双功能氢氧化物助催化剂在优化二维S型光合成系统耦合CO2还原和H2O氧化能力中的镍钴协同效应

doi:10.1016/S1872-2067(24)60174-9

催化学报 ›› 2025, Vol. 68: 311-325.DOI: 10.1016/S1872-2067(24)60174-9

双功能氢氧化物助催化剂在优化二维S型光合成系统耦合CO₂还原和H₂O氧化能力中的镍钴协同效应

胡灵萱^a^,¹, 张艳^a^,¹, 林倩^a^,¹, 曹凤莹^a, 莫伟豪^a^,^c, 仲淑贤^b, 林红军^b, 谢李燕^a^,^*(), 赵雷洪^a, 柏嵩^a^,^*()

^a浙江师范大学化学与材料科学学院, 先进催化材料教育部重点实验室, 浙江金华 321004
^b浙江师范大学地理与环境科学学院, 浙江金华 321004
^c攀枝花学院生物与化学工程学院, 四川攀枝花 617000

收稿日期:2024-08-20 接受日期:2024-09-24 出版日期:2025-01-18 发布日期:2025-01-02
通讯作者: * 电子信箱: liyanxie@zjnu.edu.cn (谢李燕), songbai@zjnu.edu.cn (柏嵩).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(21603191);浙江省自然科学基金(LQ16B010001);浙江省自然科学基金(LY20B030003);浙江省“尖兵” “领雁”研发公关计划(2022C03069);浙江省“尖兵” “领雁”研发公关计划(2023C03148);浙江省公益技术应用研究(分析测试)计划(2017C37024);金华市科技计划(20204185);国家级大学生创新创业训练计划(202310345024)

Unraveling the Ni-Co synergy in bifunctional hydroxide cocatalysts for better cooperation of CO₂ reduction and H₂O oxidation in 2D S-scheme photosynthetic systems

Lingxuan Hu^a^,¹, Yan Zhang^a^,¹, Qian Lin^a^,¹, Fengying Cao^a, Weihao Mo^a^,^c, Shuxian Zhong^b, Hongjun Lin^b, Liyan Xie^a^,^*(), Leihong Zhao^a, Song Bai^a^,^*()

^aKey Laboratory of the Ministry of Education for Advanced Catalysis Materials, College of Chemistry and Materials Science, Zhejiang Normal University, Jinhua 321004, Zhejiang, China
^bCollege of Geography and Environmental Sciences, Zhejiang Normal University, Jinhua 321004, Zhejiang, China
^cSchool of Biological and Chemical Engineering, Panzhihua University, Panzhihua 617000, Sichuan, China

Received:2024-08-20 Accepted:2024-09-24 Online:2025-01-18 Published:2025-01-02
Contact: * E-mail: liyanxie@zjnu.edu.cn (L. Xie), songbai@zjnu.edu.cn (S. Bai).
About author:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(21603191);Zhejiang Provincial Natural Science Foundation of China(LQ16B010001);Zhejiang Provincial Natural Science Foundation of China(LY20B030003);Key Research and Development Program of Zhejiang Province(2022C03069);Key Research and Development Program of Zhejiang Province(2023C03148);Public Welfare Technology Application Research Plan Project of Zhejiang Province(2017C37024);Foundation of Science and Technology Bureau of Jinhua(20204185);National College Students Innovation and Entrepreneurship Training Program(202310345024)

摘要/Abstract

摘要：

利用太阳能将CO₂和H₂O转化为高附加值化学品或燃料, 为解决温室效应和能源危机提供了一种潜在的解决方案. S型异质结光催化剂因其更宽的光吸收范围、更高的光生电荷分离效率和更强的氧化还原能力有望在该领域发挥重要作用. 但是, 由于S型异质结表面缺乏高活性的氧化还原位点, 其光催化转化CO₂的效率仍然较低. 在异质结的电子富集半导体和空穴富集半导体表面分别引入CO₂还原和H₂O氧化助催化剂, 是解决上述问题的有效方法. 目前所采用的策略主要包括利用半导体表面电子/空穴富集程度的差异来选择性地光沉积助催化剂, 以及构建中空结构的异质结以实现双助催化剂在内外表面的空间分离. 前者主要适用于贵金属助催化剂, 而后者需要复杂的模板法, 均不利于催化剂的大规模制备. 在异质结表面包裹层状过渡金属氢氧化物为实现空间分离的非贵金属CO₂还原和H₂O氧化助催化剂提供了一种简单而有效的方法. 双功能过渡金属氢氧化物不仅可以分别在异质结的电子聚集端和空穴聚集端作为还原CO₂和氧化H₂O的助催化剂, 还能防止包裹的半导体参与副反应, 并保护其免受光腐蚀. 然而, 单一金属位点限制了氢氧化物助催化剂对光催化性能的提升. 通过引入第二种金属位点以产生协同效应, 有望进一步提高其助催化效率.
本文首先制备了由Cu₂O和Fe₂O₃纳米片组成的二维S型Cu₂O/Fe₂O₃ (CF)异质结, 然后在其表面原位生长了具有不同Ni:Co摩尔比的层状镍钴双金属氢氧化物(Ni_xCo_1-_x(OH)₂, x = 1, 0.75, 0.5, 0.25和0), 合成了一系列Cu₂O/Fe₂O₃@Ni_xCo_1-_x(OH)₂(CF@NiCo)催化剂. 原位光照X射线光电子能谱、开尔文探针力显微镜以及电子顺磁共振波谱测试结果表明, 当CF@NiCo受到光激发时, Fe₂O₃的电子与Cu₂O的空穴发生复合. 同时, Cu₂O的电子和Fe₂O₃的空穴分别传输至所负载的Ni_xCo_1-_x(OH)₂助催化剂表面进行CO₂还原和H₂O氧化反应. 光电化学测试、稳态/瞬态荧光光谱、CO₂/水蒸汽吸附/程序升温脱附实验、原位漫反射傅立叶变换红外光谱和密度泛函理论计算结果表明, 适量钴掺入Ni(OH)₂, 不仅能够调控Ni_xCo_1-_x(OH)₂的能带结构, 平衡助催化剂的电子与空穴捕获能力, 提升S型异质结的电荷分离效率, 还通过调控Ni_xCo_1-_x(OH)₂的d带中心, 增强助催化剂表面对CO₂和H₂O的吸附与活化能力, 并显著降低CO₂转化为CO和H₂O转化为O₂过程中限速步骤的能垒. 光催化测试结果表明, CF@NiCo生成CO和O₂的速率以及CO的选择性均随着Ni_xCo_1-_x(OH)₂中Co含量的增加而呈现先增大后减小的趋势. 得益于镍和钴之间的协同效应, 具有最佳镍钴比的CF@Ni_0.75Co_0.25样品能够按照化学计量比还原CO₂和氧化H₂O分子. 在可见光照射下, 该样品生成CO和O₂的产率分别达到552.7和313.0 μmol g_cat^-1 h^-1, 该性能分别是CF的11.3和9.9倍, CF@Ni的1.6和1.7倍, 以及CF@Co的4.5和5.9倍.
综上所述, 利用双功能过渡金属氢氧化物助催化剂的双金属协同效应, 能够有效提升S型异质结在光催化CO₂还原耦合H₂O氧化反应中的性能, 为高性能人工光合成催化剂的设计提供了新的思路.

关键词: 镍钴协同, 双功能助催化剂, CO₂还原, H₂O氧化, 2D/2D异质结, S型光合成系统

Abstract:

Layered transition metal hydroxides show distinct advantages in separately co-catalyzing CO₂ reduction and H₂O oxidation at the electron-accumulating and hole-accumulating sites of wrapped heterojunction photocatalysts, while concurrently preventing side reactions and photocorrosion on the semiconductor surface. Herein, Ni-Co bimetallic hydroxides with varying Ni/Co molar ratios (Ni_xCo_1-_x(OH)₂, x = 1, 0.75, 0.5, 0.25, and 0) were grown in situ on a model 2D/2D S-scheme heterojunction composed of Cu₂O nanosheets and Fe₂O₃ nanoplates to form a series of Cu₂O/Fe₂O₃@Ni_xCo_1-_x(OH)₂ (CF@NiCo) photocatalysts. The combined experimental and theoretical investigation demonstrates that incorporating an appropriate amount of Co into Ni(OH)₂ not only modulates the energy band structure of Ni_xCo_1-_x(OH)₂, balances the electron- and hole-trapping abilities of the bifunctional cocatalyst and maximizes the charge separation efficiency of the heterojunction, but also regulates the d-band center of Ni_xCo_1-_x(OH)₂, reinforcing the adsorption and activation of CO₂ and H₂O on the cocatalyst surface and lowering the rate-limiting barriers in the CO₂-to-CO and H₂O-to-O₂ conversion. Benefiting from the Ni-Co synergy, the redox reactions proceed stoichiometrically. The optimized CF@Ni_0.75Co_0.25 achieves CO and O₂ yields of 552.7 and 313.0 μmol g_cat^-1 h^-1, respectively, 11.3/9.9, 1.6/1.7, and 4.5/5.9-fold higher than those of CF, CF@Ni, and CF@Co. This study offers valuable insights into the design of bifunctional noble-metal-free cocatalysts for high-performance artificial photosynthesis.

Key words: Ni-Co synergy, Bifunctional cocatalyst, CO₂ reduction, H₂O oxidation, 2D/2D heterojunction, S-scheme photosynthetic system

胡灵萱, 张艳, 林倩, 曹凤莹, 莫伟豪, 仲淑贤, 林红军, 谢李燕, 赵雷洪, 柏嵩. 双功能氢氧化物助催化剂在优化二维S型光合成系统耦合CO₂还原和H₂O氧化能力中的镍钴协同效应[J]. 催化学报, 2025, 68: 311-325.

Lingxuan Hu, Yan Zhang, Qian Lin, Fengying Cao, Weihao Mo, Shuxian Zhong, Hongjun Lin, Liyan Xie, Leihong Zhao, Song Bai. Unraveling the Ni-Co synergy in bifunctional hydroxide cocatalysts for better cooperation of CO₂ reduction and H₂O oxidation in 2D S-scheme photosynthetic systems[J]. Chinese Journal of Catalysis, 2025, 68: 311-325.

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图/表 7

Fig. 1. Synthesis and electron-microscopic characterization of CF@NiCo. (a) Schematic illustrating the synthesis of CF@NiCo; TEM (b,c). HRTEM (d), STEM and EDS-mapping (e) images of CF@Ni0.75Co0.25.

Fig. 2. Spectroscopic characterizations of CF@NiCo and reference samples. (a) XRD patterns; (b) UV-vis diffuse reflectance spectra; (c) survey XPS spectra; high-resolution XPS spectra of Cu 2p (d), Fe 2p (e), Ni 2p (f), and Co 2p (g).

Fig. 3. Photocatalytic performance of CF@NiCo. (a) H2, CO, and CH4 evolution rates and CO selectivities of CF and CF@NiCo; (b) comparison of the CO yield and selectivity of CF@Ni0.75Co0.25 with reported Cu2O and Fe2O3 based heterojunctions; (c) mass spectra of the generated 13CO (top) and 13CH4 (bottom) using 13CO2 as the gas source; (d) O2 evolution rates and hole/electron utilization ratios of CF and CF@NiCo; (e) mass spectrum of the generated 18O2 using H218O as the source; (f) recycling tests of CF@Ni0.75Co0.25.

Fig. 4. Charge kinetics analysis of CF@NiCo. Steady-state PL spectra (a), photocurrent densities (b), and average electron lifetimes (c) of CF and CF@NiCo; UPS spectra (d), Tauc plots (e), and energy band structures (f) of Cu2O, Fe2O3, and NixCo1-x(OH)2; (g) schematic illustrating the charge-transfer mechanisms in CF@NiCo samples. In Fig. 4(d)-(g), Ni0.75Co0.25(OH)2, Ni0.5Co0.5(OH)2, and Ni0.25Co0.75(OH)2 are abbreviated as Ni0.75Co0.25, Ni0.5Co0.5, and Ni0.25Co0.75, respectively.

Fig. 5. Charge separation and transfer mechanisms in CF@NiCo. AFM images (left) and KPFM potential images (right) of CF@Ni0.75Co0.25 in the dark (top) and under light irradiation (bottom) (a), and the corresponding line-scanning surface potential curves in the dark and under light irradiation (b); EPR spectra of DMPO-?OH (c) and DMPO-?O2- (d) over Cu2O, Fe2O3, CF and CF@Ni0.75Co0.25 under light irradiation; (e) schematic illustrating the charge separation and transfer mechanism in CF@Ni0.75Co0.25.

Fig. 6. Surface reaction dynamics analysis of CF@Ni, CF@Ni0.75Co0.25, and CF@Co. CO2 (a) and water vapor (d) adsorption isotherms; CO2-TPD (b) and H2O-TPD (e) profiles; LSV curves for CO2 reduction (c) and H2O oxidation (f); (g) in-situ DRIFTS of CF@Ni0.75Co0.25 during CO2 reduction coupled with H2O oxidation.

Fig. 7. DFT calculations on Ni-Co synergistic mechanisms. Charge density difference of Cu2O-NixCo1-x(OH)2 (a) and Fe2O3-NixCo1-x(OH)2 (b) heterointerfaces: Ni(OH)2 (left), Ni0.75Co0.25(OH)2 (middle), and Co(OH)2 (right) (yellow and blue colors represent the electron-accumulation zone and electron-depletion zone, respectively); (c) computed PDOS of Ni(OH)2, Ni0.75Co0.25(OH)2, and Co(OH)2; free energy diagrams and optimized configurations of key intermediates formation for CO2-to-CO reduction (d,e) and H2O-to-O2 oxidation (f,g) over Ni(OH)2, Ni0.75Co0.25(OH)2, and Co(OH) surface (Ni0.75Co0.25(OH)2 is abbreviated as Ni0.75Co0.25 in Figs.7(c), (d) and (f)).

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双功能氢氧化物助催化剂在优化二维S型光合成系统耦合CO₂还原和H₂O氧化能力中的镍钴协同效应

Unraveling the Ni-Co synergy in bifunctional hydroxide cocatalysts for better cooperation of CO₂ reduction and H₂O oxidation in 2D S-scheme photosynthetic systems

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