Full Water Splitting Electrocatalyzed by NiWO4 Nanowire Array - ACS

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Full Water Splitting Electrocatalyzed by NiWO4 Nanowire Array Yuyao Ji, Li Yang, Xiang Ren, Guanwei Cui, Xiaoli Xiong, and Xu-Ping Sun ACS Sustainable Chem. Eng., Just Accepted Manuscript • DOI: 10.1021/acssuschemeng.8b01841 • Publication Date (Web): 09 Jul 2018 Downloaded from http://pubs.acs.org on July 9, 2018

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ACS Sustainable Chemistry & Engineering

Full Water Splitting Electrocatalyzed by NiWO4 Nanowire Array Yuyao Ji,† Li Yang,# Xiang Ren,# Guanwei Cui,§ Xiaoli Xiong,†,* and Xuping Sun#,* †

College of Chemistry and Materials Science, Sichuan Normal University, Chengdu 610068, Sichuan, China, #Institute of Fundamental and Frontier Science, University of Electronic Science and Technology of China, Chengdu 610054, China, § College of Chemistry, Chemical Engineering and Materials Science, Shandong Normal University, Jinan 250014, Shandong, China. * E-mail: [email protected] (X.S.); [email protected] (X.X.) ABSTRACT: It is attractive to develop effective bifunctional electrocatalyst for full water splitting. In this Communcation, we report that NiWO4 nanowire array on Ti mesh (NiWO4/TM) is a high-performance and stable water-splitting electrocatalyst at alkaline pH. As a 3D electrocatalyst, such NiWO4/TM attains 20 mA cm–2 under overpotentials of 101 mV for cathodic water reduction and 322 mV for anodic water oxidation. We also demonstrate the use of NiWO4/TM to make a two-electrode electrolyzer capable of driving 20 mA cm–2 at a cell voltage of 1.65 V.

KEYWORDS: NiWO4 Nanowire Array, Full Water Splitting, 3D Electrocatalyst, High-performance, Alkaline Media.

INTRODUCTION

RESULTS AND DISCUSSION

Hydrogen is widely considered to be a sustainable way to take the place of the reducing fossil fuel.1,2 Water splitting can be considered as a mature commercial technique. It converts the electrical energy of intermittent renewable energy into chemical energy in hydrogen.3–5 Though providing a highly active way to fabricate high purity hydrogen, It is limited to the practical application of large-scale hydrogen production because of the powerful reaction with large potential (commercial electrolysis cells usually run under the battery voltage of 1.9-2.1 V, and it is larger than least value of 1.23 V). The catalysts for over water splitting are needed to overcome the huge overpotentials of water splitting and make the process efficiently. Platinum shows the highest activity for hydrogen evolution reaction (HER)6 and Ir-, Ru-based electrocatalysts show the highly oxygen evolution reaction (OER) activity.7 Because their high cost limits its wide application, the design of efficient catalysts based on the earth's rich elements is attractive.

NiWO4 is an interesting functional material for hydrodesulfurization36 and supercapacitors37-39. Compared to its single metal oxide, NiWO4 has higher electrical conductivity,39 promising its use as an electrocatalyst with enhanced performance. Srirapu et al. reported that NiWO4 nanoparticle is efficient for the OER and NiWO4 on nickel demands 363 mV to attain 10 mA cm-2 under alkaline conditions,40 but its use as a bifunctional catalyst for water splitting has not been explored before. Herein, we report the development of NiWO4 nanowire array on Ti mesh (NiWO4/TM) used as a durable bifunctional electrocatalyst for full water splitting. Such NiWO4 NA/TM needs 101 mV to approach 20 mA cm–2 for the HER and 322 mV for OER. We also demonstrate the use of NiWO4/TM to make a two-electrode electrolyzer, capable of driving water-splitting current of 20 mA cm–2 under a cell voltage of 1.65 V.

In recent years, considerable research has been done to develop non-noble-metal electrocatalysts for HER. (chalcogenide,8–10, nitride,11 carbides,12,13 phosphide6,14–17) and OER (oxide,18–21 hydroxide,22–25 chalcogenide,26-28 phosphide29–31). In order to maintain the full water splitting, using a bifunctional could reduce the cost and operate water splitting catalysts are essential. Recent work demonstrates that direct growth of nanoarrays has obvious advantages (for example, lowering resistance, exposing more active centers and facilitating gas diffusion.32–35) As such, it is essential to exploit bifunctional nanoarray electrocatlysts for efficient water electrolysis.

Figure 1a shows the XRD pattern of NiWO4/TM. It shows diffraction peaks at 16.3°, 31.2°, 33.6°, 35.7°, 51.2°, and 71.6° indexed to the (111), (125), (113), (365), (425), and (311) planes of crystalline NiWO4 phase (JCPDS No. 15-0755), respectively. Figure 1b shows the SEM image Ti mesh is completely overlaped by nanowire array. Cross-section analysis for NiWO4/TM shows the nanoarray is about 6.1 µm in height (Figure S1). In Figure 1d, HRTEM image taken from a NiWO4 nanowire in Figure 1c presents uniform and welldefined lattice fringes. The interval is determined as 0.53 nm, indexed to the (201) plane of NiWO4 phase.

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comparison, we also tested another three catalyst electrodes: Ti mesh, Pt/C deposited on TM, NiWO4/GCE (prepared by immobilization of NiWO4 nanowires scratched down from TM using a polymer binder on glassy carbon electrode). The iR correction is applied to initial exerimental data except otherwise stated.43 Figure 2a demonstrates the LSV curves for all four electrodes. As observed, bare TM shows poor HER activity while Pt/C on TM is highly active for catalyzing the HER. NiWO4/TM has a better HER activity, 130 mV less than that for NiWO4/GCE, outperforming many HER catalysts (Table S1). Of note, other substrates like carbon cloth and nickel foam can also be used for NiWO4 nanoarray growth with toward efficient hydrogen evolution electrocatalysis (Figure S2).

Figure 1. (a) XRD pattern and (b) SEM images of NiWO4/TM. TEM image of (c) NiWO4/TM. (d) HRTEM image of NiWO4. XPS spectra for NiWO4 in the (e) Ni 2p, (f) W 4f, and (g) O 1s regions.

Figure 1e-g shows the XPS spectra for NiWO4. The BEs at 855.4and 873.0 eV are attributed to Ni 2p3/2 and Ni 2p1/2, respectively.41 The BEs for W 4f7/2 and W 4f5/2 appear at 37.1 and 34.8 eV, respectively, which are attributed to W6+ in WO3(Figure 1f).42 In the O 1s region (Figure 2d), the peak with BE of 531.6 eV in C 1s region is attributed to carbonate.

We also applied Tafel plots to evaluate the intrinsic catalytic kinetics of catalysts (Figure 2b). NiWO4/TM shows a small Tafel (51 mV dec–1), while NiWO4/GCE has a big Tafel of 114 mV dec–1, it shows that a rapid catalytic kinetics for HER on NiWO4/TM electrode. After 500 CV cycles, the current density loss of the LSV curve of the NiWO4/TM electrode is negligible compared with the initial density (Figure 2c), suggesting the high stability of NiWO4/TM. The result of bulk water electrolysis also demonstrates the stable HER performance for 12 h under alkaline conditions (Figure 2d). The excellent activity of NiWO4/TM can be retaionally attributed to the following reasons.44 (1) Directly growing NiWO4 on TM ensures intimate contact, and excellent electrical connection between them. (2) The 1D nanoarray is capable of vectorial electron transport and the open spaces between the nanoarrays are good for more efficient use of active sites. (3) Its binder-free feature enhances the conductivity. Moreover, the impedance analysis reveals the NiWO4/TM has a better charge transfer efficiency than NiWO4/GCE (Figure S3).

Figure 3. (a) LSV of NiWO4/TM, RuO2/TM, and Ti mesh. (b) Tafel for NiWO4/TM and RuO2/TM. (c) OER for NiWO4/TM before and after 500 cycles for. (d) Chronopotentiometry curve for NiWO4/TM under 330 mV for 10 h without iR correction. Figure 2. (a) LSV curves of NiWO4/TM, Ti mesh, Pt/C, and NiWO4/GCE. (b) Tafel for Pt/C, NiWO4/TM, and NiWO4/GCE. (c) LSV curves for NiWO4/TM before and after 500 cycles. (d) Chronopotentiometry curve for NiWO4/TM under 156 mV for 10 h without iR correction. The HER activity of the NiWO4/TM electrode (NiWO4/TM loading: 1.7 mg cm–2) was probed in 1.0 M KOH. For

Our NiWO4/TM is also superior in activity for OER catalysis. Figure 3a presents the polarization curves. RuO2/TM shows good OER activity, however, the bare TM has poor OER activity. To afford 20 mA cm–2, our NiWO4/TM requires 322 mV overpotential, comparing favourably to the behaviours of many recent OER catalysts (Table S2). Note that it even compares favourably to RuO2/TM (j = 60 mA cm-2)In Figure 3b, NiWO4/TM owns a Tafel slope of 45 mV dec–1. This value is


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even smaller than that for RuO2/TM (49 mV dec–1), revealing the fast catalytic kinetics of NiWO4/TM for OER. The polarization curve for NiWO4/TM after 500 CV cycles shows almost no changes (Figure 3c). It also shows good durability (Figure 3d). It should be mentioned that although tungsten and tungsten oxides are known to be unstable in alkaline media, our NiWO4 catalyst is robust enough against the alkaline conditions. XRD analysis (Figure S4) and SEM image (Figure S5) shows that the catalyst is still NiWO4 in nature after OER electrolysis. The XPS and HRTEM results further reveal the surface oxidation of NiWO4 to form NiOOH during the OER process (Figure S6). The inductively coupled plasma mass spectrometry (ICP-MS) analysis suggest a very slight change in the molar ratio of Ni/W from roughly 1:1 to 1.0:0.97 after the stability test, excluding the possibility of catalyst dissolution to leave pure Ni. Actually, pure nickel catalyst has lower OER activity (370 mV@10 mA cm–2) and is also highly stable (Figure S7). Considering that NiWO4/TM is superior in catalytic activity, we thus made a two-electrode electrolyser using one NiWO4/TM as anode and another as cathode for full water splitting. For more fair comparison, we also examined the water splitting performance for Pt/C||RuO2 electrolyser. Figure 4a shows that Pt/C||RuO2 needs a low cell voltage of only 1.60 V@20 mA cm−2. Of note, NiWO4/TM||NiWO4/TM is also efficient for overall water splitting under a cell voltage of 1.65 V, outperforming some reported systems like EG/Co0.85Se/NiFe-LDH (1.71 V)45 and NiCoP NSAs (1.77 V).46 Table S3 shows the comparison with other catalytic. Chronopotentiometry curve of NiWO4/TM||NiWO4/TM at a constant cell voltage of 1.65 V shows that this two-electrode water electrolyser has a good electrochemical durability. (Figure 4b).

AUTHOR INFORMATION Corresponding Author *

E-mail: [email protected] (X.S.); [email protected] (X.X.)

Notes The authors declare no competing financial interest.

ACKNOWLEDGMENT This work was supported by the National Natural Science Foundation of China (No. 21575137). We also appreciate Hui Wang from the Analytical & Testing Center of Sichuan University for her help with SEM characterization.

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Figure 4. (a) LSV of Pt/C||RuO2 and NiWO4/TM||NiWO4/TM. (b) Chronopotentiometry curve of NiWO4/TM||NiWO4/TM under a constant cell voltage of 1.65 V for 10 h.

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CONCLUSIONS In summary, NiWO4 nanowire array is proposed as an efficient bifunctional electrocatalyst for alkaline water electrolysis. Such electrocatalyst needs overpotentials of 101 mV for the HER and 322 mV for OER to approach 20 mA cm–2 in 1.0M KOH. Moreover, its two-electrode water electrolyzer can attain 20 mA cm-2 water-splitting current under a low cell voltage of 1.65 V. This work not only provides us an attractive nanoarray catalyst for full water splitting, but would explored a new way to explore the tungstate nanoarrays for applications.

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ASSOCIATED CONTENT Supporting Information

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Experimental section; SEM images; Nyquist plots; LSV curves; XRD pattern; XPS survey spectrum and HRTEM image; Tables S1-S3; This material is available free of charge via the Internet at http://pubs.acs.org.

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NiWO4 nanoarray on Ti mesh (NiWO4/TM) shows a high-performance water-splitting catalyst and it two-electrode electrolyzer drives 20 mA cm–2 full water splitting current at a cell voltage of 1.65 V.

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