Ni-doped phenol resin was prepared with 1∶100 mass ratio of Ni( NO_3)_2·6H_2O to thermosetting phenol resin to optimize the structure and properties of pyrolytic carbon derived from phenol resin and increase its carbon yield. The specimens were cured at 200 ℃ and carbonized under different atmospheres( carbon-embedded atmosphere and Ar atmosphere) and at different temperatures( 600,800,1000 and 1200 ℃) for3 h,respectively. The carbon yield was measured. Thermal decomposition characteristics of Ni-doped phenol resin,and the oxidation resistance,phase composition and microstructure of pyrolytic carbon were characterized by differential scanning calorimetry,X-ray diffraction,energy dispersive spectroscopy, scanning electron microscopy and transmission electron microscopy. The results show that the carbon yield of Ni-doped phenol resin carbonized at800 or 1 000 ℃ is increased significantly,compared with that without any dopants. The graphitization degree of pyrolytic carbon structure derived from Ni-doped phenol resin increases with the increase of carbonization temperature. The massive multi-wall carbon nanotubes of 50-100 nm in diameter and of micrometre scale in length are generated at 1000 ℃. Compared with the carbonembedded atmosphere,carbon nanotubes can be more easily generated in Ar atmosphere,resulting in higher carbon yield and degree of crystallinity of the pyrolyticcarbon derived from Ni-doped phenol resin. The oxidation resistance of the pyrolytic carbon derived from Ni-doped phenol resin at 1200 ℃ is improved significantly and its highest oxidation temperature is increased by about 84℃,compared with that from Ni free phenol resin. Ni-doped phenol resin was prepared with 1: 100 mass ratio of Ni (NO_3) _2 · 6H_2O to thermosetting phenol resin to optimize the structure and properties of pyrolytic carbon derived from phenol resin and increase its carbon yield. ℃ and carbonized under different atmospheres (carbon-embedded atmosphere and Ar atmosphere) and at different temperatures (600,800, 1000 and 1200 ° C) for 3 h, respectively. Thermal decomposition characteristics of Ni-doped phenol resin, and the oxidation resistance, phase composition and microstructure of pyrolytic carbon were characterized by differential scanning calorimetry, X-ray diffraction, energy dispersive spectroscopy, scanning electron microscopy and transmission electron microscopy. The results show that the carbon yield of Ni-doped phenol resin carbonized at800 or 1 000 ℃ is increased significantly, compared with that without any dopants. The graphitization degree of pyrolytic carbon struct ure derived from Ni-doped phenol resin increases with the increase of carbonization temperature. The massive multi-wall carbon nanotubes of 50-100 nm in diameter and of micrometre scale in length at 1000 ° C. Compared with the carbonembedded atmosphere, carbon nanotubes can be more easily generated in Ar atmosphere, resulting in higher carbon yield and degree of crystallinity of the pyrolyticcarbon derived from Ni-doped phenol resin. The oxidation resistance of the pyrolytic carbon derived from Ni-doped phenol resin at 1200 ° C is improved significantly and its highest oxidation temperature is increased by about 84 ° C, compared with that from Ni free phenol resin.