Method for preparing lithium iron phosphate nanopowder
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 1 to 10 bar, and a lithium iron phosphate nanopowder prepared by the method. When compared to a common hydrothermal synthesis method, a supercritical hydrothermal synthesis method and a glycothermal synthesis method, a reaction may be performed under a relatively lower pressure. Thus, a high temperature/high pressure reactor is not necessary and process safety and economic feasibility may be secured. In addition, a lithium iron phosphate nanopowder having uniform particle size and effectively controlled particle size distribution may be easily prepared.
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 1 bar or more to less than 10 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 sequentially conducted a washing step and a drying step.
5. The method for preparing a lithium iron phosphate nanopowder for a lithium secondary battery of claim 4 , wherein the washing step is performed by sequentially 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 the 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 72 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 ), and a mixture 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)), and a mixture 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 ), and a mixture thereof.