Vapor-grown carbon fibers (VGCF) were grown from a methane-hydrogen mixture
on a reconstituted graphite support using different catalyst precursors, t
he [Fe-3(CO)(12)] complex being found to be the most efficient for the prod
uction of VGCF. The fibers thus produced were characterized and submitted t
o different oxidative treatments, namely nitric acid, plasma, air and carbo
n dioxide. From analysis performed by scanning electron microscopy (SEM), n
itrogen adsorption (BET) and X-ray photon spectroscopy (XPS) it appears tha
t the air and carbon dioxide treatments do not lead to significant increase
either of the surface area, or of the quantity of surface oxygen containin
g groups, despite the considerable weight loss attained (50%). This peculia
r observation has been interpreted by considering the presence of traces of
iron at the fibers surface, which can catalyze the gasification of carbon.
The presence of iron on the VGCF has been evidenced for the first time by
the time-of-flight secondary ion mass spectrometry technique. The cleansing
of the fibers surface with concentrated hydrochloric acid results in the r
emoval of the iron and leads, after CO2 activation, to an improvement of th
e BET surface area. The use of nitric acid or plasma as oxidation agents do
es not affect significantly the surface morphology of the fibers, but great
ly increases the number of surface oxygen functions. (C) 1998 Elsevier Scie
nce Ltd. All rights reserved.