CN106784553A - The preparation method of ceramic coating MIcroporous polyolefin film, MIcroporous polyolefin film and application - Google Patents
The preparation method of ceramic coating MIcroporous polyolefin film, MIcroporous polyolefin film and application Download PDFInfo
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- CN106784553A CN106784553A CN201611228378.2A CN201611228378A CN106784553A CN 106784553 A CN106784553 A CN 106784553A CN 201611228378 A CN201611228378 A CN 201611228378A CN 106784553 A CN106784553 A CN 106784553A
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- polyolefin film
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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
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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
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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
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
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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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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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Abstract
This application discloses a kind of preparation method of ceramic coating MIcroporous polyolefin film, MIcroporous polyolefin film and application.The preparation method of the ceramic coating MIcroporous polyolefin film of the application, including fluorination treatment is carried out to MIcroporous polyolefin film basement membrane, then the MIcroporous polyolefin film membrane surface then at fluorination treatment forms ceramic coating；Fluorination treatment includes being placed in basement membrane 20 60 seconds in the fluorine gas that concentration is 0.05%.The preparation method of the ceramic coating MIcroporous polyolefin film of the application, fluorination treatment is carried out in advance to MIcroporous polyolefin film, then it is coated with ceramic coating, the polarity and wellability on MIcroporous polyolefin film surface can be effectively improved by fluorination treatment, improve the surface bonding force of MIcroporous polyolefin film and ceramic coating, so that ceramic coating coating is uniform and difficult for drop-off.Also, the strand of fluorination treatment initiation MIcroporous polyolefin film is twined and connect, and further increases puncture resistant ability and tensile strength.
Description
Technical field
The application is related to MIcroporous polyolefin film field, more particularly to a kind of preparation side of ceramic coating MIcroporous polyolefin film
Method, the MIcroporous polyolefin film prepared by the method and application.
Background technology
At present, diaphragm for lithium ion battery is generally MIcroporous polyolefin film, including polypropylene (abbreviation PP) single layer microporous film,
Polyethylene (abbreviation PE) single layer microporous film and multilayer microporous film for being combined by PP and PE etc..MIcroporous polyolefin film has hole high
Rate, high anti-tearing strength, high antacid alkali ability, chemical-resistant reagent, it is cheap the advantages of；But, it is special when battery temperature is raised
When not being 200 DEG C of temperature, MIcroporous polyolefin film can shrink or melt, and then cause contact, short circuit between positive and negative electrode, trigger not
Security incident.Accordingly, it would be desirable to coated ceramic coating, to improve its temperature tolerance；But, PP, PE microporous barrier are non-polar, coating
Ceramic coating easily come off, or coat it is uneven, easily occur short circuit phenomenon when using.
The content of the invention
The purpose of the application is to provide a kind of preparation method of improved ceramic coating MIcroporous polyolefin film, and by the party
MIcroporous polyolefin film and its application prepared by method.
To achieve these goals, the application employs following technical scheme：
The one side of the application discloses a kind of preparation method of ceramic coating MIcroporous polyolefin film, including micro- to polyolefin
Pore membrane basement membrane carries out fluorination treatment, and then the MIcroporous polyolefin film membrane surface then at fluorination treatment forms ceramic coating；Fluorination
Treatment includes being placed in basement membrane 20-60 seconds in the fluorine gas that concentration is 0.05%.
Wherein, the concentration and process time of fluorine gas, primarily to making the micropore surface of MIcroporous polyolefin film be formed uniformly
Scattered fluorinated layer, therefore, according to different process objects, the concentration and process time of fluorine gas can be adjusted.
It should be noted that the application's it is critical that by studying discovery, fluorination treatment is carried out to MIcroporous polyolefin film
Afterwards, it is possible to increase the polarity and wellability on MIcroporous polyolefin film surface, MIcroporous polyolefin film is improved to be glued with the surface of ceramic coating
Relay so that ceramic coating coating is uniform and difficult for drop-off, so as to improve the puncture resistant ability of battery diaphragm and stretch strong
Degree；At the same time, fluorination treatment can trigger twining for strand to connect, and further improve puncture resistant ability and tensile strength.Also need
It is noted that in a kind of implementation of the application, fluorination treatment is carried out in the fluorination treatment room of sealing, its temperature
Using room temperature, the air pressure in the fluorination treatment room of sealing is standard atmospheric pressure.
Preferably, basement membrane be polyethene microporous membrane, microporous polypropylene membrane, polyethylene polypropylene composite micro porous film in wherein
It is a kind of.
It should be noted that the application is with MIcroporous polyolefin film as research object, wherein polyethene microporous membrane, poly- third
Alkene microporous barrier, polyethylene polypropylene composite micro porous film are relatively common MIcroporous polyolefin films, however not excluded that the preparation side of the application
Method is also applied for other MIcroporous polyolefin films.
Preferably, ceramic coating is aluminum oxide coating layer.
It should be noted that in a kind of implementation of the application, ceramic coating is preferably aluminum oxide coating layer；Can manage
Solution, it is critical only that for the application carry out fluorination treatment by MIcroporous polyolefin film surface, to improve MIcroporous polyolefin film surface
With the bonding force of ceramic coating, aluminum oxide coating layer is not limited in as ceramic coating, other, such as titanium dioxide, dioxy
SiClx, zirconium oxide, aluminium hydroxide, magnesium hydroxide etc. can be equally used for the application.
The another side of the application discloses ceramic coating MIcroporous polyolefin film prepared by a kind of preparation method of the application.
The another side of the application discloses a kind of ceramic coating MIcroporous polyolefin film of the application answering in battery diaphragm
With.
The another side of the application discloses a kind of battery diaphragm of the ceramic coating MIcroporous polyolefin film of the application.
It is appreciated that the preparation method of the application, the ceramic coating MIcroporous polyolefin film of preparation has excellent puncture resistant
Ability and tensile strength, lithium ion battery is applied to accordingly, as battery diaphragm, can avoid coming off or applying because of ceramic coating
Cover the uneven battery quality problem or potential safety hazard for causing.
Fluorinated polyolefin microporous barrier prepared by a kind of preparation method for simultaneously disclosing the application again of the application, fluorination is poly-
Alkene microporous barrier is included in fluorinated polyethylene microporous barrier, fluorinated polypropylene microporous barrier, fluorinated polyethylene polypropylene composite materials microporous barrier
One of which.
It should be noted that the fluorinated polyolefin microporous barrier of the application, actually according to the preparation method of the application,
The product of fluorination treatment is carried out to MIcroporous polyolefin film；In actual production, MIcroporous polyolefin film coated ceramic coating, Ke Yi
Carried out in the production in downstream, therefore, the fluorinated polyolefin microporous barrier of the application is micro- without treated polyolefin with routine
Pore membrane is compared, and with more preferable polarity and wellability, can ensure the quality of coated ceramic coating.
Because the beneficial effect using above technical scheme, the application is：
The preparation method of the ceramic coating MIcroporous polyolefin film of the application, is carried out at fluorination in advance to MIcroporous polyolefin film
Reason, is then coated with ceramic coating, and polarity and the infiltration on MIcroporous polyolefin film surface can be effectively improved by fluorination treatment
Property, improve the surface bonding force of MIcroporous polyolefin film and ceramic coating so that ceramic coating coating is uniform, and it is difficult for drop-off.
Also, the strand of fluorination treatment initiation MIcroporous polyolefin film is twined and connect, and further increases puncture resistant ability and tensile strength.
Brief description of the drawings
Fig. 1 is the electron-microscope scanning figure before MIcroporous polyolefin film fluorination treatment in the embodiment of the present application；
Fig. 2 is the electron-microscope scanning figure after MIcroporous polyolefin film fluorination treatment in the embodiment of the present application.
Specific embodiment
The application is described in further detail below by specific embodiments and the drawings.Following examples are only to the application
It is further described, should not be construed as the limitation to the application.
Embodiment
This example is tested with the PP basement membranes ZD25 that market is bought, specific as follows：
PP basement membranes ZD25 is launched, as in the fluorination treatment room of sealing, temperature is room temperature, and pressure is 1 atmospheric pressure, its
The volumetric concentration of middle fluorine gas is 0.05%, is reacted 20 seconds, obtains the fluorination basement membrane ZD25 of this example.
The various features to the basement membrane ZD25 without fluorination treatment and fluorination basement membrane ZD25 are tested respectively, including thickness
Degree, gas permeability, tensile strength MD, puncture strength, shrinkage factor MD, shrinkage factor TD are tested.
The wherein test of gas permeability uses Asahi Permeability gauges, is carried out according to GB/T 458-2008 standards.
The method of testing of tensile strength MD is：Sample is cut out into the rectangular specimens for 2 × 10cm, GB/T is compareed
12027-2004 reads experimental data using MTS universal testing machines.
The method of testing of puncture strength is：Using the puncture fixture of MTS universal testing machines, control GB/T21302-2007 marks
Quasi- experiment, reads experimental data.
The method of testing of shrinkage factor MD and shrinkage factor TD is：Sample is cut out into the square for 10 × 10cm, baking oven is placed
105 DEG C, toast within 2 hours, according to GB/T 12027-2004 result of calculations after taking-up.
Test result is as shown in table 1.
The test result of the basement membrane of table 1 and fluorination basement membrane
| Test event | Basement membrane ZD25 | Fluorination basement membrane ZD25 |
| Thickness (μm) | 24.9 | 25 |
| Gas permeability (s/100mL) | 325 | 326 |
| Tensile strength MD (Kg f/cm2) | 1403 | 1437 |
| Puncture strength (1mm tack/g) | 530 | 589 |
| 105 DEG C, 2h shrinkage factors MD (%) | 1.4 | 0.7 |
| 105 DEG C, 2h shrinkage factors TD (%) | 0.1 | 0.1 |
The result of table 1 shows that, by the fluorination basement membrane ZD25 that fluorination treatment is obtained, its tensile strength and puncture strength have
Improved, and percent thermal shrinkage declines, and stability increases.
In addition, the basement membrane ZD25 without fluorination treatment and fluorination basement membrane ZD25 are observed using electron-microscope scanning, as a result
As depicted in figs. 1 and 2, Fig. 1 is that basement membrane ZD25, Fig. 2 without fluorination treatment are fluorination basement membrane ZD25.It can be seen that, at fluorination
After reason, trigger twining for MIcroporous polyolefin film strand to connect, be conducive to improving puncture resistant ability and tensile strength, this and table 1
Result is consistent.
Additionally, this example tests dyne energy of the basement membrane ZD25 before and after fluorination treatment using dyne pen, to embody at fluorination
Manage the influence to membrane surface polarity and wellability.Test result shows that test fluid is in spot distribution on basement membrane ZD25, it is impossible to
Be covered on basement membrane ZD25 well, this with polypropylene without polarity, surface wettability the fact be consistent；And for fluorination treatment
Fluorination basement membrane ZD25 afterwards, test fluid can be uniformly covered on its surface, almost not have point-like drop, it is seen then that by fluorination
After treatment, the surface polarity and wellability of basement membrane are improved really, this lays a good foundation for the coating of ceramic coating.
Further, this example carries out ceramic coating painting to the basement membrane ZD25 without fluorination treatment and fluorination basement membrane ZD25 respectively
Cover, be respectively prepared battery diaphragm, and test two barrier film properties.It is specific as follows：
The ceramic size that this example is used is conventional aluminium oxide ceramics slurry, main material be aluminum oxide, water, thickener and
Binding agent and a small amount of dispersant.Wherein, the ratio of aluminum oxide, water, thickener, binding agent, dispersant compares 1/1.42/ for weight
0.0099/0.05/0.03.Ceramic size is obtained during each component is evenly spread into water, ceramic size is respectively coated on not
There are basement membrane ZD25 and fluorination basement membrane ZD25, the drying of fluorination treatment, that is, obtain two ceramic-coated separators.
After preparing barrier film, this example is respectively to two thickness of ceramic-coated separator, gas permeability, tensile strength MD, puncture
Intensity, shrinkage factor MD, shrinkage factor TD and peel strength have carried out contrast test.
Gas permeability, tensile strength MD, puncture strength, shrinkage factor MD, the method for testing of shrinkage factor TD are with reference to above basement membrane
The test of ZD25 and fluorination basement membrane ZD25.The method of testing of peel strength is that the sample that will scribble ceramic coating cuts 2cm wide,
20cm long.The sample that to cut out it is smooth paste a width of 2cm for pasting, on a length of 8cm double faced adhesive tapes ruler, stickup finishes vertical
Machine measurement is gone up, test speed is 300mm/min, and measuring distance is 200mm.Every test result is as shown in table 2.
Test result after the basement membrane of table 2 and fluorination basement membrane coated ceramic coating
The result of table 2 is shown, after fluorination treatment, the peel strength of ceramic coating is significantly improved, that is, improve basement membrane with pottery
The surface bonding force of porcelain coating；Also, ceramic coating is uniform, and gas permeability, tensile strength, puncture strength have different degrees of carrying
Height, heat endurance is more preferable.
Above content is to combine the further description that specific embodiment is made to the application, it is impossible to assert this Shen
Specific implementation please is confined to these explanations.For the application person of an ordinary skill in the technical field, do not taking off
On the premise of conceiving from the application, some simple deduction or replace can also be made, should all be considered as belonging to the application protection model
Enclose.
Claims (7)
1. a kind of preparation method of ceramic coating MIcroporous polyolefin film, it is characterised in that：Including entering to MIcroporous polyolefin film basement membrane
Row fluorination treatment, then then at the MIcroporous polyolefin film membrane surface formation ceramic coating of fluorination treatment；The fluorination treatment bag
Include to be placed in basement membrane in the fluorine gas that concentration is 0.05% and react 20-60 seconds.
2. preparation method according to claim 1, it is characterised in that：The MIcroporous polyolefin film basement membrane is polyethylene micropore
One of which in film, microporous polypropylene membrane, polyethylene polypropylene composite micro porous film.
3. preparation method according to claim 1, it is characterised in that：The ceramic coating is aluminum oxide coating layer.
4. the ceramic coating MIcroporous polyolefin film that prepared by the preparation method according to claim any one of 1-3.
5. application of the ceramic coating MIcroporous polyolefin film according to claim 4 in battery diaphragm.
6. a kind of battery diaphragm of the ceramic coating MIcroporous polyolefin film comprising described in claim 4.
7. the fluorinated polyolefin microporous barrier that prepared by the preparation method according to claim any one of 1-3, the fluorinated polyallyl
Hydrocarbon microporous barrier is included in fluorinated polyethylene microporous barrier, fluorinated polypropylene microporous barrier, fluorinated polyethylene polypropylene composite materials microporous barrier
One of which.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611228378.2A CN106784553B (en) | 2016-12-27 | 2016-12-27 | Preparation method of polyolefin microporous membrane with ceramic coating, polyolefin microporous membrane and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611228378.2A CN106784553B (en) | 2016-12-27 | 2016-12-27 | Preparation method of polyolefin microporous membrane with ceramic coating, polyolefin microporous membrane and application |
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| CN106784553B CN106784553B (en) | 2020-01-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107546358A (en) * | 2017-08-29 | 2018-01-05 | 湖南奥德迈能源有限责任公司 | One kind fluorination barrier film ultralow temperature lithium battery |
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| JP2001068088A (en) * | 1999-08-31 | 2001-03-16 | Sanyo Electric Co Ltd | Nonaqueous electrolyte secondary battery |
| CN102088067A (en) * | 2009-12-04 | 2011-06-08 | 索尼公司 | Diaphragm and battery |
| CN102496745A (en) * | 2011-11-28 | 2012-06-13 | 泉州劲鑫电子有限公司 | High-temperature nickel-metal hydride battery and manufacturing method thereof |
| CN104617328A (en) * | 2014-07-10 | 2015-05-13 | 天津东皋膜技术有限公司 | Long-life lithium ion secondary battery and manufacturing method thereof |
| CN105428575A (en) * | 2015-12-04 | 2016-03-23 | 中国制浆造纸研究院衢州分院 | Preparation method for plasma-induced grafting acrylic acid modified nickel-metal hydride battery diaphragm paper |
-
2016
- 2016-12-27 CN CN201611228378.2A patent/CN106784553B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001068088A (en) * | 1999-08-31 | 2001-03-16 | Sanyo Electric Co Ltd | Nonaqueous electrolyte secondary battery |
| CN102088067A (en) * | 2009-12-04 | 2011-06-08 | 索尼公司 | Diaphragm and battery |
| CN102496745A (en) * | 2011-11-28 | 2012-06-13 | 泉州劲鑫电子有限公司 | High-temperature nickel-metal hydride battery and manufacturing method thereof |
| CN104617328A (en) * | 2014-07-10 | 2015-05-13 | 天津东皋膜技术有限公司 | Long-life lithium ion secondary battery and manufacturing method thereof |
| CN105428575A (en) * | 2015-12-04 | 2016-03-23 | 中国制浆造纸研究院衢州分院 | Preparation method for plasma-induced grafting acrylic acid modified nickel-metal hydride battery diaphragm paper |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107546358A (en) * | 2017-08-29 | 2018-01-05 | 湖南奥德迈能源有限责任公司 | One kind fluorination barrier film ultralow temperature lithium battery |
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