镍掺杂扰动p-d轨道杂化调控CoSe2助催化剂用于高效光催化制氢

doi:10.1016/S1872-2067(26)65236-9

催化学报 ›› 2027, Vol. 92: 262-273.DOI: 10.1016/S1872-2067(26)65236-9

镍掺杂扰动p-d轨道杂化调控CoSe₂助催化剂用于高效光催化制氢

杜仕文, 李全美, 吕娜, 鲁巍, 黄金斗, 张振翼^*()

大连民族大学物理与材料工程学院, 辽宁省光敏材料与器件重点实验室, 国家民委新能源与稀土资源利用重点实验室, 辽宁大连 116600

收稿日期:2026-05-02 接受日期:2026-05-29 出版日期:2027-01-02 发布日期:2026-10-30
通讯作者: *电子信箱: zhangzy@dlnu.edu.cn (张振翼).
基金资助:
国家自然科学基金(U23A20102);国家自然科学基金(22472021);国家自然科学基金(22402021);国家自然科学基金(22578055);“兴辽英才计划”领军人才(XLYC2202036);辽宁省自然科学基金杰出青年基金(2025-JQ-02);中央高校基本科研业务费(044420250072);辽宁省科技计划联合基金(2024JH2/102600101);辽宁省科技计划联合基金(2025JH2/101800125);辽宁省科技计划联合基金(2025JH2/101800133)

Tailoring the d-band center of CoSe₂ cocatalyst via Ni-doping-induced p-d hybridization perturbation for enhanced photocatalytic H₂ production

Shiwen Du, Quanmei Li, Na Lu, Wei Lu, Jindou Huang, Zhenyi Zhang^*()

Key Laboratory of New Energy and Rare Earth Resource Utilization of State Ethnic Affairs Commission, Key Laboratory of Photosensitive Materials and Devices of Liaoning Province, School of Physics and Materials Engineering, Dalian Minzu University, Dalian 116600, Liaoning, China

Received:2026-05-02 Accepted:2026-05-29 Online:2027-01-02 Published:2026-10-30
Contact: *E-mail: zhangzy@dlnu.edu.cn (Z. Zhang).
Supported by:
National Natural Science Foundation of China(U23A20102);National Natural Science Foundation of China(22472021);National Natural Science Foundation of China(22402021);National Natural Science Foundation of China(22578055);Liaoning Revitalization Talents Program(XLYC2202036);Natural Science Foundation of Liaoning Province for Outstanding Young Scholars(2025-JQ-02);Fundamental Research Funds for the Central Universities(044420250072);Joint Funds of the Science and Technology Program of Liaoning Province(2024JH2/102600101);Joint Funds of the Science and Technology Program of Liaoning Province(2025JH2/101800125);Joint Funds of the Science and Technology Program of Liaoning Province(2025JH2/101800133)

摘要/Abstract

摘要：

通过光催化分解水产氢可将太阳能转化为无污染、易储存的化学能, 有望缓解日益严峻的能源危机与环境污染问题. 但单一光催化剂的载流子复合速率高、表面析氢动力学迟缓, 使太阳能-氢能转化效率远低于理想值. 助催化剂能够为反应中间体H*提供吸附活化位点、加速载流子分离, 在提升光催化析氢性能方面展示出巨大优势. 高性能析氢助催化剂需与H*的作用强度适中, 兼顾H*吸附与氢气脱附两个过程. 然而传统助催化剂中活性位点的电子构型不理想, 存在对H*吸附过强或过弱的问题, 致使反应动力学速率偏低. 因此, 精准调控活性位点电子结构、同步优化氢吸附与脱附过程, 是突破上述瓶颈、提升光催化析氢效率的关键.

本文提出一种借助过渡金属异质掺杂调控活性位点d带中心的改性策略, 设计合成了一种Ni掺杂的CoSe₂助催化剂, 有效提升了Bi₄Ti₃O₁₂ (BTO)半导体的光催化分解水制氢活性. 基于第一性原理计算的态密度分析等结果表明, Ni掺杂有效扰动了CoSe₂ (CS)中p-d轨道杂化, 从而诱导活性位点Co原子d带中心上移, 在优化H吸附吉布斯自由能的同时增强了Co活性位点对H质子的吸附能力. 实验中采用原位溶剂热法制备了Ni掺杂CoSe₂ (NCS)负载的Bi₄Ti₃O₁₂复合光催化材料(NCS/BTO), 并通过X-射线衍射分析证实了NCS选择性负载于BTO的{001}晶面. X-射线光电子能谱证实了Ni掺杂降低了Co活性位点电子密度与d电子填充度, 从而实现了其d带中心上移. 这种能带演变规律可以通过紫外光电子能谱对价带位置的变化分析得到进一步验证. H₂程序升温脱附结果表明, 改性后的复合样品对H₂分子的吸附能力更强, 进一步表明Ni掺杂有效强化了CoSe₂助催化剂表面与H质子的相互作用, 从而有利于光生电子向析氢反应中间体的快速迁移. 此外, 电化学测试(线性伏安扫描、瞬态光电流等)、原位开尔文探针力显微镜与瞬态吸收光谱等多项分析共同证实了NCS具备更强的电子捕获能力, 可显著抑制光生电子和空穴的复合, 从而使复合材料展现出高效的光催化产氢活性. 优化后NCS/BTO复合材料的产氢速率为197.17 μmol g^-1 h^-1, 相对于纯BTO和CS/BTO样品分别提高了20.1倍和1.8倍.

综上, 本研究建立了过渡金属杂原子掺杂扰动p-d轨道杂化、精准调控非贵金属助催化剂活性位点d带中心的有效策略, 为高效低成本析氢助催化剂的理性设计提供了理论与实验参考.

关键词: 光催化制氢, d带中心, d-p杂化扰动, 异质原子掺杂, 助催化剂

Abstract:

Loading cocatalysts plays a crucial role in enhancing the photocatalytic H₂ evolution performance of semiconductors. However, due to the undesirable electronic configuration of active sites, the H₂ evolution activity of intrinsic cocatalysts remains significantly limited. Herein, we propose a novel strategy for modulating the d-band center (ε_d) of transition metal active sites by transition metal heteroatom doping. The introduced heteroatoms perturb the nonmetal p-band configuration in the cocatalyst and optimize the orbital hybridization between the nonmetal p-band and the d-band of active sites. Such regulation enables precise modulation of the ε_d of active sites and the H* adsorption-desorption equilibrium, thereby ultimately boosting the photocatalytic H₂ evolution performance. This tactic is demonstrated by the Ni-doped CoSe₂ (NCS) cocatalyst and Bi₄Ti₃O₁₂ (BTO) semiconductor. Specifically, the introduction of Ni with higher electronegativity effectively promotes the rearrangement of outer-shell electrons of Co active sites, leading to an upward shift of its ε_d and thereby enhancing the H* adsorption capacity. Accordingly, the sample of BTO loaded with NCS delivers excellent photocatalytic H₂-evolution activity, which is approximately 20.1 and 1.8 times higher than that of pristine BTO and CoSe₂/BTO samples, respectively. This work provides a new insight into the rational design of high-efficiency H₂ evolution cocatalysts.

Key words: Photocatalytic H₂ evolution, d-band center, d-p hybridization perturbation, Heteroatom doping, Cocatalyst

杜仕文, 李全美, 吕娜, 鲁巍, 黄金斗, 张振翼. 镍掺杂扰动p-d轨道杂化调控CoSe₂助催化剂用于高效光催化制氢[J]. 催化学报, 2027, 92: 262-273.

Shiwen Du, Quanmei Li, Na Lu, Wei Lu, Jindou Huang, Zhenyi Zhang. Tailoring the d-band center of CoSe₂ cocatalyst via Ni-doping-induced p-d hybridization perturbation for enhanced photocatalytic H₂ production[J]. Chinese Journal of Catalysis, 2027, 92: 262-273.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65236-9

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图/表 6

Scheme 1. Schematic diagram of the heteroatom doping to optimize the d-band center of active site in cocatalyst by regulating d-p orbital hybridization.

Fig. 1. (a) DOS of bulk CoSe2 and NiSe2. (b) Partial DOS of Co atom in pure CS (111) and NCS (111) slabs. (c) Charge density difference (the yellow color and green color represented the charge accumulation and depletion, respectively) and planar-averaged charge density difference of H absorbed on pure CS and NCS (111) surface and the corresponding Bader charges of H atom. The calculated pCOHP data (d) and chemisorption energy and free energy (e) of H atom absorbed on different catalysts. (f) The schematic illustrating the d-band of Co site in CS and NCS and their optimized antibonding orbital occupancy of Co-Hads. (g) Work functions of different sample slabs. (h) Schematic diagram of photogenerated electron transfer in NCS/BTO heterojunction.

Fig. 2. XRD patterns (a), high-resolution XPS spectra of Co 2p (b) and Ni 2p (c) of different samples. SEM image (d) and HAADF STEM and corresponding EDS elemental mapping images (e) of NCS/BTO sample.

Fig. 3. Photocatalytic H2 evolution amount (a) and H2 evolution rate over different samples (b). Photographs for the viewable H2 bubbles (c) and cycling stability of the photocatalytic H2 evolution activity (d) of the optimized NCS/BTO.

Fig. 4. (a) UPS spectra of pure CoSe2 and Ni-doped CoSe2 samples. H2-TPD spectra (b), LSV polarization (c) and transient photocurrent-time (I-t) curves (d) of the obtained samples. KPFM surface potential profiles of CS/BTO (e) and NCS/BTO samples (f).

Fig. 5. Pseudocolor TA spectra (pump wavelength: 343 nm) (a,d,g), TA kinetic curves (monitored at 625 nm) (b,e,h) and corresponding schematic illustration (c,f,i) of photogenerated-electron relaxation paths of BTO (a,b,c), CS/BTO (d,e,f) and NCS/BTO (g,h,i).

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镍掺杂扰动p-d轨道杂化调控CoSe₂助催化剂用于高效光催化制氢

Tailoring the d-band center of CoSe₂ cocatalyst via Ni-doping-induced p-d hybridization perturbation for enhanced photocatalytic H₂ production

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