Method for preparing lithium iron phosphate nanopowder
View Patent ↗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 glycerol solvent, and (b) putting the mixture solution into a reactor and heating to prepare the lithium iron phosphate nanopowder under pressure conditions of 10 bar 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.
1. A method for preparing a lithium iron phosphate nanopowder, comprising the steps of:
(a) preparing a mixture solution by adding a lithium precursor, an iron precursor and a phosphorus precursor in a solvent; and
(b) putting the mixture solution into a reactor and heating to prepare the lithium iron phosphate nanopowder under pressure conditions of 10 bar to 100 bar,
wherein the solvent is non-aqueous, and the solvent is glycerol only,
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), 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,
wherein a mixing ratio of the lithium precursor, the iron precursor and the phosphorus precursor in step (a) is 0.1-1:1:0.1-1 by a molar ratio, and
wherein a particle diameter of the lithium iron phosphate nanopowder is from 30 nm to 300 nm.
2. The method for preparing a lithium iron phosphate nanopowder 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 of claim 2 , wherein the heat treating is performed by heating to a temperature range of 400° C. to 900° C.
4. The method for preparing a lithium iron phosphate nanopowder 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 of claim 4 , wherein the drying is performed at 20° C. to 160° C. for 2 to 40 hours.
6. The method for preparing a lithium iron phosphate nanopowder of claim 1 , wherein Step (b) is performed at a temperature less than or equal to a boiling point of the glycerol solvent.
7. The method for preparing a lithium iron phosphate nanopowder of claim 1 , wherein Step (b) is performed at a temperature range of 150° C. to 290° C.
8. The method for preparing a lithium iron phosphate nanopowder of claim 1 , wherein Step (b) is performed for 1 to 48 hours.
9. The method for preparing a lithium iron phosphate nanopowder 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 thereof.
10. The method for preparing a lithium iron phosphate nanopowder 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.