CN114335899A - Composite coating diaphragm and preparation method thereof - Google Patents
Composite coating diaphragm and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of lithium ion battery diaphragms, and provides a composite coating diaphragm and a preparation method thereof. The diaphragm comprises a base film and a composite coating coated on one or two surfaces of the base film, wherein the structure of the composite coating consists of a continuous phase and a disperse phase. The composite coating diaphragm of the invention has lower coating thickness, but can ensure higher performance.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a composite coating diaphragm and a preparation method thereof.
Background
With the increasing demand of new energy automobiles and consumer electronics products, the industry of diaphragm materials as an important component of lithium ion batteries is rapidly developing. In the lithium ion battery, the diaphragm can isolate the positive electrode and the negative electrode to prevent internal short circuit, and a large number of nano-scale micropores exist in the diaphragm and can provide a channel for ions in electrolyte to pass through.
In recent years, as the requirements of the market on energy density and safety of batteries are improved, the thicknesses of marketable separators are lower and lower, common polyolefin separators are difficult to meet the requirements, and coating modified separators with a multilayer composite structure become mainstream in the industry. The coating diaphragm mainly takes a polyolefin microporous membrane as a base material, and a layer of organic and/or inorganic material is added on the surface in a coating mode, so that the mechanical strength, wettability, thermal stability and other properties of the diaphragm are improved. For various types of coating diaphragms, different coating materials have different functions and characteristics, for example, aramid fiber materials have the advantages of low density, good heat resistance, high strength, high modulus and the like, PVDF can effectively improve the cohesiveness of the diaphragms and pole pieces, alumina is lower than a finished product and has good flame retardance, and boehmite materials have the advantages of low hardness, small internal resistance, low water absorption and the like.
In the prior art, in order to obtain the advantage characteristic of multiple materials simultaneously, mainly adopt the compound mode of multiple coating to realize, for example at aramid fiber coating diaphragm or ceramic coating diaphragm surface spraying one deck PVDF, can effectively improve the adhesion of diaphragm and lithium battery pole piece, but this kind of mode can cause the diaphragm gross thickness to increase, is unfavorable for the promotion of battery energy density, and coating many times simultaneously is unfavorable for improvement and the cost control of diaphragm production efficiency.
Disclosure of Invention
The invention aims to provide a composite coating diaphragm and a preparation method thereof. The composite coating diaphragm has a low coating thickness, but can ensure high performance.
The invention provides a composite coating diaphragm, which comprises a base film and a composite coating coated on one side or two sides of the base film, wherein the structure of the composite coating consists of a continuous phase and dispersion; the continuous phase is formed by aramid pulp or alumina pulp, and the dispersed phase is formed by PVDF pulp.
The second aspect of the present invention provides a method for preparing the composite coated separator, comprising: spraying a first coating slurry and a second coating slurry on the base film through a multi-cartridge coater, wherein the first coating slurry is selected from the aramid slurry or the alumina slurry, and the second coating slurry is the PVDF slurry; the multi-cartridge coating machine comprises a first coating slurry material cartridge, a second coating slurry material cartridge, a feeding pipe and a material covering cartridge moving guide rail, wherein slurry nozzles are arranged on the coating slurry material cartridges; after the material is supplied to each slurry coating material box through the material supply pipe, the slurry coating material box is driven to move through the material covering box moving guide rail, and slurry is sprayed on the base film through the slurry nozzle to form the composite coating with the continuous phase and the dispersed phase.
The composite coating structure containing multiple slurries comprises a continuous phase and a disperse phase, can effectively overcome the problem of total thickness increase of the diaphragm caused by the compounding of the traditional coating diaphragm multi-layer coating in a combined mode of embedding multiple coatings, effectively reduces the total coating thickness while obtaining multiple coatings, and is beneficial to the improvement of the energy density of a lithium ion battery.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
Exemplary embodiments of the present invention will be described in more detail by referring to the accompanying drawings.
FIG. 1 is a schematic view of a coating apparatus according to an embodiment of the present invention.
Fig. 2 to 4 are schematic structural views of the composite coatings of embodiments 1 to 3, respectively.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In a first aspect, the present invention provides a composite coated separator comprising a base film and a composite coating layer coated on one or both sides of the base film, wherein the structure of the composite coating layer consists of a continuous phase and a dispersed phase.
In the present invention, the dispersed phase is preferably a plurality of regular geometric figures uniformly distributed on the composite coating. Preferably, the individual shape of the dispersed phase is selected from one or more of a circle, a triangle (e.g., an isosceles right triangle), a rectangle, and a square. The various geometric patterns distributed on the composite coating may be the same or different. As shown in fig. 2 to 4, the dispersed phase 3 is a circle or triangle uniformly dispersed on the composite coating, and the areas of the patterns are the same.
In the invention, the distribution of the dispersion phase can be selected according to the bonding requirement of the diaphragm and the pole piece in the lithium ion battery. Typically, the dispersed phase individual pattern area is 0.2mm2～5mm2. The number of the dispersed phase patterns per square decimeter may be 9 to 500, preferably 50 to 500.
In the invention, the thickness of the composite coating can be 0.5-6 μm, and preferably 1-4 μm. For example, the composite coating may have a thickness of 1 μm, 2 μm, 2.5 μm, 3 μm, or 4 μm.
In the present invention, the aramid pulp may include an aramid dope and an inorganic filler. The aramid fiber stock solution can be selected by referring to the existing lithium ion diaphragm and can be directly obtained by commercial purchase. Preferably, the aramid fiber in the aramid fiber stock solution is selected from para-aramid fiber or meta-aramid fiber, and the mass fraction of the aramid fiber polymer in the aramid fiber stock solution is 1-6% (e.g. 1%, 2%, 3%, 4% or 5%). The aramid fiber stock solution can have an apparent viscosity of 3000-30000 cP, for example 20000cP at 25 ℃.
Preferably, the inorganic filler is selected from alumina or boehmite, and the D50 particle size of the inorganic filler is 30-300 nm.
In one embodiment, the mass ratio of the aramid raw liquid to the inorganic filler is 10 to (3-8).
In the present invention, the alumina slurry may include alumina, water, a dispersant, an aqueous binder, and a film-forming agent.
Preferably, the dispersant is sodium carboxymethylcellulose (CMC), the aqueous binder is GR-401 aqueous glue, and the film-forming agent is polyvinyl alcohol (PVA).
In one embodiment, the mass ratio of the aluminum oxide, the water, the dispersant, the water-based binder and the film forming agent is 25: 20-150: 1-5: 0.5-2: 0.05-0.2, preferably 25: 20-50: 1-5: 0.5-2: 0.07-0.15.
In the present invention, the PVDF slurry may be an oil-based PVDF slurry or a water-based PVDF slurry.
In one embodiment, the continuous phase is formed from aramid pulp and the dispersed phase is formed from oil-based PVDF pulp. In another embodiment, the continuous phase is formed from an alumina slurry and the dispersed phase is formed from an aqueous PVDF slurry.
In the present invention, the oil-based PVDF slurry may include PVDF and an organic solvent.
Preferably, the organic solvent is selected from at least one of dimethyl carbonate, N-dimethylacetamide and N-methylpyrrolidone.
In one embodiment, the mass ratio of the PVDF to the organic solvent in the oil-based PVDF slurry is 1: 20-60.
In the present invention, the aqueous PVDF slurry may contain PVDF, a dispersant, and water. The dispersing machine is preferably sodium carboxymethyl cellulose. According to one embodiment, the mass ratio of PVDF, the dispersing agent and water is 1: 0.01-0.2: 5-9. The PVDF can be selected with reference to existing lithium ion battery separators as long as it functions as a binder, and may be, for example, a PVDF product having a designation of DS 202.
In the invention, the thickness of the base film can be 2-30 μm, and preferably 5-15 μm. For example, the thickness of the base film is 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, or 12 μm.
In the present invention, the base film may be a polyolefin separator, such as a wet biaxially oriented polyolefin separator or a dry uniaxially oriented polyolefin separator. The polyolefin separator is preferably a polyethylene separator, more preferably a wet process polyethylene separator. The polyethylene film may have a number average molecular weight (Mn) of 10 to 800 ten thousand, preferably 50 to 200 ten thousand.
The second aspect of the present invention provides a method for preparing the composite coated separator, comprising: spraying a first coating slurry and a second coating slurry on the base film through a multi-box coating machine, wherein the first coating slurry is selected from the aramid slurry or the alumina slurry, and the second coating slurry is the PVDF slurry. The multi-cartridge coating machine comprises a first coating slurry material cartridge, a second coating slurry material cartridge, a feeding pipe and a material covering cartridge moving guide rail, wherein slurry nozzles are arranged on the coating slurry material cartridges; after the material is supplied to each slurry coating material box through the material supply pipe, the slurry coating material box is driven to move through the material covering box moving guide rail, and slurry is sprayed on the base film through the slurry nozzle to form the composite coating with the continuous phase and the dispersed phase.
According to one embodiment, as shown in FIG. 1, the multi-cartridge coater includes two coating slurry cartridges, a first coating slurry cartridge 2-1, a second coating slurry cartridge 3-1; the feeding pipes corresponding to the two slurry coating material boxes are respectively a first feeding pipe 2-2 and a second feeding pipe 3-2; the slurry is respectively supplied to the respective coating slurry box through the feeding pipe, and the slurry box is driven to spray the slurry to different positions of the base film 1 through the slurry nozzle 5 by the movement of the coating slurry box moving guide rail 4, so that the composite coating formed by the first coating slurry part 2-3 and the second coating slurry part 3-3 is prepared. The first coating slip forms a continuous phase and the second coating slip forms a dispersed phase with a uniformly distributed geometry. According to the invention, the position and the residence time of the material boxes on the track and the opening and closing time of the nozzle of each material box can be controlled by setting corresponding multi-material box spraying parameters in a matching software system of the coating machine, so that the composite coating with a specific dispersed phase and a specific continuous phase is obtained.
After the slurry is sprayed on the base film by the multi-cartridge coater according to the present invention, the method of the present invention further comprises a post-treatment, the manner of which can be selected according to the type of slurry selected.
According to one embodiment, the sprayed slurry is aramid slurry and oil-based PVDF slurry, and the post-treatment comprises: and solidifying, washing and drying the coated separator.
Preferably, the process of solidifying comprises: and solidifying and precipitating the coated diaphragm in saturated steam, wherein the temperature of the saturated steam is 30-65 ℃, the humidity is 60-90% RH, and the precipitation time is 10-120 s.
Preferably, the process of water washing comprises: and (4) washing the solidified diaphragm in a pure water tank for 60-300 s.
In this embodiment, the drying conditions may include: the temperature is 65-90 ℃ and the time is 20-100 s.
According to another embodiment, the sprayed slurry is an alumina slurry and a PVDF water based slurry, and the post-treatment includes: the coated separator was dried. The drying conditions may include: the temperature is 65-80 ℃ and the time is 15-80 s.
The method of the invention forms the composite coating with a combined structure by simultaneously coating a plurality of sizing agents on the base film, the method has the characteristic of simple operation, and the formed composite coating diaphragm has the characteristic of small thickness under the condition of ensuring the performance (such as ventilation value and heat shrinkage), and can reduce the consumption of raw materials.
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited to these examples.
In the following examples and comparative examples, a p-aramid stock solution was purchased from nicotintai and new materials gmbh, the mass fraction of aramid polymer was 2%, and the apparent viscosity at 25 ℃ was 20000 cP.
PVDF powder was purchased from Shandong Huaxia Shenzhou New Material Co., Ltd under the designation DS 202.
The alumina is purchased from Shandong China functional materials GmbH, under the trade name of SAO008A, and the grain diameter D50 is 0.19-0.25 μm.
Sodium carboxymethylcellulose (CMC) was purchased from the chemical industry of Japan xylonite, trade Mark CMC-2200.
The aqueous adhesive was purchased from the Hunan Gaorui Power supplies materials Ltd, under the designation GR 401.
Polyvinyl alcohol (PVA) is available from Coly corporation, Japan, under the designation PV-217.
Example 1
(1) Preparation of slurry
Aramid fiber slurry: adding alumina powder into the para-aramid stock solution, stirring for 60min by using a high-speed dispersion emulsifying machine, and filtering by using a 1000-mesh filter to obtain para-aramid slurry. Wherein the mass ratio of the alumina to the para-aramid stock solution is 0.6: 1.
Oil-based PVDF slurry: and adding the PVDF powder into dimethyl carbonate, and stirring for 60min by using a high-speed stirring dispersion machine to obtain the oil PVDF slurry. The mass ratio of PVDF to dimethyl carbonate is 1: 30.
(2) Preparation of composite coating diaphragm
The slurry was coated on a polyethylene diaphragm (base film 1) having a thickness of 12 μm using a multi-pack coater, and according to the coating structure shown in fig. 2, aramid slurry formed a continuous phase 2 and oil-based PVDF slurry formed a dispersed phase 3. Each pattern of the dispersed phase 3 was circular and 2mm in diameter, and the number of the dispersed phase patterns per square decimeter was 60. The porosity of the polyethylene-based film was 40%, the air permeability value was 200s/100cc, and the molecular weight (Mn) was 150 ten thousand.
And (3) solidifying the coated diaphragm, namely solidifying and separating out the diaphragm in saturated steam, wherein the temperature of the saturated steam is 50 ℃, the humidity of the saturated steam is 80% RH, and the separation time is 40 s.
Then, the separator after the coating layer was solidified was washed with water in a pure water tank for 100 seconds. And drying the washed diaphragm in a hot air drying oven (the drying temperature is 85 ℃, and the drying time is 25 s). Thus, a composite coated membrane of aramid and PVDF was prepared, with the thickness shown in table 1.
Example 2
(1) Preparation of slurry
Alumina slurry: adding PVA into deionized water according to the proportion of 5 parts by weight of PVA powder and 95 parts by weight of deionized water, and stirring for 60min to prepare a PVA solution with the mass fraction of 5%. And mixing deionized water, alumina powder and CMC, stirring for 30min to prepare premixed slurry, adding GR401 and PVA solution into the premixed slurry, and stirring for 4h to obtain the alumina slurry. Wherein the mass ratio of the deionized water, the alumina, the CMC, the water-based adhesive and the PVA is 25: 2: 1: 0.125.
Aqueous PVDF slurry: and mixing PVDF and deionized water, stirring and dispersing for 2 hours, adding CMC, and continuously stirring for 2 hours to obtain PVDF slurry. Wherein the mass ratio of PVDF, CMC and deionized water is 65: 1: 350.
(2) Preparation of composite coating diaphragm
The slurry was coated on a polyethylene separator (base film 1) having a thickness of 12 μm using a multi-pack coater, and according to the coating structure shown in fig. 3, alumina slurry formed a continuous phase 2 and aqueous PVDF slurry formed a dispersed phase 3. Each pattern of dispersed phase was circular with a diameter of 0.5mm and the number of patterns of dispersed phase per square decimeter was 450. The porosity of the polyethylene-based film was 40%, the permeability value was 200s/100cc, and the molecular weight (Mn) was 150 ten thousand.
And drying the coated diaphragm in a hot air drying box (the drying temperature is 70 ℃, and the drying time is 30 s). Thus, a composite coated membrane of alumina and PVDF was prepared, the thickness of which is shown in table 1.
Example 3
A composite coated membrane was prepared as in example 1, except that, at the time of coating, coating was performed using a multi-box coater in the pattern shown in fig. 4, with aramid pulp forming the continuous phase 2 and oil-based PVDF pulp forming the dispersed phase 3. Each pattern of the dispersed phase 3 was an isosceles right triangle having a right-angle side length of 0.5mm, and the number of patterns of the dispersed phase per square decimeter was 300. The polyethylene film had a thickness of 7 μm (porosity 35%, permeability value 145s/100cc, number average molecular weight 150 ten thousand) to produce a composite coated membrane of aramid combined with PVDF, with a thickness as shown in table 1.
Comparative example 1
Preparing a composite coating diaphragm by referring to the method of example 1, except that the aramid fiber slurry is coated on one side of the diaphragm by adopting a narrow-slit secondary coating method and is soaked in water for 5 s; and drying by using an oven to obtain the single-sided aramid fiber coated diaphragm. And then coating the oil PVDF slurry on the other surface which is not coated with the aramid fiber coating layer in a gravure coating mode, and drying the coated aramid fiber slurry by using an oven to obtain the composite coating diaphragm of the aramid fiber and the PVDF, wherein the thickness of the composite coating diaphragm is shown in Table 1.
Comparative example 2
A composite coated separator was prepared by referring to the method of example 2, except that gravure roll coating of alumina slurry was performed on the surface of the base film to obtain an alumina coated separator, and then spray coating of aqueous PVDF slurry was performed on the surface of the alumina to obtain a composite coated separator of PVDF and alumina, the thickness of which is shown in table 1.
Comparative example 3
Preparing a composite coating diaphragm by referring to the method of example 3, except that the aramid fiber slurry is coated on one side of the diaphragm by adopting a narrow-slit secondary coating method and is soaked in water for 5 s; and drying by using an oven to obtain the diaphragm with the single surface coated by the aramid fiber. And then coating the oil PVDF slurry on the other surface which is not coated with the aramid fiber coating layer in a gravure coating mode, and drying the coated aramid fiber slurry by using an oven to obtain the composite coating diaphragm of the aramid fiber and the PVDF, wherein the thickness of the composite coating diaphragm is shown in Table 1.
The properties of the composite coated separators prepared in examples and comparative examples were tested, wherein the air permeability and heat shrinkage of the coated membranes were performed in accordance with GB/T36363-2018. The test results are shown in table 1.
TABLE 1
As can be seen from the above table, the composite coated membrane provided by the present invention can achieve the same air permeability and thermal shrinkage as the existing composite coated membrane, and has a smaller thickness, when the same coating slurry and the same base film are used.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Claims (11)
1. A composite coating diaphragm comprises a base film and a composite coating coated on one or two surfaces of the base film, wherein the structure of the composite coating consists of a continuous phase and a disperse phase; the continuous phase is formed by aramid pulp or alumina pulp, and the dispersed phase is formed by PVDF pulp.
2. The composite coated membrane according to claim 1, wherein the shape of the dispersed phase is selected from one or more of a circle, a triangle, a rectangle, and a square.
3. The composite coated membrane according to claim 1, wherein the number of the dispersed phase patterns is 9 to 500, preferably 100 to 500 per square decimeter of the coated membrane.
4. The composite coated separator according to claim 1, wherein the composite coating has a thickness of 0.5 to 6 μm.
5. The composite coated membrane of claim 1, wherein the continuous phase is formed from aramid pulp and the dispersed phase is formed from oil-based PVDF pulp; or
The continuous phase is formed from an alumina slurry and the dispersed phase is formed from an aqueous PVDF slurry.
6. The composite coated separator of claim 1 or 5, wherein the aramid pulp comprises aramid dope and inorganic filler;
preferably, the aramid fiber in the aramid fiber stock solution is selected from para-aramid fiber or meta-aramid fiber, and the mass fraction of the aramid fiber polymer in the aramid fiber stock solution is 1-6%;
the inorganic filler is selected from alumina or boehmite, and the D50 particle size of the inorganic filler is 30-300 nm;
preferably, the mass ratio of the aramid fiber stock solution to the inorganic filler is 10 to (3-8).
7. The composite coated separator according to claim 1 or 5, wherein the alumina slurry comprises alumina, water, a dispersant, an aqueous binder, and a film former;
preferably, the mass ratio of the aluminum oxide to the water to the dispersant to the aqueous binder to the film forming agent is 25 to (20-150) to (1-5) to (0.5-2) to (0.05-0.2).
8. The composite coated separator membrane of claim 1, wherein the oil-based PVDF slurry comprises PVDF and an organic solvent; the organic solvent is at least one selected from dimethyl carbonate, N-dimethylacetamide and N-methylpyrrolidone; preferably, in the oil-based PVDF slurry, the mass ratio of PVDF to organic solvent is 1: 20-60;
the aqueous PVDF slurry comprises PVDF, a dispersant and water; preferably, in the PVDF aqueous slurry, the mass ratio of PVDF to dispersant to water is 1 to (0.01-0.2) to (5-9).
9. The composite coated separator according to claim 1, wherein the base film is a polyolefin separator, preferably a polyethylene separator, the polyethylene film having a number average molecular weight of 10 to 800 ten thousand, preferably 50 to 200 ten thousand;
preferably, the porosity of the base film is 10-80%, and the air permeability of the base film is 50-800 s/100 cc.
10. The composite coated separator according to claim 1, wherein the thickness of the base film is 2 to 30 μm, preferably 5 to 15 μm.
11. A method for preparing a composite coated separator as defined in any one of claims 1 to 10, comprising: spraying a first coating slurry and a second coating slurry on the base film through a multi-cartridge coater, wherein the first coating slurry is selected from the aramid slurry or the alumina slurry, and the second coating slurry is the PVDF slurry;
the multi-cartridge coating machine comprises a first coating slurry material cartridge, a second coating slurry material cartridge, a feeding pipe and a material covering cartridge moving guide rail, wherein slurry nozzles are arranged on the coating slurry material cartridges; after the material is supplied to each slurry coating material box through the material supply pipe, the slurry coating material box is driven to move through the material covering box moving guide rail, and slurry is sprayed on the base film through the slurry nozzle to form the composite coating with the continuous phase and the dispersed phase.
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| CN209418618U (en) * | 2018-12-28 | 2019-09-20 | 佛山市实达科技有限公司 | A kind of lithium ion battery separator |
| CN110838568A (en) * | 2019-11-18 | 2020-02-25 | 高芳 | Lithium ion battery composite diaphragm and preparation method thereof |
| WO2021174709A1 (en) * | 2020-03-06 | 2021-09-10 | 中材锂膜有限公司 | Spray separator for lithium ion battery and preparation method therefor |
| CN112490581A (en) * | 2020-10-28 | 2021-03-12 | 河北金力新能源科技股份有限公司 | Meta-aramid fiber and oil PDVF composite coating diaphragm and preparation method thereof |
| CN112531285A (en) * | 2020-12-21 | 2021-03-19 | 中材锂膜有限公司 | High-temperature-resistant para-aramid coated lithium ion battery diaphragm and preparation method thereof |
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