构建不对称结构单元实现近平衡的氢吸脱附增强a-ReSxSe2-x助剂的光催化析氢活性

doi:10.1016/S1872-2067(25)64930-8

催化学报 ›› 2026, Vol. 85: 322-332.DOI: 10.1016/S1872-2067(25)64930-8

构建不对称结构单元实现近平衡的氢吸脱附增强a-ReS_xSe_2-_x助剂的光催化析氢活性

钟威, 甘义遥, 王敬涛, 杨沛颐, 孟爱云(), 苏耀荣()

深圳技术大学新材料与新能源学院, 广东深圳 518118

收稿日期:2025-09-21 接受日期:2025-10-19 出版日期:2026-06-18 发布日期:2026-05-18
通讯作者: *电子信箱: suyaorong@sztu.edu.cn (苏耀荣),
mengaiyun@sztu.edu.cn (孟爱云).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(22178224);国家自然科学基金(22272110);国家自然科学基金(22402126);广东省基础与应用基础研究基金(2023A1515110535);深圳市科技计划资助(RCBS20231211090522041);污染物分析与资源化技术湖北省重点实验室(湖北师范大学)(PA240201);深圳市超金刚石与功能晶体应用技术重点实验室(ZDSYS20230626091303007)

Achieving near-equilibrium H_ad adsorption/desorption by introducing asymmetric S-Re-Se modules in a-ReS_xSe_2-_x cocatalysts for enhanced photocatalytic H₂ evolution

Wei Zhong, Yiyao Gan, Jingtao Wang, Peiyi Yang, Aiyun Meng(), Yaorong Su()

College of New Materials and New Energies, Shenzhen Technology University, Shenzhen 518118, Guangdong, China

Received:2025-09-21 Accepted:2025-10-19 Online:2026-06-18 Published:2026-05-18
Contact: *E-mail: suyaorong@sztu.edu.cn (Y. Su),
mengaiyun@sztu.edu.cn (A. Meng).
About author:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22178224);National Natural Science Foundation of China(22272110);National Natural Science Foundation of China(22402126);Guangdong Basic and Applied Basic Research Foundation(2023A1515110535);Shenzhen Science and Technology Program(RCBS20231211090522041);Hubei Key Laboratory of Pollutant Analysis & Reuse Technology (Hubei Normal University)(PA240201);Shenzhen Key Laboratory of Applied Technologies of Super-Diamond and Functional Crystals(ZDSYS20230626091303007)

摘要/Abstract

摘要：

将太阳能直接转化为氢能的半导体光催化分解水制氢技术, 是清洁能源领域的研究热点. 然而, 其效率常受限于光催化剂内部严重的光生电荷复合(包括体相与表面复合)以及迟缓的界面析氢反应动力学. 针对上述问题, 在光催化剂表面修饰析氢助催化剂, 通过协同提升光生电荷分离效率与表面催化反应速率, 已成为实现光催化制氢性能倍增的有效手段. 二维金属硫化物拥有一系列独特性质, 如高化学稳定性、大比表面积和可调的电子结构, 使其在光催化制氢领域极具应用潜力. 然而, 传统二维金属硫化物材料中活性S原子容易与析氢中间体(H_ad)产生强的S-H_ad键, 使得氢分子不易脱附, 导致光催化制氢性能不高. 因此, 发展有效方法调控S原子的电子结构是进一步提升二维金属硫化物助剂光催化制氢性能的重要途径.

本文提出将Se原子引入a-ReS₂的结构中打破S-Re-S单元的结构对称性, 构建不对称S-Re-Se来优化S原子的电子结构, 提高光催化析氢性能. 首先通过一步光电子还原法成功在TiO₂材料表面修饰了无定形a-ReS_xSe_2-_x纳米颗粒, 可控制备了a-ReS_xSe_2-_x/TiO₂光催化材料. 通过高倍透射电镜、X射线衍射和拉曼光谱等表征证实了具有均相结构的无定形a-ReS_xSe_2-_x纳米颗粒修饰在TiO₂颗粒表面. 光催化制氢性能测试表明, 当a-ReS_xSe_2-_x助剂中S原子与Se原子比例为1.2:0.8时, 所得a-ReS_1.2Se_0.8/TiO₂样品的光催化制氢速率为1588 μmol g^-1 h^-1, 是a-ReS₂/TiO₂和a-ReSe₂/TiO₂样品的2.12和1.53倍. X射线光电子能谱(XPS)和密度泛函理论计算结果表明, Se原子的引入能够在ReS_1.2Se_0.8中产生众多不对称S-Re-Se结构单元, 同时诱导不对称S-Re-Se结构单元产生自优化的电荷分布, 增加S原子的电子密度并形成富电子活性S⁽²⁺^δ^)-位点. 进一步理论计算结果表明, 富电子活性S⁽²⁺^δ^)-位点与H_ad结合后产生的S⁽²⁺^δ^)--H_ad键反键轨道填充度增加, 相应的S⁽²⁺^δ^)-位点上析氢吉布斯自由能为-0.06 eV, 表明不对称S-Re-Se结构单元中活性S⁽²⁺^δ^)-位点实现了接近平衡的氢吸脱附动力学. 此外, 原位XPS和光电化学测试证明, 无定形a-ReS_xSe_2-_x纳米颗粒能够快速捕获并转移TiO₂表面的光生电子, 有效抑制光生电子-空穴对的复合. 基于实验表征和理论计算分析, a-ReS_xSe_2-_x/TiO₂材料的光催化制氢活性提升机理是: 无定形a-ReS_xSe_2-_x纳米颗粒可快速捕获光生电子并将其转移至活性S⁽²⁺^δ^)-位点, 吸附在活性S⁽²⁺^δ^)-位点上的H_ad被光生电子还原后快速脱附并结合成H₂分子, 最终实现高效的光催化制氢效率.

综上, 通过Se原子掺杂产生不对称S-Re-Se结构单元, 诱导其产生自优化的电荷分布, 形成富电子活性S⁽²⁺^δ^)-位点并实现接近平衡的氢吸脱附动力学, 最终提高界面析氢催化反应动力学. 本文提出的构建不对称结构单元来优化活性位点电子结构策略为高效光催化材料的设计提供了新的思路.

关键词: 产氢, 光催化, 不对称活性单元, 自优化电子结构 a-ReS_xSe_2-_x助剂

Abstract:

Two-dimensional transition metal sulfides (MS₂) are regarded as promising cocatalyst for photocatalytic hydrogen (H₂) production, but the intrinsic symmetric S-M-S module usually causes an improper adsorption/desorption ability of H_ad on catalytic S atoms. Herein, the symmetry of S-Re-S modules in traditional ReS₂ is disrupted by incorporating selenium (Se) atoms, enabling the self-optimized electronic property of active S sites in asymmetric S-Re-Se modules for high performance photocatalytic H₂ production. Through a one-step photodeposition process, Se atoms were controllably and uniformly incorporated into a-ReS₂ nanoparticles, thereby forming a homogeneous amorphous ReS_xSe_2-_x (a-ReS_xSe_2-_x) cocatalyst on the TiO₂ surface. It is found that incorporating Se atoms into amorphous ReS₂ (a-ReS₂) structure creates massive asymmetric S-Re-Se modules and induces a steered electron transport from Se to S atoms, thus forming self-optimized electron-rich S⁽²⁺^δ^)- sites in the a-ReS_xSe_2-_x cocatalysts. Furthermore, the electron-rich S⁽²⁺^δ^)- centers interact with H_ad via a higher antibonding orbital occupancy, enabling a near-equilibrium H_ad adsorption/desorption energy for the efficient H₂ generation. Encouragingly, the photocatalytic H₂-production performance of the optimized a-ReS_1.2Se_0.8/TiO₂ photocatalyst outperforms the a-ReS₂/TiO₂ and a-ReSe₂/TiO₂ samples by factors of 2.12 and 1.53, respectively. This work constructs new asymmetric active modules to induce self-optimized charge distribution in catalytic atoms, advancing the rational design principle of highly active photocatalysts for sustainable H₂ production.

Key words: Hydrogen production, Photocatalysis, Asymmetric active modules, Self-optimized electron structure, a-ReS_xSe_2-_x cocatalysts

钟威, 甘义遥, 王敬涛, 杨沛颐, 孟爱云, 苏耀荣. 构建不对称结构单元实现近平衡的氢吸脱附增强a-ReS_xSe_2-_x助剂的光催化析氢活性[J]. 催化学报, 2026, 85: 322-332.

Wei Zhong, Yiyao Gan, Jingtao Wang, Peiyi Yang, Aiyun Meng, Yaorong Su. Achieving near-equilibrium H_ad adsorption/desorption by introducing asymmetric S-Re-Se modules in a-ReS_xSe_2-_x cocatalysts for enhanced photocatalytic H₂ evolution[J]. Chinese Journal of Catalysis, 2026, 85: 322-332.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64930-8

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图/表 8

Fig. 1. (A) Schematic diagram illustrating the formation of asymmetric S-M-Se modules with self-optimized electron structure in two-dimensional MS2 cocatalysts (M: Metal atoms). (B) Graphical illustration of the antibonding orbital occupancy between the self-optimized electron-enriched S atoms (S(2+δ)-) and Had.

Fig. 2. (A) Schematic illustration of the synthetic route for a-ReSxSe2-x/TiO2 synthesis. HRTEM (B,C), HAADF-STEM (D), and elemental mapping images (E1-E5) of typical a-ReS1.2Se0.8/TiO2 photocatalyst.

Fig. 3. XRD (A), survey XPS (B), high-resolution Re 4f (C), UV-vis (D) spectra along with optical photographs of the as-prepared photocatalysts.

Fig. 4. (A) H2 evolution rates of various photocatalysts. (B) Cycling test of the a-ReS1.2Se0.8/TiO2 photocatalyst.

Fig. 5. (A-C) The optimized structures of ReS2, ReS1.2Se0.8 and ReSe2. Local charge density difference (D) and planar-averaged electron density difference ∆ρ(z) (E) in ReS1.2Se0.8 structure. The yellow and cyan zones indicate charge gain and loss, respectively. (F) Bader charge density distributions of ReS2, ReS1.2Se0.8 and ReSe2 structures. The high-resolution XPS spectra of S 2p (G) and Se 3d (H) for the synthesized a-ReS2/TiO2, a-ReS1.2Se0.8/TiO2, and a-ReS2/TiO2. (I) Schematic diagram of the formation of the electron-rich S(2+δ)- sites in asymmetric S-Re-Se modules.

Fig. 6. (A-C) Adsorption models of H atom on ReS2, ReS1.2Se0.8 and ReSe2. (D) pDOS data of the S elements in ReS2 and ReS1.2Se0.8. (E) Gibbs energy profiles (ΔGH*) for H adsorption on the catalytic sites. (F) Schematic diagram of the weakened H adsorption on S(2+δ)- sites in ReS1.2Se0.8 by raising the antibonding-orbital occupancy.

Fig. 7. The calculated electrostatic potentials of TiO2 (A) and a-ReS1.2Se0.8 (B). In-situ XPS spectra of S 2p (C) and) Ti 2p (D) for the a-ReS1.2Se0.8/TiO2 sample before and after light illumination. (E) Schematic diagrams for the electron transfer of the a-ReS1.2Se0.8/TiO2 photocatalysts.

Fig. 8. Steady-state PL spectra (A), TRPL curves (B), photovoltage (C), EIS (D), LSV (E) and i-t curves (F) of the synthesized photocatalysts. (G) The proposed H2 evolution mechanism of the present a-ReSxSe2-x/TiO2 photocatalysts.

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构建不对称结构单元实现近平衡的氢吸脱附增强a-ReS_xSe_2-_x助剂的光催化析氢活性

Achieving near-equilibrium H_ad adsorption/desorption by introducing asymmetric S-Re-Se modules in a-ReS_xSe_2-_x cocatalysts for enhanced photocatalytic H₂ evolution

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构建不对称结构单元实现近平衡的氢吸脱附增强a-ReSxSe2-x助剂的光催化析氢活性

Achieving near-equilibrium Had adsorption/desorption by introducing asymmetric S-Re-Se modules in a-ReSxSe2-x cocatalysts for enhanced photocatalytic H2 evolution

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构建不对称结构单元实现近平衡的氢吸脱附增强a-ReS_xSe_2-_x助剂的光催化析氢活性

Achieving near-equilibrium H_ad adsorption/desorption by introducing asymmetric S-Re-Se modules in a-ReS_xSe_2-_x cocatalysts for enhanced photocatalytic H₂ evolution