CN110993865A - Lithium battery diaphragm and preparation method thereof - Google Patents
Lithium battery diaphragm and preparation method thereof Download PDFInfo
- Publication number
- CN110993865A CN110993865A CN201911301809.7A CN201911301809A CN110993865A CN 110993865 A CN110993865 A CN 110993865A CN 201911301809 A CN201911301809 A CN 201911301809A CN 110993865 A CN110993865 A CN 110993865A
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- Prior art keywords
- diaphragm
- lithium battery
- silicate powder
- stretching
- colloidal solution
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000009998 heat setting Methods 0.000 claims abstract description 13
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 12
- 238000004804 winding Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000011265 semifinished product Substances 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000005191 phase separation Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 230000002457 bidirectional effect Effects 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 230000001360 synchronised effect Effects 0.000 claims description 3
- 230000035699 permeability Effects 0.000 claims description 2
- 239000010408 film Substances 0.000 claims 4
- 239000010409 thin film Substances 0.000 claims 1
- 238000005096 rolling process Methods 0.000 abstract 1
- -1 polypropylene Polymers 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- 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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
-
- 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
-
- 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Cell Separators (AREA)
Abstract
The invention discloses a lithium battery diaphragm, which comprises polyolefin resin and silicate powder; the invention also provides a preparation method of the lithium battery diaphragm, which comprises the steps of mixing and extruding the polyolefin resin and the silicate powder, cooling, stretching, extracting, washing, drying, heat setting, rolling and the like to obtain the lithium battery diaphragm.
Description
Technical Field
The invention relates to the field of lithium battery diaphragms, in particular to a lithium battery diaphragm and a preparation method thereof.
Background
In the construction of lithium batteries, the separator is one of the key internal components. The performance of the diaphragm determines the interface structure, internal resistance and the like of the battery, directly influences the characteristics of the battery such as capacity, circulation, safety performance and the like, and the diaphragm with excellent performance plays an important role in improving the comprehensive performance of the battery.
Generally, in order to improve the conductivity of a (diaphragm/polymer electrolyte) system, a polymer with a large dielectric constant, low crystallinity, stable electrochemical properties and good thermal stability needs to be selected, for example, one or more blends of polypropylene, polyethylene, polyvinylidene fluoride, polyacrylonitrile, polymethyl methacrylate, polyoxyethylene and the like, and the problems of contradiction between high-proton conductivity and mechanical properties, poor cycle stability and the like easily occur.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a lithium battery diaphragm which effectively improves the strength and the thermal stability of the lithium battery diaphragm and a preparation method thereof.
In order to achieve the above purposes, the invention adopts the technical scheme that: a lithium battery diaphragm comprises polyolefin resin and silicate powder, wherein the weight ratio of the polyolefin resin to the silicate powder is 1: 99-3: 1, preferably 1: 19-1: 1, more preferably 1: 9-1: 2, more preferably 1: 4-1: 3.
Preferably, the membrane has a thickness of 2 to 300 μm and a permeability value of 50 to 2000s/100 cc.
Preferably, the diaphragm is including the first layer diaphragm, the second floor diaphragm and the third layer diaphragm that set gradually, first layer diaphragm and third layer diaphragm all have a plurality of bleeder vents, and are a plurality of the bleeder vent all extends along the thickness direction tortuous of diaphragm, the second floor diaphragm has a plurality of finger-like holes, and is a plurality of finger-like hole all extends along the thickness direction tortuous of diaphragm, and is a plurality of all have a plurality of mutual through holes between the pore wall in finger-like hole.
Preferably, the aperture ranges of the air holes are all between 80 nm and 300nm, the aperture ranges of the finger-shaped holes are all between 400 nm and 800nm, and the aperture ranges of the mutual through holes are all between 50nm and 200 nm.
Preferably, the porosity of the separator is 5% to 70%.
Preferably, the silicate powder has a particle size of 50nm to 1 μm.
In order to achieve the above object, the present invention provides a method for preparing a lithium battery separator, comprising the steps of:
s1: adding polyolefin resin into an organic solvent, mixing and stirring to obtain a first colloidal solution; adding silicate powder into the first colloidal solution, and continuously stirring at 20-100 ℃, wherein the stirring speed is 200-300r/min, and the stirring time is 5-30min until the silicate powder and the first colloidal solution are uniformly mixed to obtain a second colloidal solution;
s2: conveying the second colloidal solution prepared by S1 into an extruder from a first feeding hole of the twin-screw extruder, wherein the temperature of the extruder is 150 ℃ and 270 ℃, and the twin-screw extruder is provided with a vacuum exhaust port and/or a natural exhaust port;
s3: extruding the material melted and mixed by S2 through a die head, cooling and solidifying the material on a cooling roller into a thick film with the thickness of 500-3000 mu m, and carrying out solid-liquid phase separation or liquid-liquid phase separation in the solidification process to form a plurality of micropores inside the thick film;
s4: stretching the thick film prepared in the S3 along the transverse direction and the longitudinal direction, wherein the stretching temperature in the transverse direction and the longitudinal direction is 95-135 ℃, the stretching ratio is more than 5 times, and the film is obtained after stretching;
s5: extracting the film in the S4 by using an extraction device to obtain a perforated sheet;
s6: putting the hole-drawing sheet material in the step S5 into a washing device for washing to obtain a micropore forming diaphragm semi-finished product;
s7: drying the semi-finished product of the microporous forming diaphragm in the S6 by bypassing a guide roller, wherein the drying temperature is 70-80 ℃, and the drying time is 5-6 h;
s8: performing heat setting on the semi-finished product of the microporous forming diaphragm in the step S7 by using a heat setting device to obtain a finished product of the lithium battery diaphragm, wherein the heat setting temperature is 75-135 ℃, and the heat setting time is 3-5S;
s9: and (4) winding the finished lithium battery diaphragm product in the S8 by using a winding machine.
Preferably, in S4, the stretching process is bi-directional synchronous stretching or bi-directional asynchronous stretching.
The lithium battery diaphragm and the preparation method thereof provided by the invention have the beneficial effects that: through the steps S1-S9, the mixing effect of the raw materials can be improved, the lithium battery diaphragm with wider porosity control range and uniform pore diameter is finally obtained, and the added silicate powder can form a chain in the lithium battery diaphragm, so that the strength of the lithium battery diaphragm can be effectively improved, the thermal stability can be improved, the mechanical strength is excellent, and the surface tension and the thermal stability of the diaphragm are improved.
Detailed Description
The following is a detailed description of preferred embodiments of the invention in order that the advantages and features of the invention may be more readily understood by those skilled in the art, and in order that the scope of the invention may be more clearly and clearly defined.
A lithium battery diaphragm comprises polyolefin resin and silicate powder, wherein the weight ratio of the polyolefin resin to the silicate powder is 1: 99-3: 1, silicate powder is of a laminated structure and has a particle size of 50 nm-1 mu m;
the diaphragm comprises a first diaphragm, a second diaphragm and a third diaphragm which are sequentially arranged, wherein the first diaphragm and the third diaphragm are respectively provided with a plurality of air holes, the air holes are respectively extended in a zigzag manner along the thickness direction of the diaphragm, the second diaphragm is provided with a plurality of finger-shaped holes, the finger-shaped holes are respectively extended in a zigzag manner along the thickness direction of the diaphragm, a plurality of mutual through holes are respectively arranged among the hole walls of the finger-shaped holes, the aperture ranges of the air holes are respectively 80-300 nm, the aperture ranges of the finger-shaped holes are respectively 400-800 nm, the aperture ranges of the mutual through holes are respectively 50-200 nm, the porosity of the diaphragm is 5-70%, the thickness of the diaphragm is 2-300 mu m, and the ventilation value is 50-2000s/100 cc;
a preparation method of a lithium battery diaphragm is characterized by comprising the following steps:
s1: adding polyolefin resin into an organic solvent, mixing and stirring to obtain a first colloidal solution; adding silicate powder into the first colloidal solution, and continuously stirring at 20-100 ℃, wherein the stirring speed is 200-300r/min, and the stirring time is 5-30min until the silicate powder and the first colloidal solution are uniformly mixed to obtain a second colloidal solution;
s2: conveying the second colloidal solution prepared in the step S1 into an extruder from a first feeding hole of the twin-screw extruder, wherein the temperature of the extruder is 150-270 ℃, and the twin-screw extruder is provided with a vacuum exhaust port and/or a natural exhaust port;
s3: extruding the material melted and mixed by S2 through a die head, cooling and solidifying the material on a cooling roller into a thick film with the thickness of 500-3000 mu m, and carrying out solid-liquid phase separation or liquid-liquid phase separation in the solidification process to form a plurality of micropores inside the thick film;
s4: stretching the thick film prepared in the S3 along the transverse direction and the longitudinal direction, wherein the stretching temperature in the transverse direction and the longitudinal direction is 95-135 ℃, the stretching ratio is more than 5 times, and the film is obtained after stretching, and the stretching process is bidirectional synchronous stretching or bidirectional asynchronous stretching;
s5: extracting the film in the S4 by using an extraction device to obtain a perforated sheet;
s6: putting the hole-drawing sheet material in the step S5 into a washing device for washing to obtain a micropore forming diaphragm semi-finished product;
s7: drying the semi-finished product of the microporous forming diaphragm in the S6 by bypassing a guide roller at the drying temperature of 70-80 ℃ for 5-6h
S8: performing heat setting on the semi-finished product of the microporous forming diaphragm in the step S7 by using a heat setting device to obtain a finished product of the lithium battery diaphragm, wherein the heat setting temperature is 75-135 ℃, and the heat setting time is 3-5S;
s9: and (3) winding the finished lithium battery diaphragm product in the S8 by using a winding machine, wherein the winding machine comprises the following steps:
a, attaching an adhesive tape to the roller surface of a winding roller, and winding a diaphragm on the roller surface attached with the adhesive tape;
b, adjusting the distance between the winding roller and the transmission roller;
c smoothing the edge by blowing compressed air to the edge of the diaphragm.
The method of the steps S1-S9 can improve the mixing effect of the raw materials, finally obtain the lithium battery diaphragm with wider porosity control range and uniform pore diameter, and because the added silicate powder can form a chain in the lithium battery diaphragm, the strength of the lithium battery diaphragm can be effectively improved, the thermal stability can be improved, the lithium battery diaphragm has excellent mechanical strength, and the surface tension and the thermal stability of the diaphragm are improved
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the present invention is not limited thereto, and any equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.
Claims (8)
1. A lithium battery separator characterized by: the polyolefin resin silicate powder comprises polyolefin resin and silicate powder, wherein the weight ratio of the polyolefin resin to the silicate powder is 1: 99-3: 1, the silicate powder is silicate powder with a laminated structure.
2. The lithium battery separator according to claim 1, wherein: the thickness of the diaphragm is 2-300 μm, and the permeability value is 50-2000s/100 cc.
3. The lithium battery separator according to claim 1, wherein: the diaphragm is including the first layer diaphragm, the second floor diaphragm and the third layer diaphragm that set gradually, first layer diaphragm and third layer diaphragm all have a plurality of bleeder vents, and are a plurality of the bleeder vent all extends along the tortuous of thickness direction of diaphragm, the second floor diaphragm has a plurality of finger-like holes, and is a plurality of finger-like hole all extends along the tortuous of thickness direction of diaphragm, and is a plurality of all have a plurality of mutual through-holes between the pore wall in finger-like hole.
4. A lithium battery separator as defined in claim 3, wherein: the aperture range of the air holes is 80-300 nm, the aperture range of the finger-shaped holes is 400-800 nm, and the aperture range of the through holes is 50-200 nm.
5. The lithium battery separator according to claim 1, wherein: the porosity of the diaphragm is 5% -70%.
6. The lithium battery separator according to claim 1, wherein: the particle size of the silicate powder is 50 nm-1 mu m.
7. A preparation method of a lithium battery diaphragm is characterized by comprising the following steps:
s1: adding polyolefin resin into an organic solvent, mixing and stirring to obtain a first colloidal solution; adding silicate powder into the first colloidal solution, and continuously stirring at 20-100 ℃, wherein the stirring speed is 200-300r/min, and the stirring time is 5-30min until the silicate powder and the first colloidal solution are uniformly mixed to obtain a second colloidal solution;
s2: conveying the second colloidal solution prepared by S1 into an extruder from a first feed inlet of the twin-screw extruder, wherein the temperature of the extruder is 150-270 ℃, and the twin-screw extruder is provided with a vacuum exhaust port and/or a natural exhaust port;
s3: extruding the material melted and mixed by S2 through a die head, cooling and solidifying the material on a cooling roller into a thick film with the thickness of 500-3000 mu m, and carrying out solid-liquid phase separation or liquid-liquid phase separation in the solidification process to form a plurality of micropores inside the thick film;
s4: stretching the thick film prepared in the S3 along the transverse direction and the longitudinal direction, wherein the stretching temperature in the transverse direction and the longitudinal direction is 95-135 ℃, the stretching ratio is more than 5 times, and the thin film is obtained after stretching;
s5: extracting the film in the S4 by using an extraction device to obtain a perforated sheet;
s6: putting the hole-drawing sheet material in the step S5 into a washing device for washing to obtain a micropore forming diaphragm semi-finished product;
s7: drying the semi-finished product of the microporous forming diaphragm in the S6 by bypassing a guide roller, wherein the drying temperature is 70-80 ℃, and the drying time is 5-6 h;
s8: performing heat setting on the semi-finished product of the microporous forming diaphragm in the step S7 by using a heat setting device to obtain a finished product of the lithium battery diaphragm, wherein the heat setting temperature is 75-135 ℃, and the heat setting time is 3-5S;
s9: and (4) winding the finished lithium battery diaphragm product in the S8 by using a winding machine.
8. The method of claim 7, wherein: in S4, the stretching process is bidirectional synchronous stretching or bidirectional asynchronous stretching.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911301809.7A CN110993865A (en) | 2019-12-17 | 2019-12-17 | Lithium battery diaphragm and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911301809.7A CN110993865A (en) | 2019-12-17 | 2019-12-17 | Lithium battery diaphragm and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110993865A true CN110993865A (en) | 2020-04-10 |
Family
ID=70094628
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911301809.7A Pending CN110993865A (en) | 2019-12-17 | 2019-12-17 | Lithium battery diaphragm and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110993865A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107221628A (en) * | 2017-06-19 | 2017-09-29 | 武汉艾特米克超能新材料科技有限公司 | A kind of preparation method of lithium battery diaphragm, lithium battery diaphragm and lithium ion battery |
| CN108682773A (en) * | 2018-05-25 | 2018-10-19 | 杨晓丽 | A kind of lithium battery diaphragm and preparation method thereof |
| KR102017568B1 (en) * | 2018-12-26 | 2019-09-06 | 명성티엔에스 주식회사 | Separator for secondary battery, method for manufacturing the same, and secondary battery including the same |
-
2019
- 2019-12-17 CN CN201911301809.7A patent/CN110993865A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107221628A (en) * | 2017-06-19 | 2017-09-29 | 武汉艾特米克超能新材料科技有限公司 | A kind of preparation method of lithium battery diaphragm, lithium battery diaphragm and lithium ion battery |
| CN108682773A (en) * | 2018-05-25 | 2018-10-19 | 杨晓丽 | A kind of lithium battery diaphragm and preparation method thereof |
| KR102017568B1 (en) * | 2018-12-26 | 2019-09-06 | 명성티엔에스 주식회사 | Separator for secondary battery, method for manufacturing the same, and secondary battery including the same |
Non-Patent Citations (1)
| Title |
|---|
| 李祖德编, 北京：中国物资出版社 * |
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Application publication date: 20200410 |