The nucleation and growth of vanadium oxide nanotubes
(VO
x
-NT) have been followed by a combination
of numerous
ex situ techniques along the hydrothermal process. Intermediate solid
phases extracted at different reaction times have been characterized
by powder X-ray diffraction, scanning and transmission electron microscopy,
electron spin resonance, and V–K edge X-ray absorption near-edge
structure spectroscopy. The supernatant vanadate solutions extracted
during the hydrothermal treatment have been studied by liquid 51V NMR and flame spectroscopy. For short durations of the
hydrothermal synthesis, the initial V2O5-surfactant
intercalate is progressively transformed into VO
x
-NT whose crystallization starts to be detected after a hydrothermal
treatment of 24 h. Upon heating from 24 h to 7 days, VO
x
-NT are obtained in larger amount and with an improved
crystallinity. The detection of soluble amines and cyclic metavanadate
[V4O12]4– in the supernatant
solution along the hydrothermal process suggests that VO
x
-NT result from a dissolution–precipitation
mechanism. Metavanadate species [V4O12]4– could behave as molecular precursors in the polymerization
reactions leading to VO
x
-NT.