CN102610797B - Manufacturing method of lithium iron phosphate anode - Google Patents
Manufacturing method of lithium iron phosphate anode Download PDFInfo
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- CN102610797B CN102610797B CN201110424957.5A CN201110424957A CN102610797B CN 102610797 B CN102610797 B CN 102610797B CN 201110424957 A CN201110424957 A CN 201110424957A CN 102610797 B CN102610797 B CN 102610797B
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- Prior art keywords
- slurry
- positive pole
- iron phosphate
- drying
- water
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 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 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 14
- 239000000839 emulsion Substances 0.000 claims abstract description 11
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 10
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 7
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 6
- 229910001416 lithium ion Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000002474 experimental method Methods 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 claims 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 abstract description 11
- 239000006258 conductive agent Substances 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 4
- 239000000243 solution Substances 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000002033 PVDF binder Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000005955 Ferric phosphate Substances 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229940032958 ferric phosphate Drugs 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- RFGNMWINQUUNKG-UHFFFAOYSA-N iron phosphoric acid Chemical compound [Fe].OP(O)(O)=O RFGNMWINQUUNKG-UHFFFAOYSA-N 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a manufacturing method of a lithium iron phosphate anode. The manufacturing method comprises the following steps: adding a polytetrafluoroethylene emulsion to an aqueous carboxymethyl cellulose solution, stirring, adding lithium iron phosphate and a conductive agent, stirring, adding water to form a slurry, shaping by coating the slurry, drying, and sintering in an inert atmosphere, and compacting by a roller press. By using the manufacturing method provided in the invention and utilizing an aqueous solution system to manufacture the anode of a cell, the pollution of NMP (N-methyl pyrrolidone) to the environment and harms of the NMP to human bodies are avoided, and the volumetric specific energy of the cell is increased.
Description
Technical field
The present invention relates to a kind of manufacturing process of lithium ion battery positive pole, specifically the manufacture method of iron phosphate lithium positive pole.
Background technology
Ferric phosphate lithium cell is the advantage such as fail safe is good, excellent performance, aboundresources, platform stable owing to having, and production scale development in recent years rapidly, has become domestic important pillar industry.LiFePO 4 material is the core of ferric phosphate lithium cell.Domestic and international current most of LiFePO4 producer adopts oleaginous system: generally adopt NMP (1-METHYLPYRROLIDONE) to make solvent, PVDF (Kynoar) is as stick, super conductive carbon black (Super P), acetylene black, electrically conductive graphite are as conductive agent, LiFePO4 is as main active substances, suspension-turbid liquid is formed after high speed dispersion, then use coater on aluminium foil, then through baking, roll-in, point cut into pole piece.
There is many problems in above process, be first that PVDF and NMP cost is very high, and main high-quality PVDF manufacturer is all external, unfavorable to the safety of CHINESE INDUSTRIES development; Secondly, NMP has certain toxicity to human body, and the steam of volatilization can cause occupational hazards.In addition, above system needs to avoid moisture effects, and producer needs to build dry factory building, also considerably increases production cost and technique controlling difficulty.Especially, it should be noted that, the operating environment that oleaginous system needs and technique are very strict, are very easy to occur dry linting, come off, reveal the defects such as paper tinsel.
Many researchers manufactures anode pole piece in research and utilization aqueous systems, significantly can reduce costs, and improve processability.The present invention proposes a kind of water solution system of low cost that utilizes and manufactures anode sizing agent, inquires into the low cost approach of positive pole manufacturing system.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of manufacture method utilizing the aqueous systems of low cost to manufacture iron phosphate lithium positive pole, realizes low cost and the high reliability of iron phosphate lithium positive pole manufacture.
Concrete technical scheme:
A kind of manufacture method of iron phosphate lithium positive pole, comprise the following steps: to carboxymethyl cellulose (CMC, also known as sodium carboxymethylcellulose or sanlose) the aqueous solution in add polytetrafluoroethylene (PTFE) emulsion, LiFePO4 and conductive agent is added after stirring, add water after again stirring and form slurry, described slurry makes flaky material through coating aftershaping, then dry.
Wherein, carboxymethyl cellulose aqueous solution accounts for 15 ~ 40% of slurry gross mass; In the ptfe emulsion added, polytetrafluoroethylene accounts for 0.2% ~ 21% of slurry gross mass in the quality of butt; Conductive agent quality accounts for 0.3 ~ 0.8% of slurry gross mass; LiFePO4 quality accounts for 21 ~ 76% of slurry gross mass; The described quality adding water accounts for 4 ~ 35% of slurry gross mass.
Wherein, the aqueous solution of described carboxymethyl cellulose to be mass ratio be 1: 20 ~ 120 carboxymethyl cellulose and water mix and stir and obtain, the time of stirring is 2 ~ 10 hours; Described ptfe emulsion is the emulsion that polytetrafluoroethylene is scattered in water, and mass concentration is 10 ~ 65%.
Wherein, described conductive agent is selected from the one in electrically conductive graphite, acetylene black, super conductive black, Graphene or carbon nano-tube.
Wherein, described water is electronic grade ultrapure water.
Wherein, stir 0.5 ~ 5 hour after adding described ptfe emulsion, the speed of stirring is 1000-20000 rev/min; Again stir 2 ~ 8 hours after adding described LiFePO4 and electric conducting material, the speed of stirring is 1000-20000 rev/min.
Wherein, described drying divides two stages, and the temperature of first stage drying is 85 ~ 130 DEG C, and second stage drying has inert gas or nitrogen protection, and dry temperature is 250 ~ 300 DEG C.
Wherein, after described second stage drying, temperature drops to less than 100 DEG C, and also there are inert gas or nitrogen protection in the stage that temperature declines.
Wherein, dried iron phosphate lithium positive pole also uses roll squeezer compacting.
Comprise the lithium ion battery of iron phosphate lithium positive pole as claimed in claim 1.
Excellent results of the present invention is:
The manufacture method using the present invention to propose, can utilize water solution system to manufacture battery pole piece, avoid the pollution of NMP to environment and the harm of human body, increase the volumetric specific energy of battery.18650 type battery (the diameter 18mm utilizing this technology to manufacture, long 65mm cylindrical battery), battery capacity can be brought up to 2000mAh from current 1400mAh, and there is excellent cycle performance, battery discharge multiplying power can bring up to 20 ~ 30C from 5C, has increased substantially the performance of battery.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
The pure water of 35 kilograms is added in beating equipment, first adds the CMC of 0.3 kilogram of LITHIUM BATTERY, then stir 2 hours with the speed of 1000 revs/min, form uniform liquid.Then add in butt 8.4 kilograms of PTFE, (namely PTFE is scattered in the emulsion 14 kilograms of water, the mass concentration 60% of PTFE) stirs 0.5 hour again, adds 21 kg of phosphoric acid iron lithiums and 0.3 kilogram of electrically conductive graphite, then stirs 2 hours.Finally adding water to stock quality is 100 kilograms.
This slurry is coated with on coating machine, then enters oven for drying.Baking oven divides two sections, and first paragraph is dry in atmosphere, and temperature controls at 85 DEG C; Second segment is the baking oven with nitrogen protection device, and temperature controls at 300 DEG C.This section has cold-zone section after drying, and pole piece is reduced the temperature to 90 DEG C.Cooling zone needs to pass into nitrogen and carries out atmosphere protection.Dried pole piece rolling, can carry out follow-up roll-in, cut etc. is total to sequence.Gained anode pole piece and Carbon anode are assembled into 18650 type lithium ion batteries, and discharge-rate reaches 20C, and initial capacity is 2000mAh.Through 2000 cycle charge-discharge experiments, its capability retention is 95%.
Comparative example: the LiFePO4 of same quality and conductive agent, be solvent with NMP, PVDF is binding agent, and through high speed dispersion, coating, drying, roll-in, the positive plate assembled battery obtained, its initial capacity is 1400mAh.
Embodiment 2
1 ton of slurry manufacture process of above composition is as follows:
Added in beating equipment by the water of 160 kilograms, then add 8 kilograms of CMC, then high-speed stirred 10 hours, mixing speed is 5000 revs/min, forms uniform liquid.Then add in butt 3 kilograms of PTFE emulsion (PTFE is scattered in the emulsion of water, and mass concentration is 60%), then stir 5 hours, add 760 kg of phosphoric acid iron lithiums and 8 kilograms of acetylene blacks, then stir 8 hours.Finally adding water to gross weight is 1 ton.
This slurry is coated with on coating machine, then enters oven for drying.Baking oven divides two sections, and first paragraph is dry in atmosphere, and temperature controls at 130 DEG C; Second segment is the baking oven with nitrogen protection device, and temperature controls at 300 DEG C.This section has cold-zone section after drying, and pole piece is reduced the temperature to less than 50 DEG C.Cooling zone also needs to pass into nitrogen and carries out atmosphere protection.Dried positive pole rolling, the operation such as can carry out follow-up roll-in, cut.
Gained positive pole and Carbon anode are assembled into lithium ion battery, and initial capacity is 1800mAh.
Comparative example: the LiFePO4 of same quality and electric conducting material, be solvent with NMP, PVDF is binding agent, and through high speed dispersion, coating, drying, roll-in, the positive plate assembled battery obtained, discharge-rate reaches 30C, and its initial capacity is 1450mAh.Through 2000 cycle charge-discharge experiments, its capability retention is 96%.
Embodiment 3
Added in beating equipment by the water of 300g, then add the CMC of 8g, then high-speed stirred 3 hours, forms uniform liquid.Then (PTFE is scattered in the emulsion of water to add the PTFE of 20g (in butt), mass concentration is 20%), stir 1 hour again, add the LiFePO4 of 364g and the super conductive black (Super P) of 8g, then stir 4 hours.Finally adding water to gross mass is 1 kilogram.
This slurry is coated with on coating machine, then enters oven for drying.Baking oven divides two sections, and first paragraph is dry in atmosphere, and temperature controls at 105 DEG C; Second segment is the baking oven with argon protective device, and temperature controls at 280 DEG C.This section has cold-zone section after drying, and the positive pole of oven dry is reduced the temperature to 80 DEG C.Cooling zone also needs to pass into argon gas and carries out atmosphere protection.Dried anode pole piece rolling, the operation such as can carry out follow-up roll-in, cut.Gained positive pole and Carbon anode are assembled into lithium ion battery, charge-discharge magnification 35C, and initial capacity is 2050mAh.Through 2000 cycle charge-discharge experiments, its capability retention is 96%.
Comparative example: the LiFePO4 of same quality and super conductive black, be solvent with NMP, PVDF is binding agent, and through high speed dispersion, coating, drying, roll-in, the positive plate assembled battery obtained, its initial capacity is 1410mAh.
Claims (1)
1. a manufacture method for iron phosphate lithium positive pole, comprises the following steps: added in beating equipment by the water of 300g, then adds the carboxymethyl cellulose of 8g, and then high-speed stirred 3 hours, forms uniform liquid; Then add 20g in the PTFE of butt, described PTFE is the emulsion being scattered in water, and mass concentration is 20%, stir 1 hour again, add the LiFePO4 of 364g and the super conductive black Super P of 8g, then stir 4 hours, finally adding water to gross mass is 1 kilogram, forms slurry;
This slurry is coated with on coating machine, then enters oven for drying; Baking oven divides two sections, and first paragraph is dry in atmosphere, and temperature controls at 105 DEG C; Second segment is the baking oven with argon protective device, and temperature controls at 280 DEG C, and this section has cold-zone section after drying, and the positive pole of oven dry is reduced the temperature to 80 DEG C, and cooling zone also needs to pass into argon gas and carries out atmosphere protection; Dried anode pole piece rolling, carries out follow-up roll-in, point cutting process; Gained positive pole and Carbon anode are assembled into lithium ion battery, charge-discharge magnification 35C, and initial capacity is 2050mAh; Through 2000 cycle charge-discharge experiments, its capability retention is 96%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110424957.5A CN102610797B (en) | 2011-12-16 | 2011-12-16 | Manufacturing method of lithium iron phosphate anode |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110424957.5A CN102610797B (en) | 2011-12-16 | 2011-12-16 | Manufacturing method of lithium iron phosphate anode |
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| CN102610797A CN102610797A (en) | 2012-07-25 |
| CN102610797B true CN102610797B (en) | 2015-01-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102881865B (en) * | 2012-09-14 | 2014-09-10 | 北京鼎能开源电池科技股份有限公司 | Method for manufacturing positive plate of battery |
| CN105778365B (en) * | 2014-12-23 | 2018-05-08 | 新材料与产业技术北京研究院 | A kind of carbon nano-tube/poly tetrafluoroethene nano composite membrane and preparation method thereof |
| CN109904387B (en) * | 2019-02-25 | 2021-07-13 | 天津艾克凯胜石墨烯科技有限公司 | Preparation method of high-performance lithium battery positive plate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1728427A (en) * | 2004-07-29 | 2006-02-01 | 肇庆市风华锂电池有限公司 | Adhesion agent of anode, pulp for anode obtained, lithium battery ,and preparation method |
| CN101286563A (en) * | 2008-04-30 | 2008-10-15 | 东莞市迈科新能源有限公司 | Aqueous glue, lithium battery applying the aqueous glue and manufacturing method for the lithium battery |
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| CN101286564B (en) * | 2008-05-28 | 2010-06-16 | 中国科学院上海微系统与信息技术研究所 | Composite anode for direct methanol fuel cell and method for making the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1728427A (en) * | 2004-07-29 | 2006-02-01 | 肇庆市风华锂电池有限公司 | Adhesion agent of anode, pulp for anode obtained, lithium battery ,and preparation method |
| CN101286563A (en) * | 2008-04-30 | 2008-10-15 | 东莞市迈科新能源有限公司 | Aqueous glue, lithium battery applying the aqueous glue and manufacturing method for the lithium battery |
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| CN102610797A (en) | 2012-07-25 |
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