Manufacturing method of composite oxide and manufacturing method of power storage device
View Patent ↗An object is to reduce variation in shape of crystals that are to be manufactured. Raw materials are each weighed, solutions containing the respective raw materials are formed in an environment where an oxygen concentration is lower than that in air, the solutions containing the respective raw materials are mixed in an environment where an oxygen concentration is lower than that in air to form a mixture solution, and with use of the mixture solution, a composite oxide is formed by a hydrothermal method.
1. A production method of a compound comprising the steps of:
forming a solution consisting essentially of water and lithium phosphate in an atmosphere having an oxygen concentration lower than the oxygen concentration in air;
forming an aqueous solution containing a transition metal selected from the group consisting of iron (Fe), cobalt (Co), nickel (Ni), and manganese (Mn) in an atmosphere having an oxygen concentration lower than the oxygen concentration in air;
mixing the solution consisting essentially of water and lithium phosphate with the aqueous solution containing the transition metal in an atmosphere having an oxygen concentration lower than the oxygen concentration in air to form a mixture solution; and
forming a compound from the mixture solution by a hydrothermal method in which the mixture solution is subjected to heat and pressure treatment in the atmosphere having an oxygen concentration lower than an oxygen concentration in air,
wherein an oxygen concentration in the mixture solution is lower than or equal to 4.5 ppm,
wherein the compound is represented by general formula LiMPO 4 , and
wherein M denotes the transition metal selected from the group consisting of Fe, Co, Ni, and Mn.
2. The production method of a compound according to claim 1 , wherein the atmosphere having an oxygen concentration lower than the oxygen concentration in air is a nitrogen atmosphere.
3. The production method of a compound according to claim 1 , wherein the atmosphere having an oxygen concentration lower the oxygen concentration in air is a mixed atmosphere of nitrogen and hydrogen.
4. A production method of a compound comprising the steps of:
forming a solution consisting essentially of water and lithium phosphate in an atmosphere having an oxygen concentration lower than the oxygen concentration in air;
forming an aqueous solution containing a transition metal selected from the group consisting of iron (Fe), cobalt (Co), nickel (Ni), and manganese (Mn) in an atmosphere having an oxygen concentration lower than the oxygen concentration in air;
mixing the solution consisting essentially of water and lithium phosphate with the aqueous solution containing the transition metal in an atmosphere having an oxygen concentration lower than the oxygen concentration in air to form a mixture solution;
adding a reducing agent into the mixture solution; and
forming a compound from the mixture solution by a hydrothermal method in which the mixture solution is subjected to heat and pressure treatment in an atmosphere having an oxygen concentration lower than the oxygen concentration in air,
wherein an oxygen concentration in the mixture solution is lower than or equal to 4.5 ppm,
wherein the compound is represented by general formula LiMPO 4 , and
wherein M denotes the transition metal selected from the group consisting of Fe, Co, Ni, and Mn.
5. The production method of a compound according to claim 4 , wherein the atmosphere having an oxygen concentration lower than the oxygen concentration in air is a nitrogen atmosphere.
6. The production method of a compound according to claim 4 ,
wherein the atmosphere having an oxygen concentration lower than the oxygen concentration in air is a mixed atmosphere of nitrogen and hydrogen.
7. The production method of a compound according to claim 4 , further comprising the steps of:
introducing the reducing agent into a container resistant to pressure;
introducing the mixture solution into the container resistant to pressure; and
forming the compound by the hydrothermal method in the container resistant to pressure.
8. The production method of a compound according to claim 1 ,
wherein the water for forming the solution consisting essentially of water and lithium phosphate and the water for forming the aqueous solution containing transition metal are subjected to nitrogen bubbling.
9. The production method of a compound according to claim 4 ,
wherein the water for forming the solution consisting essentially of water and lithium phosphate and the water for forming the aqueous solution containing transition metal are subjected to nitrogen bubbling.