自组装3D/2D ZnIn2S4/CN-NH4构建S型异质结用于纯水中高效制备过氧化氢

doi:10.1016/S1872-2067(25)64851-0

催化学报 ›› 2026, Vol. 81: 259-271.DOI: 10.1016/S1872-2067(25)64851-0

自组装3D/2D ZnIn₂S₄/CN-NH₄构建S型异质结用于纯水中高效制备过氧化氢

王聪聪^a^,^b^,^c, 权永康^d, 石穗丽^a^,^b^,^c, 王国荣^a^,^b^,^c(), 靳治良^a^,^b^,^c

^a 北方民族大学化学与化学工程学院, 宁夏银川 750021
^b 北方民族大学宁夏太阳能化学转化技术重点实验室, 宁夏银川 750021
^c 北方民族大学, 国家民族事务委员会化学工程与技术重点实验室, 宁夏银川 750021
^d 福州大学化学工程学院, 福建福州 350116

收稿日期:2025-06-19 接受日期:2025-08-13 出版日期:2026-02-18 发布日期:2025-12-26
通讯作者: *电子信箱: guorongwang@nun.edu.cn (王国荣).
基金资助:
国家自然科学基金(U22A20147)

Self-assembling 3D/2D ZnIn₂S₄/CN-NH₄ to construct S-scheme heterojunctions for the efficient production of H₂O₂ in pure water

Congcong Wang^a^,^b^,^c, Yongkang Quan^d, Suili Shi^a^,^b^,^c, Guorong Wang^a^,^b^,^c(), Zhiliang Jin^a^,^b^,^c

^a School of Chemistry and Chemical Engineering, North Minzu University, Yinchuan 750021, Ningxia, China
^b Ningxia Key Laboratory of Solar Chemical Conversion Technology, North Minzu University, Yinchuan 750021, Ningxia, China
^c Key Laboratory for Chemical Engineering and Technology, State Ethnic Affairs Commission, North Minzu University, Yinchuan 750021, Ningxia, China
^d College of Chemical Engineering, Fuzhou University, Fuzhou 350116, Fujian, China

Received:2025-06-19 Accepted:2025-08-13 Online:2026-02-18 Published:2025-12-26
Contact: *E-mail: guorongwang@nun.edu.cn (G. Wang).
Supported by:
National Natural Science Foundation of China(U22A20147)

摘要/Abstract

摘要：

过氧化氢(H₂O₂)作为一种环境友好型氧化剂和重要的能量载体, 已广泛应用于造纸、污水处理、医疗消毒和工业生产等领域. 鉴于大规模生产H₂O₂的传统工业蒽醌工艺, 涉及高成本、高能耗以及高污染, 与追求的碳中和理念背道而驰. 开发一种低能耗、可持续的H₂O₂生产工艺势在必行. 相较于大多数传统工艺, 人工光合作用对H₂O₂的生产提供了极具吸引力的新途径. 通过太阳能将丰富的水资源以及空气中体积分数约为20%的氧气进行整合, 产生高能量密度的H₂O₂, 从而实现绿色生产. 该过程主要涉及两种途径: 双电子氧还原反应 (ORR, O₂ + 2H⁺ + 2e⁻ → H₂O₂, 0.69 V vs. NHE)和水氧化反应(WOR, 2H₂O → H₂O₂ + 2H⁺ + 2e⁻, 1.76 V vs. NHE). 由于热力学限制, 双电子WOR反应对H₂O₂的产出较为困难, 且产物易分解. 目前, 大部分研究工作主要集中双电子氧还原路径.

本文通过软模板法, 将大块的C₃N₄分解成更小的片段(CN-NH₄), 引入更多无序界面, 提供更多的界面电场, 大大弥补了材料自身的不足. 进而将低成本的CN-NH₄片段负载到花状ZnIn₂S₄上, 构建紧凑的S型异质结, 以实现环保型H₂O₂光催化合成. 通过X射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)证实催化剂单体以及ZnIn₂S₄/CN-NH₄复合催化剂的成功制备. 通过原位X射线光电子能谱(XPS)和密度泛函理论计算证实了ZnIn₂S₄/CN-NH₄复合催化剂间的典型S型电子转移机制, 电化学测试证实, ZnIn₂S₄/CN-NH4复合催化剂的构建为反应提供更多的电化学活性位点, 电子顺磁共振谱表明ZnIn₂S₄/CN-NH₄复合催化剂的制备表现出更强的氧化还原能力并通过两步单电子氧化原反应生成H₂O₂. 同时, CN-NH₄的引入增强了ZnIn₂S₄对氧气的吸附, 并降低了其两步单电子氧还原反应(ORR)的能量势垒. ZnIn₂S₄/CN-NH₄光催化剂的H₂O₂产量为2031 µmol∙g^‒1∙h^‒1, 分别是ZnIn₂S₄和CN-NH₄的2.84倍和21.39倍, 这归因于ZnIn₂S₄和CN-NH₄之间的接触, 为电子提供了快速迁移通道, 在界面处形成了强大的内电场, 并有效地延长了光生载流子的迁移寿命.

综上, 合理构建S型异质结是提高材料光催化性能的有效策略. 本文构建了S型3D/2D ZnIn₂S₄/CN-NH₄异质结,并深度探究了S型异质结构建在光催化产H₂O₂领域的关键作用, 为在纯水体系中实现高效高浓度H₂O₂的光催化生成提供新思路.

关键词: 过氧化氢, 氧还原, 超纯水, S型异质结, 硫化锌铟

Abstract:

The photocatalytic double-electron oxygen reduction pathway has become a strategic approach for the production of hydrogen peroxide (H₂O₂). In many heterojunction systems, indium zinc sulfide (ZnIn₂S₄) has received increasing attention, but it is limited by its slow REDOX kinetics and the lack of sufficient double-electron oxygen reduction active sites. In this study, low-cost CN-NH₄ fragments were loaded onto flower-like indium zinc sulfide (ZnIn₂S₄) to construct a compact S-scheme, in order to achieve environmentally friendly hydrogen peroxide photosynthesis. The H₂O₂ yield of the ZnIn₂S₄/CN-NH₄ photocatalyst was 2031 µmol g^-1 h^-1, which was 2.84 and 21.39 times that of ZnIn₂S₄ and CN-NH₄, respectively. This is attributed to the contact between ZnIn₂S₄ and CN-NH₄, providing a fast migration channel for electrons, forming a strong internal electric field at the interface, and effectively prolonging the migration lifetime of photogenerated carriers. The introduction of CN-NH₄ enhances the absorption of oxygen by ZnIn₂S₄ and simultaneously reduces the energy barrier of its two-electron oxygen reduction reaction. This study provides a new approach for constructing S-scheme heterojunction materials that can efficiently generate H₂O₂ under solar irradiation.

Key words: Hydrogen peroxide, Oxygen reduction, Pure water, S-scheme heterojunction, Zinc indium sulfide

王聪聪, 权永康, 石穗丽, 王国荣, 靳治良. 自组装3D/2D ZnIn₂S₄/CN-NH₄构建S型异质结用于纯水中高效制备过氧化氢[J]. 催化学报, 2026, 81: 259-271.

Congcong Wang, Yongkang Quan, Suili Shi, Guorong Wang, Zhiliang Jin. Self-assembling 3D/2D ZnIn₂S₄/CN-NH₄ to construct S-scheme heterojunctions for the efficient production of H₂O₂ in pure water[J]. Chinese Journal of Catalysis, 2026, 81: 259-271.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64851-0

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图/表 11

Scheme 1. Schematic illustration of the electrostatic self-assembly process for the preparation of the composite catalyst ZnIn2S4/CN-NH4.

Fig. 1. SEM images of flower-like ZnIn2S4 (a), sheet-like CN-NH4 (b), and ZnIn2S4/CN-NH4 (c). The TEM image (d), locally magnified TEM image (e), HRTEM image and corresponding SAED image (f) of ZnIn2S4/CN-NH4. EDS element mapping images of Zn (h), In (i), S (j), C (k), and N (l).

Fig. 2. XRD patterns of ZnIn2S4, CN-NH4, ZnIn2S4/CN-NH4-20 (a) and samples in various proportions (b). (c) The FT-IR spectra of ZnIn2S4, CN-NH4 and ZnIn2S4/CN-NH4-20. N2 adsorption-desorption isotherms and pore size distribution curves of ZnIn2S4 (d), CN-NH4 (e), and ZnIn2S4/CN-NH4-20 (f).

Table 1 BET surface area (ABET), pore diameter, and pore volume of ZnIn2S4, CN-NH4, and ZnIn2S4/CN-NH4-20.

Sample	A_BET(m² g^‒1)	Pore volume (cm³ g^‒1)	Average pore size (nm)
ZnIn₂S₄	107.13	0.24	4.58
CN-NH₄	37.41	0.20	18.31
ZnIn₂S₄/CN-NH₄-20	40.87	0.16	5.77

Fig. 3. (a) UV-vis DRS spectra of all samples. (b) Band gap diagram of ZnIn2S4 and CN-NH4. The M-S plots of ZnIn2S4 (c) and CN-NH4 (d) at different frequencies.

Fig. 4. In-situ XPS spectra of Zn 2p (a), In 3d (b), S 2p (c), C 1s (d), and N 1s (e). (f) Band structure diagram of ZnIn2S4 and CN-NH4.

Fig. 5. Transient photocurrent responses (a), LSV curves (b) and electrochemical active area plots (c) of ZnIn2S4, CN-NH4 and ZnIn2S4/CN-NH4. CV curves of ZnIn2S4 (d), CN-NH4 (e), and ZnIn2S4/CN-NH4 (f) at different scan rates.

Fig. 6. 2D pseudocolor TA plots of ZnIn2S4 (a), CN-NH4 (b), and ZnIn2S4/CN-NH4-20 (c). TA spectra of ZnIn2S4 (d), CN-NH4 (e), and ZnIn2S4/CN-NH4-20 (f) at indicated time delays. Normalized fs-TA decay curves of ZnIn2S4 at 710 nm (g), CN-NH4 at 388 nm (h), and ZnIn2S4/CN-NH4-20 at 710 nm (i).

Fig. 7. (a) The yield of H2O2 per 15 min of pure ZnIn2S4, CN-NH4 and samples in various proportions (mmol L?1). (b) Comparison of pure ZnIn2S4, CN-NH4 and the performance of the optimal proportion. (c) Comparison of H2O2 production performance for ZnIn2S4/CN-NH4-20 under N2 and O2 atmospheres. (d) XRD patterns of ZnIn2S4/CN-NH4-20 before and after the reaction. (e) Zeta potentials of ZnIn2S4, CN-NH4, and ZnIn2S4/CN-NH4-20. (f) ESR spectra detecting superoxide radicals (?O2?) for ZnIn2S4, CN-NH4, and ZnIn2S4/CN-NH4-20 under dark conditions and after 5 min of light irradiation. (g) A comparison chart of the H2O2 production rate of ZnIn2S4/CN-NH4-20 with some recent works.

Fig. 8. Theoretical calculation model, work function (a), density of states (b) and band gap (c) of ZnIn2S4. Theoretical calculation model, work function (d), density of states (e) and band gap (f) of CN-NH4. (g) Schematic diagram of H2O2 production by 2e? ORR in tight S-scheme ZnIn2S4/CN-NH4. (h) The Gibbs free energy distribution of the 2e? ORR process of ZnIn2S4 and ZnIn2S4/CN-NH4.

Fig. 9. Schematic illustration of the charge transfer of ZnIn2S4/CN-NH4.

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自组装3D/2D ZnIn₂S₄/CN-NH₄构建S型异质结用于纯水中高效制备过氧化氢

Self-assembling 3D/2D ZnIn₂S₄/CN-NH₄ to construct S-scheme heterojunctions for the efficient production of H₂O₂ in pure water

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[15]	陈润东, 张宇航, 夏兵全, 周贤龙, 张彦昭, 刘善堂. 双功能Zn_xCd_1-_xS_y/FePS₃阶梯(S)型异质结增强光催化产氢与苯甲醛性能[J]. 催化学报, 2026, 80(1): 123-134.