3D-ordered macroporous N-doped carbon encapsulating Fe-N alloy derived from a single-source metal-organic framework for superior oxygen reduction reaction

doi:10.1016/S1872-2067(20)63667-1

Abstract

Abstract:

Fe-N compounds with excellent electrocatalytic oxygen reduction activity are considered to be one of the most promising non-precious metal materials for fuel cells. Fe-N compounds with excellent electrocatalytic oxygen reduction activity are considered to be one of the most promising non-precious metal materials for fuel cells,which focuses on the Fe-N4 single-atom catalysts and the iron nitride materials (such as Fe2N and Fe3N). A hybridized catalyst having a hierarchical porous structure with regular macropores could enable the desired mass transfer efficiency in the catalytic process. In this study,we have constructed a new type of hybrid catalyst having iron and iron-nitrogen alloy nanoparticles (Fe-N austenite,termed as Fe-NA) embedded in the three-dimensional ordered macroporous N-doped carbon (3DOM Fe/Fe-NA@NC) by direct pyrolysis of single-source dicyandiamide-based iron metal-organic frameworks. The as-synthesized composites preserve the hierarchical porous carbon framework with ordered macropores and high specific surface area,incorporating the uniformly dispersed iron/iron-nitrogen austenite nanoparticles. Thereby,the striking architectural configuration embedded with highly active catalytic species delivers a superior oxygen reduction activity with a half-wave potential of 0.88 V and a subsequent superior Zn-air battery performance with high open-circuit voltage and continuous stability as compared to those using a commercial 20% Pt/C catalyst.

Key words: Metal-organic framework, Single-source precursor, Oxygen reduction reaction, Iron-nitrogen alloy

Ya-Ru Lv, Xue-Jing Zhai, Shan Wang, Hong Xu, Rui Wang, Shuang-Quan Zang. 3D-ordered macroporous N-doped carbon encapsulating Fe-N alloy derived from a single-source metal-organic framework for superior oxygen reduction reaction[J]. Chinese Journal of Catalysis, 2021, 42(3): 490-500.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(20)63667-1

https://www.cjcatal.com/EN/Y2021/V42/I3/490

Figures/Tables 5

Fig. 1. Schematic diagram of the process for synthesizing 3DOM Fe/Fe-NA@NC catalyst.

Fig. 2. (a) Powder XRD patterns of 3DOM Fe/Fe-NA@NC-800 and Fe/Fe-NA@NC-800; (b,c) SEM images of 3DOM Fe/Fe-NA@NC-800; (d) TEM image of 3DOM Fe/Fe-NA@NC-800; (e) HRTEM image of 3DOM Fe/Fe-NA@NC-800; (f) Elemental mapping images of 3DOM Fe/Fe-NA@NC-800 showing the uniform presence of C,N,and Fe.

Fig. 3. (a) N2 adsorption-desorption curves of Fe/Fe-NA@NC-800 and 3DOM Fe/Fe-NA@NC-800; (b) Corresponding pore size distribution curves; (c) Raman spectra of Fe/Fe-NA@NC-800 and 3DOM Fe/Fe-NA@NC-800; (d) High-resolution XPS profile of N 1s for 3DOM Fe/Fe-NA@NC-800; (e) N content for different materials; (f) High-resolution XPS profile of Fe 2p for 3DOM Fe/Fe-NA@NC-800.

Fig.4. (a) CV curves of 3DOM Fe/Fe-NA@NC-800 in O2 and N2-saturated 0.1 M KOH; (b) LSV curves of 3DOM Fe/Fe-NA@NC,Fe/Fe-NA@NC and 20% Pt/C in O2-saturated 0.1 M KOH at 1600 rpm; (c) Corresponding Tafel slopes; (d) ORR polarization curves at different rotating speeds; inset shows the corresponding K-L plots and electron transfer numbers (n) at different potentials of 3DOM Fe/Fe-NA@NC-800; (e) Electron transfer number n and HO2ˉ yield based on RRDE; (f) CV curves measured over 3DOM Fe/Fe-NA@NC-800 modified electrode 10-50 mV s-1; inset shows the corresponding scan rate dependence of the current density; (g) Chronoamperometric response; (h) Methanol tolerance for 3DOM Fe/Fe-NA@NC-800 and 20% Pt/C; (i) PXRD patterns of 3DOM Fe/Fe-NA@NC-800 after stability tests.

Fig. 5. (a) Schematic diagram of homemade Zn-air battery; (b) Open-circuit plots of a single battery of the homemade Zn-air battery using 3DOM Fe/Fe-NA@NC-800 and 20% Pt/C as the air cathode,respectively (Left: photograph of the assembled battery using the 3DOM Fe/Fe-NA@NC-800 as the air-cathode with an open-circuit voltage of 1.59 V; Right: red LED powered by two-series batteries); (c) Polarization curves and the corresponding power density curves of the homemade Zn-air batteries constructed with 3DOM Fe/Fe-NA@NC-800 and 20% Pt/C as the air-cathode catalysts,respectively; (d) Long-term cycling tests of the Zn-air battery using 3DOM Fe-N-C-800 and 20% Pt/C as the air cathode at the charging and discharging current density of 5 mA cm-2 (10 min for each cycle).

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