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Constructing a 2D Heterointerface of MoS2/MnIn2S4 with Improved Interfacial Charge Carrier Transfer for Photocatalytic H2O2 Production
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  • Uttam Kumar
    Uttam Kumar
    Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    Department of Chemistry, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005, India
    More by Uttam Kumar
    Orcidhttps://orcid.org/0000-0001-8327-8857
  • Emmanuel Picheau
    Emmanuel Picheau
    Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    More by Emmanuel Picheau
    Orcidhttps://orcid.org/0000-0002-6921-4555
  • Huanran Li
    Huanran Li
    Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    More by Huanran Li
  • Zihan Zhang
    Zihan Zhang
    Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    More by Zihan Zhang
    Orcidhttps://orcid.org/0000-0002-4047-2278
  • Takayuki Kikuchi
    Takayuki Kikuchi
    Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    More by Takayuki Kikuchi
    Orcidhttps://orcid.org/0000-0003-0588-2172
  • Indrajit Sinha*
    Indrajit Sinha
    Department of Chemistry, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005, India
    *E-mail: [email protected]
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  • Renzhi Ma*
    Renzhi Ma
    Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    *E-mail: [email protected]
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    Orcidhttps://orcid.org/0000-0001-7126-2006
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ACS Applied Energy Materials

Cite this: ACS Appl. Energy Mater. 2025, 8, 5, 3107–3119
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https://doi.org/10.1021/acsaem.4c03296
Published February 24, 2025

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Abstract

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Photocatalytic oxygen reduction to H2O2 is a promising sustainable solar fuel production pathway. Photocatalysts with heterostructure interfaces can suppress charge carrier recombination and endow photogenerated electrons and holes with improved redox potentials. This study develops a heterostructured two-dimensional (2D) MoS2/MnIn2S4 photocatalyst for photocatalytic H2O2 production. The photocatalyst with an optimal loading of MnIn2S4 on 2D MoS2 nanosheets demonstrates the maximum H2O2 production rate of 606.7 μmol g–1 h–1, approximately 4.2 and 5 times higher than pristine 2D MoS2 and MnIn2S4, respectively. The synergistic interaction between 2D MoS2 nanosheets and MnIn2S4 results in enhanced charge separation, optical absorption, stability, and recyclability. Reaction pathway studies reveal that H2O2 production is through a sequential single-electron O2 reduction reaction by accumulated photogenerated electrons on the conduction band of the 2D MoS2/MnIn2S4 heterostructure. This work presents a noble-metal-free photocatalyst responsive to visible light for solar H2O2 generation.

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1. Introduction

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The rising demand for clean energy has intensified the search for alternatives to conventional energy sources that cause substantial environmental harm. (1,2) Hydrogen peroxide (H2O2) is a promising candidate due to its high calorific value, strong oxidation capacity, eco-friendly nature, ease of storage and transportation, and clean decomposition into water and oxygen without producing toxic byproducts. (3,4) These distinctive characteristics make H2O2 indispensable in various applications, including medical sterilization, environmental remediation, (5,6) and chemical synthesis. (7) As the demand for H2O2 grows, increasing production efficiency is critical to meet its rising need. Currently, the anthraquinone process is the predominant method for large-scale H2O2 production. However, this and related methods pose challenges, such as high energy consumption, complexity, and the risk of explosion. (8)
A promising alternative is heterogeneous photocatalysis technology, which harnesses solar energy to produce H2O2. This approach is recognized as a green and sustainable process. (9,10) During photocatalysis, H2O2 can be generated either through the two-electron (2e–) reduction of O2 via the catalyst or H2O oxidation by photogenerated holes. (11) In recent decades, a wide range of photocatalysts have been explored for H2O2 production. Notable examples include titanium dioxide (TiO2)-based photocatalysts, (12) carbon nitride (g-C3N4)-based photocatalysts, (13,14) transition metal complexes, (15) transition metal sulfides, (16,17) and bismuth (Bi)-containing semiconductors. (18) Among these, metal sulfides have attracted significant interest in photocatalysis due to their tunable band gaps, favorable electronic structures, and abundant active sites. (19)
In this context, MoS2, a typical layered transition metal dichalcogenide, has attracted significant attention due to its low cost, large surface area, strong visible light response, tunable bandgap structure, and favorable photocatalytic performance. (20,21) In particular, exfoliated or few-layered MoS2 nanosheets with a 2D structure have emerged as promising photocatalysts. The unique optical and electronic properties of 2D MoS2 contribute to better photoresponse and charge separation in photocatalysts. (22) As the number of layers decreases, MoS2 exhibits enhanced properties that improve its photocatalytic performance. (23,24) To date, several studies have reported significant enhancements in photocatalytic activity using few-layer MoS2 heterojunction composites, including In2S3/MoS2, (25) CdS/MoS2, (26) MoS2/rGO/CdS, (27) WS2–MoS2, (28) MoS2/g-C3N4, (29) and MoS2/Mn0.2Cd0.8S. (30) These heterostructured photocatalysts, which couple 2D MoS2 with other semiconductors, facilitate enhanced separation of photogenerated charge carriers and broaden solar light absorption. Composite formation effectively suppresses the recombination of charge carriers, thereby improving overall photocatalytic efficiency.
On the other hand, ternary chalcogenide AB2X4 semiconductors have recently been recognized for their significant potential as visible-light-active photocatalysts, owing to their tunable optical properties, unique electronic structure, narrow band gaps, and chemical photostability. (31,32) Among them, MnIn2S4 stands out as an ideal photocatalyst due to its appropriate band gap for visible light absorption and the high reduction potential of its conduction band electrons. Chen et al. recently developed 2D/2D g-C3N4/MnIn2S4 Z-scheme heterostructured photocatalysts for H2 production and antibiotic degradation. Their study showed that heterostructure formation significantly enhanced visible light absorption and promoted efficient interfacial charge separation, resulting in superior photocatalytic performance compared to pristine g-C3N4 and MnIn2S4. (33) Similarly, Song et al. fabricated Cu7S4/MnIn2S4 semiconductor heterostructures using a simple oil bath and hydrothermal method. The nanocomposite, featuring ultrathin 2D nanosheets and Cu7S4 nanoparticles uniformly distributed on MnIn2S4, exhibited a photocatalytic hydrogen evolution rate of 13.81 μmol h–1, nearly 18 times higher than pure MnIn2S4. The enhanced performance was attributed to the forming of a p-n heterojunction that suppressed electron–hole recombination. (34) Deng et al. designed and constructed a MnIn2S4/WO3 (Yb, Tm) photocatalytic system, incorporating a Z-scheme heterojunction to regulate spatial charge separation and improve light absorption through Yb3+ and Tm3+ doping. The system was evaluated for H2O2 production, showing remarkable activity, producing 37.2 and 8.8 times more H2O2 than WO3 and MnIn2S4, respectively. (35) However, there are no prior reports on the development of a 2D/2D MoS2/MnIn2S4 heterostructure photocatalyst.
In the current study, a heterostructure was constructed by combining few-layered MoS2 with MnIn2S4, effectively integrating the advantages of both materials. This combination exhibits strong visible-light absorption, a low recombination rate of photoinduced electron–hole pairs, and excellent photocatalytic activity. Herein, we design a novel 2D MoS2/MnIn2S4 heterostructure photocatalyst that was successfully fabricated through a green hydrothermal process. As illustrated in Scheme 1, small petals of MnIn2S4 were embedded onto ultrathin 2D MoS2 nanosheets, forming a well-integrated heterostructure. The 2D morphology of both MnIn2S4 and MoS2 enhances interfacial contact and facilitates efficient charge transfer between the two components. Various characterization techniques, including X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), diffuse reflectance spectroscopy (DRS), photoluminescence (PL), contact angle, and electrochemical measurements, were employed to investigate the intrinsic relationship between the 2D heterointerface structure and the significantly enhanced photocatalytic activity of the MoS2/MnIn2S4 heterostructure. The photocatalytic activities of the resulting samples were assessed through the H2O2 production. The improved photocatalytic performance of the heterostructure systems can primarily be attributed to the Z-scheme mechanism. This mechanism effectively harnesses the strong reduction capability of photogenerated electrons in the conduction band of MnIn2S4 nanosheets and the high oxidation capability of photogenerated holes in the valence band of 2D MoS2 nanosheets. Furthermore, the mechanism of the H2O2 production process has been thoroughly investigated. The pathway is elucidated through scavenger studies, and the reactive species involved in the photocatalytic H2O2 production are identified based on confirmatory tests. Our research will guide the future design of more versatile Z-scheme sulfide/chalcogenide heterostructure composites for H2O2 production.

Scheme 1

Scheme 1. Schematic Diagram Illustrating the Synthesis Process of As-Designed MS/MnIS-x Heterostructure Photocatalysts
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2. Experimental Section

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2.1. Materials

Ammonium molybdate tetrahydrate (NH4)6Mo7O24·4H2O), indium chloride tetrahydrate (InCl3·4H2O), ethylenediaminetetraacetic acid disodium (EDTA-2Na), para-benzoquinone (p-BQ). Thiourea (NH2CSNH2), silver nitrate (AgNO3), manganese chloride tetrahydrate (MnCl2·4H2O), and nitro blue tetrazolium (NBT) were purchased from Wako Chemicals. All reagents were used as received without any further purification.

2.2. Preparation of 2D MoS2 Nanosheets

Pristine MoS2 nanosheets were prepared through a one-step hydrothermal treatment. (36) Typically, 1 mmol of (NH4)6Mo7O24·4H2O and 30 mmol of NH2CSNH2 were dissolved in 35 mL of deionized water under vigorous stirring to form a homogeneous solution. The resulting mixture was then transferred to a 50 mL Teflon-lined autoclave and maintained at 210 °C for 24 h. After the reaction, the precipitates were allowed to cool naturally to room temperature, washed multiple times with water and absolute ethanol, and collected by ultracentrifugation at 25,000 rpm. The final products were dried at 60 °C in a vacuum oven and stored for further use.
For the preparation of 2D MoS2 nanosheets, 150 mg of the synthesized MoS2 powder was initially dispersed in 80 mL of a mixed solvent of N-methyl pyrrolidone (NMP) and deionized water (50/50 (vol%)) in a stoppered conical flask. (23) The flask was then subjected to ultrasonic bath sonication for 120 min. The resulting suspension was left overnight, and the dispersion of exfoliated MoS2 was isolated. Finally, the exfoliated MoS2 was centrifuged at 25,000 rpm for 25 min, and the exfoliated MoS2 powder was collected for further use.

2.3. Preparation of MnIn2S4

First, 0.198 g of Manganese chloride tetrahydrate (1 mmol) and 0.537 g of indium chloride tetrahydrate (2 mmol) were dissolved in 35 mL of deionized water under vigorous stirring for 1 h. Then, 0.381 g of thiourea (5 mmol) was added to the solution and stirred for two more hours. The suspension was transferred to a Teflon-lined stainless steel autoclave and heated at 210 °C for 24 h. Once the reaction was complete, the samples were allowed to cool naturally to room temperature, washed with ethanol, and dried in a vacuum oven. (33)

2.4. Synthesis of 2D MoS2/MnIn2S4

The 2D MoS2/MnIn2S4 heterostructures with varying concentrations of MnIn2S4 nanosheets were synthesized using a straightforward hydrothermal method. Initially, a certain amount of 2D MoS2 nanosheets was dispersed in deionized water and subjected to ultrasonication for 60 min to form a uniform suspension. Next, manganese chloride tetrahydrate (1 mmol), indium chloride tetrahydrate (2 mmol), and thiourea (5 mmol) were dissolved in deionized water with constant stirring on a magnetic stirrer. After 1 h of stirring, the 2D MoS2 suspension was added to the mixture and stirred for an additional 2 h. The resulting mixture was then transferred to a Teflon-lined autoclave and heated at 210 °C for 24 h. Once the reaction was complete, the samples were allowed to cool naturally to room temperature, then washed multiple times with water and ethanol and collected by centrifugation. The process produced 2D MoS2/MnIn2S4 nanocomposites with varying MnIn2S4 weight ratios, designated as MS/MnIS-x, where x corresponds to 10, 20, 40, 60, and 80, representing the weight percent of MnIn2S4 relative to 2D MoS2 in the reaction system.

2.5. Photocatalytic H2O2 Production

The photocatalytic H2O2 production experiment was carried out by dispersing 5 mg of the synthesized photocatalyst powder in 20 mL of a deionized water/ethanol mixture (95:5 vol%). The dispersion was facilitated through 10 min of ultrasonic bath treatment. Afterward, oxygen was bubbled through the solution and kept in the dark for 30 min to ensure equilibrium. The suspension was then exposed to irradiation from a solar simulator. Following 1 h of photocatalytic reaction, a 2 mL aliquot was extracted, and the photocatalyst was separated from the reaction solution.
The concentration of H2O2 was quantified using the iodometric method. (37−39) To the 2 mL aliquot (post photocatalyst removal), 2 mL of 0.1 M KI and 50 μL of 0.01 M ((NH4)6Mo7O24·4H2O) were added and thoroughly mixed. The reaction mixture was kept in the dark for 20 min to allow for a complete reaction. In this process, KI is oxidized by H2O2, releasing I2, which then reacts with excess I– (from KI) to form the yellow-colored triiodide anion (I3–) through the reaction: H2O2 + 3I– + 2H+ → I3–. The amount of I3– generated is directly proportional to the concentration of H2O2 present in the sample. Finally, the absorbance of the resulting solution was measured using UV–vis spectroscopy, showing a characteristic intense absorption peak around 352 nm.
Furthermore, to achieve optimal yields in H2O2 production, the experimental conditions, including pH, were systematically optimized. The primary reactive species generated during the photocatalytic process were identified using trapping experiments under irradiation. The contributions of electrons (e–), superoxide radicals (•O2–), and holes (h+) to H2O2 production were assessed by introducing AgNO3, p-BQ, and EDTA-2Na as scavengers.

3. Characterization Methods

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Crystalline phases were characterized by powder XRD using Cu Kα radiation (Ultima IV, Rigaku, Japan) with a step size of 0.01° and scan rate of 1°/min, covering a 2θ range from 5° to 80°. The morphology and elemental mapping were analyzed using an SEM (JEOL, JSM-6010LA) and TEM/STEM (JEOL-3100). The UV–vis diffuse reflectance spectrum was obtained using a solid state spectrophotometer (SolidSpec-3700 DUV, Shimadzu, Japan), equipped with an integrating sphere assembly, using BaSO4 as a reflectance reference sample. Similarly, a UV–vis spectrophotometer (U-4100 Hitachi) was used to measure the absorbance of the liquid sample. The photoexcited charge carrier separation of as-prepared photocatalysts was analyzed using a fluorescence spectrophotometer (F-7000, Hitachi). Water/ethanol adsorption properties were examined using the contact angle instruments (Model, CA, XP).

3.1. Electrochemical Measurements Tests

The electrochemical studies, specifically Mott–Schottky (MS) and electrochemical impedance spectroscopy (EIS), were conducted using a standard three-electrode setup in an electrochemical workstation (CHI-760E). A carbon electrode was employed as the counter electrode, an Ag/AgCl electrode served as the reference electrode, and carbon paper was used as the working electrode. The working electrode was prepared as follows: 2.5 mg of the photocatalyst was dispersed in 250 μL of a deionized water/ethanol mixture (1:1 ratio) via 30 min of ultrasonic bath sonication. Then, 10 μL of Nafion reagent was added, and the mixture was sonicated for an additional 30 min. Afterward, 40 μL of the resulting suspension was evenly applied to the carbon paper within a 0.5 cm2 area and allowed to dry at room temperature to form the working electrode. Note that 0.5 M Na2SO4 electrolyte was used for the above measurements (the pH value of the electrolyte was around 7). The band potential of the photocatalysts was determined by fitting the MS plots. The potentials obtained against Ag/AgCl (reference electrode) were then converted to the normal hydrogen electrode (NHE) scale using eq 1. The photoelectrode was fabricated using the same protocol for the photocurrent measurement. A solar simulator was used as the light source to illuminate the electrode.
VNHE=V(Ag/AgCl)+0.059×pH+0.197
(1)

4. Results and Discussion

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Powder XRD was carried out to investigate the phase purity and crystal structures of the 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructures. Figure 1 shows the corresponding XRD patterns of the various samples. The XRD pattern traced in purple is of the as-prepared 2D MoS2 nanosheets. The observed diffraction peaks at two theta (2θ) values of 14.2°, 33.4°, and 58.8° can be uniquely attributed to the (002), (100), and (110) crystal planes of standard hexagonal MoS2 (2H MoS2, JCPDS card No. 731508), respectively, revealing the high purity of the sample. There is an apparent broadening of all the peaks in the diffraction patterns, which suggests the nanoscales of the crystallites in different dimensions. (36) The red trace represents the diffraction pattern of standard cubic structure MnIn2S4 phase (JCPDS No. 85-1229). The characteristic peaks of MoS2 at (002) and (110) were observed in all 2D MoS2/MnIn2S4 heterostructures, confirming that the composite structure consists of hexagonal MoS2 and cubic MnIn2S4. No diffraction peaks associated with impurities were detected, confirming the high purity of the synthesized heterostructure photocatalysts.

Figure 1

Figure 1. XRD patterns of 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts.

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The optical properties of the 2D MoS2 nanosheets, produced via liquid-phase ultrasonication, were examined using UV–visible absorbance spectrophotometry. A slight shift in the UV–visible spectral peak toward a lower wavelength (Figure S1a) suggests a change in the bandgap due to exfoliation. Additionally, the light absorbance in the visible region was significantly enhanced after exfoliation compared to bulk MoS2. Figure S1b indicates the successful and stable dispersion of exfoliated MoS2 nanosheets.
Similarly, the optical characteristics of 2D MoS2, MnIn2S4, and the MS/MnIS-x heterostructure were explored through solid-state UV–Vis NIR analysis, as shown in Figure 2. From the absorbance spectra, it is clear that 2D MoS2 shows a strong visible light absorption band at a range of 300–1350 nm. Similarly, pristine MnIn2S4 exhibited visible light absorption with a characteristic absorption edge near 680 nm. Compared to pristine MnIn2S4, the formation of the MS/MnIS-x heterostructure resulted in a significant redshift of the absorption edge, with strong absorption observed in the visible to NIR range from approximately 340 to 1350 nm. The DRS results demonstrated that the formation of 2D MoS2/MnIn2S4 heterostructures allows for more efficient exploitation of solar energy. Further, the band gap energy (Eg) of the 2D MoS2, MnIn2S4, was calculated using Tauc’s plot using eq 2.
(αhv)1/n=A(hv−Eg)
(2)

Figure 2

Figure 2. (a) Solid-state UV-DRS absorbance spectra of 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts. (b,c) Tauc plot of 2D MoS2 and MnIn2S4. Mott–Schottky plot of (d) MnIn2S4 and (e) 2D MoS2.

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Where hv and α represent the photoelectron energy and absorption coefficient, respectively. The measured band gap energies of 2D MoS2 and MnIn2S4 were 1.52 and 1.88 eV, respectively, as shown in Figure 2b,c. The calculated band gap of bulk MoS2 (before exfoliation) is provided in Figure S2a. These results indicate that, after successful exfoliation into nanosheets, the band gap energy increased from 1.31 to 1.52 eV. Furthermore, the Tauc plots of MS/MnIS-x photocatalysts are provided in Figure S2b–f.
Mott–Schottky (MS) measurements were carried out at 100 and 200 Hz to investigate the band structure and semiconductor type. Figure 2d,e shows the MS curves for 2D MoS2 and MnIn2S4 samples. Both 2D MoS2 and MnIn2S4 exhibited positive MS slopes, confirming their n-type semiconductor characteristics. The conduction band potentials were determined to be −0.1 V for 2D MoS2 and −0.81 V for MnIn2S4 versus NHE by fitting the 1/C2 vs potential plot. By combining the MS results with the energy band gaps of 2D MoS2 and MnIn2S4, as determined by the Tauc plot, the valence band positions were calculated to be 1.42 V for 2D MoS2 and 1.07 V for MnIn2S4, respectively, using the formula EVB = ECB + Eg. (40,41) Here, EVB represents the valence band edge position, and ECB denotes the conduction band edge position. It is noteworthy that the CB potentials of MnIn2S4 are more negative than the reduction potentials of O2/•O2– (−0.33 V vs NHE) and O2/H2O2 (0.68 V vs NHE). This indicates that their reduction potentials are sufficient to drive the formation of H2O2.
The morphologies and microstructures of MnIn2S4, 2D MoS2, and the MS/MnIS40 heterostructures were thoroughly characterized using SEM and TEM. The analysis revealed that both 2D MoS2 and MnIn2S4 exhibit a layered structure with lateral dimensions of several hundred nanometers, respectively. Figure 3 presents the SEM images of MnIn2S4 and the MS/MnIS40. The pure MnIn2S4 exhibits a distinctive nanoflower-like structure composed of small petal-like features, as shown in Figure 3a,b. Notably, these petal-like formations gradually orient themselves into a cohesive nanoflower morphology. This unique morphology is advantageous for photocatalytic H2O2 production, as it provides many active sites for the reaction. Figure S3 displays the SEM elemental mapping images of pristine MnIn2S4 photocatalysts, revealing the homogeneous distribution of Mn, In, and S elements in pure MnIn2S4. Similarly, the SEM images of the MS/MnIS40 heterostructure (Figure 3c,d) illustrate the formation of small petal-like nanostructures of MnIn2S4 embedded on the thin, layered 2D MoS2 nanosheets. The corresponding SEM elemental mapping images confirm the uniform distribution of Mn, In, Mo, and S elements within the MS/MnIS40 heterostructure, indicating partial coverage of the 2D MoS2 surface by MnIn2S4. However, as the MnIn2S4 loading increases, excessive deposition leads to agglomeration, resulting in the formation of nanoflowers that entirely cover the 2D MoS2 surface. Additionally, Figure S4a,b presents the SEM images and elemental mapping for the MS/MnIS60 and MS/MnIS80 samples. No extra elements are detected in these samples, confirming the high purity and successful formation of the heterostructure in the synthesized materials.

Figure 3

Figure 3. (a,b) SEM images of pristine MnIn2S4. (c) SEM images of MS/MnIS40 heterostructure photocatalysts. (d) SEM image with corresponding elemental maps (Mo, Mn, In, S) of MS/MnIS40 heterostructure photocatalysts.

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To further confirm the morphology and structure of 2D MoS2, MnIn2S4, and the MS/MnIS40 heterostructure were observed using TEM and high-resolution TEM (HRTEM).
Notably, the TEM images of the MnIn2S4 (Figure 4a) and 2D MoS2 (Figure 4d) display layered structures with a nearly transparent appearance, consistent with the presence of ultrathin nanosheets. The inverse fast Fourier transform (IFFT) images and spectra of the HRTEM images of pristine MnIn2S4, as shown in Figure 4c, reveal distinct lattice fringes of 0.32 nm, corresponding to the (311) crystal plane of MnIn2S4, which is consistent with the intense peak observed in the XRD pattern (JCPDS No. 85-1229). Figure 4d reveals that the 2D MoS2 consists of a few-layered, curled nanosheets with a scattered orientation. As shown in Figure 4e, the interlayer spacing of 6.3 Å corresponds to the (002) planes of MoS2, verifying its hexagonal (2H) structure. These nanosheets exhibit higher crystallinity and a relatively intact layered configuration, which aligns well with the XRD results. The HRTEM images of the 2D MoS2 nanosheets in Figures 4e and S5a reveal structural defects in the 2H MoS2, typically characterized by cracks and misaligned basal planes, as previously reported in the literature. (36,42) After forming the 2D MoS2 and MnIn2S4 heterostructures (MS/MnIS40), the structure exhibits an ultrathin nanosheet-on-nanosheet morphology (Figure 4f,g) with a large contact surface. The IFFT images and spectra derived from the HRTEM image of the 2D/2D heterostructure (Figure 4h) reveal lattice fringes of MnIn2S4 (0.32 nm) and 2D MoS2 (0.63 nm), confirming strong interfacial contact between the two materials and the successful formation of the heterostructure. This extensive, intimate interface enables multiple pathways for carrier migration, enhancing charge separation efficiency. Furthermore, the elemental mapping analysis of the selected region in Figure S5b for the MS/MnIS40 heterostructure clearly demonstrates the well-defined spatial distribution of Mo, Mn, In, and S (Figure 4i). The electron microscopy results clearly reveal a uniform and intimate coupling within the 2D structure of MoS2/MnIn2S4, which substantially increases the contact area. This expanded interface improves the separation of photoinduced charge carriers and facilitates more efficient electron transfer within the heterostructure, leading to a significant enhancement in photocatalytic activity. (43)

Figure 4

Figure 4. TEM, HR-TEM, and IFFT images of (a–c) pure MnIn2S4, (d,e) 2D MoS2, (f–h) MS/MnIS40 heterostructure. (i) STEM elemental mapping of MS/MnIS40 heterostructure photocatalysts.

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The X-ray photoelectron spectroscopy (XPS) analysis revealed the interfacial chemical states and interactions in the 2D MoS2, MnIn2S4, and MS/MnIS40 samples. The HR-XPS data was calibrated using a C 1s binding energy of 284.8 eV. (44) The XPS survey spectrum in Figure S6 confirms the presence of Mo and S elements in MoS2 and Mn, In, and S elements in MnIn2S4. Similarly, the survey spectrum of the MS/MnIS40 samples shows Mo, Mn, In, and S, further indicating the successful formation of heterostructures of 2D MoS2 and MnIn2S4. The high resolution (HR) Mn 2p spectra of MnIn2S4 (Figure 5a) show characteristic peaks at binding energies of 641.8 and 645.3 eV for Mn 2p3/2 and at 652.8 and 654.1 eV for Mn 2p1/2. These peaks are attributed to the Mn2+ and Mn4+ oxidation states. (35) In the Mn 2p spectra of the MS/MnIS40 heterostructure (Figure 5a), the Mn 2p3/2 and Mn 2p1/2 peaks are slightly shifted toward lower binding energies. Figure 5b shows the In 3d spectra for both MnIn2S4 and MS/MnIS40, where the binding energies of the In 3d peaks at 445.1 eV (In 3d5/2) and 452.7 eV (In 3d3/2) confirm the +3 oxidation state of In in MnIn2S4. Compared to pure MnIn2S4, the In 3d XPS peaks in the MS/MnIS40 heterostructures also shift toward lower binding energies.

Figure 5

Figure 5. XPS spectra of 2D MoS2, MnIn2S4, and MS/MnIS40: (a) Mn 2p, (b) In 3d, (c) Mo 3d, and (d) S 2p.

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The Mo 3d spectrum (Figure 5c) exhibits two distinct peaks at 229.7 and 232.9 eV, corresponding to the binding energies of Mo 3d5/2 and Mo 3d3/2, associated with the 2H phase of MoS2. These findings confirm that Mo in MoS2 is in the +4 oxidation state. An additional peak observed at a binding energy of 226.8 eV corresponds to the S 2s state, indicating the interaction between S and Mo. Compared to 2D MoS2, the characteristic Mo 3d peaks of MS/MnIS40 shift slightly to higher binding energies. Conversely, the Mn 2p and In 3d peaks in MnIn2S4 shift to lower binding energies upon forming MS/MnIS40 heterostructure, suggesting a strong interaction between 2D MoS2 and MnIn2S4. (45) A shift to lower binding energy indicates an increase in electron cloud density, while a shift to higher binding energy implies a decrease in electron cloud density. Consequently, the binding energy shifts observed in the XPS reveal the direction of electron transfer from 2D MoS2 to MnIn2S4 in the MS/MnIS40 heterostructure system. (46−49)
Figure 5d displays the HR S 2p spectra of MnIn2S4, 2D MoS2, and MS/MnIS40 heterostructure. The S 2p spectrum displays two distinct peaks at 162.2 eV for S 2p3/2 and 163.5 eV for S 2p1/2, corresponding to the binding energies of S2– ions in MoS2. (50) The S 2p binding energies of MnIn2S4 were detected at 161.6 eV for S 2p3/2 and 162.5 eV for S 2p1/2, respectively. The small peak at a binding energy of 168.9 eV is attributed to sulfate species formed by the oxidation of sulfur in air. (51)
A photoluminescence (PL) study of the photocatalytic material reveals insights into photoinduced charge carriers’ migration, transfer, and separation efficiency. Typically, a decrease in the PL emission intensity corresponds to a reduction in the charge carrier recombination rate, indicating enhanced separation of photogenerated electron–hole pairs. (38) The PL emission spectra of pristine MnIn2S4 and MS/MnIS-x, excited at 340 nm at room temperature, are shown in Figure 6a. The PL spectra of MS/MnIS10 and MS/MnIS80 are provided in Figure S7a. A prominent emission peak centered at 450 nm is observed for the as-prepared photocatalysts. In contrast, the MS/MnIS40 heterostructure exhibits the lowest PL intensity among the other photocatalysts. This suggests that incorporating 40% MnIn2S4 onto 2D MoS2 enhances the separation of electron–hole pairs on the catalyst’s surface. This enhancement likely contributes to the superior photocatalytic performance of the MS/MnIS40 heterostructure toward the oxygen reduction reaction (ORR). The primary reason is the reduced recombination rate of photogenerated electrons, which allows them to migrate efficiently to the surface of MnIn2S4, thereby enhancing the photoreduction process. Furthermore, electrochemical impedance spectroscopy (EIS) was conducted to assess the interfacial charge transfer behavior of the prepared photocatalysts. Figure 6b presents the Nyquist plots of the 2D MoS2 and MS/MnIS-x heterostructure systems. Figure S7b shows the Nyquist plot of MnIn2S4, MS/MnIS10, and MS/MnIS80 photocatalysts. As illustrated, the MS/MnIS40 system exhibits the smallest arc diameter, signifying reduced charge transfer resistance and impedance, suggesting improved charge migration. (52) In the MS/MnIS40 heterojunction, the heterostructure formation is well-balanced with a proper interface, ensuring effective electron transport from 2D MoS2 to MnIn2S4 while minimizing charge recombination. In contrast, lower MnIn2S4 loadings (10 and 20 wt%) result in insufficient heterojunction formation, leading to higher recombination losses. On the other hand, excessive MnIn2S4 content (60 and 80 wt%) causes nanosheet agglomeration, which not only covers the active sites on the 2D MoS2 surface but also leads to charge accumulation, ultimately increasing resistance. Figure S7d presents the corresponding fitting circuit along with the Rs and Rct values for 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts. Similar results were observed for these materials in the transient photocurrent responses (Figure 6c). The charge separation process is reflected in the transient photocurrent, as shown by the chronoamperometry. A significant spike in current occurs immediately upon light exposure, followed by a rapid decline when the light is turned off (Figure 6c). Notably, the MS/MnIS40 heterostructure photocatalyst exhibits a significantly higher photocurrent density compared to the other prepared photocatalysts. The photocurrent response of MnIn2S4, MS/MnIS10, and MS/MnIS80 are given in Figure S7c. The combined observations from PL, EIS, and photocurrent experiments clearly demonstrate that the MS/MnIS40 heterostructure can serve as an efficient photocatalyst, exhibiting enhanced photocatalytic H2O2 production.

Figure 6

Figure 6. (a) PL spectra of MnIn2S4 and MS/MnIS-x heterostructure photocatalysts; (b,c) Nyquist plot and photocurrent studies of 2D MoS2 and MS/MnIS-x heterostructure photocatalysts.

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To investigate the impact of photocatalyst surface properties on its activity, we performed contact angle measurements to assess the hydrophilic characteristics of photocatalysts. These experiments were carried out under similar conditions, as a reactant of 5% (vol) ethanol-containing water was used. After 2 s of contact with water/ethanol mixture droplets, the contact angle of 2D MoS2, MnIn2S4 (Figure S8), MS/MnIS10, MS/MnIS20, MS/MnIS40, MS/MnIS60, and MS/MnIS80 are 43.4°, 14.9°, 37.4°, 30.5°, 23.9°, 20.5 ° and 18.1°; results confirmed its hydrophilic nature (Figure 7). A smaller contact angle signifies better wetting of the photocatalyst particle surface by the solvent molecules. It also implies longer residence times for solvent molecules from the water/ethanol mixture, facilitating better contact between the photocatalyst particles and reactants. (53) Additionally, the hydrophilic surface improves the uniform dispersion of the photocatalyst within the reaction system, leading to increased reaction rates and selectivity.

Figure 7

Figure 7. Contact angle results: (a) 2D MoS2, (b) MS/MnIS10, (c) MS/MnIS20, (d) MS/MnIS40, (e) MS/MnIS60, and (f) MS/MnIS80.

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4.1. Photocatalytic H2O2 Production

The photocatalytic activities of 2D MoS2, MnIn2S4, and MS/MnIS-x for H2O2 production were evaluated under various controlled conditions at room temperature and atmospheric pressure. Initially, H2O2 production was tested without a catalyst or light irradiation. Under these conditions, no H2O2 was detected, confirming that the H2O2 production reaction at room temperature is driven by solar light in the presence of photocatalysts. Figure S9a illustrates the H2O2 production rates for different photocatalysts in O2-bubbled water at pH 3. The MS/MnIS-x heterostructure photocatalysts demonstrated significant H2O2 formation compared to pristine 2D MoS2 and MnIn2S4. Among the various MnIn2S4 loadings, the 40 wt% loading onto 2D MoS2 achieved a remarkable H2O2 production rate of 240.2 μmol g–1 h–1. However, further increasing the MnIn2S4 loading onto the 2D MoS2 resulted in a decline in H2O2 production, likely due to excessive 2D MoS2 active surface coverage. Moreover, the excess loading caused agglomeration of the nanosheets, as confirmed by the SEM image and elemental mapping of MS/MnIS60 and MS/MnIS80 in Figure S4a,b. This excessive coverage impairs visible light absorption and hinders efficient interfacial charge transfer, as evidenced by the EIS and PL results.
In contrast, when ethanol was introduced into the reaction mixture as a sacrificial agent, the photocatalytic H2O2 production rate was improved, as shown in Figure S9a. Figure 8a displays the time-dependent curve of photocatalytic H2O2 production of different photocatalysts. This enhancement confirms the oxidation of ethanol by the photogenerated holes. The best-performing photocatalyst, MS/MnIS40, achieved an impressive H2O2 production rate of 606.7 μmol g–1 h–1, whereas pristine 2D MoS2 and MnIn2S4 exhibited only 147.4 μmol g–1 h–1 and 121.5 μmol g–1 h–1, respectively. This corresponds to an approximately 4.2-fold increase compared to pristine 2D MoS2 and a 5-fold increase compared to MnIn2S4 alone. Notably, the H2O2 generation rate of our MS/MnIS40 surpassed that of recently reported heterostructure-based photocatalysts (Figure 8h and Table S1).

Figure 8

Figure 8. (a) The time-dependent plot of photocatalytic H2O2 production for various photocatalysts prepared in this study. (b) Kinetics plot of photocatalytic H2O2 decomposition on different photocatalysts. (c) H2O2 production at different pH levels using the optimal photocatalyst, MS/MnIS40. (d) H2O2 production under control conditions with MS/MnIS40. (e) H2O2 production with MS/MnIS40 in scavenger experiments. (f) Cycling experiments showing H2O2 production at different time intervals using MS/MnIS40. (g) XRD patterns of fresh and recycled MS/MnIS40 photocatalysts. (h) Comparison of photocatalytic H2O2 production with recently reported photocatalysts.

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It is important to note that both the formation and decomposition of H2O2 occur simultaneously during the photocatalytic process, as photogenerated charge carriers can consume H2O2. Consequently, the H2O2 production curves are fitted using a kinetic model that includes both a zero-order and a first-order term to evaluate the respective rates of H2O2 formation and decomposition. The kinetic equation, shown in eq 3, describes the changes in H2O2 concentration as a function of illumination time. (38,54)
[H2O2]=KfKd×{1−exp(−Kd×t)}
(3)
Here, Kf (μM min–1) and Kd (min–1) represent the rate constants for H2O2 generation and decomposition, respectively, while [H2O2] refers to the concentration of generated H2O2 (μM), and t denotes the reaction time (min). (55) In Figure S9b, the time-dependent H2O2 decomposition plot and kinetics plot in Figure 8b reveal that both 2D MoS2 and MnIn2S4 exhibit higher decomposition rate constants (Kd of 0.01488 min–1 and 0.00482 min–1, respectively) compared to the MS/MnIS-x heterostructure photocatalysts. The heterostructures with MnIn2S4 loadings ranging from 10 wt% to 40 wt% on 2D MoS2 effectively suppress H2O2 decomposition. However, loadings beyond 40 wt%, such as 60 and 80 wt%, result in an increase in H2O2 decomposition. These photocatalytic results suggest that enhanced photogenerated charge separation and improved light absorption contribute to higher H2O2 formation while reducing decomposition.
The photocatalytic H2O2 production activity of the best catalyst (MS/MnIS40) was further evaluated at different pH levels (1.5, 3, 5, and 7). The pH-dependent experiments showed that the activity followed the trend: pH 3 > pH 1.5 > pH 5 > pH 7. At pH 3, a significantly enhanced H2O2 production rate of 606.7 μmol g–1 h–1 was achieved (Figure 8c), suggesting that protonation-induced ionic species contribute to the improved activity. (56) At a low pH of 1.5, the solution provides an excess of protons (H+) in the reaction medium, which promotes the oxidation of H2O2 to water (H2O2 + 2H+ + 2e– → 2H2O), thereby reducing the overall H2O2 yield. Conversely, at pH 5 and 7, the lower availability of protons in the solution results in decreased H2O2 formation. Moreover, at a higher pH solution, •O2– becomes unstable, and H2O2 breaks down more quickly, further lowering its production. Hence, pH 3 was identified as the optimum pH for H2O2 production. (37,57,58)
To investigate the effect of the heterostructure in MS/MnIS40, control experiments using a physical blend of 60% 2D MoS2 and 40% MnIn2S4 photocatalyst were conducted under optimal H2O2 production conditions (Figure 8d). Under these conditions, the H2O2 production rate was only 188.4 μmol g–1 h–1, approximately 3.3 times lower than the best photocatalyst (MS/MnIS40). These results confirm that the proper formation of the heterostructure enhances visible light absorption and suppresses charge carrier recombination, leading to higher photocatalytic activity.
To gain further insight into the photocatalytic oxygen reduction reaction (ORR) pathway for H2O2 production by the MS/MnIS40 photocatalyst, control experiments with various scavengers were conducted. The photocatalytic performance of MS/MnIS40 was also evaluated under argon (Ar) atmosphere. When the reaction systems were purged with Ar, the H2O2 concentration dropped by 82%, demonstrating that O2 plays a crucial role in the photocatalytic process, with H2O2 predominantly formed via the ORR. Interestingly, 18% of the H2O2 concentration was retained even under the Ar atmosphere, suggesting that the ORR process subsequently consumes the O2 generated from water oxidation to produce H2O2 (Figure 8d). Two potential routes have been reported for synthesizing H2O2 from O2 via a 2e– redox process: a two-step ORR process involving •O2– as an intermediate species and a direct 2e– ORR process. To clarify the exact pathway, a •O2– scavenger test was conducted using p-BQ. As shown in Figure 8e, the scavenger experiment with p-BQ indicated the formation of •O2– during the photocatalytic H2O2 production pathway, as adding p-BQ reduced H2O2 production by 65%. This result confirms that O2 is reduced to form H2O2 through the •O2– intermediate via a two-step process. (59) Further validation of •O2– involvement was conducted using the NBT test. As shown in Figure S10, NBT is selectively reduced by •O2–, forming formazan. This reduction is evidenced by decreased NBT absorption intensity with prolonged illumination. The detailed experimental protocol of NBT experiments is provided in the Supporting Information. Furthermore, adding AgNO3 confirmed that photogenerated electrons play a crucial role in the photocatalytic process, significantly reducing H2O2 production. Similarly, introducing EDTA-2Na as a hole (h+) scavenger resulted in approximately a 76% reduction in H2O2 production compared to the case of no scavenger, highlighting the involvement of h+ in the photocatalytic reaction. This result suggests that •O2– radicals, e–, and h+ play a major role in photocatalytic H2O2 production (Figure 8e).
The photostability of photocatalytic materials is a critical factor influencing H2O2 production efficiency. To evaluate this, the recyclability of the MS/MnIS40 photocatalyst for H2O2 production was tested over five cycles under identical experimental conditions. After each cycle, the photocatalyst was recovered by centrifugation, rinsed with ethanol, and dried at 60 °C for 5 h to assess its reusability. The dried photocatalyst was then reused in subsequent cycles. Figure 8f illustrates the H2O2 production activity of the MS/MnIS40 photocatalyst over five reuse cycles. After five cycles, the MS/MnIS40 heterostructure demonstrated remarkable stability, with H2O2 production remaining nearly unchanged and only a slight 7.8% decrease in H2O2 formation efficiency. This indicates that the heterostructure maintains its photocatalytic activity well, which is crucial for practical applications. Moreover, we performed XRD and XPS measurements of the recycled photocatalyst, as shown in Figures 8g and S11. The XRD patterns and XPS spectra of MS/MnIS40 before and after the fifth cycle of the photocatalytic reaction show no noticeable changes, indicating that the crystal structure and chemical states remained stable throughout the recycling process. These findings strongly confirm that the MS/MnIS40 heterostructure exhibits excellent photochemical stability and reusability, which is advantageous for long-term use and continuous operation in photocatalytic H2O2 production systems.

4.2. Photocatalytic Mechanism

The photocatalytic H2O2 production of as-prepared photocatalysts performance is presented in Figure 8a. Among them, MS/MnIS40 exhibits the highest photocatalytic activity compared to the other catalysts. Based on the experimental data, a photocatalytic H2O2 production mechanism is proposed, as illustrated in Figure 9. The combination of 2D MoS2 and MnIn2S4 likely forms a Z-scheme heterojunction, as suggested by the Mott–Schottky and scavenger tests. Upon light irradiation of the MS/MnIS40 photocatalyst, photogenerated electrons accumulate in the CB of MnIn2S4, which has a more negative ECB potential at −0.81 eV (vs V NHE), closely aligning with the reduction potential of O2 at −0.33 eV (vs V NHE). The negative potential of MnIn2S4 CB and the O2/•O2– couple facilitates rapid electron transfer, promoting the two-step one electron O2 reduction necessary for H2O2 generation (eqs 4 and 5). The significant reduction in H2O2 yield in the presence of p-BQ, along with NBT experiments, confirms that •O2– is the primary active species. This suggests that H2O2 is produced through the further conversion of •O2– radicals, generated by the reduction of O2 at −0.33 eV (vs V NHE). Simultaneously, the photogenerated holes in the VB of 2D MoS2 oxidize water molecules, producing O2 and H+ (eq 6), as the VB potential of 2D MoS2 (+1.42 V vs NHE) is more positive than the H2O/O2 potential (+1.23 V vs NHE). Control experiments under “Ar” purging showed that 18% of the H2O2 concentration was retained even in the absence of external O2, suggesting that O2 is generated from water oxidation. Moreover, the addition of ethanol significantly enhances H2O2 production by facilitating its activation, as photogenerated holes are efficiently consumed in the oxidation of ethanol. This reaction also provides H+ ions, which later react with •O2– to form H2O2 (eq 7). (60) These factors are crucial for optimizing the photocatalytic ORR process to boost H2O2 production.
O2+e−→•O2−
(4)
•O2−+e−+2H+→H2O2
(5)
2H2O+2h+→O2+4H++2e−
(6)
CH3CH2OH+2h+→CH3CHO+2H+
(7)

Figure 9

Figure 9. Possible mechanism of the photocatalytic H2O2 generation on 2D MoS2/MnIn2S4 photocatalyst.

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5. Conclusions

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In conclusion, we have designed the ultrathin 2D MoS2 nanosheets embedded with MnIn2S4 heterostructure photocatalysts for solar-driven H2O2 production using a facile two-step hydrothermal method. It was observed that the optimal loading of MnIn2S4 partially covers the 2D MoS2 nanosheets, enhancing light absorption and providing more active sites. This leads to improved charge carrier separation and accelerated electron transfer, resulting in enhanced photocatalytic H2O2 production. However, excessive loading of MnIn2S4 covers the surface active sites of MoS2 and blocks light absorption, leading to poor interfacial charge carrier separation and reduced photocatalytic activity. Moreover, the poor H2O2 production activity observed in physical blending experiments (2D MoS2 + MnIn2S4) confirms that when proper heterostructures are formed, the MS/MnIS40 photocatalyst exhibits excellent H2O2 production activity, approximately 3.3 times higher than that of the physically blended mixtures. This demonstrates that the formation of an intimately connected/contacted heterostructure effectively inhibits charge recombination and accelerates charge transfer. The microscopy characterization results reveal a strong interfacial interaction between the components of 2D MoS2 and MnIn2S4. The controlled radical trapping studies confirmed that H2O2 generation preferably occurred via a dual-step, one-electron O2 reduction pathway. This study can inspire the exploration and development of effective noble-metal-free semiconductor heterostructure photocatalysts for solar-driven H2O2 generation.

Supporting Information

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The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsaem.4c03296.

  • UV visible absorbance spectra of bulk MoS2 and exfoliated MoS2 nanosheets; images of exfoliated MoS2 nanosheets dispersion; Tauc plot of bulk MoS2 and MS/MnIS-x heterostructures photocatalyst; SEM elemental mapping of MnIn2S4; SEM images with corresponding elemental mapping of MS/MnIS60 and MS/MnIS80 heterostructure photocatalysts; HRTEM images of 2D MoS2 nanosheets; TEM images of MS/MnIS40 photocatalysts; XPS survey spectra of MnIn2S4, 2D MoS2, and MS/MnIS40; PL spectra of MS/MnIS10 and MS/MnIS80; Nyquist plot of pure MnIn2S4 MS/MnIS10 and MS/MnIS80 heterostructure photocatalysts; photocurrent studies of MnIn2S4, MS/MnIS10, and MS/MnIS80 photocatalysts; EIS equivalent fitting circuit and Rs and Rct value of 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts; contact angle results of pristine MnIn2S4; photocatalytic H2O2 production rate at O2 bubbled DI and water/EtOH mixture at pH 3; photocatalytic H2O2 decomposition at different time intervals; table showing the comparison of photocatalytic H2O2 production among recently reported other photocatalytic systems; NBT experiments on MS/MnIS40 photocatalyst; XPS spectra of recycled MS/MnIS40 photocatalyst (PDF)

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Author Information

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  • Corresponding Authors
    • Indrajit Sinha - Department of Chemistry, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005, India;  Email: [email protected]
    • Renzhi Ma - Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan;  Orcidhttps://orcid.org/0000-0001-7126-2006;  Email: [email protected]
  • Authors
    • Uttam Kumar - Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan;  Department of Chemistry, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005, India;  Orcidhttps://orcid.org/0000-0001-8327-8857
    • Emmanuel Picheau - Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan;  Orcidhttps://orcid.org/0000-0002-6921-4555
    • Huanran Li - Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan
    • Zihan Zhang - Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan;  Orcidhttps://orcid.org/0000-0002-4047-2278
    • Takayuki Kikuchi - Research Center for Materials Nanoarchitectonics (WPI-MANA), National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan;  Orcidhttps://orcid.org/0000-0003-0588-2172
  • Notes
    The authors declare no competing financial interest.

Acknowledgments

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This research work was conducted under the International Cooperative Graduate Program (ICGP) of the National Institute for Materials Science (NIMS). Mr. Uttam Kumar gratefully acknowledges the support received from the IIT BHU Fellowship and the NIMS-ICGP internship program.

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    Small (2022), 18 (8), 2104561CODEN: SMALBC; ISSN:1613-6810. (Wiley-VCH Verlag GmbH & Co. KGaA)
    A review. Hydrogen peroxide (H2O2) is a mild but versatile oxidizing agent with extensive applications in bleaching, wastewater purifn., medical treatment, and chem. synthesis. The state-of-art H2O2 prodn. via anthraquinone oxidn. is hardly considered a cost-efficient and environment-friendly process because it requires high energy input and generates hazardous org. wastes. Photocatalytic H2O2 prodn. is a green, sustainable, and inexpensive process which only needs water and gaseous dioxygen as the raw materials and sunlight as the power source. Inorg. metal oxide semiconductors are good candidates for photocatalytic H2O2 prodn. due to their abundance in nature, biocompatibility, exceptional stability, and low cost. Progress has been made to enhance the photocatalytic activity toward H2O2 prodn., however, H2O2 photosynthesis is still in the lab. research phase since the productivity is far from satisfaction. To inspire innovative ideas for boosting the H2O2 yield in photocatalysis, the most well-studied metal oxide photocatalysts are selected and the modification strategies to improve their activity are listed. The mechanisms for H2O2 prodn. over modified photocatalysts are discussed to highlight the facilitating role of the modification methods. Besides, methods for the quantification of H2O2 and assocd. radical intermediates are provided to guide future studies in this field.
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  13. 13
    Xie, L.; Wang, X.; Zhang, Z.; Ma, Y.; Du, T.; Wang, R.; Wang, J. Photosynthesis of Hydrogen Peroxide Based on g-C 3 N 4: The Road of a Cost-Effective Clean Fuel Production. Small 2023, 19 (32), 2301007,  DOI: 10.1002/smll.202301007
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    Yan, J.; Li, Y.; Li, Y.; Ouyang, S.; Zhang, T. Recent Advances in Photocatalytic Hydrogen Peroxide Production, PhotoMat (In Press) , 2023.  DOI: 10.1002/phmt.8
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    Isaka, Y.; Oyama, K.; Yamada, Y.; Suenobu, T.; Fukuzumi, S. Photocatalytic Production of Hydrogen Peroxide from Water and Dioxygen Using Cyano-Bridged Polynuclear Transition Metal Complexes as Water Oxidation Catalysts. Catal. Sci. Technol. 2016, 6 (3), 681– 684,  DOI: 10.1039/C5CY01845E
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    15
    Photocatalytic production of hydrogen peroxide from water and dioxygen using cyano-bridged polynuclear transition metal complexes as water oxidation catalysts
    Isaka, Yusuke; Oyama, Kohei; Yamada, Yusuke; Suenobu, Tomoyoshi; Fukuzumi, Shunichi
    Catalysis Science & Technology (2016), 6 (3), 681-684CODEN: CSTAGD; ISSN:2044-4753. (Royal Society of Chemistry)
    Hydrogen peroxide was produced efficiently from water and dioxygen using [RuII(Me2phen)3]2+ (Me2phen = 4,7-dimethyl-1,10-phenanthroline) as a photocatalyst and cyano-bridged polynuclear transition metal complexes composed of Fe and Co as water oxidn. catalysts in the presence of Sc3+ in water under visible light irradn.
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  16. 16
    Song, H.; Wei, L.; Chen, C.; Wen, C.; Han, F. Photocatalytic Production of H2O2 and Its in Situ Utilization over Atomic-Scale Au Modified MoS2 Nanosheets. J. Catal. 2019, 376, 198– 208,  DOI: 10.1016/j.jcat.2019.06.015
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    16
    Photocatalytic production of H2O2 and its in situ utilization over atomic-scale Au modified MoS2 nanosheets
    Song, Haiyan; Wei, Lishan; Chen, Chunxia; Wen, Congcong; Han, Fuqin
    Journal of Catalysis (2019), 376 (), 198-208CODEN: JCTLA5; ISSN:0021-9517. (Elsevier Inc.)
    Au modified MoS2 nanosheets (Au@MoS2) for photocatalytic prodn. of H2O2 were prepd. via a simple pathway including the deposition-redn. and immobilization process by using a low dosage of an Au source. Nanoparticles smaller than 1 nm and single atoms, as two major forms of Au, were found to be widely dispersed on the surface of MoS2 and captured by its lattices. Au modification brought out the low recombination rate of e--h+ pairs, long lifetime of electrons, and more neg. flat band potential for MoS2. Au@MoS2 achieved efficient photocatalytic prodn. of H2O2 from H2O and air in the absence of pure O2 and org. electron donors. An optimal catalyst loading 0.50 wt% of Au enhanced the H2O2 productivity by about 2.5 times from bare MoS2. A significant finding was that higher pH was beneficial to H2O2 synthesis, and the H2O2 productivity at pH 9 was further enhanced 7.4 times from that at pH 2. Au@MoS2 was recycled more than five times without inactivation and obtained considerable 791.72 μM of H2O2 under real sunlight irradn. for 6 h, exhibiting application potential. Mn2+ as the active center for Fenton-like reactions was doped in MoS2 nanosheets before Au0 modification in order to use the photogenerated H2O2 in situ. Accordingly, a novel in situ Fenton process was proposed, and obtained significant degrdn. efficiencies for rhodamine B and methylene blue dyes, depending on the H2O2 productivity. Another important finding was that Mn2+ further increased H2O2 productivity by 2 times based on Au@MoS2.
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  17. 17
    Das, S.; Acharya, L.; Biswal, L.; Parida, K. Augmented Photocatalysis Induced by 1T-MoS2 Bridged 2D/2D MgIn2S4@1T/2H-MoS2 Z-Scheme Heterojunction: Mechanistic Insights into H2O2 and H2 Evolution. Nanoscale Adv. 2024, 6 (3), 934– 946,  DOI: 10.1039/D3NA00912B
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  18. 18
    Mase, K.; Yoneda, M.; Yamada, Y.; Fukuzumi, S. Efficient Photocatalytic Production of Hydrogen Peroxide from Water and Dioxygen with Bismuth Vanadate and a Cobalt(II) Chlorin Complex. ACS Energy Lett. 2016, 1 (5), 913– 919,  DOI: 10.1021/acsenergylett.6b00415
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    18
    Efficient Photocatalytic Production of Hydrogen Peroxide from Water and Dioxygen with Bismuth Vanadate and a Cobalt(II) Chlorin Complex
    Mase, Kentaro; Yoneda, Masaki; Yamada, Yusuke; Fukuzumi, Shunichi
    ACS Energy Letters (2016), 1 (5), 913-919CODEN: AELCCP; ISSN:2380-8195. (American Chemical Society)
    Efficient photocatalytic prodn. of H2O2 as a promising solar fuel from H2O and O2 in water has been achieved by the combination of bismuth vanadate (BiVO4) as a durable photocatalyst with a narrow band gap for the water oxidn. and a cobalt chlorin complex (CoII(Ch)) as a selective electrocatalyst for the two-electron redn. of O2 in a two-compartment photoelectrochem. cell sepd. by a Nafion membrane under simulated solar light illumination. The concn. of H2O2 produced in the reaction soln. of the cathode cell reached as high as 61 mM, when surface-modified BiVO4 with iron(III) oxide(hydroxide) (FeO(OH)) and CoII(Ch) were employed as a water oxidn. catalyst in the photoanode and as an O2 redn. catalyst in the cathode, resp. The highest solar energy conversion efficiency was detd. to be 6.6% under simulated solar illumination adjusted to 0.05 sun after 1 h of photocatalytic reaction (0.89% under 1 sun illumination). The conversion of chem. energy into elec. energy was conducted using H2O2 produced by photocatalytic reaction by the H2O2 fuel cell, where open-circuit potential and max. power d. were recorded as 0.79 V and 2.0 mW cm-2, resp.
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  19. 19
    Zhang, Y.; Huang, H.; Wang, L.; Zhang, X.; Zhu, Z.; Wang, J.; Yu, W.; Zhang, Y. Cooperation of Congenital and Acquisitus Sulfur Vacancy for Excellent Photocatalytic Hydrogen Peroxide Evolution of CdS Nanorods from Air. Chem. Eng. J. 2023, 454, 140420,  DOI: 10.1016/j.cej.2022.140420
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    19
    Cooperation of congenital and acquisitus sulfur vacancy for excellent photocatalytic hydrogen peroxide evolution of CdS nanorods from air
    Zhang, Yingge; Huang, Hongwei; Wang, Lingchao; Zhang, Xiaolei; Zhu, Zijian; Wang, Jingjing; Yu, Wenying; Zhang, Yihe
    Chemical Engineering Journal (Amsterdam, Netherlands) (2023), 454 (Part_4), 140420CODEN: CMEJAJ; ISSN:1385-8947. (Elsevier B.V.)
    Photocatalysis over semiconductors for producing hydrogen peroxide (H2O2) due to its renewable and sufficient sunlight as driving force has attracted more attention. However, the H2O2 evolution performance that is severely dependent on surface structure of photocatalysts is still inferior. Here we design sulfur vacancies (Sv)-rich CdS nanorods (CdS NRs), and disclose that the congenital Sv and acquisitus Sv in-situ created in the reaction process co-contribute to the efficient photocatalytic H2O2 prodn. The CdS NRs with abundant congenital Sv exhibit higher carrier sepn. efficiency and remarkably stronger O2 adsorption ability. Importantly, we discover that the Sv concn. in all the CdS serial samples increases after the H2O2 evolution reaction compared with that before photocatalytic reaction, and the increase level of acquisitus Sv concn. inversely correlates with congenital Sv concn. Theor. calcns. confirm that the O2 adsorption energy on the surface of CdS NRs with Sv (-0.723 eV) is much lower than that of defect-free CdS (1.293 eV). Optimized by the two types of Sv, CdS NRs-24 h delivers a superior photocatalytic H2O2 prodn. rate of 2974.7μmol g1h-1 under visible light, far exceeding the previously reported sulfide photocatalysts. This work is anticipated to offer new perspectives into designing and understanding of sulfides for photocatalytic H2O2 evolution.
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  20. 20
    Yang, Y.; Wang, Q.; Zhang, X.; Deng, X.; Guan, Y.; Wu, M.; Liu, L.; Wu, J.; Yao, T.; Yin, Y. Photocatalytic Generation of H2O2 over a Z-Scheme Fe2O3@C@1T/2H-MoS2 Heterostructured Catalyst for High-Performance Fenton Reaction. J. Mater. Chem. A 2023, 11 (4), 1991– 2001,  DOI: 10.1039/D2TA08145H
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  21. 21
    Yang, Y.; Yu, H.; Wu, M.; Zhao, T.; Guan, Y.; Yang, D.; Zhu, Y.; Zhang, Y.; Ma, S.; Wu, J.; Liu, L.; Yao, T. Dual H2O2 Production Paths over Chemically Etched MoS2/FeS2 Heterojunction: Maximizing Self-Sufficient Heterogeneous Fenton Reaction Rate under the Neutral Condition. Appl. Catal., B 2023, 325, 122307,  DOI: 10.1016/j.apcatb.2022.122307
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  22. 22
    Li, Z.; Zhou, Z.; Ma, J.; Li, Y.; Peng, W.; Zhang, G.; Zhang, F.; Fan, X. Hierarchical Photocatalyst of In2S3 on Exfoliated MoS2 Nanosheets for Enhanced Visible-Light-Driven Aza-Henry Reaction. Appl. Catal., B 2018, 237, 288– 294,  DOI: 10.1016/j.apcatb.2018.05.087
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    22
    Hierarchical photocatalyst of In2S3 on exfoliated MoS2 nanosheets for enhanced visible-light-driven Aza-Henry reaction
    Li, Zhen; Zhou, Zhou; Ma, Jingwen; Li, Yang; Peng, Wenchao; Zhang, Guoliang; Zhang, Fengbao; Fan, Xiaobin
    Applied Catalysis, B: Environmental (2018), 237 (), 288-294CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
    Exploration of appropriate photocatalysts for visible-light-driven org. synthesis is of great importance. Here we design and construct a two-dimensional hierarchical In2S3/MoS2 composite as an excellent and reusable photocatalyst for Aza-Henry reaction. The dahlia-flower-like In2S3 nanostructures are homogeneously grown on both sides of the two-dimensional MoS2 nanosheets via a hydrothermal reaction. The as-prepd. two-dimensional hierarchical In2S3/MoS2 composite exhibits higher photocatalytic performance than pure In2S3. The hierarchical heterostructure can enhance the light absorption in the visible region, facilitate the sepn. of the photo-induced electron-hole pairs, offer rich active sites for photoredox reactions and promote the generation and migration of the ·O-2 and h+. Profiting from these compositional and structural features, the two-dimensional hierarchical In2S3/MoS2 composite shows remarkably enhanced photocatalytic performance and good stability.
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  23. 23
    Kumar, U.; Das Chakraborty, S.; Sahu, R. K.; Bhattacharya, P.; Mishra, T. Improved Interfacial Charge Transfer on Noble Metal-Free Biomimetic CdS-Based Tertiary Heterostructure @ 2D MoS2-CdS-Cu2O with Enhanced Photocatalytic Water Splitting. Adv. Mater. Interfaces 2022, 9 (2), 2101680,  DOI: 10.1002/admi.202101680
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    Kumar, U.; Sinha, I.; Mishra, T. Synthesis and Photocatalytic Evaluation of 2D MoS2/TiO2 Heterostructure Photocatalyst for Organic Pollutants Degradation. Mater. Today: Proc. 2024, 112, 66– 72,  DOI: 10.1016/j.matpr.2023.08.061
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    Fang, Z.; Huang, X.; Wang, Y.; Feng, W.; Zhang, Y.; Weng, S.; Fu, X.; Liu, P. Dual-Defective Strategy Directing: In Situ Assembly for Effective Interfacial Contacts in MoS2 Cocatalyst/In2S3 Light Harvester Layered Photocatalysts. J. Mater. Chem. A 2016, 4 (36), 13980– 13988,  DOI: 10.1039/C6TA05507A
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    Zhao, H.; Fu, H.; Yang, X.; Xiong, S.; Han, D.; An, X. MoS2/CdS Rod-like Nanocomposites as High-Performance Visible Light Photocatalyst for Water Splitting Photocatalytic Hydrogen Production. Int. J. Hydrogen Energy 2022, 47 (13), 8247– 8260,  DOI: 10.1016/j.ijhydene.2021.12.171
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  27. 27
    Kumar, D. P.; Hong, S.; Reddy, D. A.; Kim, T. K. Ultrathin MoS2 Layers Anchored Exfoliated Reduced Graphene Oxide Nanosheet Hybrid as a Highly Efficient Cocatalyst for CdS Nanorods towards Enhanced Photocatalytic Hydrogen Production. Appl. Catal., B 2017, 212, 7– 14,  DOI: 10.1016/j.apcatb.2017.04.065
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    27
    Ultrathin MoS2 layers anchored exfoliated reduced graphene oxide nanosheet hybrid as a highly efficient cocatalyst for CdS nanorods towards enhanced photocatalytic hydrogen production
    Kumar, D. Praveen; Hong, Sangyeob; Reddy, D. Amaranatha; Kim, Tae Kyu
    Applied Catalysis, B: Environmental (2017), 212 (), 7-14CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
    The development of novel highly efficient noble metal-free co-catalysts for enhanced photocatalytic hydrogen prodn. is of great importance. Herein, we report the synthesis of novel and highly efficient noble metal-free ultra-thin MoS2 (UM) layers on exfoliated reduced graphene oxide (ERGO) nanosheets as a cocatalyst for CdS nanorods (ERGO/UM/CdS). A simple method different from the usual prepn. techniques is used to convert MoS2 to UM layers, graphene oxide (GO) to ERGO nanosheets, based on ultrasonication in the absence of any external reducing agents. The structure, optical properties, chem. states, and dispersion of MoS2 and CdS on ERGO are detd. using diverse anal. techniques. The photocatalytic activity of as-synthesized ERGO/UM/CdS composites is assessed by the splitting of water to generate H2 under simulated solar light irradn. in the presence of lactic acid as a hole (h+) scavenger. The obsd. extraordinary hydrogen prodn. rate of ∼234 mmol h-1 g-1 is due to the synergetic effect of the ultrathin MoS2 layers and ERGO, which leads to the effective sepn. of photogenerated charge carriers and improves the surface shuttling properties for efficient H2 prodn. Furthermore, the obsd. H2 evolution rate is much higher than that for individual noble metal (Pt), ERGO and MoS2-assisted CdS photocatalysts. Moreover, to the best of our knowledge, this is the highest H2 prodn. rate achieved by a RGO and MoS2 based CdS photocatalyst for water splitting under solar light irradn. Considering its low cost and high efficiency, this system has great potential for the development of highly efficient photocatalysts used in various fields.
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  28. 28
    Reddy, D. A.; Park, H.; Ma, R.; Kumar, D. P.; Lim, M.; Kim, T. K. Heterostructured WS2-MoS2 Ultrathin Nanosheets Integrated on CdS Nanorods to Promote Charge Separation and Migration and Improve Solar-Driven Photocatalytic Hydrogen Evolution. ChemSuschem 2017, 10 (7), 1563– 1570,  DOI: 10.1002/cssc.201601799
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    28
    Heterostructured WS2-MoS2 Ultrathin Nanosheets Integrated on CdS Nanorods to Promote Charge Separation and Migration and Improve Solar-Driven Photocatalytic Hydrogen Evolution
    Reddy, D. Amaranatha; Park, Hanbit; Ma, Rory; Kumar, D. Praveen; Lim, Manho; Kim, Tae Kyu
    ChemSusChem (2017), 10 (7), 1563-1570CODEN: CHEMIZ; ISSN:1864-5631. (Wiley-VCH Verlag GmbH & Co. KGaA)
    Solar-driven photocatalytic H evolution is important to bring solar-energy-to-fuel energy-conversion processes to reality. However, there is a lack of highly efficient, stable, and non-precious photocatalysts, and catalysts not designed completely with expensive noble metals have remained elusive, which hampers their large-scale industrial application. Here, for the 1st time, a highly efficient and stable noble-metal-free CdS/WS2-MoS2 nanocomposite was designed through a facile hydrothermal approach. When assessed as a photocatalyst for water splitting, the CdS/WS2-MoS2 nanostructures exhibited remarkable photocatalytic H-evolution performance and impressive durability. An excellent H evolution rate of 209.79 mmol/g-h was achieved under simulated sunlight irradn., which is higher than the values for CdS/MoS2 (123.31 mmol/g-h) and CdS/WS2 nanostructures (169.82 mmol/g-h) and the expensive CdS/Pt benchmark catalyst (34.98 mmol/g-h). The apparent quantum yield reached 51.4% at λ =425 nm in 5 h. The obtained H evolution rate was better than those of several noble-metal-free catalysts reported previously. The obsd. high rate of H evolution and remarkable stability may be a result of the ultrafast sepn. of photogenerated charge carriers and transport between the CdS nanorods and the WS2-MoS2 nanosheets, which thus increases the no. of electrons involved in H prodn. The proposed designed strategy is believed to potentially open a door to the design of advanced noble-metal-free photocatalytic materials for efficient solar-driven H prodn.
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  29. 29
    Zhao, M.; Guo, X.; Meng, Z.; Wang, Y.; Peng, Y.; Ma, Z. Ultrathin MoS2 Nanosheet as Co-Catalyst Coupling on Graphitic g-C3N4 in Suspension System for Boosting Photocatalytic Activity under Visible-Light Irradiation. Colloids Surf., A 2021, 631, 127671,  DOI: 10.1016/j.colsurfa.2021.127671
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    29
    Ultrathin MoS2 nanosheet as co-catalyst coupling on graphitic g-C3N4 in suspension system for boosting photocatalytic activity under visible-light irradiation
    Zhao, Mengxin; Guo, Xin; Meng, Zhe; Wang, Yinghui; Peng, Yuan; Ma, Zongqin
    Colloids and Surfaces, A: Physicochemical and Engineering Aspects (2021), 631 (), 127671CODEN: CPEAEH; ISSN:0927-7757. (Elsevier B.V.)
    In this study, ultrathin molybdenum disulfide (MoS2) nanosheets with thickness of 1.6-8.8 nm were obtained by liq.-phase exfoliating bulk MoS2. Then, they were employed as cocatalyst to build ultrathin MoS2/g-C3N4 heterojunction by self-assembly method. The degrdn. reaction of chlorimuron-Me herbicide and tetracycline antibiotics under visible light was used to evaluate the photocatalytic properties of ultrathin MoS2/g-C3N4. The results showed that ultrathin MoS2/g-C3N4 composite exhibit superior photocatalytic performance. The MoS2/g-C3N4 composite with 15 wt% of ultrathin MoS2 nanosheet exhibited the highest degrdn. efficiency with 90.4% for chlorimuron-Et and 91.7% for tetracycline in 45 min under simulated sunlight, which was 8.8 times and 13.4 times than that of bare g-C3N4, resp. The outstanding photocatalytic activity of ultrathin MoS2/g-C3N4 heterojunction thanks to the unique features of ultrathin MoS2 nanosheet that it harvesting the entire visible light, increasing the contact surface area with the support and shortened the electron and ion migration length, as well as more exposed edge sulfur atoms as redox centers. The radical scavenger expts. showed that ·OH and ·O2- plays a key role in the photocatalytic degrdn. process. This study provides a new idea for the design of high-activity a co-catalyst, i.e., ultrathin MoS2 nanosheet has a significant influence on the photocatalytic performance of MoS2/g-C3N4 heterostructure photocatalyst.
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  30. 30
    Liu, X.; Chen, X.; Xu, L.; Wu, B.; Tu, X.; Luo, X.; Yang, F.; Lin, J. Non-Noble Metal Ultrathin MoS2 Nanosheets Modified Mn0.2Cd0.8S Heterostructures for Efficient Photocatalytic H2 Evolution with Visible Light Irradiation. Int. J. Hydrogen Energy 2020, 45 (51), 26770– 26784,  DOI: 10.1016/j.ijhydene.2020.07.086
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    Shen, S.; Zhao, L.; Zhou, Z.; Guo, L. Enhanced Photocatalytic Hydrogen Evolution over Cu-Doped ZnIn 2S4 under Visible Light Irradiation. J. Phys. Chem. C 2008, 112 (41), 16148– 16155,  DOI: 10.1021/jp804525q
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    31
    Enhanced Photocatalytic Hydrogen Evolution over Cu-Doped ZnIn2S4 under Visible Light Irradiation
    Shen, Shaohua; Zhao, Liang; Zhou, Zhaohui; Guo, Liejin
    Journal of Physical Chemistry C (2008), 112 (41), 16148-16155CODEN: JPCCCK; ISSN:1932-7447. (American Chemical Society)
    A series of Cu-doped ZnIn2S4 photocatalysts has been synthesized by a facile hydrothermal method, with the copper concn. varying from 0 wt.% to 2.0 wt.%. The phys. and photophys. properties of these Cu-doped ZnIn2S4 photocatalysts were characterized by x-ray diffraction (XRD), photoluminescence spectroscopy (PL), SEM, and UV-visible diffuse reflectance spectroscopy (UV-vis). The diffuse reflectance and photoluminescence spectra of Cu-doped ZnIn2S4 shifted monotonically to longer wavelengths as the copper concn. increased from 0 wt.% to 2.0 wt.%, indicating that the optical properties of these photocatalysts greatly depended on the amt. of Cu doped. Meanwhile, the layered structure of ZnIn2S4 would be destructed gradually by Cu doping. The photoactivity of ZnIn2S4 was enhanced when Cu2+ was doped into the crystal structure. The highest photocatalytic activity was obsd. on Cu (0.5 wt.%)-doped ZnIn2S4, with the rate of hydrogen evolution to be 151.5 μmol/h under visible light irradn. (λ > 430 nm). On the basis of the calcd. energy band positions and optical properties, the effect of copper as a dopant on the photocatalytic activity of Cu-ZnIn2S4 was studied.
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  32. 32
    Zhang, B.; Shi, H.; Hu, X.; Wang, Y.; Liu, E.; Fan, J. A Novel S-Scheme MoS2/CdIn2S4 Flower-like Heterojunctions with Enhanced Photocatalytic Degradation and H2 Evolution Activity. J. Phys. D: Appl. Phys. 2020, 53 (20), 205101,  DOI: 10.1088/1361-6463/ab7563
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    Chen, W.; He, Z.-C.; Huang, G.-B.; Wu, C.-L.; Chen, W.-F.; Liu, X.-H. Direct Z-Scheme 2D/2D MnIn2S4/g-C3N4 Architectures with Highly Efficient Photocatalytic Activities towards Treatment of Pharmaceutical Wastewater and Hydrogen Evolution. Chem. Eng. J. 2019, 359, 244– 253,  DOI: 10.1016/j.cej.2018.11.141
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    33
    Direct Z-scheme 2D/2D MnIn2S4/g-C3N4 architectures with highly efficient photocatalytic activities towards treatment of pharmaceutical wastewater and hydrogen evolution
    Chen, Wei; He, Zhi-Cai; Huang, Guo-Bo; Wu, Cheng-Lin; Chen, Wu-Fei; Liu, Xiao-Heng
    Chemical Engineering Journal (Amsterdam, Netherlands) (2019), 359 (), 244-253CODEN: CMEJAJ; ISSN:1385-8947. (Elsevier B.V.)
    Semiconductor photocatalysis has been regarded as an environmentally friendly technol. in wastewater treatment and energy prodn. Here, a series of direct Z-scheme MnIn2S4/g-C3N4 (MnISCN) photocatalysts without electron mediators were fabricated by a simple hydrothermal route on the basis of in-situ loading of MnIn2S4 (MnIS) nanoflakes on the surface of g-C3N4 (CN) nanosheets. Photocatalytic performances evaluated under visible light irradn. revealed these Z-scheme heterostructured photocatalysts exhibited higher photocatalytic activities than single-component samples. The effect of wt. ratio between MnIn2S4 nanoflakes and mesoporous CN nanosheets on photocatalytic activity towards treatment of pharmaceutical wastewater was optimized to achieve highly efficient photocatalytic activities for both degrdn. of pharmaceutical wastewater and hydrogen generation compared with alone MnIS nanoflakes and isolated mesoporous CN nanosheets. The significant enhancement in photocatalytic activity could be primarily ascribed to the construction of Z-scheme MnISCN architectures, which effectively accelerated the transfer and sepn. of photogenerated charge carriers via tight interface contacts built among these two components. The recycling expts. for pharmaceutical wastewater treatment revealed the excellent stability of MnISCN nanocomposites. The advantages of highly efficient photocatalytic activity and excellent stability endowed a promising potential for MnISCN nanocomposites to apply in photocatalytic fields.
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    Cu7S4/MnIn2S4 heterojunction for efficient photocatalytic hydrogen generation
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    Journal of Alloys and Compounds (2021), 884 (), 161035CODEN: JALCEU; ISSN:0925-8388. (Elsevier B.V.)
    Heterojunction has been considered to be one of the most effective methods for efficient hydrogen evolution reaction by photocatalytic water splitting. In this work, nanostructured Cu7S4/MnIn2S4 heterojunction was successfully fabricated via a simple two-step method, which was much simpler than most heterojunction synthesis. Firstly, Cu7S4 nanoparticles were synthesized by oil bath stirring, and then the Cu7S4/MnIn2S4heterojunctions were synthesized by the hydrothermal method. The prepd. Cu7S4/MnIn2S4 composite exhibited significantly improved hydrogen evolution activity with a rate of 13.81μmol h-1 (10 mg catalyst), which was approx. 18 times higher than that of pristine MnIn2S4. This result could be attributed to the construction of p-n heterojunction for promoting the sepn. of photogenerated charge carriers and inhibiting their recombination. Possible electron transfer mechanism was proposed by the related characterization. This work will inspire the simple fabrication of nano-heterojunctions in the future.
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    Applied Catalysis, B: Environmental (2021), 299 (), 120664CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
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    Two-dimensional (2D) nanosheets materials have attracted extensive attention because of their promising practical application and theor. values. In order to enhance the photocatalytic activity of bulk C3N4, we designed a 2D fabrication in which g-C3N4 nanosheets was in the middle of MoS2/graphene layered structure. Here, we report an effective strategy to synthesize ternary g-C3N4/MoS2/graphene nanocomposite photocatalyst via an in-situ adsorption method, which exhibits superior photocatalytic activity owing to enhanced charge carrier sepn. via well-contacted interface and fast charge transfer pathway. This work indicates a new insight into the design of such 2D heterostructure and a promising cocatalyst strategy for designing a more efficient g-C3N4-based semiconductor photocatalyst toward degrdn. of org. pollutants.
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    Zhang, Z. Y.; Tian, H.; Jiao, H.; Wang, X.; Bian, L.; Liu, Y.; Khaorapapong, N.; Yamauchi, Y.; Wang, Z. L. SiO2 Assisted Cu0-Cu+-NH2 Composite Interfaces for Efficient CO2 Electroreduction to C2+ Products. J. Mater. Chem. A 2024, 12 (2), 1218– 1232,  DOI: 10.1039/D3TA05652J
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    Angewandte Chemie, International Edition (2022), 61 (26), e202203519CODEN: ACIEF5; ISSN:1433-7851. (Wiley-VCH Verlag GmbH & Co. KGaA)
    Inferior contact interface and low charge transfer efficiency seriously restrict the performance of heterojunctions. Herein, chem. bonded α-Fe2O3/Bi4MO8Cl (M=Nb, Ta) dot-on-plate Z-scheme junctions with strong internal elec. field are crafted by an in situ growth route. Exptl. and theor. results demonstrate that the internal elec. field provides a powerful driving force for vectorial migration of photocharges between Bi4MO8Cl and α-Fe2O3, and the interfacial Fe-O bond not only serves as an at.-level charge flow highway but also lowers the charge transfer energy barrier, thereby accelerating Z-scheme charge transfer and realizing effective spatial charge sepn. Impressively, α-Fe2O3/Bi4MO8Cl manifests a significantly improved photocatalytic activity for selective oxidn. of arom. alcs. into aldehydes (Con. ≥92%, Sel. ≥96%), with a performance improvement of one to two orders of magnitude. This work presents at.-level insight into interfacial charge flow steering.
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    Sulfur is a promising cathode material for lithium-sulfur batteries because of its high theor. capacity (1,675 mA h g-1); however, its low elec. cond. and the instability of sulfur-based electrodes limit its practical application. Here we report a facile in situ method for prepg. three-dimensional porous graphitic carbon composites contg. sulfur nanoparticles (3D S@PGC). With this strategy, the sulfur content of the composites can be tuned to a high level (up to 90 wt%). Because of the high sulfur content, the nanoscale distribution of the sulfur particles, and the covalent bonding between the sulfur and the PGC, the developed 3D S@PGC cathodes exhibit excellent performance, with a high sulfur utilization, high specific capacity (1,382, 1,242 and 1,115 mA h g-1 at 0.5, 1 and 2 C, resp.), long cycling life (small capacity decay of 0.039% per cycle over 1,000 cycles at 2 C) and excellent rate capability at a high charge/discharge current.
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    Nature Communications (2023), 14 (1), 6891CODEN: NCAOBW; ISSN:2041-1723. (Nature Portfolio)
    Developing efficient artificial photocatalysts for the biomimetic photocatalytic prodn. of mol. materials, including medicines and clean energy carriers, remains a fundamentally and technol. essential challenge. Hydrogen peroxide is widely used in chem. synthesis, medical disinfection, and clean energy. However, the current industrial prodn., predominantly by anthraquinone oxidn., suffers from hefty energy penalties and toxic byproducts. Herein, we report the efficient photocatalytic prodn. of hydrogen peroxide by protonation-induced dispersible porous polymers with good charge-carrier transport properties. Significant photocatalytic hydrogen peroxide generation occurs under ambient conditions at an unprecedented rate of 23.7 mmol g-1 h-1 and an apparent quantum efficiency of 11.3% at 450 nm. Combined simulations and spectroscopies indicate that sub-picosecond ultrafast electron "localization" from both free carriers and exciton states at the catalytic reaction centers underlie the remarkable photocatalytic performance of the dispersible porous polymers.
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    Proper design and fabrication of multifunctional visible-light-induced photocatalysts with high catalytic efficiency is still a huge challenge for the value-added chems. prodn. and environmental remediation. A novel 3D flower-like hierarchical CoWO4@Bi2WO6 Z-scheme hybrid was successfully fabricated via anchoring CoWO4 nanoparticles on the 2D nanopetals of Bi2WO6 microflower obtained by solvothermal assistant self-assembly. The multifunctional composite could markedly improve photocatalytic H2O2 prodn. via two-channel route (oxygen redn. and water oxidn. reaction) without using sacrificial agent. Interestingly, 3D CoWO4@Bi2WO6 also displayed a remarkable degrdn. performance on single (enrofloxacin (ENR), lomefloxacin (LOM) or ciprofloxacin hydrochloride (CIP)) and ternary mixed antibiotics (ENR + LOM + CIP) under visible light irradn. The outstanding photocatalytic activity was primarily attributed to the 3D hierarchical CoWO4@Bi2WO6 micro-flowers architecture for boosting visible light harvesting, matching energy band gaps, more exposed active sites, formation of Z-scheme based charge-transfer dynamics in a p-n heterostructure, as well as strong oxidn. and redn. capability of photoexcited h+ and e-. Therefore, it was believed that the novel multifunctional CoWO4@Bi2WO6 photocatalyst exhibited a potential application in prodn. of H2O2 and degrdn. of org. contaminants, which were more significant for the following purifn. in industrial prodn. and environmental governance.
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  • Abstract

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    Scheme 1

    Scheme 1. Schematic Diagram Illustrating the Synthesis Process of As-Designed MS/MnIS-x Heterostructure Photocatalysts
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    Figure 1

    Figure 1. XRD patterns of 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts.

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    Figure 2

    Figure 2. (a) Solid-state UV-DRS absorbance spectra of 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts. (b,c) Tauc plot of 2D MoS2 and MnIn2S4. Mott–Schottky plot of (d) MnIn2S4 and (e) 2D MoS2.

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    Figure 3

    Figure 3. (a,b) SEM images of pristine MnIn2S4. (c) SEM images of MS/MnIS40 heterostructure photocatalysts. (d) SEM image with corresponding elemental maps (Mo, Mn, In, S) of MS/MnIS40 heterostructure photocatalysts.

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    Figure 4

    Figure 4. TEM, HR-TEM, and IFFT images of (a–c) pure MnIn2S4, (d,e) 2D MoS2, (f–h) MS/MnIS40 heterostructure. (i) STEM elemental mapping of MS/MnIS40 heterostructure photocatalysts.

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    Figure 5

    Figure 5. XPS spectra of 2D MoS2, MnIn2S4, and MS/MnIS40: (a) Mn 2p, (b) In 3d, (c) Mo 3d, and (d) S 2p.

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    Figure 6

    Figure 6. (a) PL spectra of MnIn2S4 and MS/MnIS-x heterostructure photocatalysts; (b,c) Nyquist plot and photocurrent studies of 2D MoS2 and MS/MnIS-x heterostructure photocatalysts.

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    Figure 7

    Figure 7. Contact angle results: (a) 2D MoS2, (b) MS/MnIS10, (c) MS/MnIS20, (d) MS/MnIS40, (e) MS/MnIS60, and (f) MS/MnIS80.

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    Figure 8

    Figure 8. (a) The time-dependent plot of photocatalytic H2O2 production for various photocatalysts prepared in this study. (b) Kinetics plot of photocatalytic H2O2 decomposition on different photocatalysts. (c) H2O2 production at different pH levels using the optimal photocatalyst, MS/MnIS40. (d) H2O2 production under control conditions with MS/MnIS40. (e) H2O2 production with MS/MnIS40 in scavenger experiments. (f) Cycling experiments showing H2O2 production at different time intervals using MS/MnIS40. (g) XRD patterns of fresh and recycled MS/MnIS40 photocatalysts. (h) Comparison of photocatalytic H2O2 production with recently reported photocatalysts.

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    Figure 9

    Figure 9. Possible mechanism of the photocatalytic H2O2 generation on 2D MoS2/MnIn2S4 photocatalyst.

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      Design of metal-organic framework catalysts for photocatalytic hydrogen peroxide production
      Kondo, Yoshifumi; Kuwahara, Yasutaka; Mori, Kohsuke; Yamashita, Hiromi
      Chem (2022), 8 (11), 2924-2938CODEN: CHEMVE; ISSN:2451-9294. (Cell Press)
      A review. Hydrogen peroxide (H2O2) has received much attention as an environmentally friendly oxidant and a renewable energy carrier. This perspective examines metal-org. frameworks (MOFs) as highly effective materials for promoting photocatalytic H2O2 prodn. The design flexibility of MOFs enables not only the development of highly efficient photocatalysts but also the construction of rational reaction systems for photocatalytic H2O2 prodn. The goal of the present perspective is to summarize recent advances in the application of MOFs to this purpose and to provide detailed insights into the development of photocatalysts intended for H2O2 prodn.
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      Wang, L.; Zhang, J.; Zhang, Y.; Yu, H.; Qu, Y.; Yu, J. Inorganic Metal-Oxide Photocatalyst for H2O2 Production. Small 2022, 18 (8), 2104561,  DOI: 10.1002/smll.202104561
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      Inorganic Metal-Oxide Photocatalyst for H2O2 Production
      Wang, Linxi; Zhang, Jianjun; Zhang, Yong; Yu, Huogen; Qu, Yinhu; Yu, Jiaguo
      Small (2022), 18 (8), 2104561CODEN: SMALBC; ISSN:1613-6810. (Wiley-VCH Verlag GmbH & Co. KGaA)
      A review. Hydrogen peroxide (H2O2) is a mild but versatile oxidizing agent with extensive applications in bleaching, wastewater purifn., medical treatment, and chem. synthesis. The state-of-art H2O2 prodn. via anthraquinone oxidn. is hardly considered a cost-efficient and environment-friendly process because it requires high energy input and generates hazardous org. wastes. Photocatalytic H2O2 prodn. is a green, sustainable, and inexpensive process which only needs water and gaseous dioxygen as the raw materials and sunlight as the power source. Inorg. metal oxide semiconductors are good candidates for photocatalytic H2O2 prodn. due to their abundance in nature, biocompatibility, exceptional stability, and low cost. Progress has been made to enhance the photocatalytic activity toward H2O2 prodn., however, H2O2 photosynthesis is still in the lab. research phase since the productivity is far from satisfaction. To inspire innovative ideas for boosting the H2O2 yield in photocatalysis, the most well-studied metal oxide photocatalysts are selected and the modification strategies to improve their activity are listed. The mechanisms for H2O2 prodn. over modified photocatalysts are discussed to highlight the facilitating role of the modification methods. Besides, methods for the quantification of H2O2 and assocd. radical intermediates are provided to guide future studies in this field.
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      Isaka, Y.; Oyama, K.; Yamada, Y.; Suenobu, T.; Fukuzumi, S. Photocatalytic Production of Hydrogen Peroxide from Water and Dioxygen Using Cyano-Bridged Polynuclear Transition Metal Complexes as Water Oxidation Catalysts. Catal. Sci. Technol. 2016, 6 (3), 681– 684,  DOI: 10.1039/C5CY01845E
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      Photocatalytic production of hydrogen peroxide from water and dioxygen using cyano-bridged polynuclear transition metal complexes as water oxidation catalysts
      Isaka, Yusuke; Oyama, Kohei; Yamada, Yusuke; Suenobu, Tomoyoshi; Fukuzumi, Shunichi
      Catalysis Science & Technology (2016), 6 (3), 681-684CODEN: CSTAGD; ISSN:2044-4753. (Royal Society of Chemistry)
      Hydrogen peroxide was produced efficiently from water and dioxygen using [RuII(Me2phen)3]2+ (Me2phen = 4,7-dimethyl-1,10-phenanthroline) as a photocatalyst and cyano-bridged polynuclear transition metal complexes composed of Fe and Co as water oxidn. catalysts in the presence of Sc3+ in water under visible light irradn.
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      Song, H.; Wei, L.; Chen, C.; Wen, C.; Han, F. Photocatalytic Production of H2O2 and Its in Situ Utilization over Atomic-Scale Au Modified MoS2 Nanosheets. J. Catal. 2019, 376, 198– 208,  DOI: 10.1016/j.jcat.2019.06.015
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      Photocatalytic production of H2O2 and its in situ utilization over atomic-scale Au modified MoS2 nanosheets
      Song, Haiyan; Wei, Lishan; Chen, Chunxia; Wen, Congcong; Han, Fuqin
      Journal of Catalysis (2019), 376 (), 198-208CODEN: JCTLA5; ISSN:0021-9517. (Elsevier Inc.)
      Au modified MoS2 nanosheets (Au@MoS2) for photocatalytic prodn. of H2O2 were prepd. via a simple pathway including the deposition-redn. and immobilization process by using a low dosage of an Au source. Nanoparticles smaller than 1 nm and single atoms, as two major forms of Au, were found to be widely dispersed on the surface of MoS2 and captured by its lattices. Au modification brought out the low recombination rate of e--h+ pairs, long lifetime of electrons, and more neg. flat band potential for MoS2. Au@MoS2 achieved efficient photocatalytic prodn. of H2O2 from H2O and air in the absence of pure O2 and org. electron donors. An optimal catalyst loading 0.50 wt% of Au enhanced the H2O2 productivity by about 2.5 times from bare MoS2. A significant finding was that higher pH was beneficial to H2O2 synthesis, and the H2O2 productivity at pH 9 was further enhanced 7.4 times from that at pH 2. Au@MoS2 was recycled more than five times without inactivation and obtained considerable 791.72 μM of H2O2 under real sunlight irradn. for 6 h, exhibiting application potential. Mn2+ as the active center for Fenton-like reactions was doped in MoS2 nanosheets before Au0 modification in order to use the photogenerated H2O2 in situ. Accordingly, a novel in situ Fenton process was proposed, and obtained significant degrdn. efficiencies for rhodamine B and methylene blue dyes, depending on the H2O2 productivity. Another important finding was that Mn2+ further increased H2O2 productivity by 2 times based on Au@MoS2.
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    17. 17
      Das, S.; Acharya, L.; Biswal, L.; Parida, K. Augmented Photocatalysis Induced by 1T-MoS2 Bridged 2D/2D MgIn2S4@1T/2H-MoS2 Z-Scheme Heterojunction: Mechanistic Insights into H2O2 and H2 Evolution. Nanoscale Adv. 2024, 6 (3), 934– 946,  DOI: 10.1039/D3NA00912B
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      Mase, K.; Yoneda, M.; Yamada, Y.; Fukuzumi, S. Efficient Photocatalytic Production of Hydrogen Peroxide from Water and Dioxygen with Bismuth Vanadate and a Cobalt(II) Chlorin Complex. ACS Energy Lett. 2016, 1 (5), 913– 919,  DOI: 10.1021/acsenergylett.6b00415
      18
      Efficient Photocatalytic Production of Hydrogen Peroxide from Water and Dioxygen with Bismuth Vanadate and a Cobalt(II) Chlorin Complex
      Mase, Kentaro; Yoneda, Masaki; Yamada, Yusuke; Fukuzumi, Shunichi
      ACS Energy Letters (2016), 1 (5), 913-919CODEN: AELCCP; ISSN:2380-8195. (American Chemical Society)
      Efficient photocatalytic prodn. of H2O2 as a promising solar fuel from H2O and O2 in water has been achieved by the combination of bismuth vanadate (BiVO4) as a durable photocatalyst with a narrow band gap for the water oxidn. and a cobalt chlorin complex (CoII(Ch)) as a selective electrocatalyst for the two-electron redn. of O2 in a two-compartment photoelectrochem. cell sepd. by a Nafion membrane under simulated solar light illumination. The concn. of H2O2 produced in the reaction soln. of the cathode cell reached as high as 61 mM, when surface-modified BiVO4 with iron(III) oxide(hydroxide) (FeO(OH)) and CoII(Ch) were employed as a water oxidn. catalyst in the photoanode and as an O2 redn. catalyst in the cathode, resp. The highest solar energy conversion efficiency was detd. to be 6.6% under simulated solar illumination adjusted to 0.05 sun after 1 h of photocatalytic reaction (0.89% under 1 sun illumination). The conversion of chem. energy into elec. energy was conducted using H2O2 produced by photocatalytic reaction by the H2O2 fuel cell, where open-circuit potential and max. power d. were recorded as 0.79 V and 2.0 mW cm-2, resp.
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    19. 19
      Zhang, Y.; Huang, H.; Wang, L.; Zhang, X.; Zhu, Z.; Wang, J.; Yu, W.; Zhang, Y. Cooperation of Congenital and Acquisitus Sulfur Vacancy for Excellent Photocatalytic Hydrogen Peroxide Evolution of CdS Nanorods from Air. Chem. Eng. J. 2023, 454, 140420,  DOI: 10.1016/j.cej.2022.140420
      19
      Cooperation of congenital and acquisitus sulfur vacancy for excellent photocatalytic hydrogen peroxide evolution of CdS nanorods from air
      Zhang, Yingge; Huang, Hongwei; Wang, Lingchao; Zhang, Xiaolei; Zhu, Zijian; Wang, Jingjing; Yu, Wenying; Zhang, Yihe
      Chemical Engineering Journal (Amsterdam, Netherlands) (2023), 454 (Part_4), 140420CODEN: CMEJAJ; ISSN:1385-8947. (Elsevier B.V.)
      Photocatalysis over semiconductors for producing hydrogen peroxide (H2O2) due to its renewable and sufficient sunlight as driving force has attracted more attention. However, the H2O2 evolution performance that is severely dependent on surface structure of photocatalysts is still inferior. Here we design sulfur vacancies (Sv)-rich CdS nanorods (CdS NRs), and disclose that the congenital Sv and acquisitus Sv in-situ created in the reaction process co-contribute to the efficient photocatalytic H2O2 prodn. The CdS NRs with abundant congenital Sv exhibit higher carrier sepn. efficiency and remarkably stronger O2 adsorption ability. Importantly, we discover that the Sv concn. in all the CdS serial samples increases after the H2O2 evolution reaction compared with that before photocatalytic reaction, and the increase level of acquisitus Sv concn. inversely correlates with congenital Sv concn. Theor. calcns. confirm that the O2 adsorption energy on the surface of CdS NRs with Sv (-0.723 eV) is much lower than that of defect-free CdS (1.293 eV). Optimized by the two types of Sv, CdS NRs-24 h delivers a superior photocatalytic H2O2 prodn. rate of 2974.7μmol g1h-1 under visible light, far exceeding the previously reported sulfide photocatalysts. This work is anticipated to offer new perspectives into designing and understanding of sulfides for photocatalytic H2O2 evolution.
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    20. 20
      Yang, Y.; Wang, Q.; Zhang, X.; Deng, X.; Guan, Y.; Wu, M.; Liu, L.; Wu, J.; Yao, T.; Yin, Y. Photocatalytic Generation of H2O2 over a Z-Scheme Fe2O3@C@1T/2H-MoS2 Heterostructured Catalyst for High-Performance Fenton Reaction. J. Mater. Chem. A 2023, 11 (4), 1991– 2001,  DOI: 10.1039/D2TA08145H
      There is no corresponding record for this reference.
    21. 21
      Yang, Y.; Yu, H.; Wu, M.; Zhao, T.; Guan, Y.; Yang, D.; Zhu, Y.; Zhang, Y.; Ma, S.; Wu, J.; Liu, L.; Yao, T. Dual H2O2 Production Paths over Chemically Etched MoS2/FeS2 Heterojunction: Maximizing Self-Sufficient Heterogeneous Fenton Reaction Rate under the Neutral Condition. Appl. Catal., B 2023, 325, 122307,  DOI: 10.1016/j.apcatb.2022.122307
      There is no corresponding record for this reference.
    22. 22
      Li, Z.; Zhou, Z.; Ma, J.; Li, Y.; Peng, W.; Zhang, G.; Zhang, F.; Fan, X. Hierarchical Photocatalyst of In2S3 on Exfoliated MoS2 Nanosheets for Enhanced Visible-Light-Driven Aza-Henry Reaction. Appl. Catal., B 2018, 237, 288– 294,  DOI: 10.1016/j.apcatb.2018.05.087
      22
      Hierarchical photocatalyst of In2S3 on exfoliated MoS2 nanosheets for enhanced visible-light-driven Aza-Henry reaction
      Li, Zhen; Zhou, Zhou; Ma, Jingwen; Li, Yang; Peng, Wenchao; Zhang, Guoliang; Zhang, Fengbao; Fan, Xiaobin
      Applied Catalysis, B: Environmental (2018), 237 (), 288-294CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
      Exploration of appropriate photocatalysts for visible-light-driven org. synthesis is of great importance. Here we design and construct a two-dimensional hierarchical In2S3/MoS2 composite as an excellent and reusable photocatalyst for Aza-Henry reaction. The dahlia-flower-like In2S3 nanostructures are homogeneously grown on both sides of the two-dimensional MoS2 nanosheets via a hydrothermal reaction. The as-prepd. two-dimensional hierarchical In2S3/MoS2 composite exhibits higher photocatalytic performance than pure In2S3. The hierarchical heterostructure can enhance the light absorption in the visible region, facilitate the sepn. of the photo-induced electron-hole pairs, offer rich active sites for photoredox reactions and promote the generation and migration of the ·O-2 and h+. Profiting from these compositional and structural features, the two-dimensional hierarchical In2S3/MoS2 composite shows remarkably enhanced photocatalytic performance and good stability.
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    23. 23
      Kumar, U.; Das Chakraborty, S.; Sahu, R. K.; Bhattacharya, P.; Mishra, T. Improved Interfacial Charge Transfer on Noble Metal-Free Biomimetic CdS-Based Tertiary Heterostructure @ 2D MoS2-CdS-Cu2O with Enhanced Photocatalytic Water Splitting. Adv. Mater. Interfaces 2022, 9 (2), 2101680,  DOI: 10.1002/admi.202101680
      There is no corresponding record for this reference.
    24. 24
      Kumar, U.; Sinha, I.; Mishra, T. Synthesis and Photocatalytic Evaluation of 2D MoS2/TiO2 Heterostructure Photocatalyst for Organic Pollutants Degradation. Mater. Today: Proc. 2024, 112, 66– 72,  DOI: 10.1016/j.matpr.2023.08.061
      There is no corresponding record for this reference.
    25. 25
      Fang, Z.; Huang, X.; Wang, Y.; Feng, W.; Zhang, Y.; Weng, S.; Fu, X.; Liu, P. Dual-Defective Strategy Directing: In Situ Assembly for Effective Interfacial Contacts in MoS2 Cocatalyst/In2S3 Light Harvester Layered Photocatalysts. J. Mater. Chem. A 2016, 4 (36), 13980– 13988,  DOI: 10.1039/C6TA05507A
      There is no corresponding record for this reference.
    26. 26
      Zhao, H.; Fu, H.; Yang, X.; Xiong, S.; Han, D.; An, X. MoS2/CdS Rod-like Nanocomposites as High-Performance Visible Light Photocatalyst for Water Splitting Photocatalytic Hydrogen Production. Int. J. Hydrogen Energy 2022, 47 (13), 8247– 8260,  DOI: 10.1016/j.ijhydene.2021.12.171
      There is no corresponding record for this reference.
    27. 27
      Kumar, D. P.; Hong, S.; Reddy, D. A.; Kim, T. K. Ultrathin MoS2 Layers Anchored Exfoliated Reduced Graphene Oxide Nanosheet Hybrid as a Highly Efficient Cocatalyst for CdS Nanorods towards Enhanced Photocatalytic Hydrogen Production. Appl. Catal., B 2017, 212, 7– 14,  DOI: 10.1016/j.apcatb.2017.04.065
      27
      Ultrathin MoS2 layers anchored exfoliated reduced graphene oxide nanosheet hybrid as a highly efficient cocatalyst for CdS nanorods towards enhanced photocatalytic hydrogen production
      Kumar, D. Praveen; Hong, Sangyeob; Reddy, D. Amaranatha; Kim, Tae Kyu
      Applied Catalysis, B: Environmental (2017), 212 (), 7-14CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
      The development of novel highly efficient noble metal-free co-catalysts for enhanced photocatalytic hydrogen prodn. is of great importance. Herein, we report the synthesis of novel and highly efficient noble metal-free ultra-thin MoS2 (UM) layers on exfoliated reduced graphene oxide (ERGO) nanosheets as a cocatalyst for CdS nanorods (ERGO/UM/CdS). A simple method different from the usual prepn. techniques is used to convert MoS2 to UM layers, graphene oxide (GO) to ERGO nanosheets, based on ultrasonication in the absence of any external reducing agents. The structure, optical properties, chem. states, and dispersion of MoS2 and CdS on ERGO are detd. using diverse anal. techniques. The photocatalytic activity of as-synthesized ERGO/UM/CdS composites is assessed by the splitting of water to generate H2 under simulated solar light irradn. in the presence of lactic acid as a hole (h+) scavenger. The obsd. extraordinary hydrogen prodn. rate of ∼234 mmol h-1 g-1 is due to the synergetic effect of the ultrathin MoS2 layers and ERGO, which leads to the effective sepn. of photogenerated charge carriers and improves the surface shuttling properties for efficient H2 prodn. Furthermore, the obsd. H2 evolution rate is much higher than that for individual noble metal (Pt), ERGO and MoS2-assisted CdS photocatalysts. Moreover, to the best of our knowledge, this is the highest H2 prodn. rate achieved by a RGO and MoS2 based CdS photocatalyst for water splitting under solar light irradn. Considering its low cost and high efficiency, this system has great potential for the development of highly efficient photocatalysts used in various fields.
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    28. 28
      Reddy, D. A.; Park, H.; Ma, R.; Kumar, D. P.; Lim, M.; Kim, T. K. Heterostructured WS2-MoS2 Ultrathin Nanosheets Integrated on CdS Nanorods to Promote Charge Separation and Migration and Improve Solar-Driven Photocatalytic Hydrogen Evolution. ChemSuschem 2017, 10 (7), 1563– 1570,  DOI: 10.1002/cssc.201601799
      28
      Heterostructured WS2-MoS2 Ultrathin Nanosheets Integrated on CdS Nanorods to Promote Charge Separation and Migration and Improve Solar-Driven Photocatalytic Hydrogen Evolution
      Reddy, D. Amaranatha; Park, Hanbit; Ma, Rory; Kumar, D. Praveen; Lim, Manho; Kim, Tae Kyu
      ChemSusChem (2017), 10 (7), 1563-1570CODEN: CHEMIZ; ISSN:1864-5631. (Wiley-VCH Verlag GmbH & Co. KGaA)
      Solar-driven photocatalytic H evolution is important to bring solar-energy-to-fuel energy-conversion processes to reality. However, there is a lack of highly efficient, stable, and non-precious photocatalysts, and catalysts not designed completely with expensive noble metals have remained elusive, which hampers their large-scale industrial application. Here, for the 1st time, a highly efficient and stable noble-metal-free CdS/WS2-MoS2 nanocomposite was designed through a facile hydrothermal approach. When assessed as a photocatalyst for water splitting, the CdS/WS2-MoS2 nanostructures exhibited remarkable photocatalytic H-evolution performance and impressive durability. An excellent H evolution rate of 209.79 mmol/g-h was achieved under simulated sunlight irradn., which is higher than the values for CdS/MoS2 (123.31 mmol/g-h) and CdS/WS2 nanostructures (169.82 mmol/g-h) and the expensive CdS/Pt benchmark catalyst (34.98 mmol/g-h). The apparent quantum yield reached 51.4% at λ =425 nm in 5 h. The obtained H evolution rate was better than those of several noble-metal-free catalysts reported previously. The obsd. high rate of H evolution and remarkable stability may be a result of the ultrafast sepn. of photogenerated charge carriers and transport between the CdS nanorods and the WS2-MoS2 nanosheets, which thus increases the no. of electrons involved in H prodn. The proposed designed strategy is believed to potentially open a door to the design of advanced noble-metal-free photocatalytic materials for efficient solar-driven H prodn.
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    29. 29
      Zhao, M.; Guo, X.; Meng, Z.; Wang, Y.; Peng, Y.; Ma, Z. Ultrathin MoS2 Nanosheet as Co-Catalyst Coupling on Graphitic g-C3N4 in Suspension System for Boosting Photocatalytic Activity under Visible-Light Irradiation. Colloids Surf., A 2021, 631, 127671,  DOI: 10.1016/j.colsurfa.2021.127671
      29
      Ultrathin MoS2 nanosheet as co-catalyst coupling on graphitic g-C3N4 in suspension system for boosting photocatalytic activity under visible-light irradiation
      Zhao, Mengxin; Guo, Xin; Meng, Zhe; Wang, Yinghui; Peng, Yuan; Ma, Zongqin
      Colloids and Surfaces, A: Physicochemical and Engineering Aspects (2021), 631 (), 127671CODEN: CPEAEH; ISSN:0927-7757. (Elsevier B.V.)
      In this study, ultrathin molybdenum disulfide (MoS2) nanosheets with thickness of 1.6-8.8 nm were obtained by liq.-phase exfoliating bulk MoS2. Then, they were employed as cocatalyst to build ultrathin MoS2/g-C3N4 heterojunction by self-assembly method. The degrdn. reaction of chlorimuron-Me herbicide and tetracycline antibiotics under visible light was used to evaluate the photocatalytic properties of ultrathin MoS2/g-C3N4. The results showed that ultrathin MoS2/g-C3N4 composite exhibit superior photocatalytic performance. The MoS2/g-C3N4 composite with 15 wt% of ultrathin MoS2 nanosheet exhibited the highest degrdn. efficiency with 90.4% for chlorimuron-Et and 91.7% for tetracycline in 45 min under simulated sunlight, which was 8.8 times and 13.4 times than that of bare g-C3N4, resp. The outstanding photocatalytic activity of ultrathin MoS2/g-C3N4 heterojunction thanks to the unique features of ultrathin MoS2 nanosheet that it harvesting the entire visible light, increasing the contact surface area with the support and shortened the electron and ion migration length, as well as more exposed edge sulfur atoms as redox centers. The radical scavenger expts. showed that ·OH and ·O2- plays a key role in the photocatalytic degrdn. process. This study provides a new idea for the design of high-activity a co-catalyst, i.e., ultrathin MoS2 nanosheet has a significant influence on the photocatalytic performance of MoS2/g-C3N4 heterostructure photocatalyst.
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    30. 30
      Liu, X.; Chen, X.; Xu, L.; Wu, B.; Tu, X.; Luo, X.; Yang, F.; Lin, J. Non-Noble Metal Ultrathin MoS2 Nanosheets Modified Mn0.2Cd0.8S Heterostructures for Efficient Photocatalytic H2 Evolution with Visible Light Irradiation. Int. J. Hydrogen Energy 2020, 45 (51), 26770– 26784,  DOI: 10.1016/j.ijhydene.2020.07.086
      There is no corresponding record for this reference.
    31. 31
      Shen, S.; Zhao, L.; Zhou, Z.; Guo, L. Enhanced Photocatalytic Hydrogen Evolution over Cu-Doped ZnIn 2S4 under Visible Light Irradiation. J. Phys. Chem. C 2008, 112 (41), 16148– 16155,  DOI: 10.1021/jp804525q
      31
      Enhanced Photocatalytic Hydrogen Evolution over Cu-Doped ZnIn2S4 under Visible Light Irradiation
      Shen, Shaohua; Zhao, Liang; Zhou, Zhaohui; Guo, Liejin
      Journal of Physical Chemistry C (2008), 112 (41), 16148-16155CODEN: JPCCCK; ISSN:1932-7447. (American Chemical Society)
      A series of Cu-doped ZnIn2S4 photocatalysts has been synthesized by a facile hydrothermal method, with the copper concn. varying from 0 wt.% to 2.0 wt.%. The phys. and photophys. properties of these Cu-doped ZnIn2S4 photocatalysts were characterized by x-ray diffraction (XRD), photoluminescence spectroscopy (PL), SEM, and UV-visible diffuse reflectance spectroscopy (UV-vis). The diffuse reflectance and photoluminescence spectra of Cu-doped ZnIn2S4 shifted monotonically to longer wavelengths as the copper concn. increased from 0 wt.% to 2.0 wt.%, indicating that the optical properties of these photocatalysts greatly depended on the amt. of Cu doped. Meanwhile, the layered structure of ZnIn2S4 would be destructed gradually by Cu doping. The photoactivity of ZnIn2S4 was enhanced when Cu2+ was doped into the crystal structure. The highest photocatalytic activity was obsd. on Cu (0.5 wt.%)-doped ZnIn2S4, with the rate of hydrogen evolution to be 151.5 μmol/h under visible light irradn. (λ > 430 nm). On the basis of the calcd. energy band positions and optical properties, the effect of copper as a dopant on the photocatalytic activity of Cu-ZnIn2S4 was studied.
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    32. 32
      Zhang, B.; Shi, H.; Hu, X.; Wang, Y.; Liu, E.; Fan, J. A Novel S-Scheme MoS2/CdIn2S4 Flower-like Heterojunctions with Enhanced Photocatalytic Degradation and H2 Evolution Activity. J. Phys. D: Appl. Phys. 2020, 53 (20), 205101,  DOI: 10.1088/1361-6463/ab7563
      There is no corresponding record for this reference.
    33. 33
      Chen, W.; He, Z.-C.; Huang, G.-B.; Wu, C.-L.; Chen, W.-F.; Liu, X.-H. Direct Z-Scheme 2D/2D MnIn2S4/g-C3N4 Architectures with Highly Efficient Photocatalytic Activities towards Treatment of Pharmaceutical Wastewater and Hydrogen Evolution. Chem. Eng. J. 2019, 359, 244– 253,  DOI: 10.1016/j.cej.2018.11.141
      33
      Direct Z-scheme 2D/2D MnIn2S4/g-C3N4 architectures with highly efficient photocatalytic activities towards treatment of pharmaceutical wastewater and hydrogen evolution
      Chen, Wei; He, Zhi-Cai; Huang, Guo-Bo; Wu, Cheng-Lin; Chen, Wu-Fei; Liu, Xiao-Heng
      Chemical Engineering Journal (Amsterdam, Netherlands) (2019), 359 (), 244-253CODEN: CMEJAJ; ISSN:1385-8947. (Elsevier B.V.)
      Semiconductor photocatalysis has been regarded as an environmentally friendly technol. in wastewater treatment and energy prodn. Here, a series of direct Z-scheme MnIn2S4/g-C3N4 (MnISCN) photocatalysts without electron mediators were fabricated by a simple hydrothermal route on the basis of in-situ loading of MnIn2S4 (MnIS) nanoflakes on the surface of g-C3N4 (CN) nanosheets. Photocatalytic performances evaluated under visible light irradn. revealed these Z-scheme heterostructured photocatalysts exhibited higher photocatalytic activities than single-component samples. The effect of wt. ratio between MnIn2S4 nanoflakes and mesoporous CN nanosheets on photocatalytic activity towards treatment of pharmaceutical wastewater was optimized to achieve highly efficient photocatalytic activities for both degrdn. of pharmaceutical wastewater and hydrogen generation compared with alone MnIS nanoflakes and isolated mesoporous CN nanosheets. The significant enhancement in photocatalytic activity could be primarily ascribed to the construction of Z-scheme MnISCN architectures, which effectively accelerated the transfer and sepn. of photogenerated charge carriers via tight interface contacts built among these two components. The recycling expts. for pharmaceutical wastewater treatment revealed the excellent stability of MnISCN nanocomposites. The advantages of highly efficient photocatalytic activity and excellent stability endowed a promising potential for MnISCN nanocomposites to apply in photocatalytic fields.
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    34. 34
      Song, Y.; Guo, Y.; Qi, S.; Zhang, K.; Yang, J.; Li, B.; Chen, J.; Zhao, Y.; Lou, Y. Cu7S4/MnIn2S4 Heterojunction for Efficient Photocatalytic Hydrogen Generation. J. Alloys Compd. 2021, 884, 161035,  DOI: 10.1016/j.jallcom.2021.161035
      34
      Cu7S4/MnIn2S4 heterojunction for efficient photocatalytic hydrogen generation
      Song, Yibin; Guo, Yanmei; Qi, Shaopeng; Zhang, Ke; Yang, Jinfan; Li, Bingnan; Chen, Jinxi; Zhao, Yixin; Lou, Yongbing
      Journal of Alloys and Compounds (2021), 884 (), 161035CODEN: JALCEU; ISSN:0925-8388. (Elsevier B.V.)
      Heterojunction has been considered to be one of the most effective methods for efficient hydrogen evolution reaction by photocatalytic water splitting. In this work, nanostructured Cu7S4/MnIn2S4 heterojunction was successfully fabricated via a simple two-step method, which was much simpler than most heterojunction synthesis. Firstly, Cu7S4 nanoparticles were synthesized by oil bath stirring, and then the Cu7S4/MnIn2S4heterojunctions were synthesized by the hydrothermal method. The prepd. Cu7S4/MnIn2S4 composite exhibited significantly improved hydrogen evolution activity with a rate of 13.81μmol h-1 (10 mg catalyst), which was approx. 18 times higher than that of pristine MnIn2S4. This result could be attributed to the construction of p-n heterojunction for promoting the sepn. of photogenerated charge carriers and inhibiting their recombination. Possible electron transfer mechanism was proposed by the related characterization. This work will inspire the simple fabrication of nano-heterojunctions in the future.
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    35. 35
      Dang, X.; Wu, S.; Zhao, H. Enhanced Photocatalytic Production of H2O2 through Regulation of Spatial Charge Transfer and Light Absorption over a MnIn2S4/WO3(Yb, Tm) Z-Scheme System. ACS Sustainable Chem. Eng. 2022, 10 (13), 4161– 4172,  DOI: 10.1021/acssuschemeng.1c07985
      There is no corresponding record for this reference.
    36. 36
      Xie, J.; Zhang, H.; Li, S.; Wang, R.; Sun, X.; Zhou, M.; Zhou, J.; Lou, X. W.; Xie, Y. Defect-Rich MoS2 Ultrathin Nanosheets with Additional Active Edge Sites for Enhanced Electrocatalytic Hydrogen Evolution. Adv. Mater. 2013, 25 (40), 5807– 5813,  DOI: 10.1002/adma.201302685
      36
      Defect-Rich MoS2 Ultrathin Nanosheets with Additional Active Edge Sites for Enhanced Electrocatalytic Hydrogen Evolution
      Xie, Junfeng; Zhang, Hao; Li, Shuang; Wang, Ruoxing; Sun, Xu; Zhou, Min; Zhou, Jingfang; Lou, Xiong Wen; Xie, Yi
      Advanced Materials (Weinheim, Germany) (2013), 25 (40), 5807-5813CODEN: ADVMEW; ISSN:0935-9648. (Wiley-VCH Verlag GmbH & Co. KGaA)
      Defect-rich MoS2 ultrathin nanosheet with addn. active edge sites for enhanced electrocatalytic hydrogen evolution were synthesized. XRD patterns, TEM images and polarization curves were presented.
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    37. 37
      Kumar, U.; Shrivastava, A.; De, A. K.; Pai, M. R.; Sinha, I. Fenton Reaction by H2O2 Produced on a Magnetically Recyclable Ag/CuWO4/NiFe2O4 Photocatalyst. Catal. Sci. Technol. 2023, 13 (8), 2432– 2446,  DOI: 10.1039/D3CY00102D
      There is no corresponding record for this reference.
    38. 38
      Ahmed, M. T.; Abdullah, H.; Kuo, D. H. Photocatalytic H2O2 Generation over Microsphere Carbon-Assisted Hierarchical Indium Sulfide Nanoflakes via a Two-Step One-Electron Pathway. ACS Appl. Mater. Interfaces 2023, 15 (24), 29224– 29235,  DOI: 10.1021/acsami.3c05137
      There is no corresponding record for this reference.
    39. 39
      Yu, W.; Zhu, Z.; Hu, C.; Lin, S.; Wang, Y.; Wang, C.; Tian, N.; Zhang, Y.; Huang, H. Point-to-Face Z-Scheme Junction Cd0.6Zn0.4S/g-C3N4 with a Robust Internal Electric Field for High-Efficiency H2O2 Production. J. Mater. Chem. A 2023, 11 (12), 6384– 6393,  DOI: 10.1039/D2TA10074F
      There is no corresponding record for this reference.
    40. 40
      Shrivastava, A.; Kumar, U.; Sinha, I. Design and Development of the AgI/NiFe2O4 Photo-Fenton Photocatalyst. Ind. Eng. Chem. Res. 2024, 63 (36), 15721– 15734,  DOI: 10.1021/acs.iecr.4c01386
      There is no corresponding record for this reference.
    41. 41
      Fang, Z.; Li, Y.; Li, J.; Shu, C.; Zhong, L.; Lu, S.; Mo, C.; Yang, M.; Yu, D. Capturing Visible Light in Low-Band-Gap C 4 N-Derived Responsive Bifunctional Air Electrodes for Solar Energy Conversion and Storage. Angew. Chem. 2021, 133 (32), 17756– 17762,  DOI: 10.1002/ange.202104790
      There is no corresponding record for this reference.
    42. 42
      Luo, N.; Chen, C.; Yang, D.; Hu, W.; Dong, F. S Defect-Rich Ultrathin 2D MoS2: The Role of S Point-Defects and S Stripping-Defects in the Removal of Cr(VI) via Synergistic Adsorption and Photocatalysis. Appl. Catal., B 2021, 299, 120664,  DOI: 10.1016/j.apcatb.2021.120664
      42
      S defect-rich ultrathin 2D MoS2: The role of S point-defects and S stripping-defects in the removal of Cr(VI) via synergistic adsorption and photocatalysis
      Luo, Ni; Chen, Cheng; Yang, Dingming; Hu, Wenyuan; Dong, Faqin
      Applied Catalysis, B: Environmental (2021), 299 (), 120664CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
      In the field of photocatalysis, one focus is on high-performance visible light catalysis. For this study, which follows the defect engineering strategy, ultrathin two-dimensional (2D) S defect-rich MoS2 nanosheets were created in situ by ball-milling MoS2 nanosheets with ascorbic acid and then used for the removal of Cr(VI) from wastewater. The results show that ascorbic acid increases both the sp. surface area of MoS2 nanosheets and the concn. of S stripping-defects significantly. Of the samples, D-MoS2-3 (i.e., S defect-rich ultrathin 2D MoS2 nanosheets) exhibited the best Cr(VI) adsorption capacity and photocatalytic activity thanks to its large sp. surface area and a high concn. of total S defects (18.5%), 311.1% better than for P-MoS2 (i.e., pristine MoS2 nanosheets) (4.5%). The concn. of S point-defects in D-MoS2-3 is only a little greater than in P-MoS2, but the concn. of S stripping-defects is significantly greater. S point-defects at such a high concn. readily act as recombination centers for photogenerated carriers. By contrast, S stripping-defects that lack dangling Mo-S bonds trap photogenerated holes and add to the sepn. efficiency of photogenerated electron-hole pairs. As a consequence, the photocatalytic performance of D-MoS2-3 in removing Cr(VI) is significantly better. Given this finding, the present study offers a new design pathway and a ref. for the practical application of defect engineering to ultrathin 2D materials.
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    43. 43
      Tian, H.; Liu, M.; Zheng, W. Constructing 2D Graphitic Carbon Nitride Nanosheets/Layered MoS2/Graphene Ternary Nanojunction with Enhanced Photocatalytic Activity. Appl. Catal., B 2018, 225, 468– 476,  DOI: 10.1016/j.apcatb.2017.12.019
      43
      Constructing 2D graphitic carbon nitride nanosheets/layered MoS2/graphene ternary nanojunction with enhanced photocatalytic activity
      Tian, Hongwei; Liu, Ming; Zheng, Weitao
      Applied Catalysis, B: Environmental (2018), 225 (), 468-476CODEN: ACBEE3; ISSN:0926-3373. (Elsevier B.V.)
      Two-dimensional (2D) nanosheets materials have attracted extensive attention because of their promising practical application and theor. values. In order to enhance the photocatalytic activity of bulk C3N4, we designed a 2D fabrication in which g-C3N4 nanosheets was in the middle of MoS2/graphene layered structure. Here, we report an effective strategy to synthesize ternary g-C3N4/MoS2/graphene nanocomposite photocatalyst via an in-situ adsorption method, which exhibits superior photocatalytic activity owing to enhanced charge carrier sepn. via well-contacted interface and fast charge transfer pathway. This work indicates a new insight into the design of such 2D heterostructure and a promising cocatalyst strategy for designing a more efficient g-C3N4-based semiconductor photocatalyst toward degrdn. of org. pollutants.
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    44. 44
      Zhang, Z. Y.; Tian, H.; Jiao, H.; Wang, X.; Bian, L.; Liu, Y.; Khaorapapong, N.; Yamauchi, Y.; Wang, Z. L. SiO2 Assisted Cu0-Cu+-NH2 Composite Interfaces for Efficient CO2 Electroreduction to C2+ Products. J. Mater. Chem. A 2024, 12 (2), 1218– 1232,  DOI: 10.1039/D3TA05652J
      There is no corresponding record for this reference.
    45. 45
      Cheng, J.; Niu, Z.; Zhao, Z.; Pei, X.; Zhang, S.; Wang, H.; Li, D.; Guo, Z. Enhanced Ion/Electron Migration and Sodium Storage Driven by Different MoS2-ZnIn2S4 Heterointerfaces. Adv. Energy Mater. 2023, 13 (5), 2203248,  DOI: 10.1002/aenm.202203248
      There is no corresponding record for this reference.
    46. 46
      Xi, T.-L.; Liu, L.-j.; Liu, Q.; Wang, H.-W.; Zuo, L.-Y.; Fan, H.-T.; Li, B.; Wang, L.-Y. Hollow MoS2@ZnIn2S4 Nanoboxes for Improving Photocatalytic Hydrogen Evolution. Int. J. Hydrogen Energy 2024, 62, 62– 70,  DOI: 10.1016/j.ijhydene.2024.03.006
      There is no corresponding record for this reference.
    47. 47
      Fang, Z.; Xia, Y.; Zhang, L.; Liu, J.; Li, J.; Hu, B.; Li, K.; Lu, Q.; Wang, L. Building the Confined CoS2/MoS2 Nanoreactor via Interface Electronic Reconfiguration to Synchronously Enhance Activity and Stability of Heterogeneous Fenton-like Reactions. Appl. Catal., B 2024, 346, 123769,  DOI: 10.1016/j.apcatb.2024.123769
      There is no corresponding record for this reference.
    48. 48
      Zhu, Z.; Huang, H.; Liu, L.; Chen, F.; Tian, N.; Zhang, Y.; Yu, H. Chemically Bonded α-Fe2O3/Bi4MO8Cl Dot-on-Plate Z-Scheme Junction with Strong Internal Electric Field for Selective Photo-Oxidation of Aromatic Alcohols. Angew. Chem., Int. Ed. 2022, 61 (26), e202203519  DOI: 10.1002/anie.202203519
      48
      Chemically Bonded α-Fe2O3/Bi4MO8Cl( M= Nb, Ta) Dot-on-Plate Z-Scheme Junction with Strong Internal Electric Field for Selective Photo-oxidation of Aromatic Alcohols
      Zhu, Zijian; Huang, Hongwei; Liu, Lizhen; Chen, Fang; Tian, Na; Zhang, Yihe; Yu, Han
      Angewandte Chemie, International Edition (2022), 61 (26), e202203519CODEN: ACIEF5; ISSN:1433-7851. (Wiley-VCH Verlag GmbH & Co. KGaA)
      Inferior contact interface and low charge transfer efficiency seriously restrict the performance of heterojunctions. Herein, chem. bonded α-Fe2O3/Bi4MO8Cl (M=Nb, Ta) dot-on-plate Z-scheme junctions with strong internal elec. field are crafted by an in situ growth route. Exptl. and theor. results demonstrate that the internal elec. field provides a powerful driving force for vectorial migration of photocharges between Bi4MO8Cl and α-Fe2O3, and the interfacial Fe-O bond not only serves as an at.-level charge flow highway but also lowers the charge transfer energy barrier, thereby accelerating Z-scheme charge transfer and realizing effective spatial charge sepn. Impressively, α-Fe2O3/Bi4MO8Cl manifests a significantly improved photocatalytic activity for selective oxidn. of arom. alcs. into aldehydes (Con. ≥92%, Sel. ≥96%), with a performance improvement of one to two orders of magnitude. This work presents at.-level insight into interfacial charge flow steering.
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    49. 49
      Kumar, U.; Kuntail, J.; Kumar, A.; Prakash, R.; Pai, M. R.; Sinha, I. In-Situ H2O2 Production for Tetracycline Degradation on Ag/s-(Co3O4/NiFe2O4) Visible Light Magnetically Recyclable Photocatalyst. Appl. Surf. Sci. 2022, 589, 153013,  DOI: 10.1016/j.apsusc.2022.153013
      There is no corresponding record for this reference.
    50. 50
      Zhou, S.; Ma, W.; Kosari, M.; Lim, A. M. H.; Kozlov, S. M.; Zeng, H. C. Highly Active Single-Layer 2H-MoS2 for CO2 Hydrogenation to Methanol. Appl. Catal., B 2024, 349, 123870,  DOI: 10.1016/j.apcatb.2024.123870
      There is no corresponding record for this reference.
    51. 51
      Li, G.; Sun, J.; Hou, W.; Jiang, S.; Huang, Y.; Geng, J. Three-dimensional porous carbon composites containing high sulfur nanoparticle content for high-performance lithium–sulfur batteries. Nat. Commun. 2016, 7 (1), 10601,  DOI: 10.1038/ncomms10601
      51
      Three-dimensional porous carbon composites containing high sulfur nanoparticle content for high-performance lithium-sulfur batteries
      Li, Guoxing; Sun, Jinhua; Hou, Wenpeng; Jiang, Shidong; Huang, Yong; Geng, Jianxin
      Nature Communications (2016), 7 (), 10601CODEN: NCAOBW; ISSN:2041-1723. (Nature Publishing Group)
      Sulfur is a promising cathode material for lithium-sulfur batteries because of its high theor. capacity (1,675 mA h g-1); however, its low elec. cond. and the instability of sulfur-based electrodes limit its practical application. Here we report a facile in situ method for prepg. three-dimensional porous graphitic carbon composites contg. sulfur nanoparticles (3D S@PGC). With this strategy, the sulfur content of the composites can be tuned to a high level (up to 90 wt%). Because of the high sulfur content, the nanoscale distribution of the sulfur particles, and the covalent bonding between the sulfur and the PGC, the developed 3D S@PGC cathodes exhibit excellent performance, with a high sulfur utilization, high specific capacity (1,382, 1,242 and 1,115 mA h g-1 at 0.5, 1 and 2 C, resp.), long cycling life (small capacity decay of 0.039% per cycle over 1,000 cycles at 2 C) and excellent rate capability at a high charge/discharge current.
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    52. 52
      Tian, H.; Zhang, Z. Y.; Fang, H.; Jiao, H.; Gao, T. T.; Yang, J. T.; Bian, L.; Wang, Z. L. Selective Electrooxidation of Methane to Formic Acid by Atomically Dispersed CuOx and Its Induced Lewis Acid Sites on V2O5 in a Tubular Electrode. Appl. Catal., B 2024, 351, 124001,  DOI: 10.1016/j.apcatb.2024.124001
      There is no corresponding record for this reference.
    53. 53
      Sebastia-Saez, D.; Gu, S.; Ramaioli, M. Effect of the Contact Angle on the Morphology, Residence Time Distribution and Mass Transfer into Liquid Rivulets: A CFD Study. Chem. Eng. Sci. 2018, 176, 356– 366,  DOI: 10.1016/j.ces.2017.09.046
      There is no corresponding record for this reference.
    54. 54
      Zhang, X.; Yu, J.; Macyk, W.; Wageh, S.; Al-Ghamdi, A. A.; Wang, L. C3N4/PDA S-Scheme Heterojunction with Enhanced Photocatalytic H2O2 Production Performance and Its Mechanism. Adv. Sustain. Syst. 2023, 7 (1), 2200113,  DOI: 10.1002/adsu.202200113
      There is no corresponding record for this reference.
    55. 55
      Yang, Y. Y.; Guo, H.; Huang, D. W.; Li, L.; Liu, H. Y.; Sui, L.; Wu, Q.; Zhu, J. J.; Zhang, L.; Niu, C. G. Simultaneously Tuning Oxygen Reduction Pathway and Charge Transfer Dynamics toward Sacrificial Agent-Free Photocatalytic H2O2 Production for in-Situ Water Disinfection. Chem. Eng. J. 2024, 479, 147863,  DOI: 10.1016/j.cej.2023.147863
      There is no corresponding record for this reference.
    56. 56
      Wang, S.; Xie, Z.; Zhu, D.; Fu, S.; Wu, Y.; Yu, H.; Lu, C.; Zhou, P.; Bonn, M.; Wang, H. I.; Liao, Q.; Xu, H.; Chen, X.; Gu, C. Efficient Photocatalytic Production of Hydrogen Peroxide Using Dispersible and Photoactive Porous Polymers. Nat. Commun. 2023, 14 (1), 6891,  DOI: 10.1038/s41467-023-42720-6
      56
      Efficient photocatalytic production of hydrogen peroxide using dispersible and photoactive porous polymers
      Wang, Shengdong; Xie, Zhipeng; Zhu, Da; Fu, Shuai; Wu, Yishi; Yu, Hongling; Lu, Chuangye; Zhou, Panke; Bonn, Mischa; Wang, Hai I.; Liao, Qing; Xu, Hong; Chen, Xiong; Gu, Cheng
      Nature Communications (2023), 14 (1), 6891CODEN: NCAOBW; ISSN:2041-1723. (Nature Portfolio)
      Developing efficient artificial photocatalysts for the biomimetic photocatalytic prodn. of mol. materials, including medicines and clean energy carriers, remains a fundamentally and technol. essential challenge. Hydrogen peroxide is widely used in chem. synthesis, medical disinfection, and clean energy. However, the current industrial prodn., predominantly by anthraquinone oxidn., suffers from hefty energy penalties and toxic byproducts. Herein, we report the efficient photocatalytic prodn. of hydrogen peroxide by protonation-induced dispersible porous polymers with good charge-carrier transport properties. Significant photocatalytic hydrogen peroxide generation occurs under ambient conditions at an unprecedented rate of 23.7 mmol g-1 h-1 and an apparent quantum efficiency of 11.3% at 450 nm. Combined simulations and spectroscopies indicate that sub-picosecond ultrafast electron "localization" from both free carriers and exciton states at the catalytic reaction centers underlie the remarkable photocatalytic performance of the dispersible porous polymers.
      >> More from SciFinder ®
      https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BB3sXit1CnsrfJ&md5=2a609fd4897f8fc01ae349555c9f9101
    57. 57
      Li, R.; Zhang, D.; Shi, Y.; Li, C.; Long, Y.; Yang, M. Developing a Built-in Electric Field in CdS Nanorods by Modified MoS2 for Highly Efficient Photocatalytic H2O2 Production. J. Catal. 2022, 416, 322– 331,  DOI: 10.1016/j.jcat.2022.11.016
      There is no corresponding record for this reference.
    58. 58
      Wang, J.; Yang, L.; Zhang, L. Constructed 3D Hierarchical Micro-Flowers CoWO4@Bi2WO6 Z-Scheme Heterojunction Catalyzer: Two-Channel Photocatalytic H2O2 Production and Antibiotics Degradation. Chem. Eng. J. 2021, 420, 127639,  DOI: 10.1016/j.cej.2020.127639
      58
      Constructed 3D hierarchical micro-flowers CoWO4@Bi2WO6 Z-scheme heterojunction catalyzer: Two-channel photocatalytic H2O2 production and antibiotics degradation
      Wang, Jing; Yang, Lijun; Zhang, Lei
      Chemical Engineering Journal (Amsterdam, Netherlands) (2021), 420 (Part_2), 127639CODEN: CMEJAJ; ISSN:1385-8947. (Elsevier B.V.)
      Proper design and fabrication of multifunctional visible-light-induced photocatalysts with high catalytic efficiency is still a huge challenge for the value-added chems. prodn. and environmental remediation. A novel 3D flower-like hierarchical CoWO4@Bi2WO6 Z-scheme hybrid was successfully fabricated via anchoring CoWO4 nanoparticles on the 2D nanopetals of Bi2WO6 microflower obtained by solvothermal assistant self-assembly. The multifunctional composite could markedly improve photocatalytic H2O2 prodn. via two-channel route (oxygen redn. and water oxidn. reaction) without using sacrificial agent. Interestingly, 3D CoWO4@Bi2WO6 also displayed a remarkable degrdn. performance on single (enrofloxacin (ENR), lomefloxacin (LOM) or ciprofloxacin hydrochloride (CIP)) and ternary mixed antibiotics (ENR + LOM + CIP) under visible light irradn. The outstanding photocatalytic activity was primarily attributed to the 3D hierarchical CoWO4@Bi2WO6 micro-flowers architecture for boosting visible light harvesting, matching energy band gaps, more exposed active sites, formation of Z-scheme based charge-transfer dynamics in a p-n heterostructure, as well as strong oxidn. and redn. capability of photoexcited h+ and e-. Therefore, it was believed that the novel multifunctional CoWO4@Bi2WO6 photocatalyst exhibited a potential application in prodn. of H2O2 and degrdn. of org. contaminants, which were more significant for the following purifn. in industrial prodn. and environmental governance.
      >> More from SciFinder ®
      https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BB3cXitlClu7%252FJ&md5=e324b0fd94a905bafbfa772c72a2a25a
    59. 59
      Wang, F.; Yue, S.; Han, X.; Zhang, T.; Han, A.; Wang, L.; Liu, J. ZnS/C Dual-Quantum-Dots Heterostructural Nanofibers for High-Performance Photocatalytic H2O2 Production. ACS Appl. Mater. Interfaces 2024, 16 (2), 2606– 2613,  DOI: 10.1021/acsami.3c14183
      There is no corresponding record for this reference.
    60. 60
      Ma, L.; Gao, Y.; Wei, B.; Huang, L.; Zhang, N.; Weng, Q.; Zhang, L.; Liu, S. F.; Jiang, R. Visible-Light Photocatalytic H2O2 Production Boosted by Frustrated Lewis Pairs in Defected Polymeric Carbon Nitride Nanosheets. ACS Catal. 2024, 14 (4), 2775– 2786,  DOI: 10.1021/acscatal.3c05360
      There is no corresponding record for this reference.

  • Supporting Information

    Supporting Information

    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsaem.4c03296.

    • UV visible absorbance spectra of bulk MoS2 and exfoliated MoS2 nanosheets; images of exfoliated MoS2 nanosheets dispersion; Tauc plot of bulk MoS2 and MS/MnIS-x heterostructures photocatalyst; SEM elemental mapping of MnIn2S4; SEM images with corresponding elemental mapping of MS/MnIS60 and MS/MnIS80 heterostructure photocatalysts; HRTEM images of 2D MoS2 nanosheets; TEM images of MS/MnIS40 photocatalysts; XPS survey spectra of MnIn2S4, 2D MoS2, and MS/MnIS40; PL spectra of MS/MnIS10 and MS/MnIS80; Nyquist plot of pure MnIn2S4 MS/MnIS10 and MS/MnIS80 heterostructure photocatalysts; photocurrent studies of MnIn2S4, MS/MnIS10, and MS/MnIS80 photocatalysts; EIS equivalent fitting circuit and Rs and Rct value of 2D MoS2, MnIn2S4, and MS/MnIS-x heterostructure photocatalysts; contact angle results of pristine MnIn2S4; photocatalytic H2O2 production rate at O2 bubbled DI and water/EtOH mixture at pH 3; photocatalytic H2O2 decomposition at different time intervals; table showing the comparison of photocatalytic H2O2 production among recently reported other photocatalytic systems; NBT experiments on MS/MnIS40 photocatalyst; XPS spectra of recycled MS/MnIS40 photocatalyst (PDF)


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