Method for preparing lithium iron phosphate nanopowder coated with carbon

Patent metadata

Field	Value
Publication number	US-10153488-B2
Application number	US-201414421633-A
Country	US
Kind code	B2
Filing date	Jan 9, 2014
Priority date	Jul 9, 2013
Publication date	Dec 11, 2018
Grant date	Dec 11, 2018

Abstract

The present invention relates to a method for preparing a lithium iron phosphate nanopowder coated with carbon, including the steps of (a) preparing a mixture solution by adding a lithium precursor, an iron precursor and a phosphorus precursor in a glycol-based solvent, (b) putting the mixture solution into a reactor, heating and concentrating to prepare a metal glycolate slurry, (c) drying the metal glycolate slurry to form a solid content, and (d) firing the solid content to prepare the lithium iron phosphate nanopowder coated with carbon, and a lithium iron phosphate nanopowder coated with carbon prepared by the method.

First claim

What is claimed is:

1. A method for preparing a lithium iron phosphate nanopowder having a carbon coating layer, comprising the steps of:
(a) preparing a mixture solution comprising a lithium precursor, an iron precursor, a phosphorus precursor, and a glycol-based solvent;
(b) heating the mixture solution to a temperature of at least a boiling point of the glycol-based solvent used and concentrating to prepare a metal glycolate slurry;
(c) drying the metal glycolate slurry to form a solid content; and
(d) firing the solid content at a temperature ranging from 400° C. to 900° C. in an anaerobic or inert gas atmosphere to prepare the lithium iron phosphate nanopowder having the carbon coating layer.

2. The method of claim 1 , wherein the heating and concentrating in Step (b) is performed under pressure conditions less than or equal to 10 bar.

3. The method of claim 1 , wherein the drying in Step (c) is performed in a convention oven at a temperature range of 100 to 180° C.

4. The method of claim 1 , wherein the firing of Step (d) is performed at a temperature range of 400 to 900° C. for 2 to 10 hours.

5. The method of claim 1 , wherein the glycol-based solvent is selected from the group consisting of ethylene glycol, diethylene glycol and 1,4-butandiol.

6. The method 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.

7. The method 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.

8. The method 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.

9. A lithium iron phosphate nanopowder having a carbon coating layer, comprising:
second particles, wherein the second particles are agglomerates of a plurality of first particles, wherein the first particles have an olivine crystal structure; and
a carbon coating layer disposed on a portion or a whole of a surface of the first particle,
wherein an average particle diameter (D50) of the second particles is from 300 to 1,000 nm, and wherein an average particle diameter (D50) of the first particles is from 20 to 100 nm.

10. The lithium iron phosphate nanopowder having the carbon coating layer of claim 9 , wherein a thickness of the carbon coating layer is from 0.5 to 5 nm.

11. The lithium iron phosphate nanopowder having the carbon coating layer of claim 9 , wherein the lithium iron phosphate is LiFePO 4 .

12. A cathode active material comprising the lithium iron phosphate nanopowder having the carbon coating layer of claim 10 .

13. The cathode active material of claim 12 , further comprising at least one selected from a conductive agent, a binder and a filler.

14. A cathode for a lithium secondary battery comprising a cathode current collector and the cathode active material of claim 12 coated on the cathode current collector.

15. A lithium secondary battery comprising the cathode of claim 14 , an anode, a separator and a non-aqueous electrolyte comprising a lithium salt.

Assignees

• Lg Chemical Ltd

Inventors

• Jang Wook
• Cho Seung Beom
• Jun In Kook

Classifications

• H01M4/521 Primary

  of iron for aqueous cells · CPC title

• H01M4/136

  Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy · CPC title

• H01M4/366

  as layered products · CPC title

• H01M4/0402

  Methods of deposition of the material · CPC title

• H01M2004/021

  Physical characteristics, e.g. porosity, surface area · CPC title