CN103928648A - High-temperature-resistant lithium battery diaphragm and production method thereof - Google Patents
High-temperature-resistant lithium battery diaphragm and production method thereof Download PDFInfo
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- CN103928648A CN103928648A CN201410128928.8A CN201410128928A CN103928648A CN 103928648 A CN103928648 A CN 103928648A CN 201410128928 A CN201410128928 A CN 201410128928A CN 103928648 A CN103928648 A CN 103928648A
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- Prior art keywords
- polyimide film
- lithium battery
- battery diaphragm
- high temperature
- production method
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- 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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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Cell Separators (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention belongs to the technical field of battery diaphragms, and discloses a high-temperature-resistant lithium battery diaphragm and a production method thereof. A base material of the high-temperature-resistant diaphragm is a polyimide thin film, and micropores are uniformly formed in the base material. The production method comprises the steps of irradiating the polyimide thin film by heavy ions, and etching the irradiated polyimide thin film through a sodium hypochlorite solution. The high-temperature-resistant lithium battery diaphragm and the production method thereof have the advantages that the heat resistance is high, the tensile strength is high, environment pollution is avoided, the micropores are uniformly distributed, and high-current quick charging and discharging requirements for a lithium battery are met.
Description
Technical field
The invention belongs to battery diaphragm technical field, be specifically related to a kind of high temperature resistant lithium battery diaphragm and production method thereof.
Background technology
Lithium battery diaphragm is the electrical insulating property film with loose structure, is the important component part of lithium battery, and its Main Function is for intercepting positive and negative pole plate, preventing internal short-circuit of battery.But must there is duct, to make lithium ion fast transport between positive and negative electrode in charge discharge process.
Traditional barrier film production method mainly contains two kinds of dry method and wet methods, and the conventional material of these two kinds of methods is TPO film polypropylene (PP) and polyethylene (PE).Dry method is fusion drawn method, is that polyolefin film is heated to uniform temperature, and then further stretches, and crystalizing interface is peeled off, and forms loose structure.The advantage of this method is pollution-free in the relatively simple and production process of technique, and shortcoming is to control well aperture and porosity; Wet method is thermally induced phase separation, and this method can be controlled aperture and porosity preferably, and shortcoming is that complex process, cost are higher and easily bring pollution problem.Because the softening point temperature of most polyolefine materials is lower, if the fusing point of PP and PE is all lower than 150 DEG C, make the heat resistance of the lithium battery that this class material barrier film makes poor, can only below tens degree, use, can not use large electric current to carry out quick charge to it, can not carry out heavy-current discharge.
Polyimides, owing to having the performances such as good resistant of high or low temperature, chemical stability and low-expansion coefficient, is expected to for the preparation of novel lithium battery diaphragm.Ding Jun etc. disclose employing wet method and have prepared polyimides/PETG composite membrane in " chemical property of polypyromelliticimide composite diaphragm for lithium battery " literary composition.Utilize the standby barrier film thermal endurance of this legal system better, but still exist wet method to prepare some shortcomings of lithium battery diaphragm, as complex process, cost is high and solvent brings problem of environmental pollution.
Porous alumina membrane (referred to as nucleopore membranes) is a kind of high-quality microporous membrane that nucleonics ion speed technology and solid track detector technology are produced.By the heavy ion irradiation high molecular polymer film with certain kinetic energy that uses accelerator or nuclear reactor to provide, in the time that ion passes film, on the path of passing through at the inner ion of film, produce the latent track forming because of ionization damage, the long-chain of latent track place polymer molecule ruptures and produces high chemically active free radical, by using specific chemical reagent can make latent track place form micropore, can produce like this porous alumina membrane.Guoan Huoju Tech Development Co., Ltd., Zhongshan has applied for the patent of invention that denomination of invention is " a kind of lithium battery film and production method thereof " in March, 2011, this patent discloses employing PET film as base material, after high energy particle irradiation, obtains this lithium battery diaphragm with alkali lye etching.The PET barrier film that utilizes porous alumina membrane method to prepare, has micropore and is evenly distributed, and extension liquid ability is high, be easy to etching, heat resisting temperature is higher than features such as PP and PE films, but the occasion that need to carry out to lithium battery high current charge-discharge at some, and this base material still can not meet demand.
The conventional base material of porous alumina membrane method is PET and PC at present, existing open source literature does not also combine the polyimide base material of good heat resistance report with porous alumina membrane method.
Summary of the invention
(1) goal of the invention
According to the existing problem of prior art, the lithium battery diaphragm and the production method thereof that the invention provides that a kind of thermal endurance is high, hot strength are large, non-environmental-pollution problem, micropore are evenly distributed, can meet the large electric current fast charging and discharging of lithium battery needs.
(2) technical scheme
In order to solve the existing problem of prior art, the present invention is achieved by the following technical solutions:
A kind of high temperature resistant lithium battery diaphragm, key is, the base material of this barrier film is polyimide film, is evenly distributed with micropore on base material.
Preferably, described micropore is vertical with the surface of polyimide film.
Preferably, the hole density of described polyimide film is 1 × 10
7～1 × 10
10cm
-2, aperture is 0.2～3.0 μ m, the thickness of polyimide film is 5 μ m～35 μ m.
Preferably, the hole density of described polyimide film is 2 × 10
7～1 × 10
9cm
-2, aperture is 0.5～1.0 μ m, the thickness of polyimide film is 8～15 μ m.
A production method for high temperature resistant lithium battery diaphragm, key is, the method comprises the following steps:
(1) utilize the heavy ion of drawing from accelerator or reactor to carry out irradiation to polyimide film;
(2) liquor natrii hypochloritis that service quality concentration is 1%～10%, temperature be under 50 DEG C～90 DEG C conditions to the polyimide film etching 10min～150min after irradiation, obtaining aperture is the lithium battery diaphragm of 0.2 μ m～3 μ m.
Preferably, in described step (1), draw heavy ion when polyimide film is carried out to irradiation with accelerator, the energy of heavy ion is 2～15MeV/u.
Preferably, in described step (2), the liquor natrii hypochloritis who is 1%～10% in service quality concentration carries out before etching polyimide film, and the liquor potassic permanganate that is first 0.2mol/L～3mol/L by concentration soaks the polyimide film 30min～250min after irradiation under 10 DEG C～60 DEG C conditions.
Preferably, micropore described in step (1) is vertical with polyimide film surface.
Preferably, described in step (1), the hole density after polyimide film irradiation is 1 × 10
7～1 × 10
10cm
-2, the thickness of polyimide film is 5 μ m～35 μ m.
Preferably, described in step (1), the hole density after polyimide film irradiation is 2 × 10
7～1 × 10
9cm
-2, the thickness of polyimide film is 8～15 μ m.
Preferably, in described step (1), heavy ion is
32s,
40ar,
40ca,
56fe,
63cu,
65cu,
79br,
107ag,
107ag,
127i or
196au.
(3) beneficial effect
Lithium battery diaphragm provided by the invention and production method, be creatively polyimide film and porous alumina membrane method to be combined, and has following beneficial effect:
(1) good heat resistance of lithium battery diaphragm, except for conventional occasion, can also be used for needing the occasion of high current charge-discharge
Use the base material of polyimide film as lithium battery diaphragm, its heat resistance significantly improves with respect to traditional PP, PE or PET film, can at 230 DEG C, use for a long time, and can tolerate in short-term the high temperature up to 400 DEG C.Therefore, be applied in lithium battery, can adopt large electric current to charge to it, also can carry out heavy-current discharge to it, charging and discharging currents is the more than 2 times of current commercially available main flow lithium battery.
(2) solved the etch issues of polyimide film
The film micropore that porous alumina membrane method makes is evenly distributed, and is suitable for preparing lithium battery diaphragm, can etching but barrier film is necessary.Because polyimide film is insensitive to conventional acid & alkali liquid etching, limit the application of polyimide film on porous alumina membrane.The present invention creatively selects clorox, as etching solution, polyimide film is carried out to etching, and etch effect highly significant is successfully prepared the lithium battery diaphragm that aperture is 0.2～3 μ m.
In addition, the present invention also provided before clorox etching and first with potassium permanganate liquid, the polyimide film after irradiation has been soaked to this technical scheme.This technical scheme has advantages of two aspects: the one, and the etching period that can significantly shorten clorox more than 20%, has improved efficiency; The 2nd, can improve diaphragm quality, strengthen the intensity of polyimides, especially hot strength.This is also that applicant pays the selection that creative work is made simultaneously.
(3) polyimide film also has anti-flammability and certainly puts out ability, can at high temperature not melt.
Brief description of the drawings
Fig. 1 is the schematic cross-sectional view of lithium battery diaphragm provided by the invention;
Wherein 1 is polyimide film; The 2nd, micropore.
Embodiment
Below in conjunction with specification drawings and specific embodiments, the present invention is further elaborated.
Embodiment 1
A kind of high temperature resistant lithium battery diaphragm, its schematic cross-sectional view, as shown in Figure 1, the base material of this barrier film is that thickness is the polyimide film 1 of 5 μ m, is evenly distributed with micropore 2 on base material, and micropore 2 is vertical with the surface of polyimide film 1, and hole density is 1 × 10
7cm
-2, aperture is 0.2 μ m.
By the heat resistance checking to this lithium battery diaphragm, learn that this lithium battery diaphragm can use for a long time at 230 DEG C, there is anti-flammability and certainly put out ability, can at high temperature not melt, only under the high temperature of 800 degrees Celsius, ability, by coking, is insoluble to any known organic solvent.
This high temperature resistant lithium battery diaphragm, for the preparation of lithium battery sample, can be born to 2C discharges and recharges and sample battery is carried out to 2C while charging and discharging, carry out after 1000 circulations, the residual capacity after 800 circulations is initial capacity 70%.
Embodiment 2
As different from Example 1, this polyimide diaphragm base material is that thickness is the polyimide film of 15 μ m, is evenly distributed with micropore on base material, and micropore is vertical with the surface of polyimide film, and hole density is 1 × 10
8cm
-2, aperture is 1 μ m.
Embodiment 3
As different from Example 1, this polyimide diaphragm base material is that thickness is the polyimide film of 35 μ m, is evenly distributed with micropore on base material, and micropore is vertical with the surface of polyimide film, and hole density is 1 × 10
9cm
-2, aperture is 3.0 μ m.
Embodiment 4
A production method for high temperature resistant lithium battery diaphragm, key is, the method comprises the following steps:
(1) utilize the energy of drawing from accelerator for 2MeV/u's
79br ion pair polyimide film carries out irradiation, and the hole density after irradiation is 1 × 10
7cm
-2;
(2) liquor natrii hypochloritis that service quality concentration is 1%, temperature be under 70 DEG C of conditions to the polyimide film etching 30min after irradiation, obtain the lithium battery diaphragm that aperture is 0.2 μ m.
Embodiment 5
Identical, different with method, the principle of embodiment 4, in step (1), utilize energy for 8MeV/u's
32s ion carries out irradiation polyimide film, and the hole density after irradiation is 1 × 10
8.
Embodiment 6
Identical, different with method, the principle of embodiment 4, in step (1), from reactor, drawing energy is 15MeV/u
196au ion carries out irradiation polyimide film.
Embodiment 7
The liquor natrii hypochloritis identical, different with method, the principle of embodiment 4, service quality concentration is 5% in step (2), temperature be under 90 DEG C of conditions to polyimide film etching 150min, obtain the lithium battery diaphragm that aperture is 2.0 μ m.
Embodiment 8
The liquor natrii hypochloritis identical, different with method, the principle of embodiment 4, service quality concentration is 5% in step (2), temperature be under 90 DEG C of conditions to polyimide film etching 60min, obtain the lithium battery diaphragm that aperture is 1.5 μ m.
Embodiment 9
The liquor natrii hypochloritis identical, different with method, the principle of embodiment 4, service quality concentration is 10% in step (2), temperature be under 50 DEG C of conditions to polyimide film etching 10min, obtain the lithium battery diaphragm that aperture is 1.0 μ m.
Embodiment 10
The liquor natrii hypochloritis identical, different with method, the principle of embodiment 4, service quality concentration is 10% in step (2), temperature be under 50 DEG C of conditions to polyimide film etching 80min, obtain the lithium battery diaphragm that aperture is 3.0 μ m.
Embodiment 11
As different from Example 4, use liquor natrii hypochloritis to carry out before etching polyimide film in step (2), the liquor potassic permanganate that is first 0.2mol/L by concentration soaks the polyimide film 250min after irradiation under 60 DEG C of conditions.And then the service quality concentration liquor natrii hypochloritis that is 5%, temperature be under 90 DEG C of conditions to polyimide film etching 46min, obtain the lithium battery diaphragm that aperture is 1.5 μ m.
Embodiment 12
As different from Example 4, use liquor natrii hypochloritis to carry out before etching polyimide film in step (2), the liquor potassic permanganate that is first 1.0mol/L by concentration soaks the polyimide film 80min after irradiation under 30 DEG C of conditions.Then the liquor natrii hypochloritis that service quality concentration is 1%, temperature be under 70 DEG C of conditions to the polyimide film etching 10min after irradiation, obtain the lithium battery diaphragm that aperture is 0.2 μ m
Embodiment 13
As different from Example 4, use liquor natrii hypochloritis to carry out before etching polyimide film in step (2), the liquor potassic permanganate that is first 3mol/L by concentration soaks the polyimide film 100min after irradiation under 10 DEG C of conditions.And then the service quality concentration liquor natrii hypochloritis that is 5%, temperature be under 90 DEG C of conditions to polyimide film etching 40min, obtain the lithium battery diaphragm that aperture is 2.0 μ m.
Claims (10)
1. a high temperature resistant lithium battery diaphragm, is characterized in that, the base material of this barrier film is polyimide film, is evenly distributed with micropore on base material.
2. the high temperature resistant lithium battery diaphragm of one according to claim 1, is characterized in that, described micropore is vertical with the surface of polyimide film.
3. the high temperature resistant lithium battery diaphragm of one according to claim 1, is characterized in that, the hole density of described polyimide film is 1 × 10
7～1 × 10
10cm
-2, aperture is 0.2～3.0 μ m, the thickness of polyimide film is 5 μ m～35 μ m.
4. the high temperature resistant lithium battery diaphragm of one according to claim 1, is characterized in that, the hole density of described polyimide film is 2 × 10
7～1 × 10
9cm
-2, aperture is 0.5～1.0 μ m, the thickness of polyimide film is 8～15 μ m.
5. a production method for high temperature resistant lithium battery diaphragm, is characterized in that, the method comprises the following steps:
(1) utilize the heavy ion of drawing from accelerator or reactor to carry out irradiation to polyimide film;
(2) liquor natrii hypochloritis that service quality concentration is 1%～10%, temperature be under 50 DEG C～90 DEG C conditions to the polyimide film etching 10min～150min after irradiation, obtaining aperture is the lithium battery diaphragm of 0.2 μ m～3 μ m.
6. the production method of a kind of high temperature resistant lithium battery diaphragm according to claim 5, is characterized in that, in described step (1), draws heavy ion when polyimide film is carried out to irradiation with accelerator, and the energy of heavy ion is 2～15MeV/u.
7. the production method of a kind of high temperature resistant lithium battery diaphragm according to claim 5, it is characterized in that, in described step (2), the liquor natrii hypochloritis who is 1%～10% in service quality concentration carries out before etching polyimide film, and the liquor potassic permanganate that is first 0.2mol/L～3mol/L by concentration soaks the polyimide film 30min～250min after irradiation under 10 DEG C～60 DEG C conditions.
8. the production method of a kind of high temperature resistant lithium battery diaphragm according to claim 5, is characterized in that, micropore described in step (1) is vertical with polyimide film surface.
9. the production method of a kind of high temperature resistant lithium battery diaphragm according to claim 5, is characterized in that, the hole density described in step (1) after polyimide film irradiation is 1 × 10
7～1 × 10
10cm
-2, the thickness of polyimide film is 5 μ m～35 μ m.
10. the production method of a kind of high temperature resistant lithium battery diaphragm according to claim 5, is characterized in that, the hole density described in step (1) after polyimide film irradiation is 2 × 10
7～1 × 10
9cm
-2, the thickness of polyimide film is 8～15 μ m.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104377327A (en) * | 2014-09-28 | 2015-02-25 | 中山国安火炬科技发展有限公司 | Production method of novel lithium ion battery diaphragm with variable inclined holes |
| CN104393216A (en) * | 2014-09-28 | 2015-03-04 | 中山国安火炬科技发展有限公司 | Polyimide microporous membrane used as lithium ion battery separator and preparation method thereof |
| CN104399376A (en) * | 2014-09-28 | 2015-03-11 | 中山国安火炬科技发展有限公司 | Polyimides microporous membrane and production method |
| CN105514329A (en) * | 2016-01-22 | 2016-04-20 | 中山国安火炬科技发展有限公司 | PET heavy-ion microporous composite membrane for lithium battery and preparation method thereof |
| CN107078339A (en) * | 2014-10-21 | 2017-08-18 | 日本电气株式会社 | Secondary cell and its manufacture method |
| CN108281594A (en) * | 2018-01-05 | 2018-07-13 | 天津市协和医药科技集团有限公司 | A kind of lithium battery polyethylene diaphragm of nuclear pore and preparation method |
| CN111229049A (en) * | 2020-01-14 | 2020-06-05 | 西北工业大学 | Size-controllable micro-nano pore membrane and preparation method and application thereof |
| CN112635911A (en) * | 2020-12-22 | 2021-04-09 | 中国科学院近代物理研究所 | Nuclear pore membrane-based lithium ion battery diaphragm with high temperature resistance and high thermal conductivity and preparation method thereof |
| CN113629354A (en) * | 2021-08-05 | 2021-11-09 | 中国科学院近代物理研究所 | Lithium ion battery diaphragm suitable for liquid electrolyte based on heavy ion track membrane and preparation method thereof |
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| JPH0247141A (en) * | 1988-08-09 | 1990-02-16 | Japan Atom Energy Res Inst | Preparation of porous polyimide membrane |
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2014
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| JPH0247141A (en) * | 1988-08-09 | 1990-02-16 | Japan Atom Energy Res Inst | Preparation of porous polyimide membrane |
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Non-Patent Citations (1)
| Title |
|---|
| D. DOBREV等: "Novel two-step etching process for ion tracks in polyimide", 《GSI JAHRESBERICHT》, 31 December 2006 (2006-12-31), pages 321 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104377327A (en) * | 2014-09-28 | 2015-02-25 | 中山国安火炬科技发展有限公司 | Production method of novel lithium ion battery diaphragm with variable inclined holes |
| CN104393216A (en) * | 2014-09-28 | 2015-03-04 | 中山国安火炬科技发展有限公司 | Polyimide microporous membrane used as lithium ion battery separator and preparation method thereof |
| CN104399376A (en) * | 2014-09-28 | 2015-03-11 | 中山国安火炬科技发展有限公司 | Polyimides microporous membrane and production method |
| CN107078339A (en) * | 2014-10-21 | 2017-08-18 | 日本电气株式会社 | Secondary cell and its manufacture method |
| CN107078339B (en) * | 2014-10-21 | 2019-12-17 | 日本电气株式会社 | Secondary battery and method for manufacturing same |
| CN105514329A (en) * | 2016-01-22 | 2016-04-20 | 中山国安火炬科技发展有限公司 | PET heavy-ion microporous composite membrane for lithium battery and preparation method thereof |
| CN108281594A (en) * | 2018-01-05 | 2018-07-13 | 天津市协和医药科技集团有限公司 | A kind of lithium battery polyethylene diaphragm of nuclear pore and preparation method |
| CN111229049A (en) * | 2020-01-14 | 2020-06-05 | 西北工业大学 | Size-controllable micro-nano pore membrane and preparation method and application thereof |
| CN111229049B (en) * | 2020-01-14 | 2021-09-14 | 西北工业大学 | Size-controllable micro-nano pore membrane and preparation method and application thereof |
| CN112635911A (en) * | 2020-12-22 | 2021-04-09 | 中国科学院近代物理研究所 | Nuclear pore membrane-based lithium ion battery diaphragm with high temperature resistance and high thermal conductivity and preparation method thereof |
| CN113629354A (en) * | 2021-08-05 | 2021-11-09 | 中国科学院近代物理研究所 | Lithium ion battery diaphragm suitable for liquid electrolyte based on heavy ion track membrane and preparation method thereof |
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