单分散Ni簇锚定在CN上用于高效光催化析氢

doi:10.1016/S1872-2067(21)63865-2

催化学报 ›› 2022, Vol. 43 ›› Issue (2): 536-545.DOI: 10.1016/S1872-2067(21)63865-2

• 论文 • 上一篇

单分散Ni簇锚定在CN上用于高效光催化析氢

蹇亮^a, 张会珍^a, 刘冰^a, 潘成思^a, 董玉明^a^,^*(), 王光丽^a, 钟俊^b, 郑永杰^c, 朱永法^a^,^d^,^#()

^a江南大学化学与材料工程学院, 光响应功能分子材料国家级国际联合研究中心, 江苏无锡 214122
^b苏州大学功能纳米与软材料研究所, 江苏省碳基功能材料与器件重点实验室, 江苏苏州 215123
^c中国冶金地质总局青岛地质勘查院, 山东青岛 266109
^d清华大学化学系, 北京 100084

收稿日期:2021-05-10 接受日期:2021-06-16 出版日期:2022-02-18 发布日期:2021-06-28
通讯作者: 董玉明,朱永法
基金资助:
国家自然科学基金(21676123);国家自然科学基金(21575052);江苏省自然科学基金(BK20161127);江苏省自然科学基金(BK20201345);国家食品科学技术一级学科计划()(JUFSTR20180301);高等学校创新引智计划(111计划)(B13025);江南大学化学与材料工程学院中心实验室基金

Monodisperse Ni-clusters anchored on carbon nitride for efficient photocatalytic hydrogen evolution

Liang Jian^a, Huizhen Zhang^a, Bing Liu^a, Chengsi Pan^a, Yuming Dong^a^,^*(), Guangli Wang^a, Jun Zhong^b, Yongjie Zheng^c, Yongfa Zhu^a^,^d^,^#()

^aInternational Joint Research Center for Photo-responsive Molecules and Materials, School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, Jiangsu, China
^bInstitute of Functional Nano and Soft Materials Laboratory (FUNSOM), Jiangsu Key Laboratory for Carbon-Based Functional Materials & Devices, Soochow University, Suzhou 215123, Jiangsu, China
^cQingdao Geological Exploration Institute of China Metallurgical Geology Bureau, Qingdao 266109, Shandong, China
^dDepartment of Chemistry, Tsinghua University, Beijing 100084, China

Received:2021-05-10 Accepted:2021-06-16 Online:2022-02-18 Published:2021-06-28
Contact: Yuming Dong, Yongfa Zhu
Supported by:
This work was supported by the National Natural Science Foundation of China(21676123);This work was supported by the National Natural Science Foundation of China(21575052);the Natural Science Foundation of Jiangsu Province(BK20161127);the Natural Science Foundation of Jiangsu Province(BK20201345);the National First-class Discipline Program of Food Science and Technology(JUFSTR20180301);MOE & SAFEA for the 111 Project(B13025);Central Laboratory, School of Chemical and Material Engineering, Jiangnan University

摘要/Abstract

摘要：

利用太阳光在常温常压下驱动光催化反应高效进行是解决人类面临的能源、环境问题从而实现绿色化学的理想方案之一. 然而, 兼顾效率、成本和稳定性的高性能光催化体系的研究依然存在巨大的挑战. 石墨氮化碳(g-C₃N₄)基光催化剂由于高稳定性、无毒无害和适合的能带结构, 在光催化制氢方面存在巨大潜力. 然而, 表面的慢反应速率导致了光生电子和空穴的快速复合, 限制了其实际引用. 而助催化剂的负载对光催化反应起着至关重要的作用. 首先, 助催化剂能降低光催化反应的过电势; 其次, 能加快界面的电荷分离和迁移并提供更多的活性位点; 最后, 还可以抑制光腐蚀并且增强光催化剂的稳定性等. 因此, 开发合适的助催化剂提高表面反应速率对高效光催化制氢极为重要.
助催化剂的研究急需新的设计思路, 需要同时满足以下条件: (1)助催化剂定向锚定在半导体的电子富集区域捕获电子; (2)与半导体界面形成强且稳定的界面相互作用转移表面电荷; (3)高度分散的非贵金属助催化剂. 本文以具有天然表面官能团和空隙的超薄氮化碳纳米片作为载体, 设计了光化学还原制备单分散的镍原子簇新策略, 可同时满足沉积在电子富集区域、高度分散的非贵金属、界面结合作用强的要求.
高角度环形暗场扫描透射电镜、X射线吸收近边缘结构和扩展X射线吸收精细结构结果表明, 单分散的过渡金属Ni簇活性位点锚定在石墨氮化碳上. 原位光化学还原沉积法制备单分散的Ni簇锚定在石墨氮化碳表面的复合光催化剂, 可以实现高效的光催化反应制氢活性, 光催化制氢速率达到16.5 mmol·h ^‒1·g ^‒1, 并且展现出461.14 h ^‒1的总周转频率(TOF(H₂))值, 说明单分散的Ni簇提供了大量的活性位点和极大地提高了金属原子利用率. Ni-cluster/CN的C K边缘XAS光谱、N K边缘XAS光谱、XPS光谱和理论计算结果表明, 基底物质石墨氮化碳可与单分散的Ni簇形成强且稳定的界面相互作用, 其中C可充当电子受体, N可充当电子供体. 光致发光光谱、荧光寿命、瞬态光电流、表面光电压和电化学阻抗表明, 强且稳定的界面相互作用有效地促进了光生电子和空穴的分离和迁移. 本文可为原位光沉积法制备单分散稳定的Ni簇助催化剂、研究助催化剂与半导体载体之间稳定的界面相互作用及用于高效光催化反应提供借鉴.

关键词: 单分散Ni簇, 氮化碳, 界面相互作用, 光催化析氢

Abstract:

The active sites of monodisperse transition metal Ni-clusters were anchored on carbon nitride (CN) by an in situ photoreduction deposition method to promote the efficient separation of photogenerated charges and achieve high-efficiency photocatalytic activity for hydrogen evolution. The Ni-cluster/CN exhibited a photocatalytic hydrogen production rate of 16.5 mmol·h ^-1·g ^-1 and a total turnover frequency (TOF (H₂)) value of 461.14 h ^-1. X-ray absorption spectroscopy based on synchrotron radiation indicated that CN had two reaction centers to form stable interface interactions with monodispersed Ni-clusters, in which carbon can act as an electron acceptor, while nitrogen can act as an electron donor. Meanwhile, the hybrid electronic structure of the Ni-cluster/CN system was constructed, which was favorable for photocatalytic activity for hydrogen production. An in-depth understanding of the interfacial interaction between CN and Ni-clusters will have important reference significance on the mechanistic study of development based on the cocatalyst.

Key words: Monodisperse Ni-clusters, Carbon nitride, Interface interaction, Photocatalytic hydrogen evolution

蹇亮, 张会珍, 刘冰, 潘成思, 董玉明, 王光丽, 钟俊, 郑永杰, 朱永法. 单分散Ni簇锚定在CN上用于高效光催化析氢[J]. 催化学报, 2022, 43(2): 536-545.

Liang Jian, Huizhen Zhang, Bing Liu, Chengsi Pan, Yuming Dong, Guangli Wang, Jun Zhong, Yongjie Zheng, Yongfa Zhu. Monodisperse Ni-clusters anchored on carbon nitride for efficient photocatalytic hydrogen evolution[J]. Chinese Journal of Catalysis, 2022, 43(2): 536-545.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63865-2

https://www.cjcatal.com/CN/Y2022/V43/I2/536

图/表 5

Fig. 1. HRTEM (a) and HAADF-STEM (b,c) images of Ni-cluster/CN; (d) Elemental mapping.

Fig. 2. (a) XPS spectrum of Ni-cluster/CN; (b) High-resolution XPS spectrum of Ni 2p; (c) XANES curves of Ni-cluster/CN at the edge of Ni-K and Ni(OH)2 reference spectrum; (d) Corresponding Fourier transform curve of EXAFS spectrum.

Fig. 3. High-resolution XPS spectra of C 1s (a) and N 1s (b) of CN, Ni-cluster/CN and Ni(OH)2NPs/CN; XAS spectra of Ni-cluster/CN and reference samples are located at edge of C K (c) and edge of N K (d); (e) Top view of the model structure calculated by DFT: Ni-N3C2 (Note: DFT calculation was performed on the model structure established by a single Ni atom in Ni-lusters); (f) Differential charge density distribution of Ni-cluster/CN (Note: the yellow and blue areas indicate electron accumulation and consumption, respectively).

Fig. 4. (a) Schematic diagram of the Mott-Schottky contact of Ni-cluster/CN (Φ: work function, EF: Fermi level, EC: conduction band, EV: valence band); (b) Measured work functions via UV photoelectron spectroscopy analysis; (c) Ni 2p high-resolution XPS spectra of Ni(OH)2NPs/CN and Ni-cluster/CN; (d) Photocatalytic HER rate of CN, Ni(OH)2NPs/CN, and Ni-cluster/CN; (e) Cyclic stability experiment of photocatalytic hydrogen evolution; (f) Photocatalytic hydrogen evolution of Ni-cluster/CN driven by sunlight.

Fig. 5. (a) PL spectra of CN and Ni-cluster/CN at 375 nm; (b) Time-resolved photoluminescence spectra; (c) Transient photocurrent response; (d) EIS Nyquist EIS’; (e) Schematic diagram of the interface interaction between Ni-clusters and CN and Ni-cluster/CN photocatalytic reaction hydrogen production mechanism.

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单分散Ni簇锚定在CN上用于高效光催化析氢

Monodisperse Ni-clusters anchored on carbon nitride for efficient photocatalytic hydrogen evolution

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