Enhanced visible light photocatalytic H2 production over Z-scheme g-C3N4 nansheets/WO3 nanorods nanocomposites loaded with Ni(OH)x cocatalysts

doi:10.1016/S1872-2067(17)62759-1

Chinese Journal of Catalysis

Volume 38, Issue 2, February 2017, Pages 240-252

https://doi.org/10.1016/S1872-2067(17)62759-1 Get rights and content

Abstract

Novel WO₃/g-C₃N₄/Ni(OH)_x hybrids have been successfully synthesized by a two-step strategy of high temperature calcination and in situ photodeposition. Their photocatalytic performance was investigated using TEOA as a hole scavenger under visible light irradiation. The loading of WO₃ and Ni(OH)_x cocatalysts boosted the photocatalytic H₂ evolution efficiency of g-C₃N₄. WO₃/g-C₃N₄/Ni(OH)_x with 20 wt%defective WO₃ and 4.8 wt%Ni(OH)_x showed the highest hydrogen production rate of 576 μmol/(g–h), which was 5.7, 10.8 and 230 times higher than those of g-C₃N₄/4.8 wt%Ni(OH)_x, 20 wt%WO₃/C₃N₄ and g-C₃N₄ photocatalysts, respectively. The remarkably enhanced H₂ evolution performance was ascribed to the combination effects of the Z-scheme heterojunction (WO₃/g-C₃N₄) and loaded cocatalysts (Ni(OH)_x), which effectively inhibited the recombination of the photoexcited electron-hole pairs of g-C₃N₄ and improved both H₂ evolution and TEOA oxidation kinetics. The electron spin resonance spectra of ^•O₂⁻ and ^•OH radicals provided evidence for the Z-scheme charge separation mechanism. The loading of easily available Ni(OH)_x cocatalysts on the Z-scheme WO₃/g-C₃N₄ nanocomposites provided insights into constructing a robust multiple-heterojunction material for photocatalytic applications.

Graphical Abstract

The synergistic effects of Z-scheme heterojunctions (g-C₃N₄ nansheets/WO₃ nanorods) and loaded cocatalyst (Ni(OH)_x) were demonstrated, which boosted visible light photocatalytic H₂ production over g-C₃N₄ nanosheets.

Introduction

Nowadays, extensive researches are focused on the development of sustainable and environmental friendly energy. Among various energy carriers, hydrogen is considered one of the most promising, green and alternative fuel sources and a bridge to a sustainable energy future, which can effectively meet the increasing energy demands [1]. A more sustainable and green hydrogen production can be achieved by the heterogeneous photocatalysis with the aid of semiconductors and solar energy. Thus, heterogeneous hydrogen production from water splitting has gained worldwide research interest [2, 3], since the photoelectrochemical water splitting was first reported by Fujishima and Honda in 1972 [4]. Metal oxide semiconductors, such as TiO₂, are the most extensively applied photocatalysts for hydrogen generation from water splitting [5, 6, 7, 8]. Nevertheless, these semiconductors exhibit some intrinsic disadvantages, such as low quantum yield and poor visible light harvesting, which largely restrict their practical implementation [8, 9]. Efforts have been devoted to explore visible light H₂ generation photocatalysts by the modification of traditional wide band gap semiconductors or searching for new visible light semiconductors [2, 5, 8, 10, 11, 12, 13, 14].

Recently, graphitic carbon nitride (g-C₃N₄) as a metal-free visible light semiconductor has been demonstrated for photocatalytic H₂ evolution [15, 16, 17, 18, 19], CO₂ reduction [16, 20, 21, 22, 23, 24, 25] and pollutant degradation [26, 27, 28, 29, 30] where it showed superior properties, such as high chemical stability, easy fabrication, low cost, excellent absorption properties, and a suitable band gap and position [15, 21, 24, 31]. However, several challenges due to g-C₃N₄ itself, such as the rapid recombination of electron and hole pairs, and insufficient surface area and active sites leading to sluggish surface reaction kinetics and moderate oxidation ability gave a low photocatalytic H₂ evolution efficiency [21]. Therefore, various modification strategies, such as constructing Type II heterojunctions/Z-Scheme systems with other semiconductors, loading catalysts, fabricating nanostructures, and coupling with nanocarbons and their combinations have been employed to improve the visible light H₂ generation photoactivity of g-C₃N₄ photocatalysts [21, 32, 33, 34, 35, 36, 37, 38, 39]. Among these, the two interesting strategies of constructing Z-scheme systems [40, 41, 42, 43, 44] and loading catalysts [13, 21, 45, 46, 47, 48] have effectively improved the thermodynamic oxidation ability and reduction kinetics of g-C₃N₄ photocatalysts, respectively.

Compared to traditional Type II heterojunctions, the artificial heterogeneous all solid state Z-Scheme photocatalytic systems without redox pairs simultaneously feature higher spatial charge separation efficiency and stronger redox ability by combining two narrow band gap semiconductors with enhanced visible light absorption [2, 24, 49]. In the past several years, various semiconductors with weak reduction ability of photo-generated electrons, such as TiO₂ [44], Bi₂WO₆ [40], WO₃ [41, 50, 51, 52, 53], Bi₂MoO₆ [42], Ag₃PO₄ [54, 55] and ZnO [43], have been extensively employed to fabricate artificial g-C₃N₄-based Z-scheme photocatalytic systems for different applications. Among these, the WO₃/g-C₃N₄ Z-scheme photocatalysts have attracted particular attention [41, 50, 51, 52, 53]. In this Z-scheme WO₃/g-C₃N₄ photocatalytic system, the photo-generated electrons in the CB of WO₃ and the photo-generated holes in the VB of g-C₃N₄ are readily recombined, which retain the higher oxidation and reduction activity of WO₃ and g-C₃N₄, respectively, thus achieving significantly improved photocatalytic activity. For example, Cui et al. [41] synthesized Z-scheme WO₃/g-C₃N₄ composite photocatalysts by a facile one-step simultaneously heating procedure. The results indicated that the Z-scheme WO₃/g-C₃N₄ composites with 25 wt%WO₃ achieved the highest photo-degradation activity of Rhodamine B under visible light irradiation due to excellent surface properties, enhanced charge separation/migration rate and visible light absorption. Similarly, the Z-scheme WO₃/g-C₃N₄ composite photocatalysts prepared by ball milling and heat treatment exhibited greatly increased photocatalytic degradation activity towards methylene blue (MB) and fuchsin (BF) under visible light illumination. It was proposed that the photo-generated electrons and holes in g-C₃N₄ and WO₃ enhanced the formation rate of ^•O₂⁻ and active ^•OH radicals, respectively, thus leading to significantly enhanced Z-scheme photoactivity [51, 53]. In another example, Ohno et al. [52] demonstrated that the Z-scheme g-C₃N₄-WO₃ composite photocatalysts fabricated by the planetary milling of g-C₃N₄ and WO₃ mixed powders exhibited the highest photocatalytic activity for multi-electron reduction of CO₂ to CH₃OH. The loading of Au catalysts on the hybrid Z-scheme WO₃/g-C₃N₄ photocatalyst achieved 1.7 times higher photocatalytic activity, as compared to that of the hybrid photocatalyst without Au loading [52]. More interestingly, the Z-scheme reaction mechanism was also revealed by double beam photoacoustic spectroscopy, which further indicated the favorable charge separation and enhanced photocatalytic oxidation/reduction activity [52]. Katsumata et al. [50] synthesized Z-scheme WO₃/g-C₃N₄ composite H₂-evolution photocatalysts by simple calcination of the ground mixture of commercially available WO₃ nanoparticles and g-C₃N₄. The resulting 10 wt%WO₃/g-C₃N₄ composite with 2 wt%Pt catalyst showed the highest photocatalytic H₂ production rate of 110 μmol/(h–g), which was 2 times higher than that of pure g-C₃N₄. It was believed that the formation of WO₃/g-C₃N₄ Z-scheme junctions efficiently promoted charge separation, thus achieving enhanced photocatalytic H₂ evolution activity [50]. Clearly, in these Z-scheme WO₃/g-C₃N₄ composite photocatalysts, the noble metals, such as Pt, Ag and Au, were utilized as catalyst to boost the photocatalytic reduction activity of the hybrid Z-Scheme systems [50, 52]. However, their high cost and low natural abundance will significantly limit their practical large scale application. Although significant research efforts have been devoted to enhancing photocatalytic H₂ evolution over g-C₃N₄ decorated with non-noble metal catalysts [56], including nanocarbons, Ni, NiS, Ni(OH)₂, WS₂, MoS₂ and their composites [13, 16, 19, 32, 48, 57, 58, 59], there have been scarce investigations on the surface deposition of suitable readily available catalysts on a hybrid Z-Scheme WO₃/g-C₃N₄ system for photocatalytic H₂ evolution. We believe that robust composite photocatalysts can be simply constructed by combining cheap and abundant H₂ evolution catalysts and favorable Z-Scheme WO₃/g-C₃N₄ systems.

In this study, the combined effects of cheap and abundant Ni(OH)_x as electron catalyst and WO₃ with strong oxidation activity were utilized to synergistically maximize the photocatalytic H₂ evolution activity of pure g-C₃N₄ nanosheets. The robust Z-scheme WO₃/g-C₃N₄ photocatalyst was first fabricated by direct calcination of ammonium tungstate hydrate and thiourea, thus achieving intimate interfacial contact. Subsequently, the robust Ni(OH)_x nanoparticles as cocatalyst [60] were loaded onto the Z-scheme composites by in situ photo-deposition to further boost the Z-scheme charge separation and photoctalytic H₂ evolution kinetics. The fabrication of the hybrid composite is illustrated in Scheme 1. The H₂ evolution activity of the hybrid WO₃/g-C₃N₄/Ni(OH)_x Z-scheme photocatalysts under visible light irradiation was investigated using an aqueous solution containing triethanolamine as electron donor. The results revealed that the hybrid WO₃/g-C₃N₄/Ni(OH)_x Z-scheme photocatalysts exhibited significantly enhanced photocatalytic H₂ evolution activity compared to bulk g-C₃N₄ and binary hybrids of WO₃/g-C₃N₄ and g-C₃N₄/Ni(OH)_x. It was proposed that the promoted Z-scheme charge separation and transfer between g-C₃N₄ and WO₃ as well as accelerated H₂ evolution kinetics on Ni(OH)_x nanoparticles played key roles in the photocatalytic enhancement mechanism for enhanced H₂ evolution activity over the composites. It is expected that the loading of readily available cocatalysts on Z-scheme WO₃/g-C₃N₄ nanocomposites can provide more insight into boosting the activity of robust heterojunction materials for photocatalytic applications.

Section snippets

Materials

Other conditions: 100 mg g-C₃N₄, 30 mL TEOA and 30 min UV irradiation.

Ammonium tungstatehydrate ((NH₄)₁₀W₁₂O₄₁), thiourea (CH₄N₂S), sodium hypophosphite (NaH₂PO₂)_, nickel chloride (NiCl₂) and triethanolamine (TEOA) were reagent grade and used without further purification.

Synthesis of WO₃/g-C₃N₄

The WO₃/g-C₃N₄ composite was prepared by in situ heating ammonium tungstate hydrate and thiourea. In a typical synthesis, an amount of ammonium tungstate hydrate and 10 g of thiourea were dissolved in 30 mL deionized water. The

Structure and composition of the photocatalysts

The phase structure of the samples was identified by powder XRD measurement. Fig. 1 presents the comparison of the XRD patterns of different samples. As shown in Fig. 1(a), g-C₃N₄ photocatalysts exhibited two main diffraction peaks at 27.4° and 13.0°, which were indexed as the (002) and (100) diffraction planes of layered g-C₃N₄ (JCPDS, No. 87-1526) [62]. The diffraction peaks located at 27.4° and 13.0° corresponded to the distance of 0.325 and 0.681 nm, which were assigned to the interlayer

Conclusions

We fabricated high quality WO₃/g-C₃N₄/Ni(OH)_x nanocomposites by a two-step strategy of high temperature calcination and in situ photo-deposition. In the synergistic system, the photo-generated electrons and holes of g-C₃N₄ were simultaneously separated and utilized by the Ni(OH)_x cocatalysts and WO₃ Z-scheme component, respectively. The Ni(OH)_x cocatalyst effects were demonstrated by the polarization curves, while the Z-scheme charge separation mechanism was revealed by the electron spin

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This work was supported by the National Natural Science Foundation of China (51672089), the Industry and Research Collaborative Innovation Major Projects of Guangzhou (201508020098), the State Key Laboratory of Advanced Technology for Material Synthesis and Processing (Wuhan University of Technology) (2015-KF-7) and the Hunan Key Laboratory of Applied Environmental Photocatalysis (Changsha University) (CCSU-XT-04).

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Published 5 February 2017

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Article (Special Issue on the International Symposium on Environmental Catalysis (ISEC 2016))Enhanced visible light photocatalytic H2 production over Z-scheme g-C3N4 nansheets/WO3 nanorods nanocomposites loaded with Ni(OH)x cocatalysts

Abstract

Graphical Abstract

Introduction

Section snippets

Materials

Synthesis of WO3/g-C3N4

Structure and composition of the photocatalysts

Conclusions

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Chin. J. Catal.

Chin. J. Catal.

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Article (Special Issue on the International Symposium on Environmental Catalysis (ISEC 2016))
Enhanced visible light photocatalytic H₂ production over Z-scheme g-C₃N₄ nansheets/WO₃ nanorods nanocomposites loaded with Ni(OH)_x cocatalysts

Synthesis of WO₃/g-C₃N₄

J. CO₂ Util.