CN107634168A - The coating slurry of lithium ion battery separator, lithium ion battery separator and preparation method thereof - Google Patents
The coating slurry of lithium ion battery separator, lithium ion battery separator and preparation method thereof Download PDFInfo
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- CN107634168A CN107634168A CN201710743602.XA CN201710743602A CN107634168A CN 107634168 A CN107634168 A CN 107634168A CN 201710743602 A CN201710743602 A CN 201710743602A CN 107634168 A CN107634168 A CN 107634168A
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- lithium ion
- ion battery
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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
The present invention proposes a kind of coating slurry of lithium ion battery separator, lithium ion battery separator and preparation method thereof, is calculated according to percetage by weight, including following components：Water-soluble cellulose 0.01~5%, inorganic ceramic particle 12~60%, amphoteric dispersant 0.5~4%, surfactant 0.01~1%, both sexes adhesive 1~10% and deionized water 35~80%.Lithium ion battery separator：Coating slurry including MIcroporous polyolefin film and above-mentioned lithium ion battery separator, the coating slurry is coated in above the MIcroporous polyolefin film.The coating slurry does not absorb water and purpose that moisture is up to standard coated in reaching above lithium ion battery separator, and transport, packaging, storage for the coated product need not control extremely low humidity.
Description
Technical field
The invention belongs to lithium ion battery separator processing technique field, and in particular to a kind of painting of lithium ion battery separator
Cover slurry, lithium ion battery separator and preparation method thereof.
Background technology
Due to the rapid growth of power battery of pure electric automobile energy density, the requirement to rechargeable lithium ion batteries is more next
It is higher.In lithium ion battery, barrier film turns on lithium ion as electrolyte thesaurus and prevents that electronics contacts between electrode, plays
Vital effect.MIcroporous polyolefin film conventional at present due to excellent chemical stability, mechanical strength and used extensively
Make lithium ion battery separator.However, MIcroporous polyolefin film poor high temperature stability, the problem of wetting to polarity electrolyte is bad, leads
Cause that larger battery impedance, cycle performance are low, even cause internal short-circuit of battery, limit its development space significantly.
For MIcroporous polyolefin film poor high temperature stability and to polarity electrolyte wetability it is bad the problem of, people are mainly led to
Cross in microporous barrier surface coated ceramic granular materials, gelatin polymer or coated ceramic particle and gel polymer materials come simultaneously
Solves problem above.Ceramic coating is formed on MIcroporous polyolefin film surface by coated ceramic granular materials, in battery high current
Or during high power charging-discharging, inside battery heating can be effectively kept out, maintains barrier film three-dimensional structure stability.Coating gel gathers
Compound can adsorb enough electrolyte, during battery high current or high power charging-discharging, there is provided enough lithium ions
Conducted, ensure that battery performance is stable.
It is steady to solve MIcroporous polyolefin film thermal structure simultaneously for coated ceramic particle and gel polymer materials can simultaneously
It is qualitative difference and to polarity electrolyte wetting it is bad the problem of.It is domestic at present mainly to be applied using water-based system coating or oleaginous system
Cover.And it is mainly producing line cost height, difficult solvent recovery, pollution environment etc. that oleaginous system, which coats the problem of existing,.Water-based coating
The problem of be coat barrier film moisture can not control effectively, coated product is in transport or storing process due to ring
Border humidity changes, and the ceramic layer water suction of coating barrier film, causes barrier film moisture too high, and this is moved for moisture requirement is strict
It is unfavorable for power automobile batteries.
The content of the invention
The present invention proposes a kind of coating slurry of lithium ion battery separator, the coating slurry coated in lithium ion battery every
Reach above film and do not absorb water and purpose that moisture is up to standard, transport, packaging, storage for the coated product need not control
Extremely low humidity.
The technical proposal of the invention is realized in this way：
A kind of coating slurry of lithium ion battery separator, is calculated according to percetage by weight, including following components：
Water-soluble cellulose 0.01~5%, inorganic ceramic particle 12~60%, amphoteric dispersant 0.5~4%, surface are lived
Property agent 0.01~1%, both sexes adhesive 1~10% and deionized water 35~80%.
Preferably, the both sexes adhesive is total to selected from carboxylic chloroprene rubber latex, bi-component acrylic copolymer emulsion and acrylic acid
One or more in the poly resin aqueous solution, styrene-butadiene latex and organosilicon-modified acrylate.
Preferably, the amphoteric dispersant is selected from N, N- dimethyl amidos propylamine, polyethylene polyamine, octadecylamine base propylamine,
Oxirane and epoxy propane copolymer, the hydroxy terminated polypropylene acid esters and one or more in end carboxyl polyacrylate.
Preferably, the water-soluble cellulose is selected from carboxymethyl-cellulose ammonium salt, carboxymethyl cellulose sulfate, carboxymethyl
Cellulose carbonate, hydroxymethyl cellulose sulfate, hydroxymethyl cellulose carbonate, methyl hydroxyethylcellulose carbonate and first
One or more in base hydroxypropyl cellulose ammonium salt.
Preferably, the inorganic ceramic particle is selected from alundum (Al2O3), boehmite, barium sulfate, magnesium sulfate, barium titanate, two
One or more in silica, titanium dioxide, magnesium hydroxide and aluminium hydroxide.
Preferably, the surfactant is selected from neopelex, fatty glyceride, perfluorinated sulfonate, silicon
The one or more of alkane surfactant and modified polyalcohol surfactant.
It is a further object to provide a kind of lithium ion battery separator, including MIcroporous polyolefin film and above-mentioned lithium
The coating slurry of ion battery barrier film, the coating slurry is coated in above the MIcroporous polyolefin film.
It is also another object of the present invention to provide a kind of preparation method of lithium ion battery separator, comprise the following steps：
1) deionized water is heated to 50~95 DEG C, then water-soluble cellulose is added thereto, and obtains water-soluble cellulose
Dispersion liquid；
2) inorganic ceramic particle, amphoteric dispersant, surfactant and both sexes are added into water-soluble cellulose dispersion liquid
Adhesive mixing is scattered, obtains coating slurry；
3) coating slurry drying, is formed into inorganic ceramic painting coated on MIcroporous polyolefin film on MIcroporous polyolefin film
Layer, you can obtain lithium ion battery separator.
Preferably, the painting method of the step 3) is spraying, micro- rotogravure application, electrophoretic coating or flow coat.
Preferably, the thickness of the inorganic ceramic coating is 0.5~10 μm.
Further, MIcroporous polyolefin film thickness range in 5~80 μm, porosity ranges 27~85%, average pore size model
It is trapped among 0.02~1 μm.
Further, MIcroporous polyolefin film is prepared by MIcroporous polyolefin film, heating consumers prepared by melt drawn principle
MIcroporous polyolefin film, pass through spinning prepare non-woven polyolefin microporous barrier or physics lixiviation process prepare polyolefin micropore
Film.
Beneficial effects of the present invention：
Using water-soluble cellulose that is not soluble in water under normal temperature and not absorbing water, strict control coating barrier film moisture, symbol
Close the low demand of power vehicle battery moisture.Using double property dispersants and double property adhesives, applied suitable for water-based system
While covering slurry, there is the hydrophobicity of a capability, equally reach the purpose of strict control coating barrier film moisture.Due to
Coating barrier film does not absorb water, and moisture is up to standard, and the transport, packaging, storage for coated product need not control extremely low humidity,
Cost is reduced, improves efficiency.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the change of moisture content figure of lithium ion battery separator of the present invention and comparative example barrier film；
Fig. 2 is the lithium ion battery separator electron microscopic picture of the embodiment of the present invention 1.
Embodiment
Embodiment 1
The preparation method of lithium ion battery separator：
1) deionized water that heating quality percentage is 51.99% dissolves 0.5% carboxymethyl-cellulose ammonium salt to 65 DEG C,
Obtain water-based carboxymethyl-cellulose ammonium salt dispersion liquid；
2) toward in the water-based carboxymethyl-cellulose ammonium salt dispersion liquid of step 1), matter of the particle size range at 0.05-1 μm is sequentially added
Amount percentage is 45% alundum (Al2O3), 0.5% dispersant N, N- dimethyl amido propylamine, 2% adhesive organic-silicon-modified third
Coating slurry is made in olefin(e) acid ester and 0.01% perfluorinated sulfonate,
3) by micro- rotogravure application by above-mentioned steps 2) obtained by nano ceramics slurry coated in thickness be 16 microns, hole
Gap rate is 42%, and average pore size scope is on 0.02-0.07 μm of melt-pulling method single-layer polypropylene microporous barrier, obtains lithium ion
Battery diaphragm.
The scanning electron microscope (SEM) photograph for the lithium ion battery separator that the present embodiment is prepared is shown in Fig. 2.
Embodiment 2
The preparation method of lithium ion battery separator：
1) heating quality percentage be 51.49% deionized water to 65 DEG C, dissolving 0.5% carboxymethyl-cellulose ammonium salt and
0.5% hydroxymethyl cellulose carbonate, obtain water-based carboxymethyl-cellulose ammonium salt and hydroxymethyl cellulose carbonate dispersion；
2) toward in the water-based carboxymethyl-cellulose ammonium salt of step 1) and hydroxymethyl cellulose carbonate dispersion, grain is sequentially added
Footpath scope 0.05-1 μm mass percent for 45% alundum (Al2O3), 0.5% dispersant N, N- dimethyl amido propylamine,
Coating slurry is made in 2% adhesive organosilicon-modified acrylate and 0.01% perfluorinated sulfonate,
3) by micro- rotogravure application by above-mentioned steps 2) obtained by nano ceramics slurry coated in thickness be 16 microns, hole
Gap rate is 42%, and average pore size scope is on 0.02-0.07 μm of melt-pulling method single-layer polypropylene microporous barrier, obtains lithium ion
Battery diaphragm.
Embodiment 3
The preparation method of lithium ion battery separator：
1) ionized water that heating quality percentage is 51.49% dissolves 1% carboxymethyl-cellulose ammonium salt, obtained to 65 DEG C
Water-based carboxymethyl-cellulose ammonium salt dispersion liquid；
2) toward in the water-based carboxymethyl-cellulose ammonium salt dispersion liquid of step 1), matter of the particle size range at 0.05-1 μm is sequentially added
Amount percentage is 45% alundum (Al2O3), 0.5% dispersant N, N- dimethyl amido propylamine, 2% adhesive organic-silicon-modified third
Coating slurry is made in olefin(e) acid ester and 0.01% perfluorinated sulfonate,
3) by micro- rotogravure application by above-mentioned steps 2) obtained by nano ceramics slurry coated in thickness be 16 microns, hole
Gap rate is 42%, and average pore size scope is on 0.02-0.07 μm of melt-pulling method single-layer polypropylene microporous barrier, obtains lithium ion
Battery diaphragm.
Comparative example 1
1) at room temperature mass percent be 51.99% deionized water in the sodium carboxymethylcellulose of stirring and dissolving 0.5%
Salt, obtain water-based sanlose dispersion liquid；
2) toward in the water-based sanlose dispersion liquid of step 1), matter of the particle size range at 0.05-1 μm is sequentially added
Amount percentage is 45% alundum (Al2O3), 0.5% dispersant N, N- dimethyl amido propylamine, 2% adhesive organic-silicon-modified third
Coating slurry is made in olefin(e) acid ester and 0.01% perfluorinated sulfonate,
3) by micro- rotogravure application by above-mentioned steps 2) obtained by nano ceramics slurry coated in thickness be 16 microns, hole
Gap rate is 42%, and average pore size scope is on 0.02-0.07 μm of melt-pulling method single-layer polypropylene microporous barrier, completes a kind of apply
Cover the preparation of lithium battery diaphragm.
Comparative example 2
1) for the ionized water that heating quality percentage is 51.99% to 65 DEG C, high-speed stirred dissolves 0.3% carboxymethyl cellulose
Ammonium salt, obtain water-based carboxymethyl-cellulose ammonium salt dispersion liquid；
2) toward in the water-based carboxymethyl-cellulose ammonium salt dispersion liquid of step 1), matter of the particle size range at 0.05-1 μm is sequentially added
Amount percentage be 45% alundum (Al2O3), 0.5% dispersant N, N- dimethyl amido propylamine, 2% adhesive polyvinyl alcohol and
Coating slurry is made in 0.01% perfluorinated sulfonate,
3) by micro- rotogravure application by above-mentioned steps 2) obtained by nano ceramics slurry coated in thickness be 16 microns, hole
Gap rate is 42%, and average pore size scope is on 0.02-0.07 μm of melt-pulling method single-layer polypropylene microporous barrier, completes a kind of apply
Cover the preparation of lithium battery diaphragm.
Test example 1
Embodiment 1-3 and comparative example 1-2 is carried out into barrier film thermal contraction test, thickness test and battery to test,
It the results are shown in Table 1.
Barrier film thermal contraction test method：Every kind of barrier film takes 5 100mm × 100mm samples, measurement MD directions length, note
For L0, sample is put into temperature baking oven is set, taken out after the stipulated time, the length in measurement MD directions is designated as L, percent thermal shrinkage
Calculation formula is：
Δ L=(L-L0)/L0 × 100%
5 sample percent thermal shrinkages are measured, then percent thermal shrinkage, is averaged, and barrier film percent thermal shrinkage is coated for this.MD is poly-
The draw direction of propylene microcellular film melt-pulling method.
Thickness testing method：It is 100mm × 100mm samples to take barrier film size, after testing 20 points with thickness measurement equipment, is taken
Average value, as coat barrier film thickness of sample.
Battery method of testing：By positive plate, obtained coating barrier film and negative plate full of argon gas gloves
Button cell is assembled into case, battery capacity loop test is carried out on cycle charge discharge electric tester.
The embodiment 1-3 of table 1 and comparative example 1-2 membrane properties test result
Found out by table 1, embodiments of the invention and comparative example all have good heat resistance, show ceramic coating membrane
Superiority, it was found from battery, embodiments of the invention coating barrier film Capacity Ratio comparative example coating barrier film appearance
Amount loss is less, and service life is longer.
Test example 2
Embodiment 1-3 and comparative example 1-2 is subjected to moisture test, as a result sees Fig. 1.
Moisture method of testing：Every kind of coating barrier film takes 10 samples, and water is tested using karl Fischer moisture teller
Divide content, place certain time re-test moisture, average, as coat barrier film sample moisture.
As can be seen from Figure 1 embodiment 1, embodiment 2, the moisture of embodiment 3 are than comparative example 1, comparative example 2
It is low, and after certain time is placed, barrier film moisture remains unchanged, and illustrates that the coating barrier film moisture in embodiment is low,
And do not absorb water, meet current driving force automobile lithium battery or large-scale energy storage device lithium battery moisture requires low requirement, realize
The high performance of lithium battery diaphragm.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (10)
- A kind of 1. coating slurry of lithium ion battery separator, it is characterised in that calculated according to percetage by weight, including with the following group Point：Water-soluble cellulose 0.01~5%, inorganic ceramic particle 12~60%, amphoteric dispersant 0.5~4%, surfactant 0.01~1%, both sexes adhesive 1~10% and deionized water 35~80%.
- 2. the coating slurry of lithium ion battery separator according to claim 1, it is characterised in that the both sexes adhesive Selected from carboxylic chloroprene rubber latex, bi-component acrylic copolymer emulsion and the acrylic copolymeric resin aqueous solution, styrene-butadiene latex and organosilicon One or more in modification acrylate.
- 3. the coating slurry of lithium ion battery separator according to claim 1, it is characterised in that the amphoteric dispersant Selected from N, N- dimethyl amidos propylamine, polyethylene polyamine, octadecylamine base propylamine, oxirane and epoxy propane copolymer, end hydroxyl Based polyacrylic acid ester and the one or more in end carboxyl polyacrylate.
- 4. the coating slurry of lithium ion battery separator according to claim 1, it is characterised in that the water-soluble fibre Element is selected from carboxymethyl-cellulose ammonium salt, carboxymethyl cellulose sulfate, carboxymethyl cellulose carbonate, hydroxymethyl cellulose sulfuric acid One kind in salt, hydroxymethyl cellulose carbonate, methyl hydroxyethylcellulose carbonate and methylhydroxypropylcellulose ammonium salt or Person is a variety of.
- 5. the coating slurry of lithium ion battery separator according to claim 1, it is characterised in that the inorganic ceramic Grain-by-grain seed selection is from alundum (Al2O3), boehmite, barium sulfate, magnesium sulfate, barium titanate, silica, titanium dioxide, magnesium hydroxide and hydrogen-oxygen Change the one or more in aluminium.
- 6. the coating slurry of lithium ion battery separator according to claim 1, it is characterised in that the surfactant Lived selected from neopelex, fatty glyceride, perfluorinated sulfonate, silane surface active agent and modified polyalcohol surface The one or more of property agent.
- 7. a kind of lithium ion battery separator, it is characterised in that including MIcroporous polyolefin film and lithium ion as claimed in claim 1 The coating slurry of battery diaphragm, the coating slurry is coated in above the MIcroporous polyolefin film.
- 8. a kind of preparation method of lithium ion battery separator as claimed in claim 7, it is characterised in that comprise the following steps：1) deionized water is heated to 50~95 DEG C, then water-soluble cellulose is added thereto, and is obtained water-soluble cellulose and is disperseed Liquid；2) inorganic ceramic particle, amphoteric dispersant, surfactant and both sexes gluing are added into water-soluble cellulose dispersion liquid Agent mixing is scattered, obtains coating slurry；3) coating slurry drying, is formed into inorganic ceramic coating, i.e., coated on MIcroporous polyolefin film on MIcroporous polyolefin film Lithium ion battery separator can be obtained.
- 9. the preparation method of lithium ion battery separator according to claim 8, it is characterised in that the coating of the step 3) Method is spraying, micro- rotogravure application, electrophoretic coating or flow coat.
- 10. the preparation method of lithium ion battery separator according to claim 8, it is characterised in that the inorganic ceramic applies The thickness of layer is 0.5~10 μm.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807789A (en) * | 2018-05-28 | 2018-11-13 | 上海恩捷新材料科技股份有限公司 | Diaphragm and preparation method thereof for lithium ion battery |
| CN109244328A (en) * | 2018-09-25 | 2019-01-18 | 合肥先杰新能源科技有限公司 | Lithium ion battery separator and preparation method thereof |
| CN109244325A (en) * | 2018-09-25 | 2019-01-18 | 合肥先杰新能源科技有限公司 | lithium battery diaphragm and preparation method thereof |
| CN109244329A (en) * | 2018-09-25 | 2019-01-18 | 合肥先杰新能源科技有限公司 | The preparation method of fiber base lithium ion battery separator |
| CN109273649A (en) * | 2018-09-25 | 2019-01-25 | 合肥先杰新能源科技有限公司 | Lithium battery micro-pore septum and preparation method thereof |
| CN109671894A (en) * | 2018-11-29 | 2019-04-23 | 明基材料（芜湖）有限公司 | Low-water-content isolation film and its manufacturing method |
| CN109742293A (en) * | 2018-12-18 | 2019-05-10 | 乐凯胶片股份有限公司 | A kind of lithium battery coated separator and preparation method thereof with low water content |
| CN110085791A (en) * | 2019-04-11 | 2019-08-02 | 电子科技大学 | A kind of lithium ion battery separator and preparation method thereof |
| CN110492043A (en) * | 2019-09-09 | 2019-11-22 | 新乡市中科科技有限公司 | One kind is containing organic-inorganic coating septum for lithium ion battery and preparation method thereof |
| CN113659286A (en) * | 2021-08-10 | 2021-11-16 | 惠州亿纬锂能股份有限公司 | Boehmite slurry, boehmite coated diaphragm, preparation method of boehmite coated diaphragm and lithium ion battery |
| CN115101891A (en) * | 2022-07-19 | 2022-09-23 | 中材锂膜有限公司 | Preparation method of lithium ion battery diaphragm |
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| CN108807789A (en) * | 2018-05-28 | 2018-11-13 | 上海恩捷新材料科技股份有限公司 | Diaphragm and preparation method thereof for lithium ion battery |
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| CN109244329A (en) * | 2018-09-25 | 2019-01-18 | 合肥先杰新能源科技有限公司 | The preparation method of fiber base lithium ion battery separator |
| CN109273649A (en) * | 2018-09-25 | 2019-01-25 | 合肥先杰新能源科技有限公司 | Lithium battery micro-pore septum and preparation method thereof |
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| CN109671894A (en) * | 2018-11-29 | 2019-04-23 | 明基材料（芜湖）有限公司 | Low-water-content isolation film and its manufacturing method |
| CN109742293A (en) * | 2018-12-18 | 2019-05-10 | 乐凯胶片股份有限公司 | A kind of lithium battery coated separator and preparation method thereof with low water content |
| CN109742293B (en) * | 2018-12-18 | 2021-11-16 | 乐凯胶片股份有限公司 | Lithium battery coating diaphragm with low water content and preparation method thereof |
| CN110085791A (en) * | 2019-04-11 | 2019-08-02 | 电子科技大学 | A kind of lithium ion battery separator and preparation method thereof |
| CN110492043A (en) * | 2019-09-09 | 2019-11-22 | 新乡市中科科技有限公司 | One kind is containing organic-inorganic coating septum for lithium ion battery and preparation method thereof |
| CN113659286A (en) * | 2021-08-10 | 2021-11-16 | 惠州亿纬锂能股份有限公司 | Boehmite slurry, boehmite coated diaphragm, preparation method of boehmite coated diaphragm and lithium ion battery |
| CN115101891A (en) * | 2022-07-19 | 2022-09-23 | 中材锂膜有限公司 | Preparation method of lithium ion battery diaphragm |
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Application publication date: 20180126 |