In the plasma of pulsed high-voltage discharge, initiated between nickel electrodes in air, when the fluoroplastic is placed in the discharge gap, powder nanocomposite material has been synthesized. The nanocomposite contains NiF2 nanoparticles less than 5 nm in size, dispersed in a matrix consisting of carbon and fluorocarbon substances. The carbonaceous substance contains nanoscale disordered graphite-like regions. The fluorocarbon component of the composite contains fragments of PTFE molecules and fluorocarbon molecular fragments that differ in structure from PTFE molecule’s structure. After annealing the composite in air at 773 K, the initial nanocomposite is transformed into a nanocomposite containing nanosized PTFE and nanoparticles of NiF2 less than 5 nm in size, scattered in a matrix composed of nanographite and low-layer nanosized graphene, after aneling at 1173 K into a material containing NiO nanoparticles less than 10 nm in size. After annealing of the initial nanocomposite in argon atmosphere at 1073 K, the obtained nanocomposite contains Ni nanoparticles with sizes less than 5 nm and carbon and fluorocarbon components. The magnetic susceptibility of the unannealed nanocomposite is investigated. A transition to the antiferromagnetic phase at 73 K was detected. At T = 4K, exchange bias interaction of the AFM / FM type takes place in the composite. There is divergence of the FC and ZFC curves, which can be explained by the presence of a superparamagnetic phase or a spin glass phase in the sample. The field dependences of the magnetic susceptibility measured at T = 300 K show sharp changes that occur at certain values of the magnetic field. Elucidation of the nature of these changes requires additional research.