This work reports on a study conducted to achieve carbon fibre functio
nalization by means of a diazide derivative (p-(azidosulfonyl)benzoyl
azide) in two stages. The first stage comprises surface oxidation of t
he fibres, which causes an increase of the number of superficial COOH
groups. During the second stage the oxidated fibres are brought to rea
ct with the diazide derivative via the isocyanate group, obtained by m
eans of the Curtius transposition of the carbonyl azide group. Fibre o
xidation depends on reaction time, following a similar pattern as the
one described for carbon black particles. Oxidized fibre functionaliza
tion is evidenced both in the progressive decrease in SO2N3 groups in
the reagent solution and through differential scanning calorimetry ana
lysis (DSC), which shows an exothermal peak around 190-degrees-C due t
o the decomposition of the azide grafted onto the carbon fibre. The de
gree of attainable functionalization is a function of COOH group conce
ntration, generated during fibre oxidation, and the ratio of the funct
ionalizing agent with regard to the carboxy groups formed.