The present text describes an investigation of XPS study of multiwall carbon nanotube (MWNT) synthesis. The aim of the investigation was not only to improve the reaction activity by mixing nickel with vanadium, but also to understand the formation mechanism of the nanotubes. Carbon nanotubes were produced by catalytic chemical vapor deposition (CCVD) of acetylene on transition metal containing catalysts supported on zeolite ZSM-5. The samples were characterized at two different levels. At the nanoscale, they were studied by transmission electron microscopy (TEM), while at macroscopic scale mainly XPS was used to investigate the changes during the reaction. (C) 2003 Elsevier B.V. All rights reserved.