Methods for making lithium manganese phosphate and lithium manganese phosphate/carbon composite material

Patent metadata

Field	Value
Publication number	US-2017040596-A1
Application number	US-201615333907-A
Country	US
Kind code	A1
Filing date	Oct 25, 2016
Priority date	Apr 29, 2014
Publication date	Feb 9, 2017
Grant date	—

Abstract

A method for making lithium manganese phosphate is disclosed. A divalent manganese source, a lithium source and a phosphate source are mixed and dissolved in a solvothermal reaction medium to form a mixed solution. The solvothermal reaction medium includes an organic solvent and a solubilizing agent. The mixed solution is then solvothermal reacted. A method for making lithium manganese phosphate/carbon composite material is also disclosed.

First claim

What is claimed is:

1 . A method for making lithium manganese phosphate, the method comprising:
mixing and dissolving a divalent manganese source, a lithium source, and a phosphate source in a solvothermal reaction medium to form a mixed solution, the solvothermal reaction medium comprising an organic solvent and a solubilizing agent; and solvothermal reacting the mixed solution.

2 . The method of claim 1 , further comprising dissolving a metal doping source with the divalent manganese source, the lithium source, and the phosphate source in the solvothermal reaction medium to form the mixed solution comprising the metal dopant source, the divalent manganese source, the lithium source, and the phosphate source mixed with each other.

3 . The method of claim 2 , wherein the metal doping source comprises a doping element selected from the group consisting of alkaline-earth metal elements, Group-13 elements, Group-14 elements, transition metal elements, rare-earth elements, and combinations thereof.

4 . The method of claim 2 , wherein the metal doping source comprises a doping element, the doping element being Fe.

5 . The method of claim 1 , wherein the divalent manganese source is selected from the group consisting of manganese chloride, manganese nitrate, manganese sulfate, manganese acetate, and combinations thereof.

6 . The method of claim 1 , wherein the lithium source is selected from the group consisting of lithium hydroxide, lithium acetate, lithium carbonate, lithium oxalate, and combinations thereof.

7 . The method of claim 1 , wherein the phosphate source is selected from the group consisting of phosphoric acid, lithium dihydrogen phosphate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, and combinations thereof.

8 . The method of claim 1 , wherein the organic solvent is selected from the group consisting of diols, polyols, and combinations thereof.

9 . The method of claim 1 , wherein the organic solvent is selected from the group consisting of ethylene glycol, glycerol, diethylene glycol, triethylene glycol, tetraethylene glycol, butanetriol, n-butanol, isobutanol, and combinations thereof.

10 . The method of claim 1 , wherein the solubilizing agent is selected from the group consisting of alkyl phenol polyoxyethylene ether, fatty alcohol ethoxylate, polyethylene glycol, polyolester, and combinations thereof.

11 . The method of claim 1 , wherein a volume ratio of the organic solvent and the solubilizing agent is in a range from about 9:1 to about 3:2.

12 . The method of claim 1 , wherein the solvothermal reaction medium is water-free.

13 . The method of claim 1 , wherein a mass percentage of water in the mixed solution is less than 1%.

14 . The method of claim 1 , wherein the mixing and dissolving the divalent manganese source, the lithium source, and the phosphate source in the solvothermal reaction medium to form the mixed solution comprises:
providing the divalent manganese source solution, the lithium source solution, and the phosphate source solution; adding the phosphate source solution portion by portion to the divalent manganese source solution to form a first liquid solution; and adding the first liquid solution portion by portion to the lithium source solution to form the mixed solution.

15 . The method of claim 1 , wherein the solvothermal reacting is carried out at a temperature of about 120° C. to about 240° C.

16 . The method of claim 1 , further comprising heating the lithium manganese phosphate in a protective gas at a temperature range from about 200° C. to about 800° C.

17 . The method of claim 1 , wherein the solvothermal reaction medium further comprises a carbonaceous nanosized material dispersed in the organic solvent.

18 . The method of claim 17 , wherein the carbonaceous nanosized material is selected from the group consisting of graphene, carbon nanotubes, carbon nanofibers, carbon nanoballs, and combinations thereof.

19 . A method for making lithium manganese phosphate/carbon composite material comprising:
dispersing a carbonaceous material in a solvothermal reaction medium to form a dispersed solution, the solvothermal reaction medium comprising an organic solvent and a solubilizing agent; mixing and dissolving a divalent manganese source, a lithium source, and a phosphate source in the dispersed solution to form a mixed solution; and solvothermal reacting the mixed solution.

20 . The method of claim 19 , wherein the carbonaceous material is selected from the group consisting of graphene, carbon nanotubes, carbon nanofibers, carbon nanoballs, and combinations thereof.

Assignees

• Jiangsu Huadong Inst Of Li-Ion Battery Co Ltd
• Univ Tsinghua

Inventors

• Wang Li
• He xiang-ming
• Liu shao-jun
• Zhang jian-li
• Luo Jing
• Shang yu-ming
• Li Jian-Jun
• Gao Jian
• Ren Yumei
• Zhang hong-sheng

Classifications

• H01M4/5825

  Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines · CPC title

• C01B25/45 Primary

  containing plural metal, or metal and ammonium · CPC title

• H01M4/0471

  involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title

• C01P2006/40

  Electric properties · CPC title

• H01M4/625

  Carbon or graphite · CPC title