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Science 26 September 2008:
Vol. 321. no. 5897, pp. 1815 - 1817
DOI: 10.1126/science.1162369

Reports

Synthesis and Solid-State NMR Structural Characterization of 13C-Labeled Graphite Oxide

Weiwei Cai,1,2 Richard D. Piner,1 Frank J. Stadermann,3 Sungjin Park,1 Medhat A. Shaibat,4 Yoshitaka Ishii,4 Dongxing Yang,1 Aruna Velamakanni,1 Sung Jin An,5 Meryl Stoller,1 Jinho An,1 Dongmin Chen,2 Rodney S. Ruoff1*

The detailed chemical structure of graphite oxide (GO), a layered material prepared from graphite almost 150 years ago and a precursor to chemically modified graphenes, has not been previously resolved because of the pseudo-random chemical functionalization of each layer, as well as variations in exact composition. Carbon-13 (13C) solid-state nuclear magnetic resonance (SSNMR) spectra of GO for natural abundance 13C have poor signal-to-noise ratios. Approximately 100% 13C-labeled graphite was made and converted to 13C-labeled GO, and 13C SSNMR was used to reveal details of the chemical bonding network, including the chemical groups and their connections. Carbon-13–labeled graphite can be used to prepare chemically modified graphenes for 13C SSNMR analysis with enhanced sensitivity and for fundamental studies of 13C-labeled graphite and graphene.

1 Department of Mechanical Engineering and the Texas Materials Institute, University of Texas at Austin, Austin, TX 78712, USA.
2 Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100080, China.
3 Laboratory for Space Sciences, Department of Physics, Washington University, St. Louis, MO 63130, USA.
4 Department of Chemistry, University of Illinois at Chicago, 845 West Taylor Street, Chicago, IL 60607, USA.
5 National Creative Research Initiative Center for Semiconductor Nanorods and Department of Materials Science and Engineering, Pohang University of Science and Technology, Pohang, Gyeongbuk 790-784, Korea.

* To whom correspondence should be addressed. E-mail: r.ruoff{at}mail.utexas.edu

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Science. ISSN 0036-8075 (print), 1095-9203 (online)