CN1142612C - Polymer electrolyte film and lithium battery prepared with it - Google Patents
Polymer electrolyte film and lithium battery prepared with it Download PDFInfo
- Publication number
- CN1142612C CN1142612C CNB001054805A CN00105480A CN1142612C CN 1142612 C CN1142612 C CN 1142612C CN B001054805 A CNB001054805 A CN B001054805A CN 00105480 A CN00105480 A CN 00105480A CN 1142612 C CN1142612 C CN 1142612C
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- Prior art keywords
- polymer
- polymer electrolyte
- lithium battery
- electrolyte film
- film
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- Expired - Lifetime
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 24
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000005518 polymer electrolyte Substances 0.000 title abstract description 16
- 229920000642 polymer Polymers 0.000 claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 150000002484 inorganic compounds Chemical class 0.000 claims abstract description 10
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 10
- 239000000853 adhesive Substances 0.000 claims abstract description 4
- 230000001070 adhesive effect Effects 0.000 claims abstract description 4
- 229920002313 fluoropolymer Polymers 0.000 claims abstract 3
- 239000004811 fluoropolymer Substances 0.000 claims abstract 3
- 239000011244 liquid electrolyte Substances 0.000 claims description 6
- 229910017090 AlO 2 Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical group 0.000 claims description 2
- 229910052784 alkaline earth metal Chemical group 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical group 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 5
- 229920002239 polyacrylonitrile Polymers 0.000 abstract 3
- 239000008187 granular material Substances 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 229910001416 lithium ion Inorganic materials 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 239000003792 electrolyte Substances 0.000 description 9
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N activated carbon Substances [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 6
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 5
- 229920006280 packaging film Polymers 0.000 description 5
- 239000012785 packaging film Substances 0.000 description 5
- -1 polypropylene Polymers 0.000 description 5
- 230000005611 electricity Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000004831 Hot glue Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920006112 polar polymer Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
Classifications
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- Y02E60/122—
Abstract
The present invention provides a polymer electrolyte film and a technique for manufacturing a polymer lithium battery by the polymer electrolyte film. The polymer electrolyte film is characterized in that the polymer electrolyte film contains 10 to 90 wt %of inorganic compound with a micropore structure; the micropore structure of the polymer electrolyte film is a micropore network formed by the micropore of the inorganic compound and pore spaces between inorganic compound granules; an adhesive of the polymer electrolyte film comprises a fluoropolymer or polyacrylonitrile (PAN) or a mixture of the fluoropolymer and the polyacrylonitrile. The polymer lithium battery manufactured by the polymer electrolyte film has the advantages of simple method and easy industrialization.
Description
The present invention relates to after polymerization thing lithium battery.
Use the characteristics of the secondary lithium battery of non-aqueous electrolyte,, obtained on portable computer and the various removable electric terminal machine to use widely in mobile communication with its high-energy-density.At present, two class lithium ion batteries are arranged, a kind of for using the lithium ion battery of liquid organic bath, another kind of for using solid or the electrolytical lithium ion battery of colloidal polymer.The performance of polymer Li-ion battery is better than the liquid electrolyte lithium ion battery in many aspects, and for example: its manufacturing process is simple, and the shape flexibility is big, can be made into thickness less than 1 millimeter battery, and no liquid is leaked, and the holding time is long etc.In the present invention, lithium ion battery and lithium metal battery general designation lithium battery.
The main distinction of poly-lithium battery and liquid electrolyte lithium battery is that its electrolyte is the polymer film of a kind of solid or colloidal state, this polymer film and double as barrier film.The synthetic technology of preparing of polymer dielectric film is the core of poly-lithium battery technology.This polymer dielectric film should possess higher ionic conduction ability, electronic isolation performance, the electrochemical window limit mouth of broad, good mechanical intensity and processability and good and compatibility performance electrode.Polymer dielectric roughly can reduce following four classes: (1) does not contain the system of any liquid, and the formation of conductive phase is because due to containing the lithium salts dissolving or dissociating in the polar polymer matrix in this system.(2) gel polymer electrolyte will contain lithium salts dissolving or disassociation in a kind of polar liquid, add inactive polymer then to guarantee its mechanical stability.(3) plasticizing attitude polymer dielectric, this type of polymer dielectric also is a kind of colloidal state polymer electrolyte in principle, a spot ofly has the solvent of high-k very to improve conductance but keep in its matrix usually.(4) ionic rubber, this type of polymer dielectric are that a kind of low-temperature molten salt makes it become a kind of ionic conduction material through adding a small amount of high molecular polymer.(1) and (4) base polymer electrolyte still is in developing stage.(2) and (3) electrolytelike development is realistic scale closely.(BELLCORE USA) announced a kind of plasticizing attitude method for preparing polymer electrolytes (US Patent 5296318) in 1994 in U.S. bell communication research institute.They use the copolymer of Kynoar (PVdF) and hexafluoropropylene (HFP) and contain lithium salts LiFP
6, propene carbonate (PC), the mixture of ethylene carbonate (EC) is made the gel polymer electrolyte film.The content of hexafluoropropylene (HFP) in copolymer is no more than 20%.And make as the described lithium battery of United States Patent (USP) (US Patent5196279) with this film.The shortcoming of this kind polymer dielectric film is when HFP content is lower than 20%, and the ionic conductivity of this film itself does not reach the desired level of practical battery far away.Therefore, must be by plasticizing, technologies such as extraction are made microporous membrane with this film, and then pour into liquid electrolyte, become a kind of micropore colloidal film.The conduction of ion is to come now by the liquid electrolytic in the micropore.When HFP content was higher than 20%, its mechanical property and thermal stability sharply reduced.Thereby cause battery performance to worsen, even cause battery out of control.In addition, polypropylene fine (PAN) (US Patent 5219679), polyvinyl chloride (PVC) (USPatent 5252413), oxidic polyethylene (PEO) (Solid State Ionics 61 (85) 1996) class colloidal state polymer electrolyte also is used for lithium battery.But their normal temperature poorly conductive, preparation technology's relative complex or harsh to the ambient humidity requirement, the high rate during charging-discharging of battery can not satisfy modern electrical equipment requirement.
The shortcoming that the objective of the invention is to overcome above-mentioned technology provides the technology of preparing of a kind of new polymers electrolyte and film thereof, and the method that adopts this kind polymer dielectric film to make lithium battery is provided.
The method that a kind of polymer dielectric of the present invention and film thereof and this kind of employing dielectric film are made lithium battery comprises:
I. polymer dielectric film and manufacture method
The characteristics of polymer dielectric film of the present invention are, contain enough inorganic compounds with microcellular structure in the dielectric film, for example, and molecular screen material.Utilize micropore and the duct between the inorganic compound particle in the inorganic compound to form microporous network, technology that need not be other is carried out artificial pore-creating.Liquid electrolyte is poured among the microporous network of dielectric film, become the main body of ionic conduction.Polymer is mainly as adhesive.
With Kynoar (PVdF), or PVdF+ hexafluoropropylene (HPF) copolymer, or polypropylene fine (PAN) or their mixture are dissolved in acetone or N-methyl pyrrolidone (NMP) the isopolarity solvent.The concentration of polymer such as PVdF in solution is 5-25wt.%.Then, in solution, add molecular screen material M[AlO
2SiO
2], M is alkali metal or alkaline-earth metal.PVdF and the molecular screen material part by weight in solution is 25: 75.This solution becomes uniform slurry after fully mixed.Slurry is coated on the substrates such as PET film and becomes wet film.The film that will wet descended dry 15 minutes at 120 ℃, film was immersed in electrolyte such as 1M LiPF in dry environment again
6Take out after 30 seconds among+EC: the DMC (1: 1), inhale the liquid on striping surface with filter paper.Measure conductivity and be generally 2-8 * 10
-3Scm
-1
Polymer dielectric film of the present invention has very high thermal stability.After 60 minutes, irritating electrolyte 400 ℃ of heating again without the film that soaks electrolyte, the conductivity of being surveyed still is 10
-3Scm
-1About.Polymer dielectric film suitable metal lithium battery of the present invention, the electrolytical lithium ion battery of the lithium ion battery of liquid organic bath and solid or colloidal polymer.
II. the poly-lithium battery made from polymer electrolyte membrane of the present invention
Anodal: 72wt.%LiCoO
28wt.%PVdF hot glue class adhesives such as (or) PVdF+HFP, the NMP of 2wt.% acetylene activated carbon and 18wt.% or acetone mix makes uniform slurry, and to be coated in thickness be 0.02 millimeter Al paper tinsel one side or the thickness perforation Al band that is 0.05 millimeter or the both sides of Al net.Overlay thickness is generally the 0.1-0.15 millimeter.Dry under 60-150 ℃, make NMP or acetone evaporated.Cut into electrode film then.
Negative pole: 85wt.% graphite, 8wt.%PVdF (or PVdF+HFP hot glue class bonding agent), the NMP of 2wt.% acetylene activated carbon and 15wt.% or acetone mix makes uniform lotion, and to be coated in thickness be 0.02 millimeter Cu paper tinsel one side or the thickness perforation Cu band that is 0.05 millimeter or the both sides of Cu net.Applied thickness is generally the 0.06-0.12 millimeter.Dry under 60-150 ℃, make NMP or acetone evaporated.Cut into negative electrode plate then.
The dielectric film without immersing electrolyte among the I of the present invention is clipped between electrode film and the negative electrode plate, under 120-180 ℃, is hot pressed into one, i.e. the battery idiosome.Then in dry environment, after under 105-120 ℃ the battery idiosome being carried out vacuumize 20-60 minute, be immersed in electrolyte such as 1MLiPF
6Among+EC: the DMC (1: 1) 5 minutes, take out the metal-back (stainless steel, nickel plating) or be sealed in metal film+plastic composite packaging film of packing into, become battery.
Brief Description Of Drawings:
Fig. 1 adopts the polymer dielectric film of I of the present invention, according to the charging curve of the polymer Li-ion battery of the manufacture method manufacturing of the poly-lithium battery of embodiment 1.
Fig. 2 adopts the polymer dielectric film of I of the present invention, according to the discharge curve of the polymer Li-ion battery of the manufacture method manufacturing of the poly-lithium battery of embodiment 1.
Fig. 3 adopts the polymer dielectric film of I of the present invention, according to the charging curve of the polymer Li-ion battery of the manufacture method manufacturing of the poly-lithium battery of embodiment 2.
Fig. 4 adopts the polymer dielectric film of I of the present invention, according to the discharge curve of the polymer Li-ion battery of the manufacture method manufacturing of the poly-lithium battery of embodiment 2.
In order to be illustrated more clearly in the present invention, enumerate following application example.But these application examples do not have any restriction to the scope of application of the present invention.
Embodiment 1
Adopt the polymer dielectric film of I of the present invention, according to the polymer Li-ion battery of the manufacture method manufacturing of the poly-lithium battery of II of the present invention.The collector electrode of battery plus-negative plate is respectively Al net and the Cu net of thickness 50 μ m.Electrolyte is selected 1MLiPF for use
6+ EC: DMC (1: 1), positive active material are LiCoO
2, negative electrode active material is MCMB25-28 (little carbon bead graphite).Cell is sealed in the aluminium plastic composite packaging film.
The major parameter and the performance of battery are as follows:
LiCoO
2: MCMB25-28=2: 1 (weight)
Anodal thickness: 0.18mm
Negative pole thickness: 0.12mm
Polymer dielectric film thickness: 0.06mm
The thickness of battery: 0.35mm (thickness that does not comprise packaging film)
Charging cut-ff voltage: 4.2V
Discharge cut-off voltage: 2.5V
Charging current: 0.05A
Discharging current: 0.05A
Battery capacity: 115mAh (～0.5C)
Charging and discharging curve respectively as depicted in figs. 1 and 2.
Embodiment 2
Adopt the polymer dielectric film of I of the present invention, according to the manufacturing principle of liquid electrolyte lithium ion battery, with positive pole, polymer dielectric film and negative pole stack togather, and are sealed in the aluminium plastic composite packaging film.The collector electrode of battery plus-negative plate is respectively Al paper tinsel and the Cu paper tinsel of thickness 20 μ m.Electrolyte is selected 1MLiPF for use
6+ EC: DMC (1: 1), positive active material are LiCoO
2, negative electrode active material is MCMB25-28 (little carbon bead graphite).
The major parameter of battery:
LiCoO
2: MCMB25-28=2: 1 (weight)
Utmost point thickness: 0.12mm (comprising collector electrode Al net)
Utmost point thickness: 0.09mm (comprising collector electrode Cu net)
Compound dielectric film thickness: 0.06mm
The thickness in pond: 0.25mm (thickness that does not comprise packaging film)
Electricity cut-ff voltage: 4.2V
Electricity cut-ff voltage: 2.5V
Electricity electric current: 0.04A
Electricity electric current: 0.03A
Tankage: 68mAh
Discharge curve respectively as shown in Figure 3 and Figure 4.
Claims (3)
1, a kind of polymer dielectric film that uses in liquid electrolyte battery is characterized in that it comprises:
(1) contains the inorganic compound of the microcellular structure of 75～90wt.%, the microporous network that described microcellular structure is made up of the micropore and the hole between the inorganic compound particle of inorganic compound itself;
(2) adhesive of Cai Yonging is a fluoropolymer.
2, polymer dielectric film according to claim 1 is characterized in that described inorganic compound is M[AlO
2SiO
2], M is alkali metal or alkaline-earth metal.
3, the lithium battery of polymer dielectric film manufacturing according to claim 1 is characterized in that the lithium battery that adopts described polymer dielectric film to make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001054805A CN1142612C (en) | 2000-04-03 | 2000-04-03 | Polymer electrolyte film and lithium battery prepared with it |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001054805A CN1142612C (en) | 2000-04-03 | 2000-04-03 | Polymer electrolyte film and lithium battery prepared with it |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1316789A CN1316789A (en) | 2001-10-10 |
| CN1142612C true CN1142612C (en) | 2004-03-17 |
Family
ID=4577730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001054805A Expired - Lifetime CN1142612C (en) | 2000-04-03 | 2000-04-03 | Polymer electrolyte film and lithium battery prepared with it |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1142612C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI330136B (en) * | 2005-11-28 | 2010-09-11 | Lg Chemical Ltd | Organic/inorganic composite porous membrane and electrochemical device using the same |
| KR100941300B1 (en) * | 2006-09-07 | 2010-02-11 | 주식회사 엘지화학 | Gel polymer electrolyte and electrochemical device comprising the same |
| CN101626094B (en) * | 2008-07-11 | 2015-09-30 | 东莞新能源科技有限公司 | Lithium ion battery and battery thereof |
| CN101721922B (en) * | 2008-07-22 | 2011-12-28 | 山东华夏神舟新材料有限公司 | Microporous film enhanced multilayer fluorine-containing crosslinked ion-doped film and preparation method thereof |
| CN104362275A (en) * | 2014-12-01 | 2015-02-18 | 东莞市卓高电子科技有限公司 | Manufacturing method of lithium ion battery diaphragm as well as battery diaphragm prepared by manufacturing method and battery |
-
2000
- 2000-04-03 CN CNB001054805A patent/CN1142612C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1316789A (en) | 2001-10-10 |
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