Method for preparing lithium iron phosphate nanopowder

Patent metadata

Field	Value
Publication number	US-9627685-B2
Application number	US-201414429062-A
Country	US
Kind code	B2
Filing date	Jan 9, 2014
Priority date	Jan 10, 2013
Publication date	Apr 18, 2017
Grant date	Apr 18, 2017

Abstract

The present invention relates to a method for preparing a lithium iron phosphate nanopowder, including the steps of (a) preparing a mixture solution by adding a lithium precursor, an iron precursor and a phosphorus precursor in a reaction solvent, and (b) putting the mixture solution into a reactor and heating to prepare the lithium iron phosphate nanopowder under pressure conditions of 10 to 100 bar, and a lithium iron phosphate nanopowder prepared by the method. When compared to a common hydrothermal synthesis method and a supercritical hydrothermal synthesis method, a reaction may be performed under a relatively lower pressure. When compared to a common glycothermal synthesis method, a lithium iron phosphate nanopowder having effectively controlled particle size and particle size distribution may be easily prepared.

First claim

What is claimed is:

1. A method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery, comprising the steps of:
(a) preparing a mixture solution by adding a lithium precursor, an iron precursor and a phosphorus precursor in a reaction solvent; and
(b) putting the mixture solution into a reactor and heating to prepare the lithium iron phosphate nanopowder under pressure conditions of 10 to 100 bar,
wherein the reaction solvent is at least one selected from the group consisting of 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 2,3-butanediol, and an isomer thereof.

2. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , further comprising the step of (c) heat treating the lithium iron phosphate nanopowder thus prepared to form a coating layer at a portion or a whole of a surface of an individual particle of the nanopowder.

3. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 2 , wherein the heat treating is performed by heating to a temperature range of 400 to 900° C.

4. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein the lithium iron phosphate nanopowder prepared in Step (b) is consecutively washed and dried.

5. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 4 , wherein the washing is performed by consecutively using acetone and methanol.

6. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 4 , wherein the drying is performed at 20 to 160° C. for 2 to 40 hours.

7. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein Step (b) is performed at a temperature less than or equal to a boiling point of the reaction solvent.

8. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein Step (b) is performed at a temperature range of 150 to 235° C.

9. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein Step (b) is performed for 1 to 48 hours.

10. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein the lithium precursor is at least one selected from the group consisting of lithium acetate dihydrate (CH 3 COOLi.2H 2 O), lithium hydroxide monohydrate (LiOH.H 2 O), lithium hydroxide (LiOH), lithium carbonate (Li 2 CO 3 ), lithium phosphate (Li 3 PO 4 ), lithium phosphate dodecahydrate (Li 3 PO 4 .12H 2 O) and lithium oxalate (Li 2 C 2 O 4 ), or a mixture of two or more thereof.

11. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein the iron precursor is at least one selected from the group consisting of iron citrate (FeC 6 H 5 O 7 ), iron citrate hydrate (FeC 6 H 5 O 7 .nH 2 O), ferrous sulfate heptahydrate (FeSO 4 .7H 2 O), iron(II) oxalate dihydrate (FeC 2 O 4 .2H 2 O), iron acetyl acetonate (Fe(C 5 H 7 O 2 ) 3 ), iron phosphate dihydrate (FePO 4 .2H 2 O) and ferric hydroxide (FeO(OH)), or a mixture of two or more thereof.

12. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 1 , wherein the phosphorus precursor is at least one selected from the group consisting of tri-ammonium phosphate trihydrate ((NH 4 ) 3 PO 4 .3H 2 O), ammonium phosphate ((NH 4 ) 2 HPO 4 ), ammonium dihydrogen phosphate (NH 4 H 2 PO 4 ) and phosphoric acid (H 3 PO 4 ), or a mixture of two of more thereof.

Assignees

• Lg Chemical Ltd

Inventors

• Jun In Kook
• Cho Seung Beom
• Oh Myoung Hwan

Classifications

• C01P2002/30

  Three-dimensional structures · CPC title

• C01G49/009

  Compounds containing iron, with or without oxygen or hydrogen, and containing two or more other elements · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• H01M4/587

  for inserting or intercalating light metals · CPC title