CN105047843A - Preparation method of multi-layer lithium battery diaphragm with high security - Google Patents
Preparation method of multi-layer lithium battery diaphragm with high security Download PDFInfo
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- 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
- H01M50/406—Moulding; Embossing; Cutting
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- 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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- H—ELECTRICITY
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- 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
- H01M50/457—Separators, membranes or diaphragms characterised by the material having a layered structure comprising three or more layers
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- H—ELECTRICITY
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- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/491—Porosity
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/494—Tensile strength
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Abstract
The invention provides a preparation method of a multi-layer lithium battery diaphragm with high security. A microporous diaphragm is prepared by multi-layer coextrusion and unilateral stretching methods. The equipment and process technology of the method are perfect. A functional layer added with an inorganic filler or other pore-forming fillers and a polyolefin microporous membrane are subjected to composite strip casting in a multi-layer coextrusion manner; a multi-layer composite microporous membrane precursor is molded once; and then the composite membrane precursor is subjected to thermal treatment, multi-layer recombination and uniaxial stretching to obtain a high-performance microporous membrane. The microporous membrane obtained by the preparation method is uniform in pore size distribution, high in production efficiency, free of pollution, low in cost and beneficial to large-scale production; and in addition, according to the method, the pore size and distribution are easy to adjust.
Description
Technical field
The present invention relates to microporous barrier field, particularly relate to a kind of preparation method of polyolefine material microporous barrier, and the application of the microporous polyolefin film prepared by this method.
Background technology
In recent years, microporous polyolefin film is widely used in the fields such as battery diaphragm, isolated by filtration film, medical films.In application process, low-cost high-efficiency, and preparation pore size distribution and the uniform product of pore size are large technological difficulties.Especially in the application in battery diaphragm field, being uniformly distributed of hole, pore size is unanimously that one of battery superior function ensures greatly.Meanwhile, with people to the demand of clean energy resource, to the raising of the protective awareness of environment, Electric power car industry has also welcome the period of high speed development.Thus making high security, the energy-storage battery of high-discharge-rate arises at the historic moment, and receives the concern of increasing technological staff and enterpriser.
Prepare Multi-layer composite microporous barrier by difference in functionality layer, and then obtain the high micro-pore septum of fail safe, the common report of this type of technology.Chinese patent CN101779311A discloses a kind of preparation method of multilayer microporous film, high heat proof material is carried out compound through the mode of coating in microporous polyolefin film, reach the object of the fail safe improving microporous barrier, but this kind of method technological process is loaded down with trivial details, operation is various, cost is high, and efficiency is low, and its process waste material is big for environment pollution.
Summary of the invention
The present invention adopts multi-layer co-extruded method of carrying out simple tension again to prepare microporous barrier.The method apparatus and process technical perfection, carries out compound slab, the composite microporous film precursor of one-step molded multilayer by multi-layer co-extruded mode by the functional layer and microporous polyolefin film of adding inorganic filler or other pore-forming filler.After this, composite membrane presoma is through heat treatment, and MULTILAYER COMPOSITE, simple tension obtains high-performance microporous barrier.The microporous barrier even aperture distribution obtained by the method, production efficiency is high, pollution-free, and cost is low, is beneficial to large-scale production.In addition the method pore size and distribution are easy to adjustment.
The object of the present invention is to provide a kind of preparation method of Multi-layer composite high-performance microporous barrier, the microporous barrier prepared by the method possesses two-layer high strength, dystectic functional layer, for improving the security performance in battery use procedure.
Above-mentioned purpose of the present invention can be achieved by following technical solution:
A, slab: be functional layer Resin A by pore-forming filling and functional layer mixed with resin, wherein pore-forming filling accounts for weight ratio is 20% ~ 80%, carry out three-layer co-extruded with vistanex B again, wherein A:B:A tri-layers extrudes thickness proportion is 10:80:10 ~ 20:60:20, functional layer Resin A is two top layers, vistanex B is intermediate layer, prepares precursor film through this step;
B, heat treatment: by the precursor film in step a through 80 ~ 150 DEG C of temperature, heat-treat, obtain heat-treating film for 2 ~ 14 hours;
C, compound: by the heat-treating film prepared in step b, carry out compound again under 0 ~ 150 DEG C of combined temp;
D, stretching: by the heat-treating film of compound in step c, carry out stretching pore-forming, obtain final microporous barrier under 25 ~ 150 DEG C of draft temperatures and stretch ratio 1 ~ 3 times.
Pore-forming filling in described step a comprises: pore-forming filling is selected from the oxide of at least one in metal or semiconductor element, hydroxide, sulfide, nitride, carbide or its mixture.Wherein, metallic element is as Ca, Al, Si, Mg, Zn or Ba etc., and semiconductor element is as silicon, germanium, boron, selenium, tellurium or carbon etc.
Functional layer resin in described step a comprises: polyethylene, polypropylene, Kynoar (PVdF), polytetrafluoroethylene (PTFE), polyurethane, polymethylpentene (PMP), PETG (PET), Merlon (PC), polyester, polyvinyl alcohol (PVA), polyacrylonitrile (PAN), polyformaldehyde (PMO), polymethyl methacrylate (PMMA), polyoxyethylene (PEO) or cellulose, or its two or more mixture.
Vistanex in described step a is preferably polypropylene or polyethylene.
Pore-forming filling in described step a and functional layer mixed with resin, wherein, pore-forming filling preferred weight accounting is 30% ~ 70%.
The thickness proportion of extruding of the functional layer in described step a and polyolefin resin layer is: functional layer and polyolefin layer are combined as A-B-A three-decker, and the preferred thickness ratio of extruding of A:B:A is 15:70:15 ~ 20:60:20.
Heat treatment temperature in described step b is preferably 100 ~ 120 DEG C, 5 ~ 10 hours processing times.
The compound number of plies in described step c can be preferably 2 ~ 6 layers, and combined temp is preferably 80 ~ 120 DEG C.
The stretching number of plies in described steps d can be preferably 2 ~ 24 layers, draft temperature preferably 80 ~ 120 DEG C, stretch ratio 1.5 ~ 2 times.
Beneficial effect describes: the microporous barrier even aperture distribution obtained by the method, production efficiency is high, pollution-free, and cost is low, and equipment investment cost is low, is beneficial to large-scale production.In addition the method pore size and distribution are easy to adjustment, by changing pore-forming proportion of filler and stretching ratio, can change the porosity of microporous barrier easily, thus change distribution situation and the pore size in hole.The present invention introduces the concept of compound working procedure during the course, can realize multi-level synchro-draw, significantly increase production efficiency.
Accompanying drawing explanation
Fig. 1 tri-layers of membrane configuration figure
1 and 3 is the functional layer that resin and pore-forming filling are mixed with; 2 is polyolefin micropore layer; 4 is microcellular structure in functional layer and distribution; 5 is microcellular structure on polyolefin micropore layer and distribution
The pore-size distribution schematic diagram of Fig. 2 comparative sample
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
In embodiment, the thickness of sample all with 16 μm for normative reference, other conditions are shown in technique scheme, and difference will be set forth in a particular embodiment.
Embodiment 1
By calcium carbonate (CaCO
3) powder adds in polypropylene according to the mass ratio of 30%, then extrude through three-layer co-extruded casting head with acrylic resin, form the precursor film of A-B-A three-decker, A layer is CaCO
3with polypropylene mixed layer, B layer is polypropylene layer, and three layers are extruded thickness proportion is 20:60:20.Precursor film, through casting roller cooling forming, completes slab process.The heat treatment under 140 DEG C of conditions of this precursor film is obtained heat treatment in 4 hours.Heat-treating film carries out 2 layers of compound by specific complex equipment, and combined temp is 50 DEG C.
Heat-treating film after 2 layers of compound adopts 6 to unreel 12 layers of pattern stretched and stretches, and draft temperature is 140 DEG C, and stretch ratio is 2 times, obtains finished product.
Embodiment 2
By aluminium hydroxide (Al (OH)
3) powder adds in polypropylene according to the mass ratio of 50%, then extrude through three-layer co-extruded casting head with acrylic resin, form the precursor film of A-B-A three-decker, A layer is Al (OH)
3with polypropylene mixed layer, B layer is polypropylene layer, and three layers are extruded thickness proportion is 15:70:15.Precursor film, through casting roller cooling forming, completes slab process.The heat treatment under 130 DEG C of conditions of this precursor film is obtained heat-treating film in 8 hours.This heat-treating film carries out 3 layers of compound by specific complex equipment, and combined temp is 30 DEG C.
Heat-treating film volume employing 4 after 3 layers of compound unreels 12 layers of pattern stretched and stretches, and draft temperature is 120 DEG C, and stretch ratio is 1.5 times, obtains finished product.
Embodiment 3
By calcium carbonate (CaCO
3) powder adds in polyester according to the mass ratio of 30%, then extrude through three-layer co-extruded casting head with acrylic resin, form the precursor film of A-B-A three-decker, A layer is CaCO
3with polyester mixed layer, B layer is polypropylene layer, and three layers are extruded thickness proportion is 10:80:10.This precursor film, through casting roller cooling forming, completes slab process.The heat treatment under 120 DEG C of conditions of this precursor film is obtained heat-treating film in 12 hours.This heat-treating film carries out 4 layers of compound by specific complex equipment, and combined temp is 60 DEG C.
Heat-treating film volume employing 4 after 4 layers of compound unreels 16 layers of pattern stretched and stretches, and draft temperature is 100 DEG C, and stretch ratio is 2.5 times, obtains finished product.
Embodiment 4
Extruded by three-layer co-extruded casting head by acrylic resin, form the precursor film of A-B-A three-decker, A layer is polypropylene layer, and B layer is also polypropylene layer, and three layers are extruded thickness proportion is 15:70:15.Precursor film, through casting roller cooling forming, completes slab process.The heat treatment under 130 DEG C of conditions of this precursor film is obtained heat-treating film in 8 hours.This heat-treating film carries out 3 layers of compound by specific complex equipment, and combined temp is 30 DEG C.
Heat-treating film volume employing 4 after 3 layers of compound unreels 12 layers of pattern stretched and stretches, and draft temperature is 120 DEG C, and stretch ratio is 1.5 times, obtains finished product.
The performance parameter of all embodiments is as table 1
Table 1 embodiment properties of sample parameter
Note: the hot strength in what " MD hot strength " represented sample test the is direction paralleled with draw direction.
As shown in table 1, embodiment 4 does not add pore-forming filler and other functional layer resins, and products obtained therefrom is existing market microporous barrier similar performance.From embodiment 1, embodiment 2, the data result of embodiment 3 is seen, after adding functional layer, microporous barrier properties is significantly improved, especially intensity aspect, promotes significantly, significantly can promote the security performance of microporous barrier in field of lithium battery application to a great extent.
Embodiment 4
Adopt the preparation of embodiment 1 method, wherein process ratio, and test result is as shown in table 2.
Table 2
As shown in Table 2, taking into account porosity and pass distribution and large-scale situation, the preferred technical scope of the present invention, has hot strength and the better technique effect of puncture strength.
In addition, as shown in Figure 2, pore-size distribution and the size of microporous barrier can be changed easily by changing formula rate.It can also be seen that from figure, it is more concentrated that preferred technical scope can obtain pore-size distribution, pore size evenly microporous barrier, thus ensure microporous barrier performance evenly.Especially, the multilayer lithium battery diaphragm prepared by pore-forming filling accounting scope 30% ~ 70%, technique effect is more remarkable.For other functional layer resin and vistanex, there is similar technique effect.
Above-mentioned execution mode is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, change and the replacement of any unsubstantiality that those skilled in the art does on basis of the present invention all belong to the present invention's scope required for protection.
Claims (10)
1. a preparation method for Multi-layer composite lithium battery diaphragm, is characterized in that, comprises the following steps:
A, slab: be functional layer Resin A by pore-forming filling and functional layer mixed with resin, wherein pore-forming filling accounts for weight ratio is 20% ~ 80%, carry out three-layer co-extruded with vistanex B again, wherein A:B:A tri-layers extrudes thickness proportion is 10:80:10 ~ 20:60:20, functional layer Resin A is two top layers, vistanex B is intermediate layer, prepares precursor film through this step;
B, heat treatment: by the precursor film in step a through 80 ~ 150 DEG C of temperature, heat-treat, obtain heat-treating film for 2 ~ 14 hours;
C, compound: by the heat-treating film prepared in step b, carry out compound again under 0 ~ 150 DEG C of combined temp;
D, stretching: by the heat-treating film of compound in step c, carry out stretching pore-forming, obtain final microporous barrier under 25 ~ 150 DEG C of draft temperatures and stretch ratio 1 ~ 3 times.
2. according to claim 1 preparation method, it is characterized in that, described pore-forming filling preferred weight accounting is 30% ~ 70%.
3. preparation method according to claim 1, it is characterized in that, described pore-forming filling is selected from least one oxide, hydroxide, sulfide, nitride, carbide or its mixture in metal or semiconductor element.
4. preparation method according to claim 3, it is characterized in that, described metallic element is selected from Ca, Al, Si, Mg, Zn or Ba, and described semiconductor element is selected from silicon, germanium, boron, selenium, tellurium or carbon.
5. preparation method according to claim 1, it is characterized in that, described functional layer resin is selected from polyethylene, polypropylene, Kynoar (PVdF), polytetrafluoroethylene (PTFE), polyurethane, polymethylpentene (PMP), PETG (PET), Merlon (PC), polyester, polyvinyl alcohol (PVA), polyacrylonitrile (PAN), polyformaldehyde (PMO), polymethyl methacrylate (PMMA), polyoxyethylene (PEO) or cellulose, or its two or more mixture.
6. preparation method according to claim 1 or 2, is characterized in that, the preferred thickness ratio of extruding of the functional layer in described step a and the A:B:A of polyolefin resin layer is 15:70:15 ~ 20:60:20.
7. preparation method according to claim 1 or 2, is characterized in that, the heat treatment temperature in described step b is preferably 100 ~ 120 DEG C, 5 ~ 10 hours processing times.
8. preparation method according to claim 1 or 2, is characterized in that, the compound number of plies in described step c can be preferably 2 ~ 6 layers, and combined temp is preferably 80 ~ 120 DEG C.
9. preparation method according to claim 1 or 2, is characterized in that, the stretching number of plies in described steps d can be preferably 2 ~ 24 layers, draft temperature preferably 80 ~ 120 DEG C, stretch ratio 1.5 ~ 2 times.
10. a Multi-layer composite lithium battery diaphragm, is characterized in that, the method for described battery diaphragm according to the arbitrary claim of claim 1-9 prepares.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510366657.4A CN105047843B (en) | 2015-06-26 | 2015-06-26 | A kind of preparation method of the multilayer lithium battery diaphragm of high security |
| PCT/CN2015/084041 WO2016206145A1 (en) | 2015-06-26 | 2015-07-15 | Preparation method for high-safety multilayer lithium battery diaphragm |
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| CN201510366657.4A CN105047843B (en) | 2015-06-26 | 2015-06-26 | A kind of preparation method of the multilayer lithium battery diaphragm of high security |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110676420A (en) * | 2019-10-30 | 2020-01-10 | 复阳固态储能科技(溧阳)有限公司 | Lithium ion battery's lithium diaphragm of mending |
| WO2021042928A1 (en) * | 2019-09-05 | 2021-03-11 | 江苏厚生新能源科技有限公司 | Polymer battery diaphragm having interpenetrating network structure, and preparation method therefor |
| CN114361461A (en) * | 2022-01-10 | 2022-04-15 | 上海恩捷新材料科技有限公司 | Flexible current collector core layer, current collector, pole piece, battery and preparation method of flexible current collector core layer, current collector, pole piece and battery |
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| GB2585635B (en) * | 2019-05-28 | 2022-03-23 | Kafrit Ind 1993 Ltd | Compositions and methods for use in the preparation of hydrophobic surfaces |
| CN111162230B (en) * | 2020-01-21 | 2022-03-25 | 四川优源新能源有限公司 | Preparation method of high-energy-storage battery diaphragm material |
| CN113659281B (en) * | 2021-08-09 | 2023-06-09 | 界首市天鸿新材料股份有限公司 | Three-layer co-extrusion diaphragm for lithium battery and stretching process thereof |
| CN114497896B (en) * | 2022-04-14 | 2022-06-28 | 宁波长阳科技股份有限公司 | High-strength three-layer co-extrusion lithium ion battery diaphragm and preparation method thereof |
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| WO2021042928A1 (en) * | 2019-09-05 | 2021-03-11 | 江苏厚生新能源科技有限公司 | Polymer battery diaphragm having interpenetrating network structure, and preparation method therefor |
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| CN114361461A (en) * | 2022-01-10 | 2022-04-15 | 上海恩捷新材料科技有限公司 | Flexible current collector core layer, current collector, pole piece, battery and preparation method of flexible current collector core layer, current collector, pole piece and battery |
| CN114361461B (en) * | 2022-01-10 | 2024-01-16 | 上海恩捷新材料科技有限公司 | Flexible current collector core layer, current collector, pole piece, battery and preparation method of battery |
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| Publication number | Publication date |
|---|---|
| CN105047843B (en) | 2018-01-02 |
| WO2016206145A1 (en) | 2016-12-29 |
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