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Title

Atomic Force and Scanning Tunneling Microscopy Imaging of Graphene Nanosheets Derived from Graphite Oxide

AuthorsParedes Nachón, Juan Ignacio ; Villar Rodil, Silvia ; Solís Fernández, Pablo ; Martínez Alonso, Amelia ; Díez Tascón, Juan Manuel
Issue Date2009
PublisherAmerican Chemical Society
CitationLangmuir 25(10): 5957-5968 (2009)
AbstractGraphene nanosheets produced in the form of stable aqueous dispersions by chemical reduction of graphene oxide and deposited onto graphite substrates have been investigated by atomic force and scanning tunneling microscopy (AFM/STM). The chemically reduced graphene oxide nanosheets were hardly distinguishable from their unreduced counterparts in the topographic AFM images. However, they could be readily discriminated through phase imaging in the attractive regime of tapping-mode AFM, probably because of differences in hydrophilicity arising from their distinct oxygen contents. The chemically reduced nanosheets displayed a smoothly undulated, globular morphology on the nanometer scale, with typical vertical variations in the subnanometer range and lateral feature sizes of ∼5−10 nm. Such morphology was attributed to be the result of significant structural disorder in the carbon skeleton, which originates during the strong oxidation that leads to graphene oxide and remains after chemical reduction. Direct evidence of structural disorder was provided by atomic-scale STM imaging, which revealed an absence of long-range periodicity in the graphene nanosheets. Only structured domains a few nanometers large were observed instead. Likewise, the nanosheet edges appeared atomically rough and ill-defined, though smooth on the nanometer scale. The unreduced graphene oxide nanosheets could only be imaged by STM at very low tunneling currents (∼1 pA), being visualized in some cases with inverted contrast relative to the graphite substrate, a result that was attributed to their extremely low conductivity. Complementary characterization of the unreduced and chemically reduced nanosheets was carried out by thermogravimetric analysis as well as UV−visible absorption and X-ray photoelectron and Raman spectroscopies. In particular, the somewhat puzzling Raman results were interpreted to be the result of an amorphous character of the graphene oxide material.
DescriptionThis document is the Accepted Manuscript version of a Published Work that appeared in final form in Langmuir, copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see https://doi.org/10.1021/la804216z
Publisher version (URL)https://doi.org/10.1021/la804216z
URIhttp://hdl.handle.net/10261/182473
DOI10.1021/la804216z
ISSN0743-7463
E-ISSN1520-5827
Appears in Collections:(INCAR) Artículos
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