Methods of making transition metal compounds useful as cathode active materials
View Patent ↗A method for carrying out solid state reactions under reducing conditions is provided. Solid state reactants include at least one inorganic metal compound and a source of reducing carbon. The reaction may be carried out in a reducing atmosphere in the presence of reducing carbon. Reducing carbon may be supplied by elemental carbon, by an organic material, or by mixtures. The organic material is one that can form decomposition products containing carbon in a form capable of acting as a reductant. The reaction proceeds without significant covalent incorporation of organic material into the reaction product. In a preferred embodiment, the solid state reactants also include an alkali metal compound. The products of the method find use in lithium ion batteries as cathode active materials. Preferred active materials include lithium-transition metal phosphates and lithium-transition metal oxides. In a preferred embodiment, the reaction product contains carbon particles intimately mixed among crystals of the active materials.
1. A solid state method for synthesizing an inorganic metal compound comprising the steps of:
combining starting materials comprising at least one metal compound and at least one source of reducing carbon to form a mixture;
providing an atmosphere comprising a reducing gas; and
heating the mixture in the atmosphere at a temperature and for a time sufficient to form a reaction product,
wherein at least one metal ion of the starting materials is reduced in oxidation state during heating, to form the inorganic metal compound.
2. A method according to claim 1 , wherein the reducing gas comprises hydrogen.
3. A method according to claim 1 , wherein the reducing carbon comprises elemental carbon.
4. A method according to claim 1 , wherein the reducing carbon comprises a carbohydrate.
5. A method according to claim 1 , wherein the reducing carbon comprises an organic material.
6. A method according to claim 1 , wherein the reaction product comprises a lithiated mixed metal phosphate active material.
7. A method according to claim 1 , wherein the reaction product comprises a lithiated metal oxide active material.
8. A method according to claim 1 , wherein the starting materials further comprise an alkali metal compound.
9. A method according to claim 8 , wherein the alkali metal compound comprises a lithium compound.
10. A method according to claim 1 , further comprising the step of reacting an alkali metal compound with the reaction product.
11. A method according to claim 10 , wherein the alkali metal compound comprises a lithium compound.
12. A method according to claim 1 , wherein the reducing carbon is provided in stoichiometric excess.