The
mechanism of thermal defunctionalization of multiwalled carbon
nanotubes (CNTs) oxidized by nitric acid was studied. X-ray photoelectron
spectroscopy and thermal analysis under different heating rates combined
with mass spectrometry of evolved gases (TGA–MS) were used
to reveal the transformations on the CNT surface. Hydrogen–deuterium
exchange and mathematical handling of TGA–MS curves were carried
out to evaluate the impact of a small amount of residual oxygen on
CNT defunctionalization. Water, CO, CO2, and NO/CH2O mass curves recorded during TGA–MS study were curve
fitted. The resultant peaks were attributed to the different stages
of CNT defunctionalization. Deuterium exchanged CNTs allowed one to
reveal the mechanism of water release during heating. Kissinger’s
model was applied to estimate the activation energy of the decomposition
of different functional groups on the surface of CNTs.