Method for preparing lithium iron phosphate nanopowder coated with carbon

Patent metadata

Field	Value
Publication number	US-9620776-B2
Application number	US-201414429045-A
Country	US
Kind code	B2
Filing date	Jan 9, 2014
Priority date	Jan 10, 2013
Publication date	Apr 11, 2017
Grant date	Apr 11, 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 reaction 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. A lithium secondary battery including the lithium iron phosphate nanopowder coated with carbon thus prepared as a cathode active material has good capacity and stability.

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 butanediol solvent;
(b) putting the non-aqueous mixture solution into a reactor and reacting to prepare amorphous lithium iron phosphate nanoseed particle under pressure conditions of less than or equal to 10 bar; 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 the nanoseed particle.

2. The method for preparing a lithium iron phosphate nanopowder coated with carbon of claim 1 , wherein the 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 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 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 non-aqueous butanediol solvent is at least one selected from the group consisting of 1,2-butandiol, 1,3-butandiol, 1,4-butandiol, 2,3-butandiol, and an isomer thereof.

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 less than or equal to a boiling point of the non-aqueous butanediol solvent.

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 120 to 235° C. for 0.1 to 24 hours.

11. 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 to 235° C. for 0.1 to 5 hours.

12. 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 to 900° C. for 0.5 to 5 hours.

13. 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) and lithium oxalate (Li 2 C 2 O 4 ), and a mixture thereof.

14. 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) and ferric hydroxide (FeO(OH)), and a mixture thereof.

15. 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 ) and 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

• C01B25/45

  containing plural metal, or metal and ammonium · CPC title

• C01G49/009

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

• H01M10/0525

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

• H01M4/0471

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

• H01M4/136

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