostructures can not only enhance the catalytic activity of the catalyst by electron transfer between different components, but also increase the number of active centers [36,37]. The XRD measurement peaks of the powders collected in the first step belonged to Ni(OH)2 powders, corresponding to JCPDS NO. 38-0715 (Figure S1), indicating that Ni(OH)2 was successfully prepared. The XRD measurement peaks of the powders collected in the second step belonged to the MoS2 phase. The peak at (002) is significantly shifted compared to the standard card, probably because of a small change in the interlayer spacing [29].
The microstructure of the electrode was investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). NFs are interconnected three-dimensional network structures and have a smooth surface (Figure S3). Ni(OH)2/NF exhibits a layer-by-layer stack of thin nanosheet structures (Figure S4). The MoS2/NF electrode exhibits flower-like structure assembled by uniformly distributed nanosheets (Figure S5). Figure 2a and Figure S6 show that the Ni(OH)2/MoS2/NF composite electrode has the structure of Ni(OH)2 and MoS2, which can preliminarily determine the required composite electrode. Apparently, the small MoS2 assemblies grows on the large two-dimensional Ni(OH)2 lamellar structure, which can provide many composite interfaces and thus enhance the synergistic effect of the heterostructure [38,39]. We can adjust the proportion of components to prepare catalytic samples with different proportions (Figure S7). Figure 2b exhibits the TEM image of Ni(OH)2/MoS2/NF. Ni(OH)2 is a laminated structure and MoS2 assemblies are covered on the nanosheets. It can be measured from Figure 2c that the lattice spacing of 0.405 nm and 0.610 nm correspond to the (006) crystal face of Ni(OH)2 and (002) crystal face of MoS2, respectively. The results further prove that we have obtained the electrode with heterogeneous Ni(OH)2 and MoS2 structure. Figure 3 is an elemental mapping images of duan electrode, in which Ni, Mo, S and O elements are evenly distributed in the composite structure. Meanwhile, combing the SEM image and TEM image, successful preparation of integrated electrodes was demonstrated.
The OER performance of composite electrodes was tested. Simultaneously, the catalytic ability of Ni(OH)2/NF, MoS2/NF and bare NF were contrasted (see Supplementary Materials for details). The polarization curve results show that the dual Ni(OH)2/MoS2/NF electrode has the best OER catalytic activity contrasted with other comparative electrodes (Figure 4a). Figure 4b shows that the overpotential of each electrode at 50 and 100 mA·cm−2 current outputs. Generally speaking, the lower the overpotential, the better the catalytic performance [36]. Compared with the individual Ni(OH)2 or MoS2 catalyst, the Ni(OH)2/MoS2/NF exhibits the smallest overpotentials (296 mV at 50 mA·cm−2 current output, 314 mV at 100 mA·cm−2). Furthermore, the overpotential is smaller in contrast with many reported water oxidation electrocatalysts, such as Ti@NiCo2O4 (353 mV at 10 mA·cm−2), CoCr LDH (340 mV at 10 mA·cm−2) and Ni/NiO (470 mV at 10 mA·cm−2), for details see Supplementary Table S1 and Figure 5.
Electrochemical impedance spectroscopy (EIS) can describe the interface properties between electrode and the electrolyte, and it is a powerful means to indicate interfacial charge transfer. The size of the arc in the EIS is related to the electrode surface charge transfer resistance. The small arc radius in the EIS represents the small charge transfer resistance of the catalytic electrode, and also represents the fast dynamic response [40,41]. As show in Figure 4c, the arc size of the dual electrode is smallest, indicating its robust catalytic reaction kinetics. The small Tafel slope means a favorable electron transfer rate and a faster water oxidation rate [42]. As shown in Figure 4d, the Ni(OH)2/MoS2/NF possesses the smallest Tafel slope (63 mV·dec−1), indicating the robust catalytic kinetics of water oxidation [43].
Stability is an indicator of whether the catalyst can be used commercially on a large scale [44]. The stability of the composite electrode was tested using multi-step potential and multi-step current methods, as shown in Figure 6a,b, the Ni(OH)2/MoS2/NF has excellent stability. Cyclic voltammetry (CV) is an important standard to verify the durability. Figure 6c depicts the polarization curves before and after 500 CV cycles. It can be seen that the polarization curve does not change significantly. The EIS spectra in Figure 6d also exhibit the same result, indicating that the catalytic electrode has excellent stability. In the meantime, the chronoamperometric test was performed on the composite electrode. After 15 h of operation at constant potential, the composite electrode did not appear to have obvious decay (Figure S8). We studied the morphology and structure of the electrode before and after the test, and the morphology and electronic structure of the electrode can be maintained well after a long time running (Figures S9 and S10).

3. Discussion

The element valence states were analyzed using X-ray photoelectron spectroscopy (Figure S11). To ulteriorly comprehend the reason of activity enhancement, the XPS spectra of single component and composite electrodes were compared, as shown in Figure 7. In the XPS spectrum of Ni 2p, there are two main peaks (855.4 and 873 eV), corresponding to Ni 2p3/2 and Ni 2p1/2 of Ni2+ (Figure S11b) [45]. This result further confirms the existence of Ni(OH)2 [46]. Moreover, compared with the Ni(OH)2 electrode, the peaks of Ni 2p3/2 and Ni 2p1/2 in composite electrode are shifted to higher energy. Figure 7b is the XPS spectrum of Mo 3d. The peak at 232.56 eV is Mo 3d3/2 orbital. The peak at 234.84 eV is assigned to Mo6+ (Figure S11c) [47]. Comparing the Mo 3d of MoS2/NF and the combined electrode, it can be seen that the peak of Mo 3d3/2 has shifted to a lower energy. The phenomenon of peak shift indicates that the electron density of Ni and Mo ions has changed, and electron transfer has occurred in Ni(OH)2/MoS2/NF electrode [48]. According to the change of electron density, we can preliminarily determine that part of electron transfer from Ni(OH)2 to MoS2 occurred at the interface of the composite electrode [49]. The representative peaks (160.92 eV and 162.03 eV) correspond to S 2p3/2 and S 2p1/2. The nearby peak at 163.00 eV is S22−, indicating the existence of MoS2. More importantly, the peak (168.90 eV) proves the existence of the S-Ni bond. [50]. This result strongly suggests an interface between Ni(OH)2 and MoS2. The C 1s and O 1s peaks in the composite electrode were also analyzed and the results were presented in the Supplementary Material (Figure S11e,f). These results all indicate electron redistribution at the interface of the catalytic electrode, which can effectively expedite the rate of the reaction process and achieve higher catalytic activity. Furthermore, the electrochemical active area was measured (Figure S12). It was found that the Ni(OH)2/MoS2/NF composite electrode has a larger active area than the Ni(OH)2 electrode.

4. Materials and Methods

4.1. Materials

Nickel nitrate hexahydrate (Ni(NO3)2·6H2O), urea (CO(NH2)2) and ammonium fluoride (NH4F) were purchased from Tianjin Damao Chemical Reagent Factory (Tianjin, China). Ammonium tetrathiomolybdate ((NH4)2MoS4) and DMF were purchased from Aladdin Biochemical Technology Co., Ltd. (Shanghai, China). Nickel foam (NF) was used as the substrate. The thickness of the NF is about 1 mm. NF was firstly washed with HCl solution under ultrasonic, ethanol and water several times to remove the surface impurities. All the chemicals were used without further purification.

4.2. Materials Synthesis

Synthesis of Ni(OH)2/NF. An aqueous solution (25 mL) containing 1.5 mmol (0.436 g) Ni(NO3)·6H2O, 7.5 mmol (0.455 g) CO(NH2)2 and 4 mmol (0.148 g) NH4F was treated with ultrasound to accelerate dissolution. Then, the solution was encapsulated into the 50 mL PTFE-lined stainless steel reactor, and the pre-treated Ni foam was placed against the inner wall of the reactor. The reaction temperature and time were set as 120 °C and 4 h, respectively. At the end of the reaction, the nickel substrate was cleaned and dried. Powder samples from the bottom of the reactor were also collected.
Synthesis of Ni(OH)2/MoS2/NF. An amount of 0.021 g (NH4)2MoS4 and 35 mL DMF were added into a 50 mL PTFE-lined stainless steel reactor. Then, Ni(OH)2/NF was placed against the inner wall of the reactor. The reaction temperature and time were set as 200°C and 10 h, respectively. The MoS2/NF electrode was prepared by the similar method. When the quantity of (NH4)2MoS4 was set to 0.013 g and 0.030 g, the obtained samples were labeled as Ni(OH)2/MoS2/NF-13 and Ni(OH)2/MoS2/NF-30.

4.3. Materials Characterizations

XRD pattern measurements were performed using a Bruker D8 X-ray diffractometer (Bruker AXS GmbH, Karlsruhe, Germany) using Cu Kα radiation (40 kV, 30 mA, λ = 1.5406 Å). The SEM images were collected on JSM-7610F (JEOL, Tokyo, Japan) scanning electron microscope at 10 kV. TEM and HRTEM images were performed using a JEM-F200 (JEOL, Tokyo, Japan) microscope. XPS measurements were performed using the Axis Ultra DLD (Kratos, Stretford, UK) X-ray photoelectron spectrometer.

4.4. Electrochemical Characterizations

Electrochemical tests were all acquired on a CHI-660E electrochemical workstation (CHI Instruments, Shanghai, China) using a standard three-electrode system. Ni(OH)2/MoS2/NF electrodes, carbon rods and a Hg/HgO electrode served as work electrodes, counter electrode and reference electrode, respectively. The electrolyte was 1.0 M KOH. The linear sweep voltammetry (LSV) curve was scanned at a rate of 10 mV/s and calibrated using iR correction. The measurement frequency range for electrochemical impedance spectroscopy (EIS) was 0.1 to 105 Hz. The Overpotential η (mV) = ((E vs. RHE) − 1.23) × 1000. The potential was converted to the potential versus the reversible hydrogen electrode (RHE) using the relationship, ERHE = EHg/HgO + E0Hg/HgO + 0.059 pH. E0Hg/HgO = 0.098V (25 °C).

5. Conclusions

In summary, we constructed a Ni(OH)2/MoS2/NF composite electrode with heterostructures using two-step hydrothermal/solvothermal methods. The Ni(OH)2/MoS2/NF electrode displayed excellent oxygen evolution reaction performance. The Ni(OH)2/MoS2/NF possesses lower overpotential (296 mV at 50 mA·cm−2) and Tafel slope (63 mV·dec−1). The good OER performance is ascribed to the synergistic effect of composite interface, which accelerates the electron transport and increases the OER rate of the water splitting process. The method can be applied to other interface engineering to design OER catalytic electrodes.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/catal12090966/s1, Figure S1. The XRD pattern of Ni(OH)2 powder. Figure S2. The XRD pattern of MoS2 powder. Figure S3. High resolution scanning electron microscopy with NF at different magnifications. Figure S4. High resolution scanning electron microscopy of Ni(OH)2/NF at different magnifications. Figure S5. High resolution scanning electron microscopy of MoS2/NF at different magnifications. Figure S6. High resolution scanning electron microscopy of Ni(OH)2/MoS2/NF at different magnifications. Figure S7. Scanning electron microscopy images of (a) Ni(OH)2/MoS2/NF-13 and (b) Ni(OH)2/MoS2/NF-30 electrodes. Figure S8. The chronoamperometry measurement of Ni(OH)2/MoS2/NF composite electrodes. Figure S9. High-resolution XPS (a) Ni 2p, (b) Mo 3d, (c) S 2p and (d) O 1s of Ni(OH)2/MoS2/NF electrode before and after long-time stability test. Figure S10. The SEM image of Ni(OH)2/MoS2/NF electrode after long-time stability test. Figure S11. (a) XPS survey spectra, (b) Ni 2p, (c) Mo 3d, (d) S 2p, (e) C 1s and (f) O 1s of Ni(OH)2/MoS2/NF electrode. Figure S12. CV curves of the (a) Ni(OH)2/NF and (b) Ni(OH)2/MoS2/NF electrodes measured at different scan rates from 20 to 100 mV s−1 in a potential window without faradaic processes. (c) Plots of the current density vs. the scan rates for Ni(OH)2/NF and Ni(OH)2/MoS2/NF electrodes. Table S1. Comparison of OER performance of Ni(OH)2/MoS2/NF catalyst with other reports. References [51,52,53,54,55,56,57,58,59,60,61,62] are cited in the Supplementary Materials.

Author Contributions

Conducted the synthesis of the electrodes and carried out corresponding characterizations, G.L. and X.-L.W.; writing—review and editing, helped to conduct data analysis and revised the manuscript, W.-W.B., X.-H.F. and X.O.; conceptualization, J.-J.Z.; analysis, J.-J.Z.; funding acquisition J.-J.Z.; writing—original draft J.-J.Z. All authors have read and agreed to the published version of the manuscript.

Funding

This work was supported by the National Natural Science Foundation of China (Grant No. 21902123), the Fundamental Research Fund for the Undergraduate Innovation Project (S202110702085) and the support of the Research Fund for the Doctoral Program of Xi’an Technological University (Grant No. 0853-302020540).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Acknowledgments

We thank the funding support from the Science Funding Committee of China and the Science, Xi’an Technological University and Undergraduate Innovation Project.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. Schematic illustration of the synthesis.
Figure 1. Schematic illustration of the synthesis.
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Figure 2. (a) SEM image, (b) TEM image, (c) HR-TEM image of the Ni(OH)2/MoS2/NF electrocatalysts.
Figure 2. (a) SEM image, (b) TEM image, (c) HR-TEM image of the Ni(OH)2/MoS2/NF electrocatalysts.
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Figure 3. The corresponding element mapping of Ni(OH)2/MoS2/NF electrocatalysts: (a) STEM image; (b) Nickel; (c) Oxygen; (d) Molybdenum; (e) sulfur; (f) Overlay.
Figure 3. The corresponding element mapping of Ni(OH)2/MoS2/NF electrocatalysts: (a) STEM image; (b) Nickel; (c) Oxygen; (d) Molybdenum; (e) sulfur; (f) Overlay.
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Figure 4. (a) The iR-corrected polarization curves (b) a comparison of the corresponding overpotentials at 50 mA·cm−2 and 100 mA·cm−2 current outputs, (c) the electrochemical impedance spectroscopy (d) corresponding Tafel plot of the Ni(OH)2/MoS2/NF, MoS2/NF, Ni(OH)2/NF and bare NF electrodes.
Figure 4. (a) The iR-corrected polarization curves (b) a comparison of the corresponding overpotentials at 50 mA·cm−2 and 100 mA·cm−2 current outputs, (c) the electrochemical impedance spectroscopy (d) corresponding Tafel plot of the Ni(OH)2/MoS2/NF, MoS2/NF, Ni(OH)2/NF and bare NF electrodes.
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Figure 5. The comparison of OER performance for some representative non-noble electrocatalysts.
Figure 5. The comparison of OER performance for some representative non-noble electrocatalysts.
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Figure 6. (a) The multi-potential steps (b) the multi-current steps (c) the polarization curves of the Ni(OH)2/MoS2/NF electrode before and after 500 cycles cyclic voltammetry (d) electrochemical impedance spectra of Ni(OH)2/MoS2/NF electrode before and after 500 cycles of cyclic voltammetry.
Figure 6. (a) The multi-potential steps (b) the multi-current steps (c) the polarization curves of the Ni(OH)2/MoS2/NF electrode before and after 500 cycles cyclic voltammetry (d) electrochemical impedance spectra of Ni(OH)2/MoS2/NF electrode before and after 500 cycles of cyclic voltammetry.
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Figure 7. XPS spectra of (a) Ni 2p, (b) Mo 3d of Ni(OH)2, MoS2 and Ni(OH)2/MoS2/NF electrodes.
Figure 7. XPS spectra of (a) Ni 2p, (b) Mo 3d of Ni(OH)2, MoS2 and Ni(OH)2/MoS2/NF electrodes.
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Liu, G.; Ouyang, X.; Wei, X.-L.; Bao, W.-W.; Feng, X.-H.; Zhang, J.-J. Coupling Interface Construction of Ni(OH)2/MoS2 Composite Electrode for Efficient Alkaline Oxygen Evolution Reaction. Catalysts 2022, 12, 966. https://doi.org/10.3390/catal12090966

AMA Style

Liu G, Ouyang X, Wei X-L, Bao W-W, Feng X-H, Zhang J-J. Coupling Interface Construction of Ni(OH)2/MoS2 Composite Electrode for Efficient Alkaline Oxygen Evolution Reaction. Catalysts. 2022; 12(9):966. https://doi.org/10.3390/catal12090966

Chicago/Turabian Style

Liu, Ge, Xuezhi Ouyang, Xue-Ling Wei, Wei-Wei Bao, Xiao-Hua Feng, and Jun-Jun Zhang. 2022. "Coupling Interface Construction of Ni(OH)2/MoS2 Composite Electrode for Efficient Alkaline Oxygen Evolution Reaction" Catalysts 12, no. 9: 966. https://doi.org/10.3390/catal12090966

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