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Sulfur-reduced graphene oxide composite (SGC) materials with uniformly dispersed sulfur on reduced graphene oxide sheets have been prepared by a simple aqueous one-pot synthesis method, in which the formation of the composite is achieved through the simultaneous oxidation of sulfide and reduction of graphene oxide. The synthesis process has been tracked ex situ by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectroscopy, which both confirm that the majority of graphene oxide has been reduced during the synthesis reaction. The sulfur contents in the SGC, determined by thermogravimetry and elementary analysis, have been adjusted in the range from 20.9 to 72.5 wt.%. Scanning electron microscope (SEM) and transmission electron microscope (TEM) images reveal that most of the sulfur is uniformly dispersed on the reduced graphene oxide sheets, for which no sulfur in particulate form could be observed. The SGC materials have been tested as the cathode of rechargeable lithium-sulfur (Li-S) batteries, and demonstrated a high reversible capacity and good cycleability. The SGC-63.6%S can deliver a reversible capacity as high as 804 mA·h/g after 80 cycles of charge/discharge at a current density of 312 mA/g (ca. 0.186 C), and 440 mA·h/g after 500 cycles at 1250 mA/g (ca. 0.75 C).
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