锚定在有序大孔In2O3中的协同Pd物种促进太阳能驱动的CO2和H2O转化

doi:10.1016/S1872-2067(25)64919-9

催化学报 ›› 2026, Vol. 82: 238-250.DOI: 10.1016/S1872-2067(25)64919-9

锚定在有序大孔In₂O₃中的协同Pd物种促进太阳能驱动的CO₂和H₂O转化

殷付豪^a^,¹, 张迁宇^a^,¹, 徐茂^a^,¹, 魏书朋^a, 李翊^a, 陈鹏作^a, 赵彦英^b^,^*(), 李本侠^a^,^*()

^a浙江理工大学化学与化工学院, 浙江杭州 310018
^b浙江理工大学材料科学与工程学院, 浙江杭州 310018

收稿日期:2025-07-17 接受日期:2025-10-10 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: libx@zstu.edu.cn (李本侠),yyzhao@zstu.edu.cn (赵彦英).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(22371257);浙江省自然科学基金联合基金(LZY23B030006)

Synergistic Pd species anchored in ordered macroporous In₂O₃ boosting solar-driven CO₂ and H₂O conversion

Fuhao Yin^a^,¹, Qianyu Zhang^a^,¹, Mao Xu^a^,¹, Shupeng Wei^a, Yi Li^a, Pengzuo Chen^a, Yanying Zhao^b^,^*(), Benxia Li^a^,^*()

^aSchool of Chemistry and Chemical Engineering, Zhejiang Sci-Tech University, Hangzhou 310018, Zhejiang, China
^bSchool of Materials Science and Engineering, Zhejiang Sci-Tech University, Hangzhou 310018, Zhejiang, China

Received:2025-07-17 Accepted:2025-10-10 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: libx@zstu.edu.cn (B. Li),yyzhao@zstu.edu.cn (Y. Zhao).
About author:¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22371257);Joint Funds of the Zhejiang Provincial Natural Science Foundation of China(LZY23B030006)

摘要/Abstract

摘要：

实现以水(H₂O)为氢源的高效光催化二氧化碳(CO₂)还原, 关键在于协同优化CO₂还原与H₂O氧化两个半反应之间的电荷与质子转移过程. 然而, 传统研究多集中于单独强化其中一个半反应, 而忽视了两者之间的紧密耦合关系. 合理设计具备多位点协同作用的光催化剂, 对强化CO₂和H₂O同步吸附和活化过程至关重要. 在半导体表面同时构建金属单原子与团簇, 可有效满足复杂反应对于多类活性位点协同催化的需求. 研究表明, 合适的钯(Pd)位点不仅能够促进H₂O分子的吸附与活化, 提供充足的活性氢物种, 还可通过独特的氢溢流效应, 将产生的活性氢快速迁移至邻近吸附的CO₂分子及其反应中间体, 从而推动CO₂高效还原. 因此, 设计并构筑含有多种Pd催化功能中心的光催化剂, 有望显著提升光催化CO₂还原的整体催化性能.

本文利用模板辅助原位热解法合成了负载Pd单原子(Pd₁)的三维有序大孔氧化铟(3DOM In₂O₃), 随后在H₂/Ar混合气氛中进行热处理, 成功构建了Pd₁与Pd团簇(Pd_c)共存的Pd_1+c/3DOM-In₂O₃催化剂. 扫描电镜、高角环形暗场扫描透射电镜及N₂吸脱附测试结果表明, Pd_1+c/3DOM-In₂O₃催化剂具有蜂窝状的三维有序大孔结构, 孔道相互连通, 比表面积显著提升, 且Pd元素分布均匀; X射线光电子能谱、CO吸附漫反射红外傅里叶变换光谱以及X射线吸收谱分析证实, Pd₁和Pd_c在该催化剂中同时存在, 并具有不同的电子结构和配位环境. 光催化实验结果表明, 在模拟太阳光照射(320-1100 nm, 2.0 W cm^-2)且以H₂O为唯一质子与电子供体的条件下, Pd_1+c/3DOM-In₂O₃催化剂展现出优异的CO₂还原性能, CO生成速率达192.52 μmol g^-1 h^-1, 分别为纯3DOM-In₂O₃和仅含Pd₁的Pd₁/3DOM-In₂O₃催化剂的19.8倍和12.2倍. 机理研究揭示, Pd₁和Pd_c共存不仅显著提高了光生载流子的分离与迁移效率, 而且提供了协同催化的活性中心, 能够同步促进CO₂和H₂O分子的吸附和活化. 具体而言, Pd单原子为CO₂选择性转化为CO提供了最佳活性位点; 而Pd团簇不仅能加速H₂O解离以提供丰富的活性氢物种, 还协同增强了CO₂在Pd单原子位点上的吸附和活化. 此外, Pd团簇的局域表面等离子体共振效应显著增强了催化剂在可见至近红外区域的光吸收, 引发催化剂表面温度快速升高. 光催化过程与光热效应的协同作用为CO₂和H₂O向CO的选择性转化提供了更强的热力学驱动力, 从而显著加速了以H₂O为还原剂的光催化CO₂还原反应动力学.

综上, 本工作开发了一种具有金属单原子-团簇协同活性位点的光催化剂, 通过将3DOM结构、Pd₁-Pd_c协同位点以及LSPR效应有机结合, 显著提升了CO₂和H₂O向CO的光催化转化效率; 并深入揭示了金属单原子与团簇在太阳能驱动下对光热耦合过程及表面氧化还原反应的协同作用机制, 为构建新型高效的光热催化体系提供了新的设计思路.

关键词: 光催化二氧化碳还原, 光热效应, Pd物种, 协同活性位点, H₂O活化

Abstract:

Achieving efficient photocatalytic CO₂ reduction using H₂O as a hydrogen source requires the synergistic optimization of both charge and proton transfer between CO₂ reduction and H₂O oxidation half-reactions. However, conventional studies mostly focused on enhancing these half-reactions independently, overlooking the intrinsic interdependence between them. Herein, this work develops a photothermal catalyst (denoted as Pd_1+c/3DOM-In₂O₃) through engineering synergistic Pd single atoms (Pd₁) and Pd clusters (Pd_c) in three-dimensional ordered macroporous (3DOM) In₂O₃ framework. The mechanistic study reveals that the coexistence of Pd single atoms and clusters not only offers synergistic active sites to promote the reaction of CO₂ and H₂O, but also substantially improves the separation and transfer efficiencies of photogenerated electrons and holes. The Pd clusters facilitate H₂O dissociation to ensure an adequate supply of active hydrogen species as well as synergistically enhance the adsorption and activation of CO₂ at Pd single-atom sites. Furthermore, the enhanced photoabsorption in visible and near-infrared regions, attributed to the localized surface plasmon resonance of Pd clusters, leads to a significant increase in catalyst temperature under simulated solar irradiation. The integration of photocatalysis with the photothermal effect affords an intensified driving force for the selective conversion of CO₂ and H₂O into CO, thereby accelerating the reaction kinetics of the overall photocatalytic CO₂ reduction process. As a result, the Pd_1+c/3DOM-In₂O₃ catalyst exhibits excellent performance for solar-driven CO₂ reduction with H₂O vapor, achieving a remarkable CO production rate of 192.52 μmol g^-1 h^-1, which is 19.8-fold and 12.2-fold higher than those of pure 3DOM-In₂O₃ and Pd₁/3DOM-In₂O₃, respectively. This study provides valuable insights into the synergistic effect of metal single atoms and clusters toward both efficient photocatalysis and photothermal effect for solar-driven CO₂ reduction.

Key words: Photocatalytic CO₂ reduction, Photothermal effect, Pd species, Synergistic active sites, H₂O activation

殷付豪, 张迁宇, 徐茂, 魏书朋, 李翊, 陈鹏作, 赵彦英, 李本侠. 锚定在有序大孔In₂O₃中的协同Pd物种促进太阳能驱动的CO₂和H₂O转化[J]. 催化学报, 2026, 82: 238-250.

Fuhao Yin, Qianyu Zhang, Mao Xu, Shupeng Wei, Yi Li, Pengzuo Chen, Yanying Zhao, Benxia Li. Synergistic Pd species anchored in ordered macroporous In₂O₃ boosting solar-driven CO₂ and H₂O conversion[J]. Chinese Journal of Catalysis, 2026, 82: 238-250.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64919-9

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图/表 6

Scheme 1. Schematic illustration of the Pd1+c/3DOM-In2O3 photocatalyst for enhanced conversion of CO2 and H2O into CO.

Fig. 1. Synthesis and microstructure of the Pd1+c/3DOM-In2O3 catalyst. (a) Schematic diagram of the synthesis process. SEM image (b), TEM image (c), HRTEM image (d), and STEM images (e-h) with EDS element mapping images.

Fig. 2. Spectroscopic characterization of Pd1/3DOM-In2O3, Pd1+c/3DOM-In2O3 and Pdn/3DOM-In2O3 samples. XPS spectra of In 3d (a), O 1s (b), and Pd 3d (c). (d) CO-DRIFTS spectra. (e) Normalized Pd K-edge XANES spectra. (f) Fourier-transformed EXAFS spectra of k2-weighted Pd K-edge. (g-j) WT-EXAFS of k2-weighted Pd K-edge.

Fig. 3. Photocatalytic CO2 reduction performance. Evolution rates of products under different conditions: the Pd1+c/3DOM-In2O3(x) catalysts with different Pd/In molar ratios (x%) under UV-vis-NIR irradiation (a), di?erent photocatalysts under UV-vis-NIR irradiation (b), the optimal Pd1+c/3DOM-In2O3 catalyst under di?erent conditions (c), the optimal Pd1+c/3DOM-In2O3 catalyst under UV-vis-NIR irradiation at di?erent controlled temperatures (d), the optimal Pd1+c/3DOM-In2O3 catalyst under di?erent light irradiation and the surface temperature of the catalyst (e), and di?erent controlled conditions (f). (g) Mass spectrum of 13CO produced from 13CO2 photoreduction on the Pd1+c/3DOM-In2O3 catalyst. (h) Cycling test of the Pd1+c/3DOM-In2O3 catalyst in CO2 reduction reaction under UV-vis-NIR light.

Fig. 4. Investigations on H2O adsorption and activation. (a-d) Time-dependent DRIFTS spectra of H2O adsorption and activation on different catalysts. The fitted spectra (e) and peak area proportions (f) for three types of interfacial H2O adsorbed on different catalysts: (I) 3DOM-In2O3, (II) Pd1/3DOM-In2O3, (III) Pd1+c/3DOM-In2O3, and (IV) Pdn/3DOM-In2O3. (g) Fluorescence spectra for detecting ?OH radicals generated during photocatalytic CO2RR in the presence of 0.1 mmol L-1 coumarin. (h) Gibbs free energy profiles of H2O dissociation on different active sites.

Fig. 5. CO2 adsorption and reduction on the photocatalysts. (a) CO2 adsorption isotherms for different catalysts. (b) Apparent activation energy of the photocatalytic CO2RR with H2O on different catalysts. (c) In-situ DRIFTS spectrum during photocatalytic CO2RR on the Pd1+c/3DOM-In2O3 catalyst. (d) Gibbs free energy profiles for CO2 reduction at different sites of the catalysts. (e) Electron localization function of Pd1/3DOM-In2O3 and Pd1+c/3DOM-In2O3. (f) Proposed mechanism for photocatalytic conversion of CO2 and H2O to CO on the Pd1+c/3DOM-In2O3 catalyst.

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锚定在有序大孔In₂O₃中的协同Pd物种促进太阳能驱动的CO₂和H₂O转化

Synergistic Pd species anchored in ordered macroporous In₂O₃ boosting solar-driven CO₂ and H₂O conversion

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