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

Abstract

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.