CN113871795A - Wetting diaphragm and preparation method and application thereof - Google Patents

Wetting diaphragm and preparation method and application thereof Download PDF

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Publication number
CN113871795A
CN113871795A CN202111128355.5A CN202111128355A CN113871795A CN 113871795 A CN113871795 A CN 113871795A CN 202111128355 A CN202111128355 A CN 202111128355A CN 113871795 A CN113871795 A CN 113871795A
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diaphragm
coating
polyolefin
glue
discontinuous
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CN202111128355.5A
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CN113871795B (en
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谭小芳
曾汉民
林文佳
杨升
何巍
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Eve Energy Co Ltd
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Eve Energy Co Ltd
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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
    • H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
    • H01M50/417—Polyolefins
    • 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
    • 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
    • H01M50/463—Separators, membranes or diaphragms characterised by their shape
    • 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

Abstract

The invention provides an infiltration diaphragm and a preparation method and application thereof, wherein the infiltration diaphragm comprises a polyolefin-based diaphragm and coatings positioned on one side or two sides of the polyolefin-based diaphragm, the coatings comprise ceramics and glue, discontinuous concave holes are formed in the coatings, and the discontinuous concave holes are covered or not covered with the glue and can be used for storing electrolyte, so that the infiltration of the diaphragm on the electrolyte is high, and the long-term performance of a battery is excellent.

Description

Wetting diaphragm and preparation method and application thereof
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a wetting diaphragm and a preparation method and application thereof.
Background
The diaphragm is used as a key safety component of the lithium ion battery, has rich pore channel structures, and has the function of blocking the contact of active substances of the anode and the cathode and transmitting lithium ions of the lithium ion battery. With the increasing market demand for power batteries, the production of batteries with high energy density becomes a trend, and the requirement of the wettability of the diaphragm is provided for improving the problem of the electrolyte wettability of the middle part of the large power battery. The current commercial polymer coated diaphragm has the disadvantages of complicated manufacturing process, higher cost and general wetting performance.
CN110556495A discloses a lithium ion battery diaphragm and contain lithium ion battery of this diaphragm, lithium ion battery diaphragm include heat-resisting composite substrate layer, the one side of heat-resisting composite substrate layer is provided with first organic glue coating, heat-resisting composite substrate layer include the base film and set up in the ceramic layer on base film surface, the base film has a plurality of holes, and is a plurality of adhere to in the hole and have modified polyolefin coating, first organic glue coating includes first complete coating district, check intermittent type coating district and the complete coating district of second from the top edge to the lower limb of base film in proper order, its diaphragm preparation technology is loaded down with trivial details and the cohesiveness is poor.
CN112599926A discloses a self-partition functional battery diaphragm, a lithium ion battery and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a separator slurry containing foamed particles; providing a non-woven fabric base film, coating the diaphragm slurry on at least one surface of the non-woven fabric base film, and allowing the diaphragm slurry to enter the non-woven fabric base film; and baking the non-woven fabric base film coated with the diaphragm slurry to enable the diaphragm slurry to form a porous layer containing foaming particles so as to obtain the battery diaphragm, wherein the wettability of the diaphragm is poor.
The technical scheme has the problems of complicated preparation process and poor wettability of the diaphragm, so that the development of the diaphragm for the lithium ion battery, which has a simple preparation process and a good wetting effect, is very necessary.
Disclosure of Invention
The invention aims to provide an infiltration diaphragm and a preparation method and application thereof, wherein the infiltration diaphragm comprises a polyolefin-based diaphragm and coatings positioned on one side or two sides of the polyolefin-based diaphragm, discontinuous concave holes are formed in the coatings, and glue is covered or not covered on the discontinuous concave holes, so that the infiltration diaphragm can be used for storing electrolyte, the infiltration of the diaphragm to the electrolyte is high, and the long-term performance of a battery is excellent.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a wetting diaphragm, which comprises a polyolefin-based diaphragm and a coating located on one side or two sides of the polyolefin-based diaphragm, wherein the coating comprises ceramic and glue, discontinuous concave holes are formed in the coating, and the discontinuous concave holes are covered or not covered with the glue.
The wettability membrane comprises a polyolefin-based membrane and coatings positioned on one side or two sides of the polyolefin-based membrane, discontinuous concave holes are formed in the coatings, the discontinuous concave holes are covered or not covered with glue, and the discontinuous concave holes can be used for storing electrolyte, so that the wettability of the membrane on the electrolyte is high, and the long-term performance of a battery is excellent; meanwhile, compared with a commercialized polymer coating diaphragm, the diaphragm provided by the invention has the advantages of simple manufacturing process, low cost, small ionic resistance and the like.
Preferably, the average diameter of the discontinuous concave holes is 0.2-200 μm, for example: 0.2 μm, 1 μm, 5 μm, 10 μm, 50 μm, 100 μm, 200 μm, or the like.
Preferably, the discontinuous recesses are irregularly shaped.
Preferably, the particle size of the covering glue on the discontinuous concave holes is 2-50 μm, for example: 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, or 50 μm, etc.
Preferably, the polyolefin-based separator includes any one of a polyethylene separator, a polypropylene separator, or a polyethylene-polypropylene composite separator, or a combination of at least two thereof.
Preferably, the polyolefin-based separator has a thickness of 4 to 20 μm, for example: 4 μm, 8 μm, 10 μm, 12 μm, 15 μm, 20 μm, or the like.
Preferably, the polyolefin-based separator has a pore size of 10 to 400nm, for example: 10nm, 50nm, 100nm, 200nm, 300nm, 400nm, etc.
Preferably, the ceramic comprises any one of boehmite, alumina, magnesium hydroxide, magnesium oxide, titanium dioxide, barium titanate, zinc oxide, barium sulfate, or a combination of at least two thereof.
Preferably, the mass fraction of the ceramic is 80-90% based on 100% of the mass of the coating, such as: 80%, 82%, 85%, 88%, 90%, etc.
Preferably, the glue monomer covered on the discontinuous concave hole comprises any one or a combination of at least two of acrylic acid, ammonium acrylate, methyl acrylate, ethyl acrylate, butyl acrylate, methacrylic acid, methyl methacrylate, ethyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, N-hydroxymethyl acrylamide, hydroxyethyl methacrylate, glycidyl acrylate, styrene alcohol, styrene acrylate, vinyl acid methyl ester, vinylidene fluoride, hexafluoropropylene and tetrafluoroethylene.
Preferably, the thickness of the glue covered on the discontinuous concave holes is 5-70% calculated by taking the coating thickness as 100%, for example: 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, or the like.
Preferably, the area of the discontinuous concave holes accounts for 1-20% of the area of the coating, for example: 1%, 5%, 10%, 15%, 20%, etc.
In a second aspect, the present invention provides a method for preparing the wettability membrane according to the first aspect, wherein the preparation method comprises the following steps:
(1) mixing ceramic powder, glue and a hydrosolvent to obtain coating slurry;
(2) coating the coating slurry obtained in the step (1) on one side or two sides of a polyolefin-based diaphragm, and drying;
(3) soaking the diaphragm obtained in the step (2) in an organic solvent, taking out after 12-36 h, and drying to obtain the wettability diaphragm;
wherein, the organic solvent comprises any one of dimethyl carbonate, ethyl methyl carbonate or ethylene carbonate or the combination of at least two of the dimethyl carbonate, the ethyl methyl carbonate or the ethylene carbonate.
In a third aspect, the present invention provides a lithium ion battery, which includes the wettability membrane according to the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) the wetting diaphragm is provided with the coating on the surface of the polyolefin-based diaphragm, discontinuous concave holes in the coating are covered or not covered with glue, and the size of the discontinuous concave holes is 0.2-200 mu m, so that the wetting diaphragm can be used for storing electrolyte, the wetting performance of the diaphragm on the electrolyte is high, and the long-term performance of a battery is excellent.
(2) The diaphragm provided by the invention has the advantages of simple manufacturing process, low cost and small ionic resistance.
Drawings
FIG. 1 is an SEM image of a wetting membrane according to example 1 of the present invention.
FIG. 2 is a schematic view of the structure of the wettable membrane of example 1 of the invention, 1-discrete recess locations, 2-coating, 3-base film.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a wettability membrane, which is prepared by the following method:
(1) mixing alumina powder, acrylate group and styryl group-containing glue with the particle size of 20 mu m and water to obtain coating slurry, wherein the mass percentage of alumina in the coating slurry is 80%;
(2) coating the coating slurry obtained in the step (1) on two sides of a polyethylene diaphragm with the average pore diameter of 40nm and the thickness of 9 microns, and drying;
(3) and (3) soaking the diaphragm obtained in the step (2) in dimethyl carbonate, taking out the diaphragm after 12-36 hours, and drying to obtain the wettability diaphragm, wherein the thickness of the coating is 2 microns, and the average diameter of discontinuous concave holes is 10 microns.
The SEM of the resulting wetted membrane is shown in FIG. 1.
The structural schematic diagram of the prepared wetting diaphragm is shown in fig. 2, the coating 2 is positioned on the surface of the base film 3, and discontinuous irregular concave hole positions 1 are arranged on the surface of the coating.
Example 2
The embodiment provides a wettability membrane, which is prepared by the following method:
(1) mixing boehmite powder, glue with 25 mu m of particle size and containing methyl methacrylate group and water to obtain coating slurry, wherein the mass ratio of boehmite in the coating slurry is 85%;
(2) coating the coating slurry obtained in the step (1) on two sides of a polyethylene diaphragm with the average pore diameter of 70nm and the thickness of 9 microns, and drying;
(3) and (3) soaking the diaphragm obtained in the step (2) in dimethyl carbonate, taking out the diaphragm after 12-36 hours, and drying to obtain the wettability diaphragm, wherein the thickness of the coating is 2 microns, and the average diameter of discontinuous concave holes is 10 microns.
Example 3
This example is different from example 1 only in that the mass ratio of alumina in the coating slurry in step (1) is 75%, and other conditions and parameters are exactly the same as those in example 1.
Example 4
This example is different from example 1 only in that the mass ratio of alumina in the coating slurry in step (1) is 95%, and other conditions and parameters are exactly the same as those in example 1.
Example 5
This example is different from example 1 only in that the thickness of the polyethylene separator in step (2) is 3 μm, and other conditions and parameters are exactly the same as those in example 1.
Example 6
This example is different from example 5 only in that the thickness of the polyethylene separator in step (2) is 25 μm, and other conditions and parameters are exactly the same as those in example 5.
Comparative example 1
This comparative example is different from example 1 only in that alumina and a glue are sequentially layered-coated on the surface of a polyolefin-based separator, and other conditions and parameters are exactly the same as those of example 1.
Comparative example 2
The comparative example differs from example 1 only in that no glue is added, and the other conditions and parameters are exactly the same as in example 1.
And (3) performance testing:
testing the liquid absorption rate, the liquid retention rate and the ionic resistance of the diaphragm provided by each embodiment and the comparative example, and assembling the diaphragm with a positive plate and a negative plate to form a battery cell, wherein the mass ratio of nickel cobalt lithium manganate, acetylene black and polyvinylidene fluoride in the positive plate is 9.5:0.2:0.3, the mass ratio of graphite, acetylene black, sodium carboxymethylcellulose and styrene butadiene rubber in the negative plate is 9.5:0.2:0.15:0.15, injecting an electrolyte, and the electrolyte is LiPF6After preparing a lithium ion battery from/EC + DEC + DMC (EC, DEC and DMC in a volume ratio of 1:1:1), carrying out 45 ℃ cycle test, wherein the test method is as follows:
testing the liquid absorption rate and the liquid retention rate: winding the diaphragm and the same positive and negative pole pieces into a naked electric core and weighing the naked electric core with the mass of W0Immersing into a mixed solution of Ethylene Carbonate (EC) and Propylene Carbonate (PC) at the same volume ratio of 1:1 at room temperature, standing for 2h, sucking the electrolyte on the surface with filter paper, weighing, and recording the mass as W1The liquid absorption rate is (W)1-W0)/W0(ii) a Then the mixture is placed in the air at room temperature for 12 hours, weighed again and recorded as W2The retention rate is (W)2-W0)/(W1-W0)。
And (3) testing the ionic resistance: the inert stainless steel electrode is adopted to manufacture a symmetrical battery for testing, the resistance of the battery is correspondingly increased along with the increase of the number of layers of the diaphragm, and the battery resistance is in a linear relation, and the corresponding slope is the diaphragm resistance.
And (3) battery core circulation test at 45 ℃: charging and discharging 0.5C/1C to the cell at 45 deg.C, and recording the 1 st circle discharge capacity C0And then discharge capacity per cycle CnRetention rate of discharge capacity ═ Cn*100/C0
The test results are shown in table 1:
TABLE 1
Figure BDA0003279549490000071
As can be seen from table 1, the separators obtained in examples 1 to 6 had good wettability, low ionic resistance, and excellent long-term performance.
By comparing the example 1 with the example 2, the coating slurry can be coated on the polyolefin-based diaphragm with any aperture, and the obtained diaphragm has good wettability and excellent long-term performance.
Comparing the embodiment 1 with the embodiment 3-4, the quality ratio of the ceramic in the coating slurry influences the performance of the prepared wetting diaphragm, the quality ratio of the ceramic in the coating slurry is controlled to be 80-90%, the diaphragm with excellent performance can be prepared, if the quality ratio of the ceramic in the coating slurry is too low, the area ratio of discontinuous concave holes in the coating is too high, the thermal shrinkage performance of the diaphragm is reduced, and the safety performance is reduced, and if the quality ratio of the ceramic in the coating slurry is too high, the area ratio of the discontinuous concave holes in the coating is too low, the wetting performance of the diaphragm is reduced, and the liquid absorption rate and the liquid retention rate are reduced.
As can be seen from comparison between example 1 and examples 5-6, the thickness of the base film in step (2) affects the performance of the obtained wettable membrane, and the thickness of the base film is controlled to be 4-20 μm, so that the wettable membrane with excellent performance can be obtained.
Compared with the comparative example 1, the heat-resistant material and the glue are prepared into the coating slurry and coated on the surface of the polyolefin-based diaphragm, so that the preparation method is simple in preparation process, low in cost and small in ionic resistance.
As can be seen from comparison of example 1 with comparative example 2, the separator of the present invention has good wettability and the battery has excellent long-term performance.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. The utility model provides an infiltration nature diaphragm, its characterized in that, infiltration nature diaphragm includes polyolefin-based diaphragm and is located the coating of polyolefin-based diaphragm one side or both sides, the coating includes pottery and glue, be provided with discontinuous shrinkage pool on the coating, cover or not cover on the discontinuous shrinkage pool and glue.
2. The infiltrative separator according to claim 1, wherein the discontinuous recesses have an average diameter of 0.2 to 200 μm;
preferably, the discontinuous recesses are irregularly shaped;
preferably, the particle size of the covering glue on the discontinuous concave holes is 2-50 μm.
3. The infiltrant membrane according to claim 1 or 2, wherein the polyolefin-based membrane comprises any one of a polyethylene membrane, a polypropylene membrane, or a polyethylene-polypropylene composite membrane, or a combination of at least two thereof.
4. The infiltrative separator according to any one of claims 1 to 3, wherein the polyolefin-based separator has a thickness of 4 to 20 μm;
preferably, the polyolefin-based separator has a pore size of 10 to 400 nm.
5. The infiltrative separator according to any one of claims 1 to 4, wherein the ceramic includes any one of boehmite, alumina, magnesium hydroxide, magnesium oxide, titanium dioxide, barium titanate, zinc oxide, barium sulfate, or a combination of at least two thereof;
preferably, the mass fraction of the ceramic is 80-90% based on 100% of the mass of the coating.
6. The infiltrative membrane according to any one of claims 1-5, wherein the glue monomer covering the discontinuous recessed holes comprises any one of acrylic acid, ammonium acrylate, methyl acrylate, ethyl acrylate, butyl acrylate, methacrylic acid, methyl methacrylate, ethyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, N-methylol acrylamide, hydroxyethyl methacrylate, glycidyl acrylate, styrene alcohol, styrene enoate, styrene nitrile, styrene acrylate, vinyl acid, methyl vinyl acetate, vinylidene fluoride, hexafluoropropylene, tetrafluoroethylene, or a combination of at least two thereof.
7. An infiltrative membrane according to any one of claims 1-6, wherein the thickness of the glue covering the discontinuous recesses is 5-70% calculated on the basis of 100% of the thickness of the coating.
8. An infiltrative separator according to any one of claims 1-6, wherein the discontinuous recesses have an area ratio of 1-20% based on 100% of the area of the coating.
9. A method for manufacturing the impregnating membrane according to any one of claims 1 to 8, comprising the steps of:
(1) mixing ceramic powder, glue and a hydrosolvent to obtain coating slurry;
(2) coating the coating slurry obtained in the step (1) on one side or two sides of a polyolefin-based diaphragm, and drying;
(3) soaking the diaphragm obtained in the step (2) in an organic solvent, taking out after 12-36 h, and drying to obtain the wettability diaphragm;
wherein, the organic solvent comprises any one of dimethyl carbonate, ethyl methyl carbonate or ethylene carbonate or the combination of at least two of the dimethyl carbonate, the ethyl methyl carbonate or the ethylene carbonate.
10. A lithium ion battery comprising the wettable membrane of any one of claims 1 to 8.
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Citations (9)

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Publication number Priority date Publication date Assignee Title
KR20060003665A (en) * 2004-07-07 2006-01-11 주식회사 엘지화학 New organic/inorganic composite porous film and electrochemical device prepared thereby
US20130084483A1 (en) * 2011-04-06 2013-04-04 Lg Chem, Ltd. Separator and electrochemical device comprising the same
CN103441230A (en) * 2013-08-21 2013-12-11 东莞新能源科技有限公司 Organic/inorganic composite porous isolating membrane, preparation method thereof and electrochemical device
CN105140451A (en) * 2015-07-06 2015-12-09 佛山荷韵特种材料有限公司 Lithium-ion battery diaphragm and preparation method thereof
WO2016034019A1 (en) * 2014-09-02 2016-03-10 深圳市星源材质科技股份有限公司 Aqueous polymer and inorganic nanoparticle composite lithium battery separator and preparation method thereof
CN106549128A (en) * 2017-01-19 2017-03-29 宁德卓高新材料科技有限公司 A kind of non-all standing formula coats the preparation method of barrier film
CN109817872A (en) * 2019-03-07 2019-05-28 武汉中兴创新材料技术有限公司 A kind of non-all standing coated separator and preparation method thereof and device
CN110556495A (en) * 2019-08-22 2019-12-10 惠州锂威新能源科技有限公司 lithium ion battery diaphragm and lithium ion battery containing same
CN113178663A (en) * 2021-04-28 2021-07-27 惠州亿纬锂能股份有限公司 Composite diaphragm and preparation method and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060003665A (en) * 2004-07-07 2006-01-11 주식회사 엘지화학 New organic/inorganic composite porous film and electrochemical device prepared thereby
US20130084483A1 (en) * 2011-04-06 2013-04-04 Lg Chem, Ltd. Separator and electrochemical device comprising the same
CN103441230A (en) * 2013-08-21 2013-12-11 东莞新能源科技有限公司 Organic/inorganic composite porous isolating membrane, preparation method thereof and electrochemical device
WO2016034019A1 (en) * 2014-09-02 2016-03-10 深圳市星源材质科技股份有限公司 Aqueous polymer and inorganic nanoparticle composite lithium battery separator and preparation method thereof
CN105140451A (en) * 2015-07-06 2015-12-09 佛山荷韵特种材料有限公司 Lithium-ion battery diaphragm and preparation method thereof
CN106549128A (en) * 2017-01-19 2017-03-29 宁德卓高新材料科技有限公司 A kind of non-all standing formula coats the preparation method of barrier film
CN109817872A (en) * 2019-03-07 2019-05-28 武汉中兴创新材料技术有限公司 A kind of non-all standing coated separator and preparation method thereof and device
CN110556495A (en) * 2019-08-22 2019-12-10 惠州锂威新能源科技有限公司 lithium ion battery diaphragm and lithium ion battery containing same
CN113178663A (en) * 2021-04-28 2021-07-27 惠州亿纬锂能股份有限公司 Composite diaphragm and preparation method and application thereof

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