MOF-derived nanocarbon materials for electrochemical catalysis and their advanced characterization
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摘要: 鉴于对清洁和可持续能源的需求，来自金属有机框架（MOFs）的纳米炭衍生物正崭露头角，成为电催化能量转化的独特催化剂。这些MOF衍生的纳米炭材料不仅保持了MOFs组成可定制和结构多样性等优势，而且在热解过程中可有效防止金属纳米颗粒和金属氧化物的聚集。因此，它们提高了电催化效率，改善了电导率，并在燃料电池和金属-空气电池等绿色能源技术中发挥了关键作用。该综述以MOF衍生碳基材料的炭化机制为起点，随后深入探讨了固有炭缺陷、金属和非金属原子掺杂，并研究了这些材料的合成策略。此外，全面介绍了先进的表征技术，包括原位映射和原位光谱学。最后，对MOF衍生碳基材料作为电催化剂的研究前景提供了见解。该综述的主要目标是为当前MOF衍生碳基电催化剂的状况提供更清晰的视角，鼓励更高效电催化材料的发展。Abstract: Because of the demand for clean and sustainable energy sources, nanocarbons, modified carbons and their composite materials derived from metal-organic frameworks (MOFs) are emerging as distinct catalysts for electrocatalytic energy conversion. These materials not only inherit the advantages of MOFs, like customizable dopants and structural diversity, but also effectively prevent the aggregation of nanoparticles of metals and metal oxides during pyrolysis. Consequently, they increase the electrocatalytic efficiency, improve electrical conductivity, and may play a pivotal role in green energy technologies such as fuel cells and metal-air batteries. This review first explores the carbonization mechanism of the MOF-derived carbon-based materials, and then considers 3 key aspects: intrinsic carbon defects, metal and non-metal atom doping, and the synthesis strategies for these materials. We also provide a comprehensive introduction to advanced characterization techniques to better understand the basic electrochemical catalysis processes, including mapping techniques for detecting localized active sites on electrocatalyst surfaces at the micro- to nano-scale and in-situ spectroscopy. Finally, we offer insights into future research concerning their use as electrocatalysts. Our primary objective is to provide a clearer perspective on the current status of MOF-derived carbon-based electrocatalysts and encourage the development of more efficient materials.
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Key words:
- MOFs /
- Nanocarbon materials /
- Electrochemical catalysis /
- Advanced characterizations
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Figure 1. (a-b) Schematic illustration of the ZIF-8 derived highly graphitized NGPCs. (c) The corresponding rhombic dodecahedron-like structural models of ZIF-8 and NGPCs. (d-e) TEM images of typical ZIF-8 and NGPC polyhedron nanoparticle, respectively[14]. Reproduced with permission. Copyright @ 2014 Royal Society of Chemistry. (f) Schematic illustration of the FA/MOF-5 composites derived highly porous carbon and its corresponding SEM image[17]. Reproduced with permission Copyright © 2008 American Chemical Society. (g) Schematic of the self-assembly process of the ZIF-8 and chitosan aerogel for the formation of ZCCA composite(up) and their corresponding SEM images (bottom)[41]. Reproduced with permission. Copyright @ 2020 Elsevier Ltd.
Figure 2. (a) Synthetic process of the GO/ZIF-67 composites and GO/Co@CN nanosheets. (b) Randomly aligned GO/Co@CN nanosheets with electrode. (c) Horizontally aligned GO/Co@CN nanosheets with electrode. (d) The cross-sectional SEM image and (e) SAED pattern of the HAGO/Co@CN electrodes[19]. Reproduced with permission. Copyright@ 2022 The Royal Society of Chemistry. (f) Schematic illustration of the preparation of the Co@N–HCCs@NG derived from GO/ZIF-67 composites. (g-h) TEM images of Co@N–HCCs@NG. (i) HRTEM image of Co@N–HCCs@NG and (j) SAED pattern of the HAGO/Co@CN electrode[34]. Reproduced with permission. Copyright @ 2021 Elsevier Ltd.
Figure 3. (a) High-angle annular dark-field imaging of various carbon structural defects[36]. Reproduced with permission. Copyright @ 2016 Wiley-VCH GmbH. (b) Scheme of the carbon structural defects[47]. Reproduced with permission. Copyright @ 2016 Wiley-VCH GmbH. (c) DFT calculation of free energy for ORR activities at different defects[48]. Reproduced with permission. Copyright © 2015 American Chemical Society. (d) Volcano plot of both ORR and OER for the adsorption energy of OH* at different carbon defects, (e) free energy diagrams of ORR substeps on C5+7 active site[47]. Reproduced with permission. Copyright @ 2016 Wiley-VCH GmbH. (f) Cyclic voltammetry and ORR performance of carbon structural defects [35]. Reproduced with permission. Copyright @ 2016 Royal Society of Chemistry
Figure 4. (a) N 1s XPS spectra of N-modified HOPG. (b) ORR results for corresponding N-modified HOPG in (a). (c) N 1s XPS of the N-modified HOPG sample catalyst before and after ORR. (d) Catalysis mechanism of the active site[53]. Reproduced with permission. Copyright @ 2016 American Association for the Advancement of Science. (e) Schematic of the formation of N-doped hollow carbon from ZIF-8. (f) Current density measured at 0.75 V (vs. RHE). (g) ORR curves and (h) discharge curve and corresponding power density of N-doped hollow carbon[21]. Reproduced with permission. Copyright @ 2020 Elsevier Ltd. (i) Schematic of the formation of N, P co-doped carbon from ZnO@ZIF-8. Linear sweep voltammetry curves of (j) ORR and (k) both ORR and OER at 1600 r min−1 in the whole in O2-saturated 0.1 mol L−1 KOH solution[59]. Reproduced with permission. Copyright @ 2018 Elsevier Ltd.
Figure 5. (a) Schematic of the formation of Co nanoparticle grafted on N-doped carbon. (b) The corresponding linear sweep voltammetry curves for both ORR and OER at 1600 r min−1. (c) Discharge curve and corresponding power density[63]. Reproduced with permission. Copyright @ 2022 Elsevier Ltd. (d) Schematic of the formation of Fe single-atom catalysts. (e) The corresponding linear sweep voltammetry and (f) NH3 yield[76]. Reproduced with permission. Copyright @ 2022 Elsevier Ltd.
Figure 6. (a) Scheme and the (b) optical photograph of the SECCM measured on the HOPG, (c) ORR linear sweep voltammetry curves within a droplet on the edge and the basal region of the HOPG[15]. Reproduced with permission. Copyright @ 2014 Wiley-VCH GmbH. (d) Atomic Force Microscope (AFM) and (e) SECCM current density image of the graphene device of the proton transfer process[99]. Reproduced with permission. Copyright @ 2023 Macmillan Publisher Ltd.. (f) Schematic representation of the SECM measurement[104]. Reproduced with permission. Copyright @ 2017 Royal Society of Chemistry. (g) Current density from SECM and (h) G peak mapping from Raman of the graphene sample[107]. Reproduced with permission. Copyright @ 2018 American Chemical Society. (i) AMF image and (j) ORR current image measured from SECM of the HOPG sample, (k) AMF image and (l) ORR current image measured from SECM of Fe-N doped HOPG sample[108]. Reproduced with permission. Copyright @ 2018 Royal Society of Chemistry
Figure 7. In-situ Raman spectra of (a) honeycomb carbon nanofibers with abundant oxygenated functional groups and (b) solid carbon nanofibers[113]. Reproduced with permission. Copyright @ 2021 Wiley-VCH GmbH. (c) Spin trapping results of the superoxide radicals using the DMPO, EPR spectra of (d) graphene oxide, (e) graphene oxide washed by base and acid solutions to remove Mn2+ impurities and oxidized debris and (f) quenched graphene oxide with phenyl carboxylic acid groups[117]. Reproduced with permission. Copyright @ 2012 Macmillan Publisher Ltd. (g) In situ EPR spectra of the N-doped graphene in KOH electrolyte[124]. Reproduced with permission. Copyright @ 2020 Elsevier Ltd. (h) Scheme of the in situ FTIR setup, (i) in situ FTIR spectra of high-entropy single-atom activated carbon catalysts, (j) summarised peak density at 1347 cm−1, (k) in situ FTIR spectra at 1082 cm−1[133]. Reproduced with permission. Copyright @ 2023 Macmillan Publisher Ltd.
Table 1. Summary of the recent MOF-derived carbon-based electrochemical catalysts for ORR
ORR Catalysts Electrolytes Onset potential
(Eonset (vs. RHE)/V)Half-wave potential
(E1/2 (vs. RHE)/V)Limiting current density
(JL/(mA cm−2)) at 1600 r min−1Durability Refs NHCP-1000 0.1 M KOH 0.98 0.86 ~5.7 36000 s (~96%) [21] Co@N–HCCs@NG 0.1 M KOH ~0.97 0.86 ~5.8 6 h (99%) [34] Carbon defects graphene 0.1 M KOH 0.91 0.76 ~4.6 5 h (90%) [36] Nitrogen-doped graphene mesh (NGM) 0.1 M KOH ~0.89 ~0.77 ~6.4 10 h (100%) [47] NPCTC-850 0.1 M KOH 0.92 0.83 ~5.4 20000 s (96%) [59] D-Co@NC 0.1 M KOH ~0.95 ~0.85 ~5.8 30000 s (98.4%) [63] ZnCo2@NCNTs-800 0.1 M KOH ~0.94 ~0.85 ~6.2 30000 s (97.5%) [77] Fe/Fe3C-N-CNTs 0.1 M KOH 1.02 0.88 ~5.7 20000 s (94%) [78] 0.05CoOx@PNC 0.1 M KOH 0.98 0.88 ~6.5 12 h (100%) [79] BTC-Co-O-Cu-BTA 0.1 M NaOH 1.06 0.95 ~6.0 20000 s (99%) [80] C-ZIF-CuPt 0.1 M KOH ~0.99 ~0.87 5.5 10000 cycles [81] CoP-NC@NFP 0.1 M KOH ~0.92 ~0.83 ~6.1 200 h (82%) [82] Fe3C-Co-NC 0.1 M KOH 1.20 0.89 ~4.5 20000 s (97%) [83] Note: M: mol L−1 
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Table 2. Summary of the recent MOF-derived carbon-based electrochemical catalysts for OER
Catalysts Electrolytes Tafel slopes/(mV dec−1) Over potential
(at 10 mA cm−2)Durability Refs Co@N–HCCs@NG 1 M KOH 114.4 1.6 V (onset potential) 21600 s (98%) [34] Carbon defects graphene 1 M KOH 97 1.57 V (onset potential) 35000 s (100%) [36] NPCTC-850 0.1 M KOH 115 210 mV [59] D-Co@NC 0.1 M KOH ~101 488 mV 10000 s (89%) [63] ZnCo2@NCNTs-800 0.1 M KOH ~76 1.58 V (onset potential) 30000 s (92.4%) [77] Fe/Fe3C-N-CNTs 0.1 M KOH ~78 1.57 (onset potential) 30000 s (95%) [78] CoNiP/CoNi 1 M KOH 72 300 mV 10 h (95%) [84] NiCoZnP/NC 1 M KOH 85 228 mV 45 h (91%) [85] CoP-NC@NFP 1 M KOH 84 320 mV 40 h (100%) [82] 2D Co@NC 1 M KOH 110 ~380 mV − [86] 2D Mo2C@NC 1 M KOH 100 ~370 mV − H-2D Co/Mo2C@NC 1 M KOH 48 ~256 mV 10 h (100%) CoNi/NC-YS 1 M KOH ~54 292 mV 24 h (100%) [87] Fe3C-Co-NC 1 M KOH 59 −338 mV 30000 s (100%) [83] Note: M: mol L−1
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Table 3. Summary of the recent MOF-derived carbon-based electrochemical catalysts for HER
Catalysts Electrolytes Tafel slopes/(mV dec−1) Over potential/(mV at 10 mA cm−2) Durability Refs Carbon defects graphene 1 M KOH 118 320 35000 s [36] 0.5 M H2SO4 55 150 35000 s CoNiP/CoNi/N-RGO 1 M KOH 97 150 10 h [84] CoZnP/NC 1 M KOH ~121 308 at 100 mA cm−2 45 h [85] NiCoZnP/NC 1 M KOH ~48 133 at 100 mA cm−2 45 h Co3O4/C 0.1 M NaOH ~68 ~183 at 100 mA cm−2 12 h [88] 0.5 M H2SO4 ~72 ~195 12 h HNi/NiO/C 1 M KOH 91 87 at 100 mA cm−2 12 h [89] Ru–MoO2@PC/rGO 1 M KOH 43 126 8 h [90] C-ZIF-CuPt 0.1 M KOH 45 46 1000 cycles [81] PtCu-Mo2C@C (0.75:1) 0.5 M H2SO4 29 26 25 h [91] NiSe2/NiS2@NC 0.5 M H2SO4 46 188 2000 cycles [92] 1 M KOH ~93 211 2000 cycles CoP-NC@NFP 1 M KOH 108 200 50 h [82] Note: M: mol L−1
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