新型钯-铜纳米点析氢助催化剂: 优化界面氢脱附以实现高效光催化活性

doi:10.1016/S1872-2067(21)63830-5

催化学报 ›› 2022, Vol. 43 ›› Issue (2): 215-225.DOI: 10.1016/S1872-2067(21)63830-5

新型钯-铜纳米点析氢助催化剂: 优化界面氢脱附以实现高效光催化活性

许家超^a, 高朵朵^a, 余火根^a^,^b^,^#(), 王苹^a, 朱必成^b, 王临曦^b^,^*(), 范佳杰^c

^a武汉理工大学化学化工与生命科学学院化学系, 湖北武汉 430070
^b中国地质大学(武汉)材料与化学学院太阳燃料实验室, 湖北武汉 430074
^c郑州大学材料科学与工程学院, 河南郑州 450001

收稿日期:2021-07-30 接受日期:2021-08-27 出版日期:2022-02-18 发布日期:2021-05-20
通讯作者: 余火根,王临曦
基金资助:
国家自然科学基金(51872221);国家自然科学基金(21771142);国家自然科学基金(22075220);中央高校基础研究经费(WUT 2019IB002)

Palladium-copper nanodot as novel H₂-evolution cocatalyst: Optimizing interfacial hydrogen desorption for highly efficient photocatalytic activity

Jiachao Xu^a, Duoduo Gao^a, Huogen Yu^a^,^b^,^#(), Ping Wang^a, Bichen Zhu^b, Linxi Wang^b^,^*(), Jiajie Fan^c

^aDepartment of Chemistry, School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, Hubei, China
^bLaboratory of Solar Fuel, Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430074, Hubei, China
^cSchool of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450002, Henan, China

Received:2021-07-30 Accepted:2021-08-27 Online:2022-02-18 Published:2021-05-20
Contact: Huogen Yu, Linxi Wang
Supported by:
This work was supported by the National Natural Science Foundation of China(51872221);This work was supported by the National Natural Science Foundation of China(21771142);This work was supported by the National Natural Science Foundation of China(22075220);the Fundamental Research Funds for the Central Universities(WUT 2019IB002)

摘要/Abstract

摘要：

助剂修饰是提高单相光催化剂催化制氢活性的有效策略之一. 贵金属Pt是光催化制氢体系中较为理想的助催化剂, 但价格高、储量少, 严重限制了其广泛应用. 在过去几十年中, 研究者研发了一系列低成本的非Pt助催化剂, 如金属氧化物、碳化物、氮化物、硫化物和磷化物等, 并应用于光催化制氢, 但其催化活性与Pt助催化剂相比有较大差距. 近年来, 与Pt具有相似的物化性质,但价格较低的其他铂族金属得到了广泛关注和研究.
贵金属Pd不仅具有良好的导电性和稳定性, 而且相对于Pt, Pd的储量更丰富且廉价(Pd: 124.9元/克, Pt: 224.8元/克), 因而被认为是一种很有应用前景的析氢助催化剂. 然而, Pd金属助剂在实际应用中的析氢活性并不理想, 主要是因为Pd对氢原子(H)的吸附强度过高, 严重限制了后续的氢脱附过程, 导致材料整体的析氢反应速率较慢. 因此, 发展合适的方法来优化Pd的电子结构以弱化其对氢的吸附强度, 对进一步提升Pd助剂的催化析氢活性具有重要意义.
本文通过一种简易的NaH₂PO₂介导的共沉积策略, 成功地将过渡金属Cu引入金属Pd的晶格中, 并通过Pd-Cu合金化作用弱化了Pd对氢的吸附强度, 进而有效提高界面H₂释放速率. 通过X射线衍射、高分辨率透射电镜、X射线光电子能谱和电感耦合等离子体等技术对Pd_100-_xCu_x合金的结构和形貌进行了分析. 结果表明, Pd_100-_xCu_x合金纳米点(2-5 nm)成功修饰于TiO₂表面, 所得的Pd_100-_xCu_x/TiO₂光催化剂表现出显著增强的光催化制氢性能. 其中, Pd₇₅Cu₂₅/TiO₂样品的催化性能达到269.2 μmol h ^-1, 是纯TiO₂的90倍. 此外, 原位X射线光电子能谱和密度泛函理论的结果表明, 所形成的Pd_100-_xCu_x合金纳米点因其自身优异的导电性可以有效促进光生电荷的分离; 同时, Cu的成功引入弱化了Pd对氢的吸附强度, 从而促进了Pd₇₅Cu₂₅合金上的氢解吸过程, 最终有效提升了光催化剂的制氢活性. Pd₇₅Cu₂₅合金对H吸附强度降低的原因是: 引入弱电负性的Cu元素后, Cu的部分电子转移至Pd上形成富电子的Pd, 进而降低了Pd对H的吸附强度. 本文通过优化电子结构以促进界面反应活性的策略为开发高效光催化剂提供了新的见解.

关键词: 光催化产氢, 二氧化钛, Pd_100-_xCu_x合金, 富电子Pd, 氢脱附

Abstract:

Noble metal palladium (Pd) is well-known as excellent photocatalytic cocatalyst, but its strong adsorption to hydrogen causes its limited H₂-evolution activity. In this study, the transition metal Cu was successfully introduced into the metallic Pd to weaken its hydrogen-adsorption strength to improve its interfacial H₂-evolution rate via the Pd-Cu alloying effect. Herein, the ultrasmall Pd_100-_xCu_x alloy nanodots (2-5 nm) as a novel H₂-evolution cocatalyst were integrated with the TiO₂ through a simple NaH₂PO₂-mediated co-deposition route. The resulting Pd_100-_xCu_x/TiO₂ sample shows the significantly enhanced photocatalytic H₂-generation performance (269.2 μmol h ^-1), which is much higher than the bare TiO₂. Based on in situ irradiated X-ray photoelectron spectroscopy (ISI-XPS) and density functional theory (DFT) results, the as-formed Pd_100-_xCu_x alloy nanodots can effectively promote the separation of photo-generated charges and weak the adsorption strength for hydrogen to optimize the process of hydrogen-desorption process on Pd₇₅Cu₂₅ alloy, thus leading to high photocatalytic H₂-evolution activity. Herein, the weakened H adsorption of Pd₇₅Cu₂₅cocatalyst can be ascribed to the formation of electron-rich Pd after the introduction of weak electronegativity Cu. The present work about optimizing electronic structure for promoting interfacial reaction activity provides a new sight for the development of the highly efficient photocatalysts.

Key words: Photocatalytic H₂ evolution, TiO₂, Pd_100-xCu_xalloy, Electron-rich Pd, Hydrogen desorption

许家超, 高朵朵, 余火根, 王苹, 朱必成, 王临曦, 范佳杰. 新型钯-铜纳米点析氢助催化剂: 优化界面氢脱附以实现高效光催化活性[J]. 催化学报, 2022, 43(2): 215-225.

Jiachao Xu, Duoduo Gao, Huogen Yu, Ping Wang, Bichen Zhu, Linxi Wang, Jiajie Fan. Palladium-copper nanodot as novel H₂-evolution cocatalyst: Optimizing interfacial hydrogen desorption for highly efficient photocatalytic activity[J]. Chinese Journal of Catalysis, 2022, 43(2): 215-225.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63830-5

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Fig. 1. Schematic diagram illustrating the controllable preparation for Pd100-xCux/TiO2 photocatalyst.

Fig. 2. XRD patterns (a) and the slow-scan patterns (b) of metal PdCu for various samples. (1) TiO2; (2) Pd95Cu5/TiO2; (3) Pd75Cu25/TiO2; (4) Pd55Cu45/TiO2.

Fig. 3. TEM (a,b) and HRTEM (c) images of Pd75Cu25/TiO2 photocatalyst; (d) HAADF-STEM and its EDS mapping images; (e) The corresponding line-scan results of single Pd75Cu25 nanodot.

Fig. 4. XPS survey spectra (a) and high-resolution XPS spectra of Pd 3d (b), Cu 2p (c) for TiO2 (1), Pd95Cu5/TiO2 (2), Pd75Cu25/TiO2 (3) and Pd55Cu45/TiO2 (4).

Fig. 5. UV-vis spectra for TiO2 (1), Pd100Cu0/TiO2 (2), Pd95Cu5/TiO2 (3), Pd75Cu25/TiO2 (4), and Pd55Cu45/TiO2 (5).

Fig. 6. (a) The photocatalytic H2-generation rate of various samples: (1) TiO2; (2) Pd100Cu0/TiO2; (3) Pd95Cu5/TiO2; (4) Pd75Cu25/TiO2; (5) Pd55Cu45/TiO2; (6) Pd37Cu63/TiO2; (7) Pd25Cu75/TiO2. (b) photocatalytic H2-generation cycling tests of Pd75Cu25/TiO2 sample; (c) Proposed photocatalytic H2-generation mechanism of the Pd100-xCux nanodot-modified TiO2 photocatalyst.

Fig. 7. ISI-XPS spectra of Ti 2p (a) and Pd 3d (b) for the Pd75Cu25/TiO2 sample; (c) Schematic diagrams for the electron transfer of the Pd75Cu25/TiO2.

Fig. 8. Theoretical calculations of the HER activation energy of the Pd75Cu25 alloy. (a) Atomic configurations of the water-dissociation step on the surface of the Pd75Cu25 alloy. Color codes: blue and deep orange represent Pd and Cu atoms, while red and green represent O and H atoms in a single H2O molecule, respectively; (b) Calculated water-dissociation barriers diagram; (c) Calculated Free energies of H adsorption diagram.

Fig. 9. Bulk model of Pd75Cu25 alloy (a) and corresponding charges transformation (b) obtained from Bader charge analysis; (c) XPS results of Pd element in the Pd100Cu0/TiO2 and Pd75Cu25/TiO2 samples.

Fig. 10. Transient-state photoluminescence spectra (a), linear sweep voltammetry curves (b), transient photocurrent responses (c) and electrochemical impedance spectra (d) for TiO2 (1), Pd100Cu0/TiO2 (2), and Pd75Cu25/TiO2 (3).

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新型钯-铜纳米点析氢助催化剂: 优化界面氢脱附以实现高效光催化活性

Palladium-copper nanodot as novel H₂-evolution cocatalyst: Optimizing interfacial hydrogen desorption for highly efficient photocatalytic activity

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新型钯-铜纳米点析氢助催化剂: 优化界面氢脱附以实现高效光催化活性

Palladium-copper nanodot as novel H2-evolution cocatalyst: Optimizing interfacial hydrogen desorption for highly efficient photocatalytic activity

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Palladium-copper nanodot as novel H₂-evolution cocatalyst: Optimizing interfacial hydrogen desorption for highly efficient photocatalytic activity