Niobium carbide (NbC) synthesis was studied by the temperature-program
med reaction (TPR) between niobium oxide precursors of different textu
ral properties and a 20% (v/v) CH4-H-2 mixture. Surface areas ranging
between 13 and 74 m(2)/g were obtained depending on the temperature an
d on the nature of the precursor (Nb2O5 or an aerogel precursor). The
high synthesis temperatures (1173-1373 K) caused surface contamination
by carbon from methane decomposition and led to low CO uptakes (15-28
mu mol/g). Environmental scanning electron microscopy (ESEM) analysis
showed that the transformation oxide carbide is a pseudomorphous proc
ess. The results suggest that the reaction occurs in two steps: reduct
ion by H-2 leading to NbO2 formation and carburization/reduction of th
e NbO2 to NbC.