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Graphite and multiwall carbon nanotube surfaces were functionalized by vacuum-ultraviolet induced photochemistry in NH3 or O2, in order to introduce amino- (NH2) or hydroxyl (OH) functionalities, respectively. Modified surfaces were characterized by X-ray photoelectron spectroscopy (XPS), which showed significant incorporation of nitrogen (N) and oxygen (O) at the materials surface. While high-resolution XP spectra did not yield much specific information about the incorporated functional groups, chemical derivatization with 4-trifluoromethyl benzaldehyde and trifluoroacetic anhydride accompanied by XPS enabled quantification of NH2 and OH groups, respectively. Using near edge X-ray absorption fine structure spectroscopy, we assessed the conservation of the aromatic structure following functionalization treatments.
A toluene solution of 4,4´-methylenebis(2,6-diethylaniline) was spin coated on Si wafers. The samples were derivatized with pentafluorobenzaldehyde (PFB) in order to determine the primary amino groups on the surface. XPS C 1s and N 1s and C and N K-edge NEXAFS of underivatized and derivatized films were carefully analyzed. The result was that after 10 min of exposure the gas-surface reaction was already completed. A reasonable derivatization reaction yield in the order of 90% is derived from the experiments. This number correlates well to a reaction yield obtained by a wet chemical approach.