Research ArticleFUNCTIONAL CARBONS

Gelatin-derived sustainable carbon-based functional materials for energy conversion and storage with controllability of structure and component

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Science Advances  27 Feb 2015:
Vol. 1, no. 1, e1400035
DOI: 10.1126/sciadv.1400035
  • Fig. 1 Illustration of the preparation procedure of IAG-C catalysts and Fe3O4@AGC electrode materials.
  • Fig. 2

    (A) TEM image of intermediate Fe3O4/carbon composite produced at 350°C. (B and C) TEM and HRTEM images of IAG-C catalyst. (D) Nitrogen adsorption-desorption curves of four samples prepared with different precursors.

  • Fig. 3

    (A) CVs of Pt/C, G-C, and IAG-C in 0.1 M KOH at 5 mV s−1. (B) LSV curves for G-C, AG-C, IG-C, IAG-C, and Pt/C in O2-saturated 0.1 M KOH at 5 mV s−1 at 1600 revolutions per minute (rpm). (C) LSV curves for IAG-C at different rotation rates in O2-saturated 0.1 M KOH at 5 mV s−1; inset shows the K-L plots. (D) Tafel plots of IAG-C and Pt/C for ORR derived by the mass-transport correction of corresponding RDE data. (E) Chronoamperometric response of IAG-C and Pt/C in O2-saturated 0.1 M KOH followed by addition of 3 M methanol. (F) Chronoamperometric response of IAG-C and Pt/C in O2-saturated 0.1 M KOH solution at 0.65 V at 1600 rpm.

  • Fig. 4

    (A and B) N 1s XPS spectra (A) and the relative content of pyridinic and graphitic N (B) in the four samples prepared with different precursors. (C and D) Mössbauer spectra for IG-C and IAG-C. (E) Relative content of D1, D2, and D3 sites in all the Fe species for both Fe-containing catalysts. (F) Possible structure model of IAG-C.

  • Fig. 5

    (A and B) TEM (A) and HRTEM (B) images of Fe3O4@AGC electrode material. (C and D) Comparison of rate capabilities (C) and cycle performance (D) of Fe3O4@AGC and bare Fe3O4.

Supplementary Materials

  • Supplementary material for this article is available at http://advances.sciencemag.org/cgi/content/full/1/1/e1400035/DC1

    Materials and Methods

    Fig. S1. Photographs of precursor solution (A), composite gel (B), and the final catalyst (C).

    Fig. S2. Comparison of photographs and UV-visible spectroscopy of different solutions.

    Fig. S3. (A) SEM image of composite gel after sol-gel; (B to E) mapping analysis of the composite gel: (B) C element from gelatin, (C) N and (D) O elements from gelatin and ammonium nitrate, and (E) Fe element from iron ferric hydroxide.

    Fig. S4. Comparison of the products derived from different precursor solution containing different components at the same treatment conditions: (A) only gelatin; (B) gelatin and ammonium nitrate; and (C) gelatin and iron nitrate.

    Fig. S5. Comparison of gels obtained by using cobalt nitrate (A) and nickel nitrate (B) as metal salts with the same treatment conditions of iron nitrate.

    Fig. S6. (A) FT-IR spectra, (B) N 1s spectra, and (C) XRD patterns of gelatin, amorphous Fe(OH)3, and gelatin-Fe(OH)3 gel.

    Fig. S7. (A) SEM image of composite gel after sol-gel; (B) SEM image and (C) XRD pattern of the product obtained by calcining the gel at 350°C; (D) TEM image of the above HCl-washed product.

    Fig. S8. TEM images of AG-C (A), IG-C (B), and G-C (C); (D) pore size distributions of four samples prepared with different precursors.

    Fig. S9. Raman spectra (A) and ID/IG ratio (B) of four samples prepared with different precursors. (C) Comparison of XRD patterns of IAG-C and G-C.

    Fig. S10. (A) Temperature effect of IAG-C activity for ORR; (B) comparison of the electron transfer number of catalysts at 0.65 V; (C) stability of IAG-C after 3 months in air.

    Fig. S11. LSV curves of IAG-C before and after adding KCN in O2-saturated 0.1 M KOH at 1600 rpm: (A) 10 mM KCN and (B) 50 mM KCN. The green line is the LSV curve after CN poisoning tests, electrode washing, and immersion in fresh 0.1 M KOH for IAG-C.

    Fig. S12. LSV curves at different rotation rates in O2-saturated 0.1 M KOH at 5 mV s−1, and the inset shows the corresponding K-L plots: (A) G-C, (B) AG-C, (C) IG-C, and (D) Pt/C; (E) electron transfer number (n) and (F) peroxide yield of G-C, AG-C, IG-C, IAG-C, and commercial 20 wt % Pt/C in O2-saturated 0.1 M KOH.

    Fig. S13. (A) Linear sweep voltammetry (LSV) curves for G-C, AG-C, IG-C, IAG-C, and Pt/C in O2-saturated 0.1 M HClO4 at 5 mV s−1 at 1600 rpm; LSV curves for IAG-C (B) and Pt/C (C) at different rotation rates in O2-saturated 0.1 M HClO4 at 5 mV s−1, and the inset shows the K-L plots.

    Fig. S14. (A) Electron transfer number and (B) peroxide yield (n) of G-C, AG-C, IG-C, IAG-C, and commercial 20 wt % Pt/C in O2-saturated 0.1 M HClO4; (C) chronoamperometric response of IAG-C and Pt/C in O2-saturated 0.1 M HClO4 followed by addition of 3 M methanol; (D) chronoamperometric response of IAG-C and Pt/C in O2-saturated 0.1M HClO4 solution at 0.5 V (versus RHE) at 1600 rpm.

    Fig. S15. (A) High-angle annular dark-field scanning transmission electron microscopy (STEM) image of the IAG-C catalyst; (B) C-, (C) N-, (D) O-, and (E) Fe-elemental mapping of the square region.

    Fig. S16. (A) High-angle annular dark-field scanning transmission electron microscopy (STEM) image of the IAG-C catalyst; (B) C-, (C) N-, (D) O-, and (E) Fe-elemental mapping of the square region after stability test. (F) N 1s XPS spectra of IAG-C after stability test.

    Fig. S17. TEM images of Fe3O4@AGC with different content of Fe3O4 in the hybrids: (A) Fe3O4@AGC-4, (B) Fe3O4@AGC, and (C) Fe3O4@AGC-6; (D) TG curves of the three hybrids to determine the content of carbon; (E) XRD patterns of three hybrids. The diffraction peaks of the composites are perfectly indexed to pure-phase Fe3O4 (JCPDS No.65-3107).

    Fig. S18 Charge-discharge curves of Fe3O4@AGC (A), bare Fe3O4 (B), and AGC (C) at a current density of 100 mA g−1; (D) Nyquist plots for the Fe3O4@AGC and bare Fe3O4-based cells with lithium metal as counter electrode.

    Fig. S19. The calibration CV curves of Ag/AgCl electrode (A) in 0.1 M KOH and (B) in 0.1 M HClO4 with respect to RHE.

  • Supplementary Materials

    This PDF file includes:

    • Materials and Methods
    • Fig. S1. Photographs of precursor solution (A), composite gel (B), and the final catalyst (C).
    • Fig. S2. Comparison of photographs and UV-visible spectroscopy of different solutions.
    • Fig. S3. (A) SEM image of composite gel after sol-gel; (B to E) mapping analysis of the composite gel: (B) C element from gelatin, (C) N and (D) O elements from gelatin and ammonium nitrate, and (E) Fe element from iron ferric hydroxide.
    • Fig. S4. Comparison of the products derived from different precursor solution containing different components at the same treatment conditions: (A) only gelatin; (B) gelatin and ammonium nitrate; and (C) gelatin and iron nitrate.
    • Fig. S5. Comparison of gels obtained by using cobalt nitrate (A) and nickel nitrate (B) as metal salts with the same treatment conditions of iron nitrate.
    • Fig. S6. (A) FT-IR spectra, (B) N 1s spectra, and (C) XRD patterns of gelatin, amorphous Fe(OH)3, and gelatin-Fe(OH)3 gel.
    • Fig. S7. (A) SEM image of composite gel after sol-gel; (B) SEM image and (C) XRD pattern of the product obtained by calcining the gel at 350°C; (D) TEM image of the above HCl-washed product.
    • Fig. S8. TEM images of AG-C (A), IG-C (B), and G-C (C); (D) pore size distributions of four samples prepared with different precursors.
    • Fig. S9. Raman spectra (A) and ID/IG ratio (B) of four samples prepared with different precursors. (C) Comparison of XRD patterns of IAG-C and G-C.
    • Fig. S10. (A) Temperature effect of IAG-C activity for ORR; (B) comparison of the electron transfer number of catalysts at 0.65 V; (C) stability of IAG-C after 3 months in air.
    • Fig. S11. LSV curves of IAG-C before and after adding KCN in O2-saturated 0.1 M KOH at 1600 rpm: (A) 10 mM KCN and (B) 50 mM KCN. The green line is the LSV curve after CN−1 poisoning tests, electrode washing, and immersion in fresh 0.1 M KOH for IAG-C.
    • Fig. S12. LSV curves at different rotation rates in O2-saturated 0.1 M KOH at 5 mV s−1, and the inset shows the corresponding K-L plots: (A) G-C, (B) AG-C, (C) IG-C, and (D) Pt/C; (E) electron transfer number (n) and (F) peroxide yield of GC, AG-C, IG-C, IAG-C, and commercial 20 wt % Pt/C in O2-saturated 0.1 M KOH.
    • Fig. S13. (A) Linear sweep voltammetry (LSV) curves for G-C, AG-C, IG-C, IAG-C, and Pt/C in O2-saturated 0.1 M HClO4 at 5 mV s−1 at 1600 rpm; LSV curves for IAG-C (B) and Pt/C (C) at different rotation rates in O2-saturated 0.1 M HClO4 at 5 mV s−1, and the inset shows the K-L plots.
    • Fig. S14. (A) Electron transfer number and (B) peroxide yield (n) of G-C, AG-C, IG-C, IAG-C, and commercial 20 wt % Pt/C in O2-saturated 0.1 M HClO4; (C) chronoamperometric response of IAG-C and Pt/C in O2-saturated 0.1 M HClO4 followed by addition of 3 M methanol; (D) chronoamperometric response of IAGC and Pt/C in O2-saturated 0.1M HClO4 solution at 0.5 V (versus RHE) at 1600 rpm.
    • Fig. S15. (A) High-angle annular dark-field scanning transmission electron microscopy (STEM) image of the IAG-C catalyst; (B) C-, (C) N-, (D) O-, and (E) Fe-elemental mapping of the square region.
    • Fig. S16. (A) High-angle annular dark-field scanning transmission electron microscopy (STEM) image of the IAG-C catalyst; (B) C-, (C) N-, (D) O-, and (E) Fe-elemental mapping of the square region after stability test. (F) N 1s XPS spectra of IAG-C after stability test.
    • Fig. S17. TEM images of Fe3O4@AGC with different content of Fe3O4 in the hybrids: (A) Fe3O4@AGC-4, (B) Fe3O4@AGC, and (C) Fe3O4@AGC-6; (D) TG curves of the three hybrids to determine the content of carbon; (E) XRD patterns of three hybrids. The diffraction peaks of the composites are perfectly indexed to pure-phase Fe3O4 (JCPDS No.65-3107).
    • Fig. S18 Charge-discharge curves of Fe3O4@AGC (A), bare Fe3O4 (B), and AGC (C) at a current density of 100 mA g−1; (D) Nyquist plots for the Fe3O4@AGC and bare Fe3O4-based cells with lithium metal as counter electrode.
    • Fig. S19. The calibration CV curves of Ag/AgCl electrode (A) in 0.1 M KOH and (B) in 0.1 M HClO4 with respect to RHE.

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