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化学进展 2020, Vol. 32 Issue (5): 505-518 DOI: 10.7536/PC190938   后一篇

所属专题： 电化学有机合成

• 综述 •

石墨烯基单原子催化剂的合成、表征及分析

祁建磊, 徐琴琴, 孙剑飞, 周丹, 银建中**   

  • 修回日期:2020-01-10 出版日期:2020-05-15 发布日期:2020-02-20
  • 通讯作者: 银建中
  • 基金资助:
    国家自然科学基金项目(U1662130); 国家自然科学基金项目(21978043)
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Synthesis, Characterization and Analysis of Graphene-Supported Single-Atom Catalysts

Jianlei Qi, Qinqin Xu, Jianfei Sun, Dan Zhou, Jianzhong Yin**   

  • Revised:2020-01-10 Online:2020-05-15 Published:2020-02-20
  • Contact: Jianzhong Yin
  • About author:
    ** e-mail:
  • Supported by:
    National Natural Science Foundation of China(U1662130); National Natural Science Foundation of China(21978043)

单原子催化剂具有配位数低、配位环境特殊、原子利用率极高和催化位点高度均一等优点,是沟通均相和异相催化剂之间的桥梁,有助于更好地认识催化反应的本质。本文综述了近年来国内外石墨烯基单原子催化剂的多种合成方法,包括原子层沉积法、浸渍-煅烧法、缺陷捕获法、配位锚定法和其他新颖方法的制备过程、合成原理和表征。在此基础上,本文对石墨烯基金属单原子催化剂在催化方面的性能进行阐述和分析,以期为单原子催化剂制备提供指导和参考。

关键词： 单原子, 催化剂, 石墨烯, 性能与表征, 制备

Single-atom catalyst has the advantages of low coordination number, special coordination environment, high atomic utilization, and high uniformity of catalytic sites. It is the bridge between homogeneous and heterogeneous catalysts, which helps to better understand the nature of catalytic reaction. In this paper, the synthetic methods of graphene-based single-atom catalysts in recent years are reviewed, including atomic layer deposition, impregnation-calcination, defect trapping, coordination anchoring and some other novel methods, with a focus on the preparation process, principle and characterization results of these methods. Based on this, the performance of graphene-based metal single-atom catalysts in catalysis is illustrated and analyzed, and the purpose is to provide guidance and reference for the preparation of single-atom catalysts.

Contents

1 Introduction

2 Synthetic method

2.1 Atomic layer deposition method

2.2 Impregnation-calcination method

2.3 Defect trapping method

2.4 Coordination anchoring method

2.5 Other methods

3 Performance evaluation and characterization

3.1 Hydrogen evolution reaction

3.2 Carbon dioxide reduction reaction

3.3 Oxidation reaction

3.4 Hydrogenation reaction

4 Conclusion and outlook

Key words: single-atom, catalyst, graphene, performance and characterization, preparation
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表1 不同循环次数对应Pt负载的相关参数
Table 1 The related parameters of Pt loading with different cycle times
Carrier Cycle index Partical
size(nm)		 Loading
(wt%)		 ref
rGO 50 0.5 1.52 42
100 1~2 2.67 42
150 2~4 10.5 42
N-doped graphene 50 - 2.1 45
100 - 7.6 45
图1 (a) Pt单原子团簇的HAADF-STEM图[42];(b) Pd单原子的HAADF-STEM图[49];(c) Pt双原子的HAADF-STEM图[51];(d) 原子层沉积法制备单原子示意图[52]
Fig. 1 (a) HAADF-STEM images of Pt atom clusters[42];(b) HAADF-STEM images of Pd atom[49];(c) HAADF-STEM images of Pt diatomics[51];(d) schematic diagram of single atom prepared by atomic layer deposition[52]
图2 (a) Co-NG的HAADF-STEM图[24];(b) Fe/NG 的合成过程示意图[62];(c) Ni-NG/CdS复合材料[26];(d) EDX扫描Ni-NG选定区域内的元素映射[26]
Fig. 2 (a) HAADF-STEM images of Co-NG[24];(b) schematic of the synthesis process of the Fe/NG catalyst[62];(c) the Ni-NG/CdS composite materials[26];(d) EDX elemental mapping of Ni-NG within the selected area[26]
图3 (a) 催化剂的大规模生产[65];(b) Co-NG-MW的制备路线示意图[66]
Fig. 3 (a) The mass production of catalyst[65];(b) Schematic illustration of preparation route to Co-NG-MW[66]
图4 (a) 掺杂镍的纳米多孔石墨烯的制备工艺示意图[76];(b)掺杂镍石墨烯的HAADF-STEM图[76];(c) 单原子催化剂FeN4和FeN5的合成路线[79]
Fig. 4 (a) Schematic illustration of the fabrication process of Ni-doped np-G[76];(b) HAADF-STEM image of Ni-doped graphene[76];(c) synthetic route towards single-atom FeN4 and FeN5 catalysts[79]
图5 (a) 2 mV·s-1扫描速率时NG, Co-G、Co-NG和Pt/C在0.5 M H2SO4中的LSV曲线[24];(b) 不同材料在平衡电势下HER的吉布斯自由能[76];(c) 氮掺杂石墨烯Pt原子构型[45];(d) 不同溶解时间下的材料的XPS图谱[76]
Fig. 5 (a) LSV of NG, Co-G, Co-NG and Pt/C in 0.5 M H2SO4 at scan rate of 2 mV·s-1[24];(b) Gibbs free energy of HER at equilibrium potential for different materials[76];(c) illustration of Pt atoms configurations on N-doped graphene[45];(d) XPS spectra of materials at different dissolution times[76]
表2 不同催化剂析氢反应的过电势
Table 2 Overpotential of hydrogen evolution reaction with different catalysts
Catalyst Electrolyte Overpotential of
10 mA/cm2		 ref
Co-NG 0.5 M H2SO4 147 24
Co-NG-MW 0.5 M H2SO4 175 66
Ni-doped np-G 0.5 M H2SO4 180 76
ALD50Pt/NGNs 0.5 M H2SO4 <50 45
A-Ni@NG 0.5 M H2SO4 70 32
Pt/C 0.5 M H2SO4 50~70 32, 66, 76
图6 (a) 可见光照射下Ni-NG/ CdS、Pt/ CdS、NG/ CdS和纯CdS的光催化产氢率[26];(b) 各类催化剂在氨硼烷水解中的催化活性[51]
Fig. 6 (a) Photocatalytic hydrogen production rate over Ni-NG/CdS, Pt/CdS, NG/CdS and bare CdS under visible light irradiation[26];(b) catalytic activities of various Pt catalysts in AB hydrolysis[51]
图7 (a) Ni-N-MEGO、NiPc, N-MEGO 和MEGO在CO2饱和的0.5 M KHCO3中的LSV曲线[63];(b) 氮配位铁的催化位点的理论计算与提出的机理[62]
Fig. 7 (a) LSV of Ni-N-MEGO, NiPc, N-MEGO and MEGO in CO2 saturated 0.5 M KHCO3 solution[63];(b) theoretical calculations and proposed mechanism on the nitrogen-coordinated Fe catalytic site[62]
图8 每个电势下甲酸的法拉第效率和催化剂的TOF值[65]
Fig. 8 Faradaic efficiencies for formate at each applied potentials and TOF of the catalyst[65]
图9 (a) Pt foil、Pt/C、ALD150Pt/GNS、Pt/GNS、ALD100Pt/GNS、ALD50Pt/GNS在Pt L3边的XANES谱图[42];(b) 单原子Pd1/graphene催化剂丁烯选择性提高的示意图[49];(c) 125 ℃条件下Pd1/N-graphene催化剂24 h耐久性测试实验[67]
Fig. 9 (a) The XANES spectra at Pt L3 edge of Pt foil, Pt/C, ALD150Pt/GNS, Pt/GNS, ALD100Pt/GNS, ALD50Pt/GNS[42];(b) schematic illustration of improvement of butenes selectivity on single atom Pd1/graphene catalyst[49];(c) durability test for the Pd1/N-graphene catalyst for over 24 h at 125 ℃[67]
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