CN101575093A - Preparation process of lithium iron phosphate material - Google Patents
Preparation process of lithium iron phosphate material Download PDFInfo
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- CN101575093A CN101575093A CNA2009100651270A CN200910065127A CN101575093A CN 101575093 A CN101575093 A CN 101575093A CN A2009100651270 A CNA2009100651270 A CN A2009100651270A CN 200910065127 A CN200910065127 A CN 200910065127A CN 101575093 A CN101575093 A CN 101575093A
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- Prior art keywords
- lithium
- lifepo
- carbon source
- hour
- iron phosphate
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- -1 polyoxyethylene Polymers 0.000 claims abstract description 7
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 6
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- 229930006000 Sucrose Natural products 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 229960004887 ferric hydroxide Drugs 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 125000000185 sucrose group Chemical group 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000002270 dispersing agent Substances 0.000 abstract 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 abstract 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000002083 X-ray spectrum Methods 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation process of a lithium iron phosphate material. The process includes the following steps of: step 1: formulating lithium salt solution containing dispersant polyoxyethylene; step 2: putting ferric orthophosphate into the formulated lithium salt solution step by step, continuously stirring the mixed solution to fully react, mix and form colloidal solution in which the total mol rate of lithium to iron is 1.05-1.0; step 3: adding carbon source to the prepared colloidal solution with the adding amount being 20-40g/mol (Li<+>), and drying after uniform mixing; and step 4: sintering the dried material of step 3 under the protection of nitrogen and preparing the finished product of lithium iron phosphate. After being ground and sieved, the lithium iron phosphate material produced by using the preparation process has the carbon content of 3.8-5.2%, compact density of 1.0-1.3g/mL and testing volume up to 150-160mA/h (0.2C). The volume is improved by over 15% compared with that of a solid ball milling method.
Description
Technical field
The present invention relates to a kind of LiFePO 4 material, especially relate to a kind of preparation technology who can be used as the iron lithium phosphate of power lithium-ion battery positive electrode material.
Background technology
Characteristics such as LiFePO 4 material has that security is good, cycle performance is excellent, environmental friendliness, raw material sources are extensive are acknowledged as the first-selected positive electrode material of lithium ion battery of new generation, have become the primary study and the developing direction of main developed country in the world today.Since the complicated process of preparation of this material, the technical threshold height, and industrialization speed is also relatively slow, only has the fewer companies of indivedual developed countries to realize batch process at present.
The starting material that the preparation LiFePO 4 material needs have two or more more, and each material all is solid powders, and how each starting material being mixed is one of key issue that influences material settling out.At present; lithium iron phosphate preparation method mostly adopts high temperature solid-state method, mixes general solid ball milling or the solid-alcohol ball milling of adopting early stage, and these class methods can only guarantee that each stock yard reaches the mixing of micron level; not only influence the performance of LiFePO 4 material, also limited its large-scale production.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology of LiFePO 4 material of suitable batch process.
For achieving the above object, the present invention can take following technical proposals:
The preparation technology of LiFePO 4 material of the present invention, it comprises the steps:
The first step: preparation contains the lithium salt solution of dispersion agent polyoxyethylene glycol: use deionized water as solvent, add lithium hydroxide, lithium concentration is 2～5mol/L, and the polyoxyethylene glycol add-on is 25～100 grams per liters, be heated to 60～90 ℃, be stirred to solid and dissolve stand-by fully;
Second step: Orthophosphoric acid Ferrum is progressively put in the above-mentioned lithium salt solution for preparing, be continuously stirring to abundant reaction, mixing, generate and contain Fe
3+, PO
4 3-, Li
+Ferric hydroxide colloid solution, in the described colloidal solution, total lithium, iron mol ratio are 1.05: 1.0;
The 3rd goes on foot: go on foot in the colloidal solution that makes second and add carbon source, the addition of described carbon source is 20～40g/mol (Li
+), mix the back oven dry;
The 4th step: the material after the oven dry of the 3rd step is carried out sintering under nitrogen protection, make the iron lithium phosphate finished product.
The sintering process in described the 4th step is: material is placed in the sintering oven, feeds nitrogen protection, be warming up to 350～500 ℃ in 1～2 hour, constant temperature 3～5 hours; After be warming up to 600～700 ℃ in 1～2 hour, constant temperature 7～9 hours; Be warming up to 700～750 ℃ through 0.2～1 hour again, constant temperature 1～2 hour; After be cooled in 4～6 hours below 45 ℃, make finished product and come out of the stove and get final product.
After adding carbon source in described the 3rd step, mix, under 100 ℃ of conditions, dry.
Described carbon source is sucrose, glucose or white sugar.
The invention has the advantages that and adopted the liquid phase colloid to mix when mix early stage, make each raw material in solution, reach the degree of mixing of ionic level.Adopt above-mentioned hybrid mode, on the one hand the mixture homogeneity of raw material is greatly improved, reach the degree that mixes of ionic level; Liquid phase colloid blending means in solution has good repeatability on the other hand, is more suitable for producing in batches.In the sintering procedure in later stage, adopt once sintered method, can reduce energy consumption, shorten sintering time, increase the output in the unit time.
The LiFePO 4 material that adopts preparation technology of the present invention to produce, through crushing screening, carbon content is 3.8～5.2%, tap density is 1.0～1.3g/mL, test capacity reaches 150～160mA/h (0.2C), compares with the solid ball milled, and capacity has improved more than 15%.
From the laser particle size distribution plan of iron lithium phosphate product, as can be seen, adopt prepared LiFePO 4 material narrow particle size distribution, the particle diameter that goes out of the present invention little; Maximum particle diameter is less than 20 microns, and meso-position radius is 2～3 microns.
As can be seen, adopting the prepared LiFePO 4 material that goes out of the present invention is pure olivine-type iron lithium phosphate, does not have other assorted peaks from the X-ray spectra of iron lithium phosphate product.
Description of drawings
Fig. 1 is the laser particle size distribution plan of iron lithium phosphate product.X-coordinate is a size, unit: micron, ordinate zou is a volume percent, represents that powder granule volume under the corresponding particle diameter accounts for the size of cumulative volume.
Fig. 2 is the X-ray spectra of iron lithium phosphate product.X-coordinate is 2 θ angles, and ordinate zou is represented the intensity size at peak.
Embodiment
Embodiment 1:
Take by weighing 45 gram LiOH*H
2O is dissolved in 300 ml deionized water, adds 30 gram polyoxyethylene glycol, stirs, is heated to 60 degree, and dissolving forms uniform solution; Take by weighing 190 gram FePO
4* xH
2O progressively drops into, continuously stirring, and heating keeps temperature 60 degree; FePO
4* xH
2After the O adding finishes, add 30 gram sucrose; Heated and stirred stopped heating in 30 minutes, continued to stir until the mixture temperature to be lower than 30 degree; At last the material that mixes is put into 100 degree drying in oven, the material after the oven dry is inserted in the tubular type retort furnace, is fed under the nitrogen protection, is warming up to 350 ℃ through 1 hour, constant temperature 3 hours; After be warming up to 600 ℃ in 1 hour, constant temperature 7 hours; Be warming up to 700 ℃ through 0.2 hour again, constant temperature 1 hour; After be cooled in 4 hours below 45 ℃ and can make the iron lithium phosphate finished-product material by sintering.Products obtained therefrom is through crushing screening, and test capacity reaches 155mA/h (0.2C), and carbon content is 5.2%, and tap density is 1.02g/mL.
Embodiment 2:
Take by weighing 45 gram LiOH*H2O, be dissolved in 300 ml deionized water, add 10 gram polyoxyethylene glycol, stir, be heated to 70 degree, dissolving forms uniform solution; Take by weighing 190 gram FePO
4* xH
2O progressively drops into, continuously stirring, and heating keeps temperature 70 degree; FePO
4* xH
2After the O adding finishes, add 20 gram sucrose; Heated and stirred stopped heating in 30 minutes, continued to stir until the mixture temperature to be lower than 30 degree; Mixture was put into 100 degree drying in oven 4 hours; After the oven dry, material is inserted in the tubular type retort furnace, is fed under the nitrogen protection, is warming up to 500 ℃ through 2 hours, constant temperature 5 hours; After be warming up to 700 ℃ in 2 hours, constant temperature 9 hours; Be warming up to 750 ℃ through 1 hour again, constant temperature 2 hours; After be cooled in 6 hours below 45 ℃, sintering is made the iron lithium phosphate finished-product material.Products obtained therefrom is through crushing screening, and test capacity reaches 152mA/h (0.2C).Carbon content is 3.8%, and tap density is 1.24g/mL.
Claims (4)
1, a kind of preparation technology of LiFePO 4 material, it is characterized in that: it comprises the steps:
The first step: preparation contains the lithium salt solution of dispersion agent polyoxyethylene glycol: as solvent, add lithium hydroxide with deionized water, lithium concentration is 2～5mol/L, the polyoxyethylene glycol add-on is 25～100 grams per liters, be heated to 60～90 ℃, be stirred to solid and dissolve fully, stand-by;
Second step: Orthophosphoric acid Ferrum is progressively put in the above-mentioned lithium salt solution for preparing, be continuously stirring to abundant reaction, mixing, generate and contain Fe
3+, PO
4 3-, Li
+Ferric hydroxide colloid solution, in the described colloidal solution, total lithium, iron mol ratio are 1.05: 1.0;
The 3rd goes on foot: go on foot in the colloidal solution that makes second and add carbon source, the addition of described carbon source is 20～40g/mol Li
+, mix the back oven dry;
The 4th step: the material after the oven dry of the 3rd step is carried out sintering under nitrogen protection, make the iron lithium phosphate finished product.
2, the preparation technology of LiFePO 4 material according to claim 1 is characterized in that: the sintering process in described the 4th step is: material is placed in the sintering oven, feeds nitrogen protection, be warming up to 350～500 ℃ in 1～2 hour, constant temperature 3～5 hours; After be warming up to 600～700 ℃ in 1～2 hour, constant temperature 7～9 hours; Be warming up to 700～750 ℃ through 0.2～1 hour again, constant temperature 1～2 hour; After be cooled in 4～6 hours below 45 ℃, make finished product and come out of the stove and get final product.
3, the preparation technology of LiFePO 4 material according to claim 1 is characterized in that: after adding carbon source in described the 3rd step, mix, dry under 100 ℃ of conditions.
4, according to the preparation technology of claim 1,2 or 3 described LiFePO 4 materials, it is characterized in that: described carbon source is sucrose, glucose or white sugar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100651270A CN101575093B (en) | 2009-06-05 | 2009-06-05 | Preparation process of lithium iron phosphate material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100651270A CN101575093B (en) | 2009-06-05 | 2009-06-05 | Preparation process of lithium iron phosphate material |
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| Publication Number | Publication Date |
|---|---|
| CN101575093A true CN101575093A (en) | 2009-11-11 |
| CN101575093B CN101575093B (en) | 2011-04-06 |
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|---|---|---|---|
| CN2009100651270A Expired - Fee Related CN101575093B (en) | 2009-06-05 | 2009-06-05 | Preparation process of lithium iron phosphate material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891181A (en) * | 2010-08-11 | 2010-11-24 | 河北工业大学 | Preparation method of pure-phase high-crystallinity lithium iron phosphate |
| CN102005564A (en) * | 2010-09-28 | 2011-04-06 | 烟台卓能电池材料有限公司 | Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid |
| CN102040211A (en) * | 2010-10-29 | 2011-05-04 | 北京工业大学 | Method for synthesizing lithium ion battery cathode material LiFePO4 |
| CN102208625A (en) * | 2011-05-04 | 2011-10-05 | 合肥国轩高科动力能源有限公司 | Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery |
| CN102447109A (en) * | 2011-12-10 | 2012-05-09 | 桂林理工大学 | Method for preparing lithium vanadium phosphate and lithium manganese phosphate composite anode material through rheological phase reaction |
| CN103400986A (en) * | 2013-08-09 | 2013-11-20 | 郑州瑞普生物工程有限公司 | Preparation method of lithium iron phosphorus oxide |
| CN108675276A (en) * | 2018-05-24 | 2018-10-19 | 深圳市毓丰新材料有限公司 | LiFePO4 and preparation method thereof |
-
2009
- 2009-06-05 CN CN2009100651270A patent/CN101575093B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891181A (en) * | 2010-08-11 | 2010-11-24 | 河北工业大学 | Preparation method of pure-phase high-crystallinity lithium iron phosphate |
| CN101891181B (en) * | 2010-08-11 | 2012-01-04 | 河北工业大学 | Preparation method of pure-phase high-crystallinity lithium iron phosphate |
| CN102005564A (en) * | 2010-09-28 | 2011-04-06 | 烟台卓能电池材料有限公司 | Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid |
| CN102040211A (en) * | 2010-10-29 | 2011-05-04 | 北京工业大学 | Method for synthesizing lithium ion battery cathode material LiFePO4 |
| CN102040211B (en) * | 2010-10-29 | 2012-07-04 | 北京工业大学 | Method for synthesizing lithium ion battery cathode material LiFePO4 |
| CN102208625A (en) * | 2011-05-04 | 2011-10-05 | 合肥国轩高科动力能源有限公司 | Preparation method of lithium iron phosphate of cathode material of lithium ion secondary battery |
| CN102447109A (en) * | 2011-12-10 | 2012-05-09 | 桂林理工大学 | Method for preparing lithium vanadium phosphate and lithium manganese phosphate composite anode material through rheological phase reaction |
| CN103400986A (en) * | 2013-08-09 | 2013-11-20 | 郑州瑞普生物工程有限公司 | Preparation method of lithium iron phosphorus oxide |
| CN108675276A (en) * | 2018-05-24 | 2018-10-19 | 深圳市毓丰新材料有限公司 | LiFePO4 and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101575093B (en) | 2011-04-06 |
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