TiO2上原子分散的Fe位点促进光催化CO2还原: 增强的催化活性、 DFT计算和机制洞察

doi:10.1016/S1872-2067(23)64484-5

催化学报 ›› 2023, Vol. 51: 145-156.DOI: 10.1016/S1872-2067(23)64484-5

TiO₂上原子分散的Fe位点促进光催化CO₂还原: 增强的催化活性、 DFT计算和机制洞察

李嘉明¹, 李源¹, 王小田, 杨直雄, 张高科^*()

武汉理工大学矿物资源加工与环境湖北省重点实验室, 硅酸盐建筑材料国家重点实验室, 湖北武汉430070

收稿日期:2023-05-18 接受日期:2023-06-28 出版日期:2023-08-18 发布日期:2023-09-11
通讯作者: *电子信箱: gkzhang@whut.edu.cn (张高科).
作者简介:第一联系人：¹共同第一作者.
基金资助:
深圳市科技规划项目(JCYJ20200109150225155);国家自然科学基金(92163125)

Atomically dispersed Fe sites on TiO₂ for boosting photocatalytic CO₂ reduction: Enhanced catalytic activity, DFT calculations and mechanistic insight

Jiaming Li¹, Yuan Li¹, Xiaotian Wang, Zhixiong Yang, Gaoke Zhang^*()

Hubei Key Laboratory of Mineral Resources Processing and Environment, State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070, Hubei, China

Received:2023-05-18 Accepted:2023-06-28 Online:2023-08-18 Published:2023-09-11
Contact: *E-mail: gkzhang@whut.edu.cn (G. Zhang).
About author:First author contact:¹Contributed equally to this work.
Supported by:
Science and Technology Planning Project of Shenzhen Municipality(JCYJ20200109150225155);National Natural Science Foundation of China(92163125)

摘要/Abstract

摘要：

光催化CO₂高效、环保地转化为高附加值化工产品(CH₄,CO,CH₃OH等),能够有效降低环境污染并且促进资源利用.商用P25(TiO₂)因其具有无毒、化学稳定性和强氧化还原电位而被广泛研究.然而,TiO₂的带隙高达3.0eV,只有在紫外光激发下才能产生光生载流子,这极大地限制了其在光催化领域的应用.单原子催化剂(SACs)具有金属原子利用率高、选择性高和活性高等优点,可用于精细化工合成、氧还原和污染物降解等催化领域.由于单个原子具有极高的表面自由能,因此如何稳定地保持原子分散,避免原子团聚成为SACs制备和反应过程中的一大挑战.
本文通过简单的负压封装后热解方法实现了Fe在TiO₂表面的原子级分散负载,所制备的Fe SA/TiO₂催化剂展现出高效的光催化CO₂还原性能,并且利用多种表征手段及理论计算研究了TiO₂表面Fe位点促进CO₂高效转化的反应机制.扫描透射电子显微镜高角环形暗场像(HADDF-STEM)表明Fe以单原子形式分散在TiO₂表面.利用X射线吸收光谱研究了10Fe SA/TiO₂的配位情况和价态,结果表明,Fe的平均价态在Fe²⁺和Fe³⁺之间,10Fe SA/TiO₂中存在Fe−O键而不是Fe−Fe键.光电化学性能测试结果表明,Fe单原子的引入有利于光生载流子的分离,提高了可见光的利用率.光催化CO₂还原实验结果表明,最优的10Fe SA/TiO₂催化剂展示了最好的光催化CO₂转化为CO(48.2μmol·g^‒1·h^‒1)和CH₄(113.4μmol·g^‒1·h^‒1)性能,而TiO₂体系仅产生少量CO(2.7μmol·g^‒1·h^‒1). ¹³C同位素标记结果表明,产物中的C来自CO₂的催化转化.通过密度泛函理论计算对Fe单原子引入增强的CO₂还原性能机理进行探究,结果表明,CO₂在Fe位点的吸附能显著高于TiO₂中的Ti位点,Fe SA/TiO₂的d带中心向费米能级的偏移进一步证实了Fe位点的引入促进了催化剂对C1小分子的吸附.CO₂吸附在催化剂表面的差分电荷密度分布表明,Fe SA/TiO₂上的电子沿Ti-O-Fe-C路径快速转移.吉布斯自由能的计算结果表明,Fe SA/TiO₂表面形成*COOH所需能量(0.89eV)明显低于TiO₂(1.51eV),且CO*在Fe位点转化为CHO*和进一步加氢生成CH₄在热力学上都是有利的.采用原位红外对CO₂在催化剂表面反应的中间产物进行检测,结果发现*CO,*COOH,CHO*等中间产物的存在,基于上述研究提出了Fe SA/TiO₂光催化还原CO₂可能的反应路径.综上,本文为设计CO₂转化为高附加值产物的单原子催化剂提供了有效策略.

关键词: 光催化CO₂还原, 负压封装, Fe SA/TiO₂, 单原子催化剂, d带中心

Abstract:

The design of photocatalysts for the stable and efficient photocatalytic reduction of CO₂ without sacrificial agents remains challenging. In this study, Fe atoms were anchored on the surface of TiO₂ with atomic-level dispersion using a novel negative-pressure encapsulation and pyrolysis strategy. The photoelectrochemical test results confirmed that the introduction of single Fe atoms accelerated the separation of photogenerated carriers and enhanced the TiO₂utilization rate of visible light. The optimal catalyst with atomically dispersed Fe showed excellent photocatalytic conversion of CO₂ to CO (48.2 μmol·g^-1·h^-1) and CH₄ (113.4 μmol·g^-1·h^-1), whereas the TiO₂ system produced only trace amounts of CO (2.7 μmol·g^-1·h^-1). The increased CO₂ adsorption energy and movement of the d-band center toward the Fermi level confirmed that single Fe sites were more favorable for the adsorption of CO₂. The differential charge density distribution of CO₂ adsorbed on the catalyst surface confirmed the rapid transfer of electrons along the Ti-O-Fe-C path, and the Gibbs free energy calculation further confirmed that the Fe sites were conducive to reducing the energy barrier required for the reaction. In addition, the key intermediate (*COOH) of CO₂ conversion to CH₄ was detected by in situ diffuse reflectance infrared Fourier transform spectroscopy, and a possible reaction pathway was proposed. This work provides an effective strategy for designing single-atom catalysts that can efficiently reduce CO₂ to high-value-added products.

Key words: Photocatalytic reduction of CO₂, Negative-pressure encapsulation, Fe SA/TiO₂, Single atom catalyst, d-Band center

李嘉明, 李源, 王小田, 杨直雄, 张高科. TiO₂上原子分散的Fe位点促进光催化CO₂还原: 增强的催化活性、 DFT计算和机制洞察[J]. 催化学报, 2023, 51: 145-156.

Jiaming Li, Yuan Li, Xiaotian Wang, Zhixiong Yang, Gaoke Zhang. Atomically dispersed Fe sites on TiO₂ for boosting photocatalytic CO₂ reduction: Enhanced catalytic activity, DFT calculations and mechanistic insight[J]. Chinese Journal of Catalysis, 2023, 51: 145-156.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64484-5

https://www.cjcatal.com/CN/Y2023/V51/I8/145

图/表 6

Fig. 1. XRD patterns (a), Raman spectra (b), and FTIR spectra (c) of TiO2 and Fe SA/TiO2 catalysts. High resolution TEM images (d), HAADF-STEM images (e,f), and corresponding elemental mapping images (g?j) of 10Fe SA/TiO2.

Fig. 2. (a) Normalized XANES spectra at the Fe K-edge of 10Fe SA/TiO2 in comparison with FeO, Cu foil, and Fe2O3 references. (b) Comparison of the Fourier-transformed magnitudes of the experimental Fe K-edge. XPS survey spectra (c) and high-resolution Ti 2p (d), O 1s (e), and Fe 2p (f) XPS spectra of Fe SA/TiO2.

Fig. 3. UV-visible DRS (a), Tauc plot(b), XPS valence band spectrum (c), band structure (d), time-resolved PL spectra (e), and electrochemical impedance spectroscopy (f) of TiO2 and Fe SA/TiO2.

Fig. 4. Production rates of CH4 (a) and CO2 (b) from the photocatalytic reduction of CO2 under full spectrum irradiation within 4 h. Comparison of the photocatalytic property under full spectrum (Insert selective calculation results) (c) and visible light irradiation (d) of TiO2 and Fe SA/TiO2. Conditional control experiment (e) and 13C isotope labeling experiment (f). (g) Cycling performance test of 10Fe SA/TiO2. (h) XRD patterns of fresh and used 10Fe SA/TiO2 catalysts. (i) Comparison of CO2 performance for the photocatalytic reduction of different systems.

Fig. 5. (a) Calculated DOS of TiO2 and Fe SA/TiO2 catalysts with different crystal phases. (b-g) Differential charge density distribution of CO2 adsorbed on TiO2 and Fe SA/TiO2 catalysts.

Fig. 6. (a) CO2 adsorption and temperature-programmed isotherms of TiO2 and Fe SA/TiO2. (b) In situ DRIFTS spectra of 10Fe SAs/TiO2. (c) Schematic diagram of the CO2 reaction path for the surface photocatalytic reduction of 10Fe SAs/TiO2. (d) Gibbs free energy (ΔG) diagrams of CO2 photoreduction to CO and CH4 through different paths over TiO2 and Fe SA/TiO2.

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TiO₂上原子分散的Fe位点促进光催化CO₂还原: 增强的催化活性、 DFT计算和机制洞察

Atomically dispersed Fe sites on TiO₂ for boosting photocatalytic CO₂ reduction: Enhanced catalytic activity, DFT calculations and mechanistic insight

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