CN101232104B - Method for manufacturing iron phosphate lithium power polymer lithium ion battery - Google Patents
Method for manufacturing iron phosphate lithium power polymer lithium ion battery Download PDFInfo
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- CN101232104B CN101232104B CN2007100668041A CN200710066804A CN101232104B CN 101232104 B CN101232104 B CN 101232104B CN 2007100668041 A CN2007100668041 A CN 2007100668041A CN 200710066804 A CN200710066804 A CN 200710066804A CN 101232104 B CN101232104 B CN 101232104B
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to the preparation method of a lithium iron phosphate power polymer lithium ion battery. The method mainly comprises following steps: preparing electrode slurry, processing a current collector, preparing a positive electrode sheet, preparing a negative electrode sheet, preparing a membrane and preparing a single battery sheet. By adopting lithium iron phosphate as the positive electrode material and stacking process, the invention can significantly improve the safety performance, cycle performance, etc. of the battery to well meet the performance requirement of power supply.
Description
Technical field
The present invention relates to a kind of manufacture method of lithium ion battery, particularly a kind of with the manufacture method of LiFePO4 as the electrokinetic cell of anodal key component.
Background technology
Advantages such as LiFePO4 is reliable with its fail safe, have extended cycle life, charge and discharge platform is stable become one of power lithium-ion battery positive electrode that has application prospect.
Business-like at present ferric phosphate lithium cell is mainly liquid lithium system.Yet, in the preparation process of positive plate, coating is difficulty very, easy and the collector disengaging of positive electrode after the oven dry, the colleague exists positive plate to occur the problem of serious dry linting phenomenon easily, and the capacity that has influenced battery is largely brought into play and cycle performance, therefore, the ferric phosphate lithium cell of liquid lithium system, processing difficulties, production efficiency is lower.
Summary of the invention
The invention provides a kind of positive pole by lithium ion being provided and can carrying out the preparation method that lithium embedded/took off the battery that the lithium-iron phosphate active material of embedding constitutes, solved the problem of security performance, cycle performance, memory property and the high-temperature electrochemical properties deficiency of existing in prior technology battery.
Simultaneously, for solving dry linting and the coating difficult problem in the liquid lithium system, the invention provides the stacked manufacturing process of polymeric system.
Above-mentioned technical purpose of the present invention solves by the following technical programs:
The manufacture method of iron phosphate lithium power polymer lithium ion battery, it may further comprise the steps:
(1) make the electrode slip: with LiFePO4 be dissolved in the organic solvent after conductive agent, copolymer, plasticizer mix, stirring makes anode sizing agent; Embedding lithium formula material with carbon element with after copolymer, plasticizer, conductive agent fully mix, is dissolved in the organic solvent and stirs and make cathode size;
(2) collector is handled: dry under 50～90 ℃ of temperature after applying collector preliminary treatment slurry on the collector equably;
(3) preparation of positive plate: the anode sizing agent that makes is injected film-making machine, make the heavy uniform iron phosphate lithium positive pole diaphragm of film, a slice cathode film and collector are hot pressed into positive plate under 90～160 ℃;
(4) preparation of negative plate: cathode size is injected film-making machine, make the heavy uniform cathode membrane of film, with the collector two sides, stacked two cathode membrane, negative plate is made in hot pressing;
(5) preparation of barrier film: copolymer, inorganic filler, plasticizer are mixed with organic solvent, make slurry, inject film-making machine then, make barrier film;
(6) making of battery monomer: with the sequential cascade of positive plate/barrier film/negative plate/barrier film/positive plate together, battery monomer is made in hot pressing.
As preferably, LiFePO4 when (1) making anode sizing agent in the step, conductive agent, copolymer, the weight portion of plasticizer is respectively: 60～90,5～25,5～20,5～15, described conductive agent is an acetylene black, acetone is black, Supper S, Supper P, one or more of graphite powder, described copolymer is a Kynoar, the copolymer of vinylidene and hexafluoropropylene, polyacrylonitrile, polymethacrylates, polyacrylate, polyethylene, polypropylene, polyvinyl acetate, one or more of acrylonitrile and acrylic acid copolymer, described plasticizer is a repefral, dibutyl phthalate, ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, one or more of dipropyl carbonate, described organic solvent is an acetone, butanone, cyclohexanone, oxolane and cyclohexane, isobutanol, the N-methyl pyrrolidone, N, dinethylformamide, one or more of ethyl acetate.
As preferably, the weight portion of embedding lithium formula material with carbon element, copolymer, conductive agent, plasticizer is respectively when making the negative pole anode sizing agent in the step (1): 60～80,5～15,5～20,10～25, and described embedding lithium formula material with carbon element is one or more of carbonaceous mesophase spherules, native graphite, Delanium, graphitized carbon fibre.
As preferably, copolymer in the step (2), the weight portion of conductive agent are respectively: 20～40,60～80, and described copolymer is one or more of polyacrylonitrile, polymethacrylates, polyacrylate, polyethylene, polypropylene, polyvinyl acetate, ethylene acrylic acid co polymer.
As preferably, the weight portion of copolymer, plasticizer, inorganic filler is respectively in the step (5): 40～75,25～40,10～30, and described inorganic filler is one or more of silicon dioxide, alundum (Al, zirconium dioxide, lead titanates, di-iron trioxide, titanium dioxide, calcium silicates.
As preferably, the hot pressing temperature scope in the step (4) is 90～160 ℃.
As preferably, the hot pressing temperature scope in the step (6) is 90～160 ℃.
Battery production method of the present invention also should comprise following removal plasticizer, weldering collector, injects electrolyte, the changing into of battery packages, battery after above-mentioned steps is handled, this is familiar with by those of ordinary skill.Usually removing plasticizer is that battery monomer is repeatedly extracted with absolute methanol, then oven dry; The weldering collector is with bonding machine that aluminium, copper collector and the nickel lug of positive and negative electrode is welded together; Injecting electrolyte is after the battery that welding is good is dried, to inject an amount of electrolyte; Battery packages is to use the aluminum-plastic composite membrane battery pack; Changing into of battery is that the cell that obtains more than the general after packaged battery is discharged and recharged with the suitable system of changing into carries out connection in series-parallel according to instructions for use, is assembled into and satisfies the battery pack of using.
Owing to adopt among the present invention LiFePO4 as positive electrode, adopts stacked manufacture craft, the security performance, cycle performance etc. of battery are significantly improved, ten minutes meets the performance requirement of electrical source of power.
Embodiment
Below by instantiation, technical scheme of the present invention is described in further detail.
Embodiment 1:
1, anodal preparation
1.1 the preparation of cathode film, material
LiFePO4 (LiFePO
4): 700g
Polyvinylidene fluoride (PVDF): 130g
Acetylene black: 70g
Dimethyl carbonate: 80g
N-methyl pyrrolidone: 2000g
Above-mentioned material mixed stir into slurry, mixing speed is 2800r/min, and stirring the duration is 3 hours.Make film with film-making machine and heavily be 250g/m
2Cathode film, film-making machine walking speed 10cm/s, bake out temperature are 90 ℃.
1.2 collector preliminary treatment
Acetylene black 100g
Second polyacrylate: 30g
N-methyl pyrrolidone: 1200g
Above material even stirring in mixer made slurry, mixing speed 3000r/min, mixing time 3 hours is sprayed on slurry on the aluminium collector with spray net machine then, and spray pressure is 3 atmospheric pressure, and distance is 0.5m, again with 120 ℃ of oven dry.
1.3 anodal last preparation
Cathode film is cut into the size of 200*130mm, carry out hot pressing after cathode film that a slice cuts and the stack of a slice aluminium collector, hot pressing temperature is 110 ℃, pressure gap 50 μ m.
The preparation of 2 negative poles
2.1 the preparation of negative electrode film, material:
Carbonaceous mesophase spherules 300g
Polyvinylidene fluoride (PVDF): 60g
Acetylene black: 30g
Dimethyl carbonate: 40g
N-methyl pyrrolidone: 2500g
Above-mentioned material even stirring in mixer made slurry, mixing speed 3000r/min, mixing time two hours.Make film with film-making machine and heavily be 110g/m
2Cathode film, film-making machine walking speed 10cm/s, bake out temperature are 80 ℃.
2.2 the two sides preliminary treatment of copper collector is identical with above-mentioned aluminium collector processing mode.
2.3 the last preparation of negative pole
Negative electrode film is cut into the size of 200*130mm, a slice copper collector two sides two negative electrode film of stack are carried out hot pressing, hot pressing temperature is 130 ℃, pressure gap 45 μ m.
3, barrier film preparation, material:
Polyvinylidene fluoride (PVDF): 350g
Dimethyl carbonate: 175g
Silicon dioxide: 120g
N-methyl pyrrolidone: 5000g
Above-mentioned material is mixed in mixer, mixing speed 6000r/min, mixing time is four hours, uses film-making machine to make the barrier film that thickness is 40 μ m, and walking speed is 100mm/s, and bake out temperature is 80 ℃.
4, the preparation of monolithic electricity core
Mode with positive pole/barrier film/negative pole/barrier film/positive pole stacks gradually, and carries out hot pressing on hot press, 130 ℃ of hot pressing temperatures, and the thickness after the hot pressing is 0.7mm.
5, extraction
Battery after synthetic is put in the absolute methanol extracts, in order to remove the plasticizer in the battery, 60 ℃ of dryings 15 hours in baking oven then.
6, the welding of lug
The positive and negative electrode collector of per 10 monolithics welds together with the nickel lug respectively, forms the exit of positive and negative electrode.
7, annotate electrolyte and battery pack
Use the aluminum-plastic composite membrane battery pack; the inlet that keeps electrolyte; in the glove box of argon shield, be that the mixture of 1: 1 ethylene carbonate and diethyl carbonate, the electrolyte of hexafluoro phosphorus lithium that solute is 1mol/L inject the aluminum-plastic composite membrane bag with organic solvent, seal inlet.
8, battery changes into
Battery was placed 6 hours, changed into the 0.3C system of changing into again.
9, the ageing of battery
With one week of battery ageing after changing into.
Cell circulated for 200 weeks through 1C, and capability retention is 93%.Above-mentioned battery parallel connection and series connection are assembled into battery pack, with practical requirement.
Embodiment 2:
1, anodal preparation
1.1 the preparation of cathode film, material
LiFePO4 (LiFePO
4): 800g
Polyvinylidene fluoride (PVDF): 140g
Acetylene black: 70g
Dimethyl carbonate: 70g
N-methyl pyrrolidone: 2500g
Above-mentioned material mixed stir into slurry, mixing speed is 3000r/min, and stirring the duration is 3 hours.Make film with film-making machine and heavily be 230g/m
2Cathode film, film-making machine walking speed 10cm/s, bake out temperature are 80 ℃.
1.2 collector preliminary treatment
Acetylene black 140g
Polyacrylate: 60g
N-methyl pyrrolidone: 2000g
Above material even stirring in mixer made slurry, mixing speed 3000r/min, mixing time 3 hours is sprayed on slurry on the aluminium collector with spray net machine then, and spray pressure is 3 atmospheric pressure, and distance is 0.5m, again with 110 ℃ of oven dry.
1.3 anodal last preparation
Cathode film is cut into the size of 215*140mm, carry out hot pressing after cathode film that a slice cuts and the stack of a slice aluminium collector, hot pressing temperature is 130 ℃, pressure gap 50 μ m.
The preparation of 2 negative poles
2.1 the preparation of negative electrode film, material:
Carbonaceous mesophase spherules 350g
Polyvinylidene fluoride (PVDF): 100g
Acetylene black: 30g
Dimethyl carbonate: 50g
N-methyl pyrrolidone: 3500g
Above-mentioned material even stirring in mixer made slurry, mixing speed 3000r/min, mixing time two hours.Make film with film-making machine and heavily be 110g/m
2Negative electrode film, film-making machine walking speed 10cm/s, bake out temperature are 80 ℃.
2.2 the two sides preliminary treatment of copper collector is identical with above-mentioned aluminium collector processing mode.
2.3 the last preparation of negative pole
Negative electrode film is cut into the size of 215*140mm, a slice copper collector two sides two negative electrode film of stack are carried out hot pressing, hot pressing temperature is 115 ℃, pressure gap 45 μ m.
3, barrier film preparation, material:
Polyvinylidene fluoride (PVDF): 350g
Dimethyl carbonate: 120g
Silicon dioxide: 110g
N-methyl pyrrolidone: 5000g
Above-mentioned material is mixed in mixer, mixing speed 6000r/min, mixing time is four hours, uses film-making machine to make the barrier film that thickness is 40 μ m, and walking speed is 100mm/s, and bake out temperature is 90 ℃.
4, the preparation of monolithic electricity core
Order with positive plate/barrier film/negative plate/barrier film/positive plate stacks gradually, and carries out hot pressing on hot press, 125 ℃ of hot pressing temperatures, and the thickness after the hot pressing is 0.7mm.
5, extraction
Battery after synthetic is put in the absolute methanol extracts, in order to remove the plasticizer in the battery, 60 ℃ of dryings 15 hours in baking oven then.
6, the welding of lug
The positive and negative electrode collector of per 10 monolithics welds together with the nickel lug respectively, forms the exit of positive and negative electrode.
7, annotate electrolyte and battery pack
Use the aluminum-plastic composite membrane battery pack; the inlet that keeps electrolyte; in the glove box of argon shield, be that the mixture of 1: 1 ethylene carbonate and diethyl carbonate, the electrolyte of hexafluoro phosphorus lithium that solute is 1mol/L inject the aluminum-plastic composite membrane bag with organic solvent, seal inlet.
8, battery changes into
Battery was placed 6 hours, changed into the 0.3C system of changing into again.Test result is as follows:
Discharge capacity is 11.5Ah first.
9, the ageing of battery
With one week of battery ageing after changing into.
Cell circulated for 200 weeks through 1C, and capability retention is 94.6%.Above-mentioned battery parallel connection and series connection are assembled into battery pack, with practical requirement.
Claims (4)
1. the manufacture method of iron phosphate lithium power polymer lithium ion battery, it may further comprise the steps:
(1) makes the electrode slip: with LiFePO4 and conductive agent, copolymer, plasticizer is dissolved in the organic solvent after mixing, stir and make anode sizing agent, wherein said LiFePO4, conductive agent, copolymer, the weight portion of plasticizer is respectively: 60～90,5～25,5～20,5～15, described conductive agent is an acetylene black, acetone is black, in the graphite powder one or more, described copolymer is a Kynoar, the copolymer of vinylidene and hexafluoropropylene, polyacrylonitrile, polymethacrylates, polyacrylate, polyethylene, polypropylene, polyvinyl acetate, in acrylonitrile and the acrylic acid copolymer one or more, described plasticizer is a repefral, dibutyl phthalate, ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, in the dipropyl carbonate one or more, described organic solvent is an acetone, butanone, cyclohexanone, oxolane and cyclohexane, isobutanol, the N-methyl pyrrolidone, N, dinethylformamide, in the ethyl acetate one or more; With embedding lithium formula material with carbon element with after copolymer, plasticizer, conductive agent fully mix, be dissolved in the organic solvent and stir and make cathode size, the weight portion of wherein said embedding lithium formula material with carbon element, copolymer, conductive agent, plasticizer is respectively: 60～80,5～15,5～20,10～25, and described embedding lithium formula material with carbon element is one or more in carbonaceous mesophase spherules, native graphite, Delanium, the graphitized carbon fibre;
(2) collector is handled: dry under 50～90 ℃ of temperature after applying collector preliminary treatment slurry on the collector equably, wherein said preliminary treatment slurry contains copolymer and conductive agent, the weight portion of copolymer, conductive agent is respectively: 20～40,60～80, and described copolymer is one or more in polyacrylonitrile, polymethacrylates, polyacrylate, polyethylene, polypropylene, polyvinyl acetate, the ethylene acrylic acid co polymer;
(3) preparation of positive plate: the anode sizing agent that makes is injected film-making machine, make the heavy uniform iron phosphate lithium positive pole diaphragm of film, under 90～160 ℃, positive plate is made in hot pressing with a slice cathode film and collector;
(4) preparation of negative plate: cathode size is injected film-making machine, make the heavy uniform cathode membrane of film, with the collector two sides, stacked two cathode membrane, negative plate is made in hot pressing;
(5) preparation of barrier film: copolymer, inorganic filler, plasticizer are mixed with organic solvent, make slurry, inject film-making machine then, make barrier film, the weight portion of wherein said copolymer, plasticizer, inorganic filler is respectively: 40～75,25～40,10～30, and described inorganic filler is one or more in silicon dioxide, alundum (Al, zirconium dioxide, lead titanates, di-iron trioxide, titanium dioxide, the calcium silicates;
(6) making of battery monomer: with the sequential cascade of positive plate/barrier film/negative plate/barrier film/positive plate together, battery monomer is made in hot pressing.
2. the manufacture method of iron phosphate lithium power polymer lithium ion battery according to claim 1, it is characterized in that: the hot pressing temperature scope in the step (4) is 90～160 ℃.
3. the manufacture method of iron phosphate lithium power polymer lithium ion battery according to claim 1, it is characterized in that: the hot pressing temperature scope in the step (6) is 90～160 ℃.
4. the manufacture method of iron phosphate lithium power polymer lithium ion battery according to claim 1, it is characterized in that: the other branch of weight portion of embedding lithium formula material with carbon element, copolymer, conductive agent, plasticizer is when making the negative pole anode sizing agent in the step (1): 60～80,5～15,5～20,10～25, and described embedding lithium formula material with carbon element is one or more in carbonaceous mesophase spherules, native graphite, Delanium, the graphitized carbon fibre; The weight portion of copolymer, conductive agent is respectively in the step (2): 20～40,60～80, and described copolymer is one or more in polyacrylonitrile, polymethacrylates, polyacrylate, polyethylene, polypropylene, polyvinyl acetate, the ethylene acrylic acid co polymer; Hot pressing temperature scope in the step (4) is 90～160 ℃; Hot pressing temperature scope in the step (6) is 90～160 ℃.
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| CN2007100668041A CN101232104B (en) | 2007-01-22 | 2007-01-22 | Method for manufacturing iron phosphate lithium power polymer lithium ion battery |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102971816B (en) * | 2010-06-28 | 2015-10-07 | 株式会社村田制作所 | Electric energy storage device and manufacture method thereof |
| CN102332600A (en) * | 2010-12-17 | 2012-01-25 | 东莞新能源科技有限公司 | Lithium ion battery |
| CN102163744B (en) * | 2011-03-07 | 2013-11-06 | 湖北能一郎新能源研究院 | Mixed polymer colloid lithium-ion battery and manufacturing method thereof |
| CN102903888A (en) * | 2012-11-01 | 2013-01-30 | 能一郎科技股份有限公司 | Cathode film of lithium iron phosphate polymer lithium ion battery |
| CN103022423A (en) * | 2012-11-28 | 2013-04-03 | 上海锦众信息科技有限公司 | Method for preparing lithium-ion safe negative pole |
| CN104143655A (en) * | 2014-07-31 | 2014-11-12 | 天津力神电池股份有限公司 | Flexible and pliable lithium ion secondary battery and manufacturing method thereof |
| CN105958012A (en) * | 2016-06-07 | 2016-09-21 | 程建聪 | Single high-capacity polymer lithium ion battery negative plate and manufacturing method therefor |
| CN105870489B (en) * | 2016-06-07 | 2019-03-01 | 程建聪 | Monomer-polymer lithium ion battery manufacturing method and its assemble method |
| CN105932290A (en) * | 2016-06-07 | 2016-09-07 | 程建聪 | Unit high-capacity polymer lithium ion battery positive plate and production method thereof |
| CN105914322B (en) * | 2016-06-07 | 2019-08-16 | 程建聪 | The manufacturing method of monomer high capacity polymer lithium ion battery |
| CN111200101B (en) * | 2018-11-16 | 2021-02-09 | 宁德时代新能源科技股份有限公司 | Positive pole piece and electrochemical device |
| CN113991185A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | Energy storage lithium ion battery based on nano electrode and preparation method thereof |
| CN113991062A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | High-capacity energy storage lithium ion battery and preparation method thereof |
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