CN105047843B - A kind of preparation method of the multilayer lithium battery diaphragm of high security - Google Patents
A kind of preparation method of the multilayer lithium battery diaphragm of 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- 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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
- 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
- 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
- H01M50/489—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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- 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
- H01M50/489—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 present invention prepares microporous barrier using the multi-layer co-extruded method for carrying out simple tension again.The method apparatus and process technical perfection, the functional layer for adding inorganic filler or other pore-forming fillers is carried out by compound slab, the composite microporous film precursor of one-step molded multilayer with MIcroporous polyolefin film by multi-layer co-extruded mode.Hereafter, compound film precursor is thermally treated, MULTILAYER COMPOSITE, and simple tension obtains high-performance microporous barrier.The microporous barrier even aperture distribution obtained by the method, production efficiency is high, and pollution-free, cost is low, beneficial to large-scale production.In addition this method pore size and distribution are easy to adjust.
Description
Technical field
The present invention relates to microporous barrier field, more particularly to a kind of preparation method of polyolefine material microporous barrier, Yi Jiyou
The application of MIcroporous polyolefin film prepared by this method.
Background technology
In recent years, MIcroporous polyolefin film is widely used in battery diaphragm, is separated by filtration the fields such as film, medical films.
In application process, low-cost high-efficiency, and it is a big technological difficulties to prepare pore size distribution and the uniform product of pore size.Especially exist
The application in battery diaphragm field, hole are uniformly distributed, and pore size is unanimously a big guarantee of battery superior function.Meanwhile companion
Demand with people to clean energy resource, the raising to the protective awareness of environment, Electric power car industry have also welcome high speed development
Period.So that high security, the energy-storage battery of high-discharge-rate arises at the historic moment, by increasing technological staff and
The concern of enterpriser.
Multi-layer composite microporous barrier is prepared by difference in functionality layer, and then obtains safe micro-pore septum, such skill
Art common report.Chinese patent CN101779311A discloses a kind of preparation method of multilayer microporous film, and high heat proof material is passed through
The mode of coating carries out compound in MIcroporous polyolefin film, reaches the purpose for the security for improving microporous barrier, but such a method work
Skill flow is cumbersome, and process is various, and cost is high, and efficiency is low, and its process waste material is big for environment pollution.
The content of the invention
The present invention prepares microporous barrier using the multi-layer co-extruded method for carrying out simple tension again.The method apparatus and process technology is complete
It is kind, the functional layer for adding inorganic filler or other pore-forming fillers is carried out with MIcroporous polyolefin film by multi-layer co-extruded mode
Compound slab, the composite microporous film precursor of one-step molded multilayer.Hereafter, compound film precursor is thermally treated, MULTILAYER COMPOSITE, unidirectionally
Stretching obtains high-performance microporous barrier.The microporous barrier even aperture distribution obtained by the method, production efficiency is high, pollution-free, into
This is low, beneficial to large-scale production.In addition this method pore size and distribution are easy to adjust.
It is an object of the invention to provide a kind of preparation method of Multi-layer composite high-performance microporous barrier, pass through party's legal system
Standby microporous barrier possesses two layers of high intensity, dystectic functional layer, for improving the security performance during battery use.
The above-mentioned purpose of the present invention can be achieved by following technical solution：
A, slab：Pore-forming filling and functional layer resin are mixed into functional layer Resin A, wherein pore-forming filling accounts for weight ratio and is
20%~80%, then carry out three-layer co-extruded, wherein A with vistanex B:B:Tri- layers of extrusion thickness proportions of A are 10:80:10~
20:60:20, functional layer Resin A is two top layers, and vistanex B is intermediate layer, and precursor film is prepared through the step；
B, it is heat-treated：Precursor film in step a is passed through into 80~150 DEG C of temperature, is heat-treated within 2~14 hours, obtained
To heat-treating film；
C, it is compound：The heat-treating film that will be prepared in step b, carried out again under 0~150 DEG C of combined temp compound；
D, stretch：By heat-treating film compound in step c, under 1~3 times of 25~150 DEG C of draft temperatures and stretch ratio
Stretching pore-forming is carried out, obtains final microporous barrier.
Pore-forming filling in the step a includes：Pore-forming filling is selected from least one of metal or semiconductor element
Oxide, hydroxide, sulfide, nitride, carbide or its mixture.Wherein, metallic element such as Ca, Al, Si, Mg, Zn
Or Ba etc., semiconductor element such as silicon, germanium, boron, selenium, tellurium or carbon etc..
Functional layer resin in the step a includes：Polyethylene, polypropylene, Kynoar (PVdF), polytetrafluoroethylene (PTFE)
(PTFE), polyurethane, polymethylpentene (PMP), polyethylene terephthalate (PET), makrolon (PC), polyester, poly-
Vinyl alcohol (PVA), polyacrylonitrile (PAN), polyformaldehyde (PMO), polymethyl methacrylate (PMMA), polyoxyethylene (PEO) or
Cellulose, or its two or more mixture.
Vistanex in the step a is preferably polypropylene or polyethylene.
Pore-forming filling in the step a mixes with functional layer resin, wherein, pore-forming filling preferred weight accounting is 30%
~70%.
The extrusion thickness proportion of functional layer and polyolefin resin layer in the step a is：Functional layer and polyolefin layer group
It is combined into A-B-A three-deckers, A:B:A extrusion preferred thickness ratio is 15:70:15~20:60:20.
Heat treatment temperature in the step b is preferably 100~120 DEG C, 5~10 hours processing times.
The compound number of plies in the step c is preferably 2~6 layers, and combined temp is preferably 80~120 DEG C.
The stretching number of plies in the step d is preferably 2~24 layers, preferably 80~120 DEG C of draft temperature, 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, into
This is low, and equipment investment cost is low, beneficial to large-scale production.In addition this method pore size and distribution are easy to adjust, and pass through change
Pore-forming filler ratio and stretching ratio, it can easily change the porosity of microporous barrier, so as to change the distribution situation in hole and aperture
Size.The present invention introduces the concept of compound working procedure in the process, and multi-level synchro-draw can be achieved, and production effect is significantly increased
Rate.
Brief description of the drawings
Fig. 1 three-layer membrane structure charts
1 and 3 be the functional layer that resin is mixed with pore-forming filling；2 be polyolefin micropore layer；4 be micro- in functional layer
Pore structure and distribution；5 be microcellular structure and distribution on polyolefin micropore layer
The pore-size distribution schematic diagram of Fig. 2 comparative samples
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
In embodiment, for the thickness of sample with 16 μm for normative reference, other conditions are shown in above-mentioned technical proposal, difference
It will illustrate in a particular embodiment.
Embodiment 1
By calcium carbonate (CaCO3) powder is added in polypropylene according to 30% mass ratio, then with acrylic resin through three
Layer coextrusion casting die head extrusion, forms the precursor film of A-B-A three-deckers, A layers are CaCO3With polypropylene mixed layer, B layers are
Polypropylene layer, three layers of extrusion thickness proportion are 20:60:20.Precursor film is cooled and shaped by casting roller, completes slab process.
The precursor film is heat-treated 4 hours under the conditions of 140 DEG C and is heat-treated.Heat-treating film carries out 2 by specific complex equipment
Layer is compound, and combined temp is 50 DEG C.
The pattern that heat-treating film through 2 layers after compound unreels 12 layers of stretching using 6 is stretched, draft temperature 140
DEG C, stretch ratio is 2 times, obtains finished product.
Embodiment 2
By aluminium hydroxide (Al (OH)3) powder is added in polypropylene according to 50% mass ratio, then with acrylic resin
Extruded through three-layer co-extruded casting head, form the precursor film of A-B-A three-deckers, A layers are Al (OH)3Mixed with polypropylene
Layer, B layers are polypropylene layer, and three layers of extrusion thickness proportion are 15:70:15.Precursor film is cooled and shaped by casting roller, completes casting
Piece process.The precursor film is heat-treated 8 hours under the conditions of 130 DEG C and obtains heat-treating film.The heat-treating film passes through special multiple
It is compound to close 3 layers of equipment progress, combined temp is 30 DEG C.
The pattern that heat treatment film roll through 3 layers after compound unreels 12 layers of stretching using 4 is stretched, and draft temperature is
120 DEG C, stretch ratio is 1.5 times, obtains finished product.
Embodiment 3
By calcium carbonate (CaCO3) powder is added in polyester according to 30% mass ratio, then with acrylic resin through three layers
Coextrusion casting die head is extruded, and forms the precursor film of A-B-A three-deckers, A layers are CaCO3With polyester mixed layer, B layers are poly- third
Alkene layer, three layers of extrusion thickness proportion are 10:80:10.The precursor film is cooled and shaped by casting roller, completes slab process.Will
The precursor film is heat-treated 12 hours under the conditions of 120 DEG C and obtains heat-treating film.The heat-treating film is entered by specific complex equipment
4 layers of row is compound, and combined temp is 60 DEG C.
The pattern that heat treatment film roll through 4 layers after compound unreels 16 layers of stretching using 4 is stretched, and draft temperature is
100 DEG C, stretch ratio is 2.5 times, obtains finished product.
Embodiment 4
Acrylic resin is extruded by three-layer co-extruded casting head, forms the precursor film of A-B-A three-deckers, A layers
For polypropylene layer, B layers are also polypropylene layer, and three layers of extrusion thickness proportion are 15:70:15.Precursor film cools down by casting roller
Shaping, complete slab process.The precursor film is heat-treated 8 hours under the conditions of 130 DEG C and obtains heat-treating film.The heat-treating film
Compound by 3 layers of specific complex equipment progress, combined temp is 30 DEG C.
The pattern that heat treatment film roll through 3 layers after compound unreels 12 layers of stretching using 4 is stretched, and draft temperature is
120 DEG C, stretch ratio is 1.5 times, obtains finished product.
The performance parameter of all embodiments such as table 1
The embodiment sample performance parameter of table 1
Note：What " MD tensile strengths " represented sample test is the tensile strength in the direction parallel with draw direction.
As shown in table 1, embodiment 4 is not added with 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 is each
Item performance is significantly improved, and especially in terms of intensity, lifting is notable, can largely be obviously improved microporous barrier in lithium battery
The security performance of application field.
Embodiment 4
Prepared using the method for embodiment 1, wherein ratio is processed, and test result is as shown in table 2.
Table 2
As shown in Table 2, porosity and pass distribution and large-scale situation, currently preferred technical scope, tool are being taken into account
There are tensile strength and puncture strength superior technique effect.
In addition, as shown in Fig. 2 it can easily change the pore-size distribution and size of microporous barrier by changing formula rate.
From this figure it can be seen that preferable technical scope can obtain pore-size distribution and more concentrate, the microporous barrier of pore size evenly,
So as to ensure micropore film properties evenly.Especially, the multilayer lithium battery prepared by pore-forming filling accounting scope 30%~70% every
Film, technique effect are more notable.There is similar technique effect with vistanex for other functional layer resins.
Above-mentioned embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (8)
1. a kind of preparation method of Multi-layer composite lithium battery diaphragm, it is characterised in that comprise the following steps：
A, slab：Pore-forming filling and functional layer resin are mixed into functional layer Resin A, wherein pore-forming filling accounts for weight ratio as 40%
~60%, then carry out three-layer co-extruded, wherein A with vistanex B:B:Tri- layers of extrusion thickness proportions of A are 10:80:10~15:
70:15, functional layer Resin A is two top layers, and vistanex B is intermediate layer, and precursor film is prepared through the step；
B, it is heat-treated：Precursor film in step a is passed through into 80~150 DEG C of temperature, is heat-treated within 2~14 hours, obtains heat
Process film；
C, it is compound：The heat-treating film that will be prepared in step b, it is compound that 2-6 layer heat-treating films are carried out under 0~150 DEG C of combined temp；
D, stretch：By heat-treating film compound in step c, carried out under 25~150 DEG C of longitudinal stretchings, 1.5~3 times of stretch ratio
Pore-forming is stretched, obtains final microporous barrier.
2. preparation method according to claim 1, it is characterised in that the pore-forming filling is in metal or semiconductor element
At least one oxide, hydroxide, sulfide, nitride, carbide or its mixture.
3. preparation method according to claim 2, it is characterised in that the metallic element is selected from Ca, Al, Mg, Zn or Ba, institute
State semiconductor element and be selected from silicon, germanium, boron, selenium, tellurium or carbon.
4. preparation method according to claim 1, it is characterised in that the functional layer resin includes：Polyethylene, polypropylene,
Kynoar (PVdF), polytetrafluoroethylene (PTFE) (PTFE), polyurethane, polymethylpentene (PMP), polyethylene terephthalate
(PET), makrolon (PC), polyvinyl alcohol (PVA), polyacrylonitrile (PAN), polyformaldehyde (PMO), polymethyl methacrylate
(PMMA), polyoxyethylene (PEO) or cellulose, or its two or more mixture.
5. preparation method according to claim 1, it is characterised in that the heat treatment temperature in the step b is 100~120
DEG C, 5~10 hours processing times.
6. preparation method according to claim 1, it is characterised in that the compound number of plies in the step c is 2~6 layers, compound
80~120 DEG C of temperature.
7. preparation method according to claim 1, it is characterised in that the stretching number of plies in the step d is 2~24 layers, is drawn
Stretch 80~120 DEG C of temperature, 1.5~2 times of stretch ratio.
8. a kind of Multi-layer composite lithium battery diaphragm, it is characterised in that described battery diaphragm is according to any power of claim 1-7
The method that profit requires described is prepared.
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| 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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| CN105047843B true CN105047843B (en) | 2018-01-02 |
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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 |
| CN110518178B (en) | 2019-09-05 | 2020-09-01 | 江苏厚生新能源科技有限公司 | Polymer battery diaphragm with interpenetrating network structure and preparation method thereof |
| CN110676420B (en) * | 2019-10-30 | 2022-04-12 | 复阳固态储能科技(溧阳)有限公司 | Lithium ion battery's lithium diaphragm of mending |
| 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 |
| 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 |
| 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 |
| CN115029073B (en) * | 2022-06-28 | 2024-06-11 | 常州斯威克光伏新材料有限公司 | High-cohesiveness high-temperature-resistant tab adhesive and preparation method thereof |
| CN116365171B (en) * | 2023-06-01 | 2023-08-29 | 合肥长阳新能源科技有限公司 | High-ion-conductivity composite lithium battery diaphragm and preparation method thereof |
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| US20020136945A1 (en) * | 2000-01-18 | 2002-09-26 | Call Ronald W. | Multilayer battery separators |
| US6878226B2 (en) * | 2002-01-08 | 2005-04-12 | Wei-Ching Yu | Continuous methods of making microporous battery separators |
| CN101997102B (en) * | 2009-08-26 | 2013-11-06 | 比亚迪股份有限公司 | Lithium ion battery diaphragm and manufacturing method thereof |
| CN102544416A (en) * | 2010-12-08 | 2012-07-04 | 重庆纽米新材料科技有限责任公司 | Multilayer polyolefin battery diaphragm and preparation method thereof |
| CN102064299A (en) * | 2010-12-25 | 2011-05-18 | 佛山塑料集团股份有限公司 | Polyolefin multi-layer porous diaphragm for lithium ion battery and preparation method thereof |
| CN102738427B (en) * | 2012-07-19 | 2015-01-28 | 河南义腾新能源科技有限公司 | Inorganic composite microporous membrane serving as lithium ion battery diaphragm and preparation method thereof |
| CN103786349A (en) * | 2014-01-22 | 2014-05-14 | 广东工业大学 | Method for preparing multi-layer polyolefin microporous film |
| CN104022249B (en) * | 2014-06-26 | 2016-03-30 | 佛山市盈博莱科技有限公司 | A kind of three layers of lithium battery diaphragm and preparation method thereof |
| CN104085101B (en) * | 2014-07-02 | 2016-06-29 | 湖南锂顺能源科技有限公司 | A kind of battery diaphragm simple tension micro molding equipment |
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