CuxP/g-C3N4异质结催化剂Cu和P双位点协同光催化C-C偶联制备C2H4

doi:10.1016/S1872-2067(24)60183-X

催化学报 ›› 2025, Vol. 69: 58-74.DOI: 10.1016/S1872-2067(24)60183-X

Cu_xP/g-C₃N₄异质结催化剂Cu和P双位点协同光催化C-C偶联制备C₂H₄

温东晓^a, 王楠^a, 彭嘉禾^b, 真嶋哲朗^a^,^c, 江吉周^b^,^*()

^a华中科技大学化学化工学院, 能量转化与存储材料化学教育部重点实验室, 湖北武汉 430074, 中国
^b武汉工程大学材料科学与工程学院, 国家磷资源开发利用工程技术研究中心, 绿色化工过程教育部重点实验室, 湖北武汉 430205, 中国
^c大阪大学科学产业研究所, 大阪, 日本

收稿日期:2024-09-06 接受日期:2024-10-15 出版日期:2025-02-18 发布日期:2025-02-10
通讯作者: *电子信箱: 027wit@163.com (江吉周).
基金资助:
国家自然科学基金(62004143);国家自然科学基金(21976063);湖北省重点研发计划(2022BAA084)

Collaborative photocatalytic C-C coupling with Cu and P dual sites to produce C₂H₄ over Cu_xP/g-C₃N₄ heterojunction

Dongxiao Wen^a, Nan Wang^a, Jiahe Peng^b, Tetsuro Majima^a^,^c, Jizhou Jiang^b^,^*()

^aKey Laboratory of Material Chemistry for Energy Conversion and Storage, Ministry of Education, School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074, Hubei, China
^bKey Laboratory of Green Chemical Engineering Process of Ministry of Education, Engineering Research Center of Phosphorus Resources Development and Utilization of Ministry of Education, School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430205, Hubei, China
^cThe Institute of Scientific and Industrial Research (SANKEN), Osaka University, Ibaraki, Osaka, 567-0047, Japan

Received:2024-09-06 Accepted:2024-10-15 Online:2025-02-18 Published:2025-02-10
Contact: *E-mail: 027wit@163.com (J. Jiang).
Supported by:
National Natural Science Foundation of China(62004143);National Natural Science Foundation of China(21976063);Key R&D Program of Hubei Province(2022BAA084)

摘要/Abstract

摘要：

作为石油化工的基本原料, 乙烯(C₂H₄)广泛应用于水果成熟、药物合成、高科技材料生产和生态农业实践. 传统的C₂H₄生产通常是通过煤基化学得到. 然而, 由于原料稀缺、生产工艺复杂、成本高、选择性差以及碳排放等问题, 煤基化学生产C₂H₄面临挑战. 作为一种可持续、低成本的替代方案, 光驱动二氧化碳还原反应(CO₂RR)正成为一种将温室气体CO₂转化为增值燃料的理想方法.然而, 尽管在过去的几十年里, 人们在光催化CO₂RR方面做了较多努力, 但在实现其高活性和选择性方面仍存在巨大挑战. 在大多数已报道的光催化CO₂RR中, 由于C1产物在动力学上的优势, 主要得到的通常为CO, CH₄, HCOOH, HCOH等C1产物. 通过C−C耦合过程将CO₂转化为C2+化合物, 不仅需要进一步将*CO中间体氢化, 更需要克服比形成“C−H”和“C−O”慢得多的动力学障碍和更高的能垒. 因此, 通过光驱动的CO₂RR将CO₂和H₂O直接高活性和选择性的转化为高能量密度的C₂H₄燃料仍是一个重大挑战.

本文基于理论计算预测了Cu₃P/g-C₃N₄异质结的光催化电子转移能力, 及其CO₂和H₂O分子的吸附能力, 并以NaH₂PO₂·H₂O为磷源, 原位磷化Cu-g-C₃N₄制备了Cu_xP/g-C₃N₄异质结用于光催化CO₂RR. 通过X射线粉末衍射、红外光谱和拉曼光谱证实了得到的Cu_xP/g-C₃N₄中的Cu_xP主要由Cu₃P组成. X射线光电子能谱结果进一步证明了Cu_xP与g-C₃N₄的成功杂化. 扫描电镜、高分辨透射电镜、电感耦合等离子体-原子发射光谱、元素分析和氮气等温吸附-脱附曲线结果表明, 原位磷化制备的Cu_xP/g-C₃N₄为Cu_xP纳米颗粒与g-C₃N₄纳米片紧密结合并均匀分布在其表面的多孔纳米材料. 光催化CO₂RR活性实验结果表明, 制备的Cu_xP/g-C₃N₄实现了协同光催化CO₂和H₂O转化生成CO和C₂H₄作为主要产物. 值得注意的是, 由Cu_xP/g-C₃N₄产生的C₂H₄产物的选择性达到了64.25%, 是Cu_xP(6.52%)的9.85倍. 同位素标记¹³CO₂RR测试和对照实验结果表明, 这些产物主要来自CO₂的还原, 而不是其他可能的碳源. 紫外-可见漫反射光谱结果表明, Cu_xP的复合使Cu_xP/g-C₃N₄在紫外可见-近红外光谱范围内具有较好的光吸收能力. 光电性能测试和时间分辨光致发光光谱结果表明, 复合型Cu_xP/g-C₃N₄异质结中光生载流子分离效率显著提高. 时间分辨荧光光谱、飞秒瞬态吸收光谱测试验证了Cu_xP/g-C₃N₄异质结中的超快速界面电子传输机制. g-C₃N₄导带上大部分光生e⁻在超强的界面内建电场作用下超快的转移到Cu_xP的导带上, 增加了Cu_xP/g-C₃N₄异质结表面有效光生e⁻的寿命, 促进了光催化CO₂转化率的提高. 原位辐照X射线光电子能谱结果直接验证了在CO₂RR过程中这些长寿命光生e⁻从g-C₃N₄向Cu_xP的超快转移过程. 此外, H₂O吸附实验证实了Cu_xP对H₂O分子的强亲和力. 密度泛函理论计算结果表明, 这些被吸附的H₂O分子在P位点裂解生成*H, 且g-C₃N₄的存在使杂化后的Cu_xP/g-C₃N₄具有适度的加氢能力, 促进了CO₂RR过程中的多步加氢反应过程. 黑暗条件下的原位漫反射红外光谱结果为H₂O和CO₂分子的共吸附提供了直接证据. 在Cu_xP/g-C₃N₄光催化还原CO₂过程中原位漫反射红外光谱检测到了*COOH, *CO, *CHO, *CH₃O和*CH_x吸附态中间体, 基于这些中间体, DFT计算优化后的CO₂RR过程结果表明, 由于受g-C₃N₄影响和调制的不对称Cu和P双位点的存在, 使得在Cu_xP/g-C₃N₄表面生成的*CHO在能量上有利于C−C耦合形成*CHOCHO中间体, 该耦合的中间体可进一步接受激发的光生e⁻和*H, 深度还原生成C₂H₄.

综上所述, 本文利用原位磷化策略制备了Cu_xP/g-C₃N₄异质结用于光催化CO₂高选择性转化为C₂H₄. 结合实验和DFT计算结果详细阐明了Cu_xP/g-C₃N₄异质结催化剂在光反应(电子转移过程)和催化CO₂RR反应(C-C偶联和氢化)过程中的机制. 该发现为开发基于Cu_xP的异质结催化剂通过光驱动CO₂RR将CO₂转化为C2+增值燃料提供了有价值的参考.

关键词: 光催化CO₂还原, C-C偶联, 乙烯, Cu_xP/g-C₃N₄异质结

Abstract:

Light-driven CO₂ reduction reaction (CO₂RR) to value-added ethylene (C₂H₄) holds significant promise for addressing energy and environmental challenges. While the high energy barriers for *CO intermediates hydrogenation and C−C coupling limit the C₂H₄ generation. Herein, Cu_xP/g-C₃N₄ heterojunction prepared by an in-situ phosphating technique, achieved collaborative photocatalytic CO₂ and H₂O, producing CO and C₂H₄ as the main products. Notably, the selectivity of C₂H₄ produced by Cu_xP/g-C₃N₄ attained to 64.25%, which was 9.85 times that of Cu_xP (6.52%). Detailed time-resolution photoluminescence spectra, femtosecond transient absorption spectroscopy tests and density functional theory (DFT) calculation validate the ultra-fast interfacial electron transfer mechanism in Cu_xP/g-C₃N₄ heterojunction. Successive *H on P sites caused by adsorbed H₂O splitting with moderate hydrogenation ability enables the multi-step hydrogenation during CO₂RR process over Cu_xP/g-C₃N₄. With the aid of mediated asymmetric Cu and P dual sites by g-C₃N₄ nanosheet, the produced *CHO shows an energetically favorable for C−C coupling. The coupling formed *CHOCHO further accepts photoexcited efficient e⁻ and *H to deeply produce C₂H₄ according to the C2+ intermediates, which has been detected by in-situ diffuse reflectance infrared Fourier transform spectroscopy and interpreted by DFT calculation. The novel insight mechanism offers an essential understanding for the development of Cu_xP-based heterojunctions for photocatalytic CO₂ to C2+ value-added fuels.

Key words: Photocatalytic CO₂ reduction, C-C coupling, Ethylene, Cu_xP/g-C₃N₄ heterojunction

温东晓, 王楠, 彭嘉禾, 真嶋哲朗, 江吉周. Cu_xP/g-C₃N₄异质结催化剂Cu和P双位点协同光催化C-C偶联制备C₂H₄[J]. 催化学报, 2025, 69: 58-74.

Dongxiao Wen, Nan Wang, Jiahe Peng, Tetsuro Majima, Jizhou Jiang. Collaborative photocatalytic C-C coupling with Cu and P dual sites to produce C₂H₄ over Cu_xP/g-C₃N₄ heterojunction[J]. Chinese Journal of Catalysis, 2025, 69: 58-74.

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图/表 9

Fig. 1. DFT calculated work function (Φ) and corresponding electronic structure of g-C3N4 (a), Cu3P (b), and Cu3P/g-C3N4 (c). Charge density difference (d,e) and the mechanism of Φ tuning (f) of Cu3P/g-C3N4. The selected two Cu atom sites (Cu1, Cu2) on Cu3P and Cu3P/g-C3N4 (g). Calculated H2O and CO2 molecules adsorption energy on the different active sites of Cu3P (h) and Cu3P/g-C3N4 (i).

Fig. 2. Rotes of preparation for CuxP/g-C3N4 (a). XRD patterns (b), FTIR (c), Raman spectra (d), HR-XPS spectra of N 1s (e), Cu 2p (f), and P 2p (g) of different photocatalyst.

Fig. 3. SEM (a), TEM (b) and HR-TEM (c,d), HAADF (e-g) and corresponding EDX elemental mapping (h) images of CuxP/g-C3N4. Blue and pink circles in (d) refer to Cu3P with (e) d = 0.21 nm (300), (f) d = 0.19 nm (113), and CuP2 with (g) d = 0.29 nm (-112) respectively.

Fig. 4. Time profiles of the evolution of CO (a), C2H4 (b), and CH4 (c), and r values and product selectivity (d) of different photocatalyst. Different mass ratio of NaH2PO2·H2O:Cu-g-C3N4 (wt%) effect in CuxP/g-C3N4 during photocatalytic CO2RR (e). Time profiles of the productions during the photocatalytic CO2RR using CuxP/g-C3N4 for five consecutive runs (f).

Fig. 5. UV-vis DRS spectra (a) and (inset) Tauc-plots of (αhv)2 vs. energy of the exciting energy. UPS spectra (b), photocurrent responses (c), PL (d) and TR-PL (e) spectra with excitation at 340 nm of different photocatalyst, and the proposed electron transfer mechanism based on the band structures (f).

Fig. 6. The in-situ irradiated HR-XPS spectra of C 1s (a), N 1s (b), Cu 2p (c), and P 2p (d) of CuxP/g-C3N4

Fig. 7. 2D pseudo-color maps of fs-TA spectra (a,d,g), transient fs-TA spectra (b,e,h), kinetic time profiles (c,f,i) of normalized transient absorption at 462 nm, and the decay pathways (j) of photogenerated e- in g-C3N4, CuxP and CuxP/g-C3N4 under 340 nm laser pulse irradiation.

Fig. 8. CO2-TPD results (a), adsorption kinetic adsorption-desorption (b) of D2O at 2536 cm?1. The in-situ DRIFTS spectra of adsorbed CO2 and H2O under dark (c), and photocatalytic CO2RR under light irradiation (d) over CuxP/g-C3N4.

Fig. 9. DFT calculations. Free energy diagram of water splitting (a) over Cu3P and Cu3P/g-C3N4. CO2RR pathways to produce CO over Cu3P (b) and C2H4 over Cu3P/g-C3N4 (c). Proposed steps with optimized geometric structures in mechanism (d) for photocatalytic CO2 to C2H4 over CuxP/g-C3N4.

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Cu_xP/g-C₃N₄异质结催化剂Cu和P双位点协同光催化C-C偶联制备C₂H₄

Collaborative photocatalytic C-C coupling with Cu and P dual sites to produce C₂H₄ over Cu_xP/g-C₃N₄ heterojunction

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