Method for preparing lithium iron phosphate nanopowder coated with carbon

Patent metadata

Field	Value
Publication number	US-9742006-B2
Application number	US-201414516810-A
Country	US
Kind code	B2
Filing date	Oct 17, 2014
Priority date	Jan 10, 2013
Publication date	Aug 22, 2017
Grant date	Aug 22, 2017

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 triethanolamine solvent, (b) putting the mixture solution into a reactor and reacting to prepare amorphous lithium iron phosphate nanoseed particle, and (c) heat treating the lithium iron phosphate nanoseed particle thus to prepare the lithium iron phosphate nanopowder coated with carbon on a portion or a whole of a surface of a particle, and a lithium iron phosphate nanopowder coated with carbon prepared by the above method. The lithium iron phosphate nanopowder coated with carbon having controlled particle size and particle size distribution may be prepared in a short time by performing two simple steps.

First claim

What is claimed is:

1. A method for preparing a lithium iron phosphate nanopowder coated with carbon, comprising the steps of:
(a) preparing a non-aqueous mixture solution by adding a lithium precursor, an iron precursor and a phosphorus precursor in a non-aqueous triethanolamine solvent;
(b) reacting the non-aqueous mixture solution to prepare an amorphous lithium iron phosphate nanoseed particle; and
(c) heat treating the amorphous lithium iron phosphate nanoseed particle to prepare a lithium iron phosphate nanopowder coated with carbon on a portion or a whole of a surface thereof,
wherein the step (b) is performed under pressure conditions of less than or equal to 10 bar.

2. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , wherein the amorphous lithium iron phosphate nanoseed particle prepared in the above Step (b) go through at least one step among a cooling step, a washing step and a drying step.

3. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 2 , wherein the washing is performed by consecutively using acetone and methanol.

4. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 2 , wherein the drying is performed at a temperature range of 20° C. to 160° C. for 2 to 40 hours.

5. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , further comprising the step of adding an organic compound in the above Step (a), Step (b), or Step (c).

6. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 5 , wherein the organic compound is at least one selected from the group consisting of glucose, sucrose, galactose, fructose, lactose, starch, mannose, ribose, aldohexose, ketohexose, and a mixture thereof.

7. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 5 , wherein the amount of the organic compound is 0.1 wt % to 5 wt % based on a total amount of the lithium iron phosphate nanoseed particle prepared in Step (b).

8. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , wherein the above Step (b) is performed at a temperature less than or equal to a boiling point of the triethanolamine solvent.

9. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , wherein the above Step (b) is performed at a temperature range of 120° C. to 335° C. for 0.1 to 24 hours.

10. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , wherein the above Step (b) is performed at a temperature range of 150° C. to 335° C. for 0.1 to 5 hours.

11. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , wherein the above Step (c) is performed at a temperature range of 400° C. to 900° C. for 0.5 to 5 hours.

12. The method for preparing a lithium iron phosphate nanopowder coated with carbon 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), lithium oxalate (Li 2 C 2 O 4 ), and a mixture thereof.

13. The method for preparing a lithium iron phosphate nanopowder coated with carbon 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), ferric hydroxide (FeO(OH)), and a mixture thereof.

14. The method for preparing a lithium iron phosphate nanopowder coated with carbon 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 ), phosphoric acid (H 3 PO 4 ), and a mixture thereof.

Assignees

• Lg Chemical Ltd

Inventors

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

Classifications

• H01M4/049

  Manufacturing of an active layer by chemical means · CPC title

• H01M4/587

  for inserting or intercalating light metals · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title

• H01M4/58

  of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title