Abstract: Calcium lignosulfonate-phenol-formaldehyde resin (LPF) was prepared by the polymerization of a mixture of calcium lignosulfonate and phenol with formaldehyde using a NaOH catalyst. Nickel nitrate was used as a catalyst for the carbon formation and was added to the LPF before dehydration and curing. The LPF was carbonized at 800, 1 000 and 1 200 ℃ for 3 h. The dispersion of the catalyst (Ni) in the cured LPF and the microstructure of the carbon were investigated by SEM, HR-TEM, XRD and Raman spectroscopy. Results show that Ni is dispersed homogeneously in the LPF. The carbon is a kind of foam with closed cells. The metallic Ni in the carbon catalyzes the formation of carbon nanotubes that extend from the carbon matrix into the closed cells. The number and length of the carbon nanotubes increase and their crystallinity is improved with increasing carbonization temperature and/or the amount of nickel nitrate added.