Photocatalytic H2 evolution on a novel CaIn2S4 photocatalyst under visible light irradiation

A novel visible-light-driven photocatalyst CaIn₂S₄ was synthesized using a facile hydrothermal method followed by a post-calcination process. The influence of the calcination temperature and time on the activities of the photocatalyst was investigated. CaIn₂S₄ exhibits optical absorption predominantly in visible region with an optical band gap of 1.76 eV. Considerable activity for hydrogen evolution from pure water was observed without any sacrificial agents or cocatalysts under visible light irradiation. The maximum hydrogen evolution rate achieved was 30.92 μmol g⁻¹ h⁻¹ without obvious deactivation of the photocatalytic activity for four consecutive runs of 32 h.     

Fabrication of graphene/CaIn2O4 composites with enhanced photocatalytic activity from water under visible light irradiation

A series of graphene/CaIn₂O₄ composites were synthesized using a facile solvothermal method to improve the photocatalytic performance of CaIn₂O₄. The reduction of graphene oxide to graphene and the deposition of CaIn₂O₄ nanoparticles on the graphene sheets can be achieved simultaneously during the solvothermal process. The photocatalytic activities of as-prepared graphene/CaIn₂O₄ composites for hydrogen evolution from CH₃OH/H₂O solution were investigated under visible light irradiation. It was found that graphene exhibited an obvious influence on the photocatalytic activity of CaIn₂O₄. The graphene/CaIn₂O₄ composite reached a high H₂ evolution rate of 62.5 μmol h⁻¹ from CH₃OH/H₂O solution when the content of graphene was 1 wt%. Furthermore, the 1 wt% graphene/CaIn₂O₄ composite did not show deactivation for H₂ evolution for longer than 32 h. This work could provide a new insight into the fabrication of visible light driven photocatalysts with efficient and stable performance.     

Highly exposed (001) facets Ni(OH)2 induced formation of nickle phosphide over cadmium sulfide nanorods for efficient photocatalytic hydrogen evolution

An efficient Ni₂P–CdS photocatalyst for photocatalytic hydrogen evolution was synthesized by phosphorizing β-Ni(OH)₂ nanosheet with exposed (001) facets on CdS nanorods. The obtained Ni₂P–CdS composite displays an outstanding and stable photocatalytic hydrogen generation rate of 68.47 mmol g⁻¹ h⁻¹ in 10 vol% lactic acid under visible light irradiation, more than 17 times higher than that for pure CdS nanorods. The transient photocurrent response, EIS measurement, Mott-Schottky plots, acidic LSV measurement, and PL spectra have proved that Ni₂P loading can significantly improve the separation of photo-excited electron-hole pairs in CdS nanorods and enhance the hydrogen evolution capability for CdS. These improvements are achieved by features of Ni₂P such as the high capability of trapping photo-generated electrons from CdS, lifting the total Fermi level and lowering the hydrogen evolution overpotential of the composite. The results show that β-Ni(OH)₂ precursor with a high exposure degree of (001) facet is contributed to the epitaxial formation of (001)-facet-exposed Ni₂P co-catalyst on CdS nanorods, resulting in that the Fermi level and the hydrogen evolution overpotential of the composite can be further lifted and lowered. This study has provided a novel precursor-derived route to fabricate high-performance co-catalysts with highly exposed active facets on CdS nanorods for effective photocatalytic hydrogen evolution.     

An anti-symmetric dual (ASD) Z-scheme photocatalytic system: (ZnIn2S4/Er3+:Y3Al5O12@ZnTiO3/CaIn2S4) for organic pollutants degradation with simultaneous hydrogen evolution

An anti-symmetric dual (ASD) Z-scheme ZnIn₂S₄/Er³⁺:Y₃Al₅O₁₂@ZnTiO₃/CaIn₂S₄ photocatalyst was prepared by isoelectric point and calcination methods. The photocatalytic activity is estimated via degradation of Acid Orange II as a target organic contaminant with simultaneous hydrogen evolution under simulated solar-light irradiation. The prepared ASD Z-scheme ZnIn₂S₄/Er³⁺:Y₃Al₅O₁₂@ZnTiO₃/CaIn₂S₄ photocatalyst has a high photocatalytic activity, which can be assigned to the enlarged photoresponse range, increased reduction surface and enhanced separation efficiency of photo-induced carriers. Furthermore, the cyclic experiment proves that the prepared ASD Z-scheme ZnIn₂S₄/Er³⁺:Y₃Al₅O₁₂@ZnTiO₃/CaIn₂S₄ photocatalyst still maintains a high photocatalytic activity within five repetitive cycles. Moreover, the mechanism on photocatalytic degradation of organic pollutants with simultaneous hydrogen evolution caused by ASD Z-scheme ZnIn₂S₄/Er³⁺:Y₃Al₅O₁₂@ZnTiO₃/CaIn₂S₄ photocatalyst is proposed. It is wished that this study could provide a promising pathway for effective degradation and rapid hydrogen production.     

Facile strategy to fabricate Ni2P/g-C3N4 heterojunction with excellent photocatalytic hydrogen evolution activity

Transition metal phosphides are considered as the most prospective replacements for noble metal cocatalysts used for H₂ evolution during photocatalytic water splitting. In this work, Ni₂P/g-C₃N₄ composite photocatalyst was synthesized using a simple in-situ hydrothermal method by one step. Benefiting from the excellent light trapping, efficient transfer of charge carriers and strong stability of Ni₂P nanoparticles, as well as the stable interface contact between Ni₂P and g-C₃N₄, the Ni₂P/g-C₃N₄ exhibit greatly enhanced H₂ evolution performance during photocatalytic water splitting. The optimized H₂ evolution rate can reach 3344 μmol h^?1 g^?1 over 17.5 wt% Ni₂P/g-C₃N₄, which is 68.2 times greater than that of pure g-C₃N₄ and even much greater than that of 15 wt% Pt/g-C₃N₄. The apparent quantum efficiency (QE) is about 9.1% under 420 nm monochromatic. The enhancement mechanism was demonstrated in detail by transient photocurrent responses, photoluminescence spectra and electrochemical impedance spectroscopy. This work develops a facile strategy to fabricate transition metal phosphide/semiconductor heterojunction systems with potential application for photocatalytic H₂ evolution.     

Charge transfer behaviors over MOF-5@g-C3N4 with NixMo1−xS2 modification

The composite photocatalyst Ni_xMo_1?xS₂/MOF-5@g-C₃N₄ was successfully synthesized by means of hydrothermal with two step methods and the effective photocatalytic activity improvement was obtained. With the introduction of Ni_xMo_1?xS₂, the H₂ production reached the maximum about 319 μmol under continuous visible light irradiation for 5 h, which was 30 times higher than that of pure g-C₃N₄ photocatalyst. A series of characterization results shown that the MOF-5@g-C₃N₄ on the surface of Ni_xMo_1?xS₂ provided the more active sites and improved the efficiency of photo-generated charge separation with SEM, XRD, TEM, EDX, XPS, UV–vis DRS, BET, FTIR, transient fluorescence and electro-chemistry etc. and the results of which were in good mutual corresponding with each other. Furthermore, the reaction mechanism over the compound catalyst Ni_x-Mo_1?xS₂/MOF-5@g-C₃N₄ was proposed.     

In situ metal–organic framework-derived c-doped Ni3S4/Ni2P hybrid co-catalysts for photocatalytic H2 production over g-C3N4 via dye sensitization

Controlled integration of metal-based sulfides with phosphides possessing strong coupling effects is a promising way to accelerate electron transfer by modulating the electronic structures of the host species. In this work, a c-doped Ni₃S₄/Ni₂P (C@Ni₃S₄/Ni₂P) hybrid co-catalyst produced by in situ sulfuration and phosphidation of Ni-MOF was decorated on g-C₃N₄ and subsequently used for photocatalytic H₂ evolution under visible-light irradiation. Among the prepared composites tested herein, the optimized g-C₃N₄/C@Ni₃S₄/Ni₂P-30 composite showed the highest H₂ evolution rate (14.49 mmol g⁻¹ h⁻¹) with 1.0 mmol L⁻¹ of Eosin Y (EY)-sensitization, which is 10 times higher than that of pristine g-C₃N₄ (1.33 mmol g⁻¹ h⁻¹). The enhanced photocatalytic activity of this composite can be attributed to: (i) electronic interactions between Ni₂P and Ni₃S₄ (which synergistically increased the electron transfer rate) and (ii) staggered band alignment of excited-stated EY, g-C₃N₄, Ni₃S₄, and Ni₂P. This work may provide some perspectives for utilization of MOF-derived hybrid co-catalysts as substitutes of noble metals for effective photocatalytic H₂ evolution.     

NiS2 Co-catalyst decoration on CdLa2S4 nanocrystals for efficient photocatalytic hydrogen generation under visible light irradiation

NiS₂ nanoparticles as noble metal-free co-catalysts were deposited onto the CdLa₂S₄ nanocrystals through a hydrothermal process. The loading of NiS₂ co-catalyst resulted in remarkable enhancement for H₂ production over the CdLa₂S₄ photocatalyst under visible light irradiation. The optimal hybrid photocatalyst with 2 wt% NiS₂ loading exhibited a H₂ production rate of 2.5 mmol h⁻¹ g⁻¹, which was more than 3 times higher than that of the pristine CdLa₂S₄ photocatalyst. The promoted photocatalytic H₂ production by NiS₂-loading is attributed to the enhanced separation of photogenerated electrons and holes as well as the activation effect of NiS₂ for H₂ evolution.     

Highly efficient visible-light-assisted photocatalytic hydrogen generation from water splitting catalyzed by Zn0.5Cd0.5S/Ni2P heterostructures

Development of heterostructured photocatalysts which can facilitate spatial separation of photo-generated charge carriers is crucial for achieving improved photocatalytic H₂ production. Consequently, herein, we report the synthesis of Zn_0.5Cd_0.5S/Ni₂P heterojunction photocatalysts with varying amount of Ni₂P, 0.5 (S1), 1 (S2), 3 (S3), 5 (S4) and 10wt% (S5) for the efficient visible-light-assisted H₂ generation by water splitting. The heterostructures were characterized thoroughly by PXRD, FE-SEM, EDS, HR-TEM and XPS studies. FE-SEM and HR-TEM analyses of the samples unveiled the presence of Zn_0.5Cd_0.5S microspheres composed of smaller nanocrystals with the surface of the microspheres covered with Ni₂P nanosheets and the intimate contact between the Zn_0.5Cd_0.5S and the Ni₂P. Further, visible-light-assisted photocatalytic investigation of the samples showed excellent water splitting activity of the heterostructure, Zn_0.5Cd_0.5S/1wt%Ni₂P (S2) with very high H₂ generation rate of 21.19 mmol h^?1g^?1 and the AQY of 21.16% at 450 nm with turnover number (TON) and turnover frequency (TOF) of 251,516 and 62,879 h^?1 respectively. Interestingly, H₂ generation activity of S2 was found to be about four times higher than that of pure Zn_0.5Cd_0.5S (5.0 mmol h^?1g^?1) and about 240 times higher than that of CdS/1wt%Ni₂P. The enhanced H₂ generation activity of S2 has been attributed to efficient spatial separation of photogenerated charge carriers and the presence of highly reactive Ni₂P sites on the surface of Zn_0.5Cd_0.5S microspheres. A possible mechanism for the enhanced photocatalytic H₂ generation activity of Zn_0.5Cd_0.5S/1wt%Ni₂P (S2) has been proposed and is further supported by photoluminescence and photocurrent measurements. Furthermore, the catalyst, S2 can be recycled for several cycles without significant loss of catalytic activity and photostability. Remarkably, the H₂ generation activity of S2 was found to be even higher than the reported examples of Zn_xCd_1-xS doped with noble metal cocatalysts. Hence, the present study highlights the importance of Zn_0.5Cd_0.5S/Ni₂P heterostructures based on non-noble metal co-catalyst for efficient visible-light-driven H₂ production from water splitting.     

Direct Z-scheme ZnIn2S4/LaNiO3 nanohybrid with enhanced photocatalytic performance for H2 evolution

The direct Z-scheme ZnIn₂S₄/LaNiO₃ nanohybrid based on ZnIn₂S₄ nanosheets and LaNiO₃ cubes was synthesized by a facile hydrothermal method. The ZnIn₂S₄/LaNiO₃ nanohybrid showed improved photocatalytic H₂ evolution and stability. The photocatalytic H₂ evolution activity of ZnIn₂S₄/LaNiO₃ nanohybrid is 3-fold enhanced than that of bare ZnIn₂S₄. The enhanced performance of ZnIn₂S₄/LaNiO₃ nanohybrid is mainly ascribed to the formation of heterojunction between LaNiO₃ and ZnIn₂S₄. The heterojunction can facilitate charge transport on the interface between LaNiO₃ and ZnIn₂S₄ and suppress the recombination of photo-generated charge carriers over ZnIn₂S₄/LaNiO₃ nanohybrid, which were well demonstrated by photoelectrochemical tests. Moreover, the direct Z-scheme photocatalytic reaction mechanism was proposed to elucidate the improved performance of ZnIn₂S₄/LaNiO₃ nanohybrid photocatalyst. This study may provide some guidance on the construction of direct Z-scheme photocatalytic system for photocatalytic H₂ evolution.     

Fabrication of the SnS2/ZnIn2S4 heterojunction for highly efficient visible light photocatalytic H2 evolution

A series of SnS₂/ZnIn₂S₄ (x-SS/ZIS) photocatalysts with different mass ratios of SnS₂ were prepared by a hydrothermal method. The resulted composites were used for photocatalytic hydrogen evolution under visible light excitation. All the SS/ZIS composites exhibited significantly enhanced photocatalytic activity for H₂ evolution. Obviously, the highest H₂ evolution rate of 769 μmol g^?1 h^?1 was observed over 2.5-SS/ZIS, which was approximately 10.5 times that of the ZnIn₂S₄ (73 μmol g^?1 h^?1). The enhanced photocatalytic performance was attributed to the successful construction of SnS₂/ZnIn₂S₄ heterojunctions, leading to rapid charge separation and fast transfer of the photo-generated electrons and holes under light irradiation. On the basis of PL, electrochemical impedance spectroscopy (EIS), photocurrent measurements and the H₂ evolution tests, a plausible photocatalytic mechanism was proposed.     

Mesoporous g-C3N4 decorated by Ni2P nanoparticles and CdS nanorods together for enhancing photocatalytic hydrogen evolution

Ni₂P nanoparticles and CdS nanorods were grew together on a mesoporous g-C₃N₄ through a facile in-situ solvothermal approach. Under visible light (λ > 400 nm), the as-prepared ternary PCN–CdS-5% Ni₂P composite displays a high H₂ evolution rate with 2905.86 μmol g^?1 h^?1, which is about 14, 18 and 279 times that of PCN–CdS, PCN–Ni₂P and PCN, respectively. The enhanced photocatalytic activity is mainly attributed to the improved separation efficiency of the photocarriers by the type II PCN–CdS heterojunction and the effective extraction of photogenerated electrons by Ni₂P. Meanwhile, Ni₂P acts as co-catalyst to provide the photocatalytic active site for hydrogen reduction. In addition, PCN–CdS-5% Ni₂P composite exerts good stability in 12-h cycles.     

Solvothermal fabrication of MoS2 anchored on ZnIn2S4 microspheres with boosted photocatalytic hydrogen evolution activity

The MoS₂/ZnIn₂S₄ composites with MoS₂ anchored on the surface of ZnIn₂S₄ microspheres were fabricated by a facile solvothermal method. To clarify the crystal phases, morphologies, chemical compositions, optical properties, and special surface areas of the obtained photocatalysts, the corresponding characterization measurements were performed. The photocatalytic H₂ evolution activities of MoS₂/ZnIn₂S₄ composites were evaluated and compared with using lactic acid as sacrificial reagents. The results showed that integrating MoS₂ with ZnIn₂S₄ could remarkably boost the photocatalytic H₂ evolution performance and the maximum H₂ evolution rate of 201 μmol h^?1 was achieved over 1 wt% MoS₂ loading on the ZnIn₂S₄, corresponding to the apparent quantum efficiency (AQE) about 3.08% at 420 nm monochromatic light. The photoelectrochemical tests and photoluminescence spectra (PL) versified that the efficient charge transfer and separation were achieved over MoS₂/ZnIn₂S₄ composite in contrast with single ZnIn₂S₄, which would significantly benefit the enhancement of photocatalytic H₂ activity. This work provides a desired strategy to design and synthesize the visible-light-response photocatalysts with MoS₂ as cocatalysts to enhance the photocatalytic activity.     

0D/2D heterojunction constructed by high-dispersity Mo-doped Ni2P nanodots supported on g-C3N4 nanosheets towards enhanced photocatalytic H2 evolution activity

Development of low cost and efficient non-noble-metal cocatalyst is still a hot topic to improve the activity of g-C₃N₄ in photocatalytic water splitting to produce H₂. As a potential cocatalyst in photocatalytic application, transition metal phosphides (TMPs) have been proved to greatly enhance the photocatalytic H₂ evolution performance comparable to noble metal Pt. Modifying TMPs by incorporation of hetero-metal has also been reported as an effective strategy for their electronic structure regulation and optimizing the intermediates absorption energy, however, which is rarely reported in the field of photocatalysis. Herein, the 0D/2D heterojunction is constructed by high-dispersity Mo-doped Ni₂P nanodots supported on g-C₃N₄ nanosheets, which exhibits the significantly improved photocatalytic H₂ evolution performance compared with that of Ni₂P/g-C₃N₄ and Pt/g-C₃N₄. Specifically, the optimal H₂ evolution rate reaches 67.6 μmol h⁻¹ over Mo–Ni₂P/g-C₃N₄ sample, which is 6.0 and 2.4 times higher than those of Pt/g-C₃N₄ and Ni₂P/g-C₃N₄, respectively. The fascinating result mainly stems from the improved separation efficiency of charge carriers and more effective electron donating reaction sites resulted from the electronic structure adjustment through doping Mo element into Ni₂P as cocatalyst. This work provides a valid evidence for the modification of cocatalyst to realize high H₂ evolution performance, opening up new opportunities and possibilities for the application of TMPs in the photocatalytic field.     

Microwave-assisted hydrothermal synthesis of transition-metal doped ZnIn2S4 and its photocatalytic activity for hydrogen evolution under visible light

Aiming at the enhancement of photocatalytic activity for hydrogen evolution over ZnIn₂S₄, different transition metals (Cr, Mn, Fe, Co) are doped into the lattices of ZnIn₂S₄ to narrow the band gap. The doped ZnIn₂S₄ is characterized by XRD, Raman, UV-vis spectra, photoluminescence spectra, SEM and XPS techniques. The photocatalytic evaluation shows that Mn-doped ZnIn₂S₄ performs photocatalytic activity 20% higher than undoped ZnIn₂S₄, while Cr-, Fe-, and Co-doped ZnIn₂S₄ perform poorer activities in an order of Cr > Fe > Co. Based on the combined characterization results, the band structures of doped ZnIn₂S₄ are schematically depicted, which illustrates the different effects of transition-metal doping on the photocatalytic activity for hydrogen evolution. For Mn-doped ZnIn₂S₄, the enhancement of photocatalytic activity could be due to narrowed band gap induced by Mn doping. However, for Cr-, Fe-, and Co-doped ZnIn₂S₄, the suppressed photocatalytic activities should be attributed to the dopant-related impurity energy levels localizing the charge carriers or acting as non-radiative recombination centers for photoexcited electrons and holes. Hence, this study indicates that it is of great importance to make the in-depth investigation on the effects of band structures on the photocatalytic activity, especially for the doped semiconducting photocatalysts.     

Photoelectrochemical performance of TiO2 nanotube arrays modified with Ni2P Co-catalyst

Solar-driven water splitting to produce hydrogen is an important solution to the problem of energy shortage and environmental pollution. The photolysis of water to produce hydrogen requires highly efficient and stable photocatalysts, and the anode used as catalyst for oxygen evolution is a bottleneck in this process. In this paper, the a-TNTAs/Ni₂P composite photo-anode was constructed by electrodeposition to anchor the Ni₂P co-catalyst for oxygen evolution at the active site of TiO₂ nanotube arrays (TNTAs). The a-TNTAs/Ni₂P delivered excellent oxygen evolution at a photocurrent density of 1.058 mA cm^-2, an improvement of 2.78 times, 13.2 times, and 15.8 times over a-TNTAs, TNTAs/Ni₂P, and TNTAs photo-anodes, respectively. The Mott-Schottky curve showed that Ni₂P as co-catalyst for oxygen evolution accelerated the rates of separation and transfer of the photogenerated electrons. This research provides a simple and efficient method to promote the OER performance of optical semiconductors.     

Ternary Ni2P/reduced graphene oxide/g-C3N4 nanotubes for visible light-driven photocatalytic H2 production

Developing low cost co-catalysts is crucial for both fundamental research and practical application of g-C₃N₄. In this work, we prepared ternary Ni₂P/rGO/g-C₃N₄ nanotubes with different Ni₂P contents for visible-light-driven photocatalytic H₂ generation from triethanolamine aqueous solution. The optimal Ni₂P/rGO/g-C₃N₄ produced H₂ at a rate of 2921.9 μmol h⁻¹ g⁻¹, which is about 35, 16 and 9 times as large as that of g-C₃N₄, binary rGO/g-C₃N₄ and Ni₂P/g-C₃N₄, respectively. The apparent quantum efficiency of optimal Ni₂P/rGO/g-C₃N₄ was 5.6% at λ = 420 nm. We believe that the improved photocatalytic performance of Ni₂P/rGO/g-C₃N₄ originates from the synergistic effect of rGO as electron transfer medium and Ni₂P as reaction site, which is supported by photoelectrochemical and photoluminescence measurements. Cyclic experiment demonstrated an excellent stability of Ni₂P/rGO/g-C₃N₄. Moreover, we further studied the effect of other nickel-based compounds by replacing Ni₂P with NiS, Ni₃C, and Ni₃N, respectively. The order of the H₂-generation rate is Ni₂P/rGO/CNNT > NiS/rGO/CNNT > Ni₃C/rGO/CNNT > Ni₃N/rGO/CNNT, which could be reasonably explained based on Mott–Schottky plots. Our work reveals that Ni₂P can be used as a promising cocatalyst for photocatalytic H₂ evolution.     

In situ photodeposition of metalloid Ni2P co-catalyst on Mn0.5Cd0.5S for enhanced photocatalytic H2 evolution with visible light

Developing a suitable and low-cost co-catalyst is highly desired for promoting photocatalytic water splitting of H₂ production. Herein, we adopted a simple in situ photodeposition strategy by coupling Mn_0.5Cd_0.5S with non-noble co-catalyst Ni₂P to construct Ni₂P/Mn_0.5Cd_0.5S composites and achieved obviously improved H₂ amount (31.83 mmol/h/g) in visible-light region, which is nearly 2.8 times than that of pure Mn_0.5Cd_0.5S. Such photocatalytic performance is in a relatively superior position among Mn_xCd_1?xS-based photocatalysts. The apparent quantum efficiency of Ni₂P/Mn_0.5Cd_0.5S-7 composites reaches 32% at 420 nm. Through optical and photoelectrochemical measurements, a possible mechanism was proposed, it was found that the interface between metalloid Ni₂P and Mn_0.5Cd_0.5S contacts closely, which facilitates transfer and separation of charge carriers, thus promotes the reduction of H⁺ to H₂. This study provides a new design of cut-price, high-efficiency photocatalyst for H₂ evolution.     

Visible-light-driven ZnIn2S4/CdIn2S4 composite photocatalyst with enhanced performance for photocatalytic H2 evolution

ZnIn₂S₄/CdIn₂S₄ composite photocatalysts (x = 0–1) were successfully synthesized via a hydrothermal route. Compositions of ZnIn₂S₄/CdIn₂S₄ composite photocatalysts were optimized according to the photocatalytic H₂ evolution rate. XRD patterns indicate the as-prepared samples are mixtures of hexagonal and cubic structures. FESEM and TEM images show that the as-prepared samples are composed of flower-like microspheres with wide distribution of diameter. There is obviously distinguishing distribution of Zn, Cd elements among the composite architectures. UV–vis absorption spectra of different compositions exhibit that absorption edges of ZnIn₂S₄/CdIn₂S₄ composites slightly move towards longer wavelengths with the increment of CdIn₂S₄ component. A typical time course of photocatalytic H₂ evolution from an aqueous Na₂SO₃ and Na₂S solution over unloaded and PdS-loaded ZnIn₂S₄/CdIn₂S₄ composite photocatalyst is carried out. The initial activity for H₂ evolution over 0.75 wt% PdS-loaded sample is up to 780 μmol h⁻¹. And the activity of unloaded sample also reaches 490 μmol h⁻¹ with consistent stability.     

Sonochemistry synthesis of Bi2S3/CdS heterostructure with enhanced performance for photocatalytic hydrogen evolution

Photocatalytic hydrogen evolution from water splitting is an efficient, eco-friendly method for the conversion of solar energy to chemical energy. A great number of photocatalysts have been reported but only a few of them can respond to visible-light. Metal sulfides, a class of visible-light response semiconductor photocatalysts for hydrogen evolution and organic pollutant degradation, receive a lot of attention due to their narrow band gaps. Herein, we report the sonochemical synthesis of Bi₂S₃/CdS nanocrystal composites with microsphere structure at mild temperature. The phases of Bi₂S₃ and CdS can be observed obviously in HRTEM image. The heterostructure consisting of the two species of nanocrystals plays a key role in separating photo-generated charge carriers. Photocatalytic activities for water splitting are investigated under visible-light irradiation (λ > 400 nm) and an enhanced photocatalytic activity is achieved. The initial rate of H₂ evolution is up to 5.5 mmol h⁻¹ g⁻¹ without resorting to any cocatalysts.