Novel process for the preparation of finely divided, nano-structured, olivine lithium metal phosphates (LiMPO.sub.4) (where metal M is iron, cobalt, manganese, nickel, vanadium, copper, titanium and mix of them) materials have been developed. This so called Polyol” method consists of heating of suited precursor materials in a multivalent, high-boiling point multivalent alcohol like glycols with the general formula HO—(—C2H4O—).sub.n-H where n=1-10 or HO—(—C3H6O—).sub.n.-H where n=1-10, or other polyols with the general formula HOCH2—(—C3H5OH—).sub.n-H where n=1-10, like for example the tridecane-1,4,7,10,13-pentaol. A novel method for implementing the resulting materials as cathode materials for Li.-ion batteries is also developed.