The present invention relates to a method for preparing a metal phosphate
which comprises milling in a carbonaceous vessel a lithium source, a
phosphate source, such as LiH.sub.2PO.sub.4, and a metal oxide containing
a metal ion wherein the metal ion is capable of being reduced, to
produced a milled mixture and heating the milled mixture in an inert
atmosphere at a temperature and for a time sufficient to form a metal
phosphate wherein the metal ion of the metal oxide is reduced in
oxidation state without the direct addition of a reducing agent to the
starting materials. In another embodiment the present invention relates
to a method for preparing a mixed metal phosphate which comprises milling
a lithium source and a phosphate source, such as LiH.sub.2PO.sub.4, a
metal oxide and another metal compound wherein at least one of the metal
compounds contains a metal ion capable of being reduced to produce a
milled mixture and heating the resulting milled mixture in an inert
atmosphere at a temperature and for a time sufficient to form a mixed
metal phosphate, wherein the oxidation state of at least one of the metal
ions is reduced in oxidation state without the direct addition of a
reducing agent to the reactants. It is another object of the invention to
provide electrochemically active materials produced by said methods.