在Pt/DUT-67(Zr)表面生成氢物种增强光催化合成氨

doi:10.1016/S1872-2067(26)65110-8

催化学报 ›› 2026, Vol. 88: 247-258.DOI: 10.1016/S1872-2067(26)65110-8

在Pt/DUT-67(Zr)表面生成氢物种增强光催化合成氨

黄芸^a^,^b, 陈奇^a^,^b, 陈月铃^a^,^b, 杨泽锋^a^,^b, 吴炯桦^a^,^c^,^*(), 余济美^b^,^d^,^*(), 吴棱^a^,^b^,^*()

^a 福州大学化学学院, 核生化危害防护国家重点实验室, 福建福州 350116
^b 福州大学化学学院, 能源与环境光催化国家重点实验室, 福建福州 350116
^c 福州大学物理与信息工程学院, 微纳器件与太阳能电池研究所, 福建福州 350116
^d 香港中文大学化学系, 香港新界沙田 999077

收稿日期:2025-12-17 接受日期:2026-02-27 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: JionghuaWu@fzu.edu.cn (吴炯桦),
jimyu@cuhk.edu.hk (余济美),
wuling@fzu.edu.cn (吴棱).
基金资助:
国家自然科学基金(22272026);国家自然科学基金(52102217);高等教育学科创新项目(D16008)

Effective generation of active hydrogen species for nitrogen fixation on Pt/DUT-67(Zr)

Yun Huang^a^,^b, Qi Chen^a^,^b, Yueling Chen^a^,^b, Zefeng Yang^a^,^b, Jionghua Wu^a^,^c^,^*(), Jimmy C. Yu^b^,^d^,^*(), Ling Wu^a^,^b^,^*()

^a State Key Laboratory of Chemistry for NBC Hazards Protection, College of Chemistry, Fuzhou University, Fuzhou 350116, Fujian, China
^b State Key Laboratory of Photocatalysis on Energy and Environment, College of Chemistry, Fuzhou University, Fuzhou 350116, Fujian, China
^c Institute of Micro-Nano Devices and Solar Cells, College of Physics and Information Engineering, Fuzhou University, Fuzhou 350116, Fujian, China
^d Department of Chemistry, Chinese University of Hong Kong, Shatin, New Territories, Hong Kong 999077, China

Received:2025-12-17 Accepted:2026-02-27 Online:2026-09-18 Published:2026-09-05
Supported by:
The National Natural Science Foundation of China(22272026);The National Natural Science Foundation of China(52102217);The Higher Education Discipline Innovation Project(D16008)

摘要/Abstract

摘要：

氨(NH₃)是一种具有广泛应用的重要工业化学品, 既是氮肥的主要原料, 也是制药、制冷剂、塑料和炸药的原料. 哈伯-博世法作为应用最广泛的工业氨合成技术存在操作复杂、设备庞大、能耗高及污染严重的缺陷. 通过温和的光催化法将氮还原为氨, 不仅解决了传统工艺能耗高、污染严重的问题, 而且可以满足对氨的迫切需求. 目前, 对光催化合成氨的研究主要集中在催化剂能带结构的选择和促进氮的吸附和活化上, 而对于氮还原为氨的中间体加氢过程关注较少. 因此, 本研究在强化催化剂氮气吸附活化性能的同时, 重点实现活性氢(H*)物种的稳定高效生成.
本文从光催化固氮(PNRR)的反应机理入手, 分析了MOF光催化固氮所面临的挑战以及相关的修饰改进策略, 结合已有研究成果, 选择了具有良好光催化固氮潜力的DUT-67, 并在其已突破氮的吸附和活化挑战的基础上, 进一步考虑提高其活性氢(H*)的供应. Pt作为卓越的氢活化位点助催化剂, 可降低*H迁移能垒并促进H₂O解离. 并且, 还注意到DUT-67噻吩环上携带孤对电子的独特S原子, 展现出与N原子相当的金属-配体配位能力. 该S原子促进Pt原子以单原子形态高效均匀地分散于DUT-67表面, 从而建立电子传递通路. 首先, 通过光还原策略将Pt引入DUT-67, 制备了一系列不同质量比的Pt/DUT-67复合催化剂. 在模拟日光条件下开展了光催化氨合成实验, 实现了高效的光催化固氮性能78.8 μmol g^‒1 h^‒1. 透射电子显微镜、球差矫正高角度暗场扫描透射电子显微镜及X射线光电子能谱(XPS)结果揭示了规则形态的催化剂中同时具有存在表面的0价Pt簇与高分散的单原子态+4价Pt. XPS与傅里叶变换红外光谱(FT-IR)结果表明, Pt通过与DUT-67结构中的S原子形成配位键而被稳定锚定, 同时锆氧簇中存在丰富的不饱和Zr位点, 可作为氮气的吸附活化中心. 通过一系列光电化学测试, 证实催化剂中的缺陷与原子级分散的Pt⁴⁺能有效增强光生载流子迁移效率. 原位漫反射FT-IR和密度泛函理论结果表明, Pt/DUT-67比DUT-67具有更强的N₂吸附与活化能力, 而Pt簇的存在促进了活性氢的产生, 并且降低N₂以及中间体的氢化能垒. 最后, 基于上述表征和理论计算, 提出一种潜在的光催化固氮机制. 在光照条件下, DUT-67通过脱除部分氧原子形成氧空位与不饱和Zr位点, 从而吸附并活化N₂. 配体上的S原子与Pt⁴⁺形成独特的电子通路, 促进电子转移并加速光生载流子的传输. 同时, Pt簇驱动H₂O氧化生成活性氢物种*H和O₂. 最后, 活化的*N₂中间体协同*H, 在光生电子的作用下还原生成NH₃, 实现光催化固氮过程.
综上, 本文通过光还原策略构筑了Pt/DUT-67复合催化剂, 混合价态Pt⁰/Pt⁴⁺与不饱和Zr中心协同促进了活性氢物种的产生与氮气的配位活化, 从而实现高效光催化固氮, 本文通过多维协同设计, 为后续催化剂的设计提供了独特视角.

关键词: Pt/DUT-67, 铂簇, 铂单原子, 协同效应, 光催化固氮

Abstract:

The generation of active hydrogen species (H*) is an essential step in the photocatalytic conversion of nitrogen molecules (N₂) to ammonia (NH₃). Metal-organic frameworks (MOFs) are versatile porous structures but they do not exhibit sufficient photocatalytic activities for nitrogen fixation. Adding appropriate amounts of noble metal species as a cocatalyst to MOFs can often improve their activities. This work uses a photoreduction strategy to reduce the right amount of Pt⁴⁺ to Pt clusters, and confines the remaining Pt⁴⁺ uniformly onto DUT-67(Zr). This is realized by taking advantage of a unique Pt-S electron channel, and the unsaturated Zr sites are concurrently in-situ generated under light exposure. The unsaturated Zr sites adsorb and activate N₂, while the Pt clusters are involved in the water splitting process on DUT-67(Zr) to generate more H*, leading to continuous H* supply that would speed up the catalytic hydrogenation of nitrogen intermediate NH_x. The Pt-S electronic channel formed between highly dispersed single atoms Pt and DUT-67(Zr) facilitates the separation and transfer of photo-generated charge carriers. Consequently, with the synergistic effect of unsaturated Zr sites, Pt clusters and Pt-S electron channels, a high photocatalytic nitrogen fixation performance of 78.8 μmol g^‒1 h^‒1 can be achieved. This is 10.4 times higher than that of the sample DUT-67-L with only unsaturated Zr sites and no Pt loading. This work provides an insight to rational design of uniform dispersed precious metal-based MOF photocatalyst for efficient photocatalytic ammonia synthesis.

Key words: Pt/DUT-67, Pt clusters, Pt single atoms, Synergistic effect, Photocatalytic nitrogen fixation

黄芸, 陈奇, 陈月铃, 杨泽锋, 吴炯桦, 余济美, 吴棱. 在Pt/DUT-67(Zr)表面生成氢物种增强光催化合成氨[J]. 催化学报, 2026, 88: 247-258.

Yun Huang, Qi Chen, Yueling Chen, Zefeng Yang, Jionghua Wu, Jimmy C. Yu, Ling Wu. Effective generation of active hydrogen species for nitrogen fixation on Pt/DUT-67(Zr)[J]. Chinese Journal of Catalysis, 2026, 88: 247-258.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65110-8

https://www.cjcatal.com/CN/Y2026/V88/I9/247

图/表 8

Fig. 1. (A,B) SEM images, (C) EDS elemental mappings (C: red, O: green, Zr: cyan, S: yellow, Cl: blue, Pt: pink), (D,E) AC-HAADF-STEM images of 5%Pt/DUT-67.

Fig. 2. (A) O 1s, (B) EPR, (C) Zr 3d, (D) S 2p XPS spectra of DUT-67 and 5%Pt/DUT-67. (E) Pt 4f XPS spectrum of 5%Pt/DUT-67. (F) Relative content of Pt with different valence states.

Fig. 3. (A) Magnified view of high wavenumber region. (B) FT-IR spectra of DUT-67 and 5%Pt/DUT-67. (C) Magnified view of low wavenumber region.

Fig. 4. (A) UV-Vis DRS spectra, (B) Tauc plots, (C) Band structure diagram, (D) Valence band XPS spectra of DUT-67 and 5%Pt/DUT-67. (E) N2 adsorption-desorption isotherms. (F) Pore size distribution curves.

Fig. 5. (A) Photocatalytic nitrogen fixation activity of various catalysts. (B) Eight cyclic stability tests of 5%Pt/DUT-67. (C) Time-dependent ammonia yield (0-8 h). (D) Activity of 5%Pt/DUT-67 under different reaction atmospheres. (E) 1H NMR spectra of NH4+ from 14N2 and 15N2. (F) GC signals of N2 and O2. (G) Activity comparison with reported catalysts.

Fig. 6. A) In-situ DRIFT spectra under dark atmosphere, (B) In-situ DRIFT spectra under irradiation, (C) PL spectra, (D) TRPL spectra, (E) Transient photocurrent curves, (F) EIS Nyquist plots.

Fig. 7. (A) Contact angle results of DUT-67 and 5%Pt/DUT-67. (B) Catalytic activity in N2-H2 mixed atmosphere. (C) Activity after adding TBA radical scavenger. (D) Gibbs free energy profiles of different reaction pathways. (E) Gibbs free energy for photocatalytic nitrogen fixation.

Fig. 8. Schematic diagram of the mechanism for photocatalytic nitrogen fixation on Pt/DUT-67.

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在Pt/DUT-67(Zr)表面生成氢物种增强光催化合成氨

Effective generation of active hydrogen species for nitrogen fixation on Pt/DUT-67(Zr)

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