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In the field of materials for Lithium ion batteries, the lithium iron phosphate LiFePO4 has been proven for use as a positive electrode due to its good resistance to thermal degradation and overcharge, safety and low cost. The use of nanostructured materials would improve its efficiency. This work shows the results of the synthesis of nanostructured materials with functional properties for Lithium batteries through aerosol techniques. The Spray Pyrolysis method allows synthesizing nanostructured particles with spherical geometry, not agglomerates, with narrow distribution of particle size and homogeneous composition in respect to a precursor solution. Experimental techniques were focused on the morphological (SEM and TEM), structural (XRD and HRTEM-SAED), chemical (EDS) and electrochemical characterization.