High-quality graphene via microwave reduction of solution-exfoliated graphene oxide

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Science  23 Sep 2016:
Vol. 353, Issue 6306, pp. 1413-1416
DOI: 10.1126/science.aah3398
  • Fig. 1 Physical characterization of MW-rGO compared with pristine GO, rGO, and graphene grown by CVD.

    (A) Scanning electron microscopy of the single-layer GO flakes deposited on a silicon wafer. GO nanosheets typically have a lateral dimension of ~50 μm. (B) High-resolution x-ray photoelectron spectra from the C1s regions for microwaved reduced graphene oxide (MW-rGO) compared with pristine graphene oxide (GO), reduced graphene oxide (rGO), graphene grown by chemical vapor deposition (CVD graphene), and graphite. Each spectrum can be deconvoluted with components from the carbon-carbon bonds (sp3: C–C and sp2: C=C) as well as oxygen functional groups (C–O, C=O, and C–O=O), allowing quantification of the oxygen content. a.u., arbitrary units. (C) Raman spectra of MW-rGO and other graphene-based samples. The spectrum obtained for MW-rGO is similar to the spectrum of CVD graphene, with the presence of a high and symmetrical 2D band together with a minimal D band. Sharp Raman peaks indicate high crystallinity of MW-rGO and demonstrate the quality of microwave reduction. (D) Evolution of the I2D/IG ratio versus the crystal size (La) for MW-rGO, GO, rGO, highly ordered pyrolytic graphite (HOPG), dispersed graphene, and graphene from (3) (i.e., CVD graphene). We report 62 measurements on about five different MW-rGO samples. I2D/IG ratios and La values for MW-rGO are approaching those of graphene and are substantially higher than the values for rGO and dispersed graphene.

  • Fig. 2 High-resolution transmission electron microscopy (HR-TEM) of MW-rGO nanosheets.

    (A) HR-TEM of single-layer rGO presenting high density of defects. The red arrow denotes a hole; the blue arrow indicates an oxygen functional group. Bilayer (B) and trilayer (C) HR-TEM of MW-rGO showing highly ordered structure. Scale bars, 1 nm.

  • Fig. 3 Characterization of the electronic and electrocatalytic properties of MW-rGO.

    (A) Transfer characteristics of MW-rGO and rGO measured at drain voltage (Vds) = 50 mV. MW-rGO displays ambipolar behavior with a Dirac cone at gate voltage (Vg) ~ 0.5 V. Id, drain current. (Inset) Evolution of the MW-rGO conductivity with the carrier density. n, carrier concentration; σ, conductivity. (B) Polarization curves obtained from Ni-Fe layered double hydroxide (LDH) deposited on MW-rGO (Ni-Fe@MW-rGO), rGO (Ni-Fe@rGO), and glassy carbon (Ni-Fe@GC). (Inset) Magnification of the onset potential. J, current density. (C) Tafel plot of Ni-Fe LDH deposited on MW-rGO compared with GC and rGO. (Inset) Nyquist plots of the different samples obtained by electrochemical impedance spectroscopy at η = 200 mV. Ni-Fe@MW-rGO clearly shows a reduced internal resistance and minimal charge transfer resistance that can be attributed to the high conductivity of the MW-rGO nanosheets. Re (Z), real part of the impedance; -Im (Z), imaginary part of the impedance. (D) Galvanostatic measurements showing the electrocatalytic stability of Ni-Fe LDH deposited on glassy carbon and MW-rGO when driving a 10 mA/cm2 current density over 15 hours. The MW-rGO support shows the best stability with minimal change of the overpotential. Contrastingly, the activity from the Ni-Fe LDH on glassy carbon decreases rapidly.

Supplementary Materials

  • High-quality graphene via microwave reduction of solution-exfoliated graphene oxide

    Damien Voiry, Jieun Yang, Jacob Kupferberg, Raymond Fullon, Calvin Lee, Hu Young Jeong, Hyeon Suk Shin, Manish Chhowalla</p

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