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. 2018 Feb 7;8(11):6136-6145.
doi: 10.1039/c7ra13514a. eCollection 2018 Feb 2.

One-pot synthesis of amine-functionalized graphene oxide by microwave-assisted reactions: an outstanding alternative for supporting materials in supercapacitors

C C Caliman  1 , A F Mesquita  1 , D F Cipriano  2 , J C C Freitas  2 , A A C Cotta  3 , W A A Macedo  3 , A O Porto  4
Affiliations

One-pot synthesis of amine-functionalized graphene oxide by microwave-assisted reactions: an outstanding alternative for supporting materials in supercapacitors

C C Caliman et al. RSC Adv. .

Abstract

A simple and straightforward method using microwave-assisted reactions is presented for the functionalization of graphene oxide with aromatic and non-aromatic amines, notedly dibenzylamine (DBA), p-phenylenediamine (PPD), diisopropylamine (DPA) and piperidine (PA). The as-synthesized amine-functionalized graphene oxide materials (amine-GO) were characterized using spectroscopic techniques including XRD, FTIR, 13C NMR, XPS, TEM for imaging and thermogravimetric analysis (TGA). The characterization confirmed the functionalization for all amines, reaching relatively high surface nitrogen atomic concentrations of up to 8.8%. The investigations of electrochemical behavior for the amine-GOs show the significant improvement in GO's electrochemical properties through amine functionalization, exhibiting long life cycle stability and reaching specific capacitance values of up to 290 F g-1 and 260 F g-1 for GO-PA and GO-DPA samples, respectively, confirming their potential application as alternative supporting materials in supercapacitors.

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Conflict of interest statement

There are no conflicts to declare.

Figures

Fig. 1
Fig. 1. XRD patterns of GO, GO-DBA, GO-DPA,GO-PPD and GO-PA.
Fig. 2
Fig. 2. TEM images for GO (a), GO-DBA (b), GO-DPA (c), GO-PA (d) and GO-PPD (e).
Fig. 3
Fig. 3. N2 adsorption–desorption isotherm for GO: (a) BET surface area measurement and (b) BJH pore size distribution.
Fig. 4
Fig. 4. N2 adsorption–desorption isotherm for GO-DBA: (a) BET surface area measurement and (b) BJH pore size distribution.
Fig. 5
Fig. 5. FTIR spectra for GO, GO-DBA, GO-DPA, GO-PPD and GO-PA.
Fig. 6
Fig. 6. TG curves of GO, GO-DBA, GO-DPA, GO-PPD and GO-PA.
Fig. 7
Fig. 7. 13C NMR spectra of GO and GO-amines. The asterisks indicate spinning sidebands.
Fig. 8
Fig. 8. XPS survey spectra of GO and GO-amine samples.
Fig. 9
Fig. 9. C 1s high resolution XPS spectra obtained for GO, GO-DBA, GO-DPA, GO-PPD and GO-PA.
Fig. 10
Fig. 10. O 1s (a) and N 1s (b) high resolution XPS spectra of GO, GO-DBA, GO-DPA, GO-PPD and GO-PA.
Fig. 11
Fig. 11. Cyclic voltammograms in 1.0 M H2SO4 of (a) amine-functionalized GOs at 10 mV s−1 and (b) GO-PA at different scan rates.
Fig. 12
Fig. 12. Galvanostatic charge–discharge curves in 1.0 M H2SO4 for (a) GO and amine-functionalized GO at 1.0 mA cm−2 and for (b) GO-DPA at different current densities.
Fig. 13
Fig. 13. Cyclic stability tests for the amine-functionalized electrodes at 1 mA cm−2 discharge current density in aqueous 1.0 M H2SO4 electrolyte solution.
Fig. 14
Fig. 14. Electrochemical impedance spectroscopy (EIS) of GO and the amine-functionalized electrodes in aqueous 1.0 M H2SO4 electrolyte solution.
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