The methods for the synthesis of lithium iron phosphate LiFePO4 with olivine structure have been developed. New materials based on lithium iron phosphate, including doped with metals, the «LiFePO4 + carbon» composites obtained by pyrolysis of organic compounds have been synthesized. Crystallographic characterization of the synthesized materials was carried out; their electrochemical characteristics of the extraction and intercalation of lithium have been identified. A correlation between the crystallographic and electrochemical characteristics of the materials was found. It was confirmed that an effective way to improve the electrical conductivity of LiFePO4 is to create a carbon shell of the products of pyrolysis of organic compounds on the material's particles surface. A correlation of electrical conductivity and temperature of synthesis of the material was determined. The sequence of chemical interaction between precursors for the synthesis of LiFePO4 is defined; the mechanism of solid-phase interaction is described.