The different methods of the phosphorus-containing copper/carbon nanocomposites formation are considered in this chapter. The difference of methods is concluded as follows: (1) The mixing-grinding of reagents in relation 1:1; (2) The mixing-grinding of reagents with addition of water small qualities; and (3) the mixing-grinding of reagents with last vacuum using. The estimation of investigation results is carried out by 162the means of IR-spectroscopy and X-ray photoelectron spectroscopy. Better results were obtained when the second variant was utilized. In this case, the atomic magnetic moment is increased from 1.3 to 3 Bohr Magneton, and the oxidation state of phosphorus atom is decreased from +5 to 0, according to X-ray photoelectron spectra. These data correspond to IR spectra.