Using Raman spectroscopy and X-ray photoelection spectroscopy (XPS), synthesized lithium iron(II) phosphate (LiFePO4) and carbon coated nanocomposites LiFePO4/С, synthesized by annealing LiFePO4 with glucose for 1 and 12 hours at 700 °C, have been investigated. According to XPS data, the synthesis conditions of LiFePO4/С nanocomposite (700 °C, 1 hour) facilitate the reduction of iron, Fe 3+ → Fe 2+ , on the sample surface. Also according to C1s spectra, sp 2 C-sp 2 C is the main bond type in the samples under investigation. Contributions relating to C-O, C=O, C-O-C, O-C=O functional groups are also present. According to X-ray diffraction analysis, a 12-hour synthesis of LiFePO4/C nanocomposite leads to the formation of impurities. According to Raman spectra, the annealing time does not affect the quality of carbon coating: the peak intensity ratio of bands D and G has a value of 1.06 for the material annealed for 1 hour and 1.04 for LiFePO4/С nanocomposite after annealing for 12 hours.