CN109192902B - Preparation method of multi-stage safety protection lithium battery diaphragm and lithium battery diaphragm - Google Patents
Preparation method of multi-stage safety protection lithium battery diaphragm and lithium battery diaphragm 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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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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
- H01M50/463—Separators, membranes or diaphragms characterised by their shape
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The application discloses a preparation method of a multi-stage safety protection lithium battery diaphragm and a lithium battery diaphragm. The preparation method comprises the steps of co-extruding polypropylene and polyethylene by twin-screw or single-screw casting to prepare PP and PE double-layer casting films; annealing the double-layer casting film at high temperature; laminating, compounding, stretching and forming holes on the annealed 4-32 double-layer casting films, wherein the multiplying power is 1.5-3.0; layering the multilayer diaphragms formed by stretching and hole forming, and stripping out a PP and PE double-layer film; forming a high temperature resistant layer on the surface of the PE. The preparation method can simply and efficiently prepare the three-layer multi-stage safety protection lithium battery diaphragm consisting of the PP layer, the PE layer and the high temperature resistant layer. According to the lithium battery diaphragm prepared by the application, PE can rapidly close the hole at a lower temperature, so that the battery can be protected from being broken; carrying out secondary hole closing and further carrying out open circuit protection on the PP when the temperature of the PP is continuously raised; the high-temperature resistant layer plays a role in supporting at high temperature, can ensure that the battery diaphragm does not deform and break, and improves the safety performance of the battery.
Description
Technical Field
The application relates to the field of lithium ion battery diaphragms, in particular to a preparation method of a multi-stage safety protection lithium battery diaphragm and a lithium battery diaphragm.
Background
With the development of new energy industry, the importance of lithium batteries is gradually highlighted. The lithium battery diaphragm is one of the most important components in the lithium battery, and the preparation of the microporous membrane which is safe, environment-friendly and low in cost is difficult in the production process. At present, the manufacturing methods of the lithium battery diaphragm include a wet method and a dry method. The wet process needs a large amount of organic diluent, and has the disadvantages of complex equipment, high cost and easy environmental pollution. Compared with the wet method, the dry method has the advantages of simple equipment, low cost and no environmental pollution. The dry method is mainly divided into dry unidirectional stretching and dry bidirectional stretching technologies. The pore-forming of the microporous membrane prepared by the dry biaxial stretching technology is not uniform, mainly because the pore-forming position and pore-forming size of the polypropylene in the process of converting the beta crystal form into the alpha crystal form can not be controlled. So the mainstream technology of the dry-method diaphragm is dry-method uniaxial tension. The process has been well established in the united states and japan over decades and is now used by Celgard corporation, UBE corporation, japan, to produce membranes.
The structure and performance of the lithium battery diaphragm are crucial to the safety of the lithium battery: on one hand, the single-layer lithium battery diaphragm is easy to have a small amount of defects, and the production process is difficult to control, so the defects of each single-layer diaphragm are preferably covered by the design of a multilayer diaphragm; on the other hand, in the initial stage of the temperature rise of the battery short circuit, if the diaphragm can be broken in time, the short circuit is further stopped or prevented, and the safety of the lithium battery can be greatly improved. The existing wet-process diaphragm is usually prepared by ultra-high molecular weight polyethylene, the melt flow speed is slow, the thermal shrinkage is large in the temperature rise process, and the hole cannot be closed in time. The dry-process polypropylene diaphragm has high closed pore temperature and large thermal shrinkage in the temperature rise process, so that the dry-process polypropylene diaphragm cannot respond quickly and can not protect the battery, only the polyethylene layer is used for protection in the dry-process polypropylene (abbreviation PP)/polyethylene (abbreviation PE)/polypropylene three-layer diaphragm, and particularly under the condition that the PE layer is very thin, the diaphragm can be broken when the temperature is further increased, so that short circuit can be caused continuously. In addition, the ceramic coated membrane, which usually has only one layer of protection, cannot effectively protect the membrane when the temperature is further increased due to the accumulated heat.
Disclosure of Invention
The application aims to provide an improved preparation method of a multistage safety protection lithium battery diaphragm and a lithium battery diaphragm prepared by the improved preparation method.
In order to achieve the purpose, the following technical scheme is adopted in the application:
one aspect of the application discloses a method for preparing a multi-stage safety protection lithium battery diaphragm, which comprises the following steps,
(1) carrying out double-screw or single-screw casting coextrusion on polypropylene and polyethylene materials to form a film, and preparing a double-layer casting film consisting of a PP layer and a PE layer with the thickness of 10-40 microns;
(2) annealing the prepared double-layer casting film at the high temperature of 100-135 ℃ to form regular platelets;
(3) laminating and compounding 4-32 annealed double-layer casting films, and stretching and forming holes together, wherein the stretching ratio is 1.5-3.0 times;
(4) layering the multi-layer diaphragm after the stretching and hole forming, and stripping a double-layer film consisting of a PP layer and a PE layer;
(5) the PE layer surface at the double-layer membrane that PP layer and PE layer are constituteed forms high temperature resistant layer, obtains the three-layer composite diaphragm that PP layer, PE layer and high temperature resistant layer are constituteed, the multistage safety protection lithium battery diaphragm of this application promptly.
The preparation method comprises the steps of firstly co-extruding PP and PE into a double-layer casting film, then laminating and compounding a plurality of double-layer casting films for stretching, and then stripping the double-layer film formed by the PP layer and the PE layer, so that the production efficiency is greatly improved, and the prepared lithium battery diaphragm can meet the use requirement of multi-stage safety protection.
Preferably, in the preparation method, the high-temperature resistant layer is a ceramic coating and/or an aramid coating.
Preferably, in the step (5), the high temperature resistant layer is formed on the surface of the PE layer of the two-layer film by at least one of gravure printing, roll coating, dip coating, doctor blade coating and spray coating.
Preferably, in the preparation method, the polypropylene has the isotacticity of more than or equal to 96 percent and the melt index of 0.3-5g/10 min; the polyethylene is high density polyethylene with a melt index of 0.05-5g/10 min.
The application further discloses a lithium battery diaphragm prepared by the preparation method, and the lithium battery diaphragm is a three-layer composite diaphragm consisting of a PP layer, a PE layer and a high-temperature-resistant layer.
Preferably, in the lithium battery separator of the present application, the high temperature resistant layer is a ceramic coating and/or an aramid coating.
Preferably, the ceramic coating is formed by coating at least one of alumina, silica, titania, zirconia, barium titanate and barium sulfate as a main component.
Preferably, in the lithium battery diaphragm, the PE layer is a first fused closed pore layer, and the fusing temperature of the PE layer is 125-135 ℃; the PP layer is a second fused closed-pore layer, and the fusing temperature of the PP layer is 155-165 ℃; the heat-resistant temperature of the high-temperature resistant layer is higher than 200 ℃.
It should be noted that, according to the lithium battery diaphragm of the present application, the melting point of the PE layer is about 130 degrees, the melting point of the PP layer is about 160 degrees, the heat-resistant temperature of the high temperature-resistant layer is higher than 200 ℃, the high temperature-resistant layer plays a role of high temperature support, when the lithium battery is heated to 130 degrees due to a short circuit, the PE layer first melts and closes the pores to open the circuit, thereby protecting the battery, when the temperature continues to rise, the polyethylene on the PE layer can permeate into the polypropylene pores on the PP layer, and meanwhile, the PP layer can also melt and close the pores, thereby performing the second-level protection, and achieving the effect of multi-level safety protection.
Preferably, in the lithium battery separator of the present application, the raw material of the PE layer is high density polyethylene having a melt index of 0.05 to 5g/10 min.
Preferably, the porosity of the PE layer is 20% to 60%.
Preferably, in the lithium battery separator, the PP layer is made of polypropylene with a melt index of 0.3-5g/10min and an isotacticity of greater than or equal to 96%.
Preferably, the porosity of the PP layer is 20% to 60%.
It should be noted that the high-density polyethylene with the melt index of 0.05-5g/10min is adopted in the application, so as to ensure that the cell can be closed rapidly at a lower temperature in the process of increasing the temperature of the cell; and the PP layer uses polypropylene with the isotacticity of more than or equal to 96 percent and the melt index of 0.3-5g/10min, and also aims to ensure secondary pore closing in the process of heating the battery.
Preferably, the thickness of the lithium battery separator is 10-40 microns; wherein, the thickness of the PP layer is 4-20 microns, and the thickness of the PE layer is 4-20 microns; the thickness of the high temperature resistant layer is 1-8 microns, and the porosity of the high temperature resistant layer is 10% -70%.
Due to the adoption of the technical scheme, the beneficial effects of the application are as follows:
the preparation method can simply and efficiently prepare the three-layer multi-level safety protection lithium battery diaphragm consisting of the PP layer, the PE layer and the high temperature resistant layer, and lays a foundation for large-scale batch production of high-quality lithium battery diaphragms. According to the multi-stage safety protection lithium battery diaphragm prepared by the application, the PE layer is a first melting closed hole layer, and the hole is closed rapidly at a lower temperature, so that the battery is subjected to open circuit safety protection; the PP layer is a second melting hole-closing layer, secondary hole closing is carried out under the condition that the temperature of the battery is continuously increased, and further the safety protection of the battery is carried out, so that the effect of strengthening the safety protection of the open circuit is achieved; and in the whole process of heating and fusing, the high-temperature-resistant layer plays a role of high-temperature support, so that the battery diaphragm can not deform and break at high temperature, and the safety performance of the battery is further improved.
Drawings
FIG. 1 is a schematic structural diagram of a lithium battery separator with enhanced open circuit safety protection in an embodiment of the present application.
Detailed Description
The present application is described in further detail below with reference to specific embodiments and the attached drawings. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application.
Example one
The multi-stage safety protection lithium battery diaphragm of the embodiment is a three-layer composite diaphragm composed of a PP layer 1, a PE layer 2 and a high temperature resistant layer 3, as shown in figure 1. The high-temperature resistant layer of the embodiment is a ceramic coating, and particularly adopts alumina with D50 being 1 micron to prepare the high-temperature resistant coating. The PP layer of this example was prepared from polypropylene having an isotacticity of 98% and a melt index of 2g/10min, and the PE layer was high density polyethylene having a melt index of 0.5g/10 min.
The preparation method of the multi-stage safety protection lithium battery diaphragm comprises the following steps:
(1) carrying out twin-screw casting coextrusion film forming on polypropylene and polyethylene materials to prepare a double-layer casting film consisting of a PP layer and a PE layer with the thickness of 17 microns;
(2) annealing the prepared double-layer casting film at the high temperature of 130 ℃ to form regular platelets;
(3) laminating and compounding the annealed 32 double-layer casting films, and stretching and forming holes together, wherein the stretching ratio is 1.5 times;
(4) layering the multi-layer diaphragm after the stretching and hole forming, and stripping a double-layer film consisting of a PP layer and a PE layer;
(5) and forming a ceramic coating on the surface of the PE layer of the double-layer film consisting of the PP layer and the PE layer to obtain a three-layer composite diaphragm consisting of the PP layer, the PE layer and the high-temperature-resistant layer, namely the multi-stage safety protection lithium battery diaphragm.
In the step (5), the preparation method of the ceramic coating comprises the following steps:
weighing aluminum oxide powder, dispersing the aluminum oxide powder in deionized water, and adding a dispersing agent, a binder and the like to prepare coating slurry. And coating the coating slurry on the surface of the PE layer in a roller coating mode, and drying to obtain the three-layer composite diaphragm consisting of the PP layer, the PE layer and the high-temperature-resistant layer.
The multi-stage safety protection lithium battery diaphragm of the embodiment is observed by a scanning electron microscope, wherein the thickness of the PP layer is 7 microns, the thickness of the PE layer is 7 microns, and the thickness of the high-temperature resistant layer is 2 microns.
The air permeability values at normal temperature, MD heat shrinkage, TD heat shrinkage, and air permeability values after heat treatment at 130 ℃, 150 ℃, and 170 ℃ respectively of the multi-stage safety protection lithium battery separator of this example were tested, and the test results are shown in table 1. Wherein, the ventilation values after heat treatment at 130 ℃, 150 ℃ and 170 ℃ are used for representing the safety of open circuit, and the larger the ventilation value is, the lower the lithium ion passing rate in the battery is, and the more obvious the open circuit effect is.
Example two
The multi-stage safety protection lithium battery diaphragm of the embodiment is a three-layer composite diaphragm composed of a PP layer, a PE layer and a high temperature resistant layer, which is the same as the embodiment I. The high temperature resistant layer of this example is an aramid coating. The PP layer of this example was prepared from polypropylene with an isotacticity of 97% and a melt index of 0.5g/10min, and the PE layer was high density polyethylene with a melt index of 0.3g/10 min.
The preparation method of the multi-stage safety protection lithium battery diaphragm comprises the following steps:
(1) the polypropylene and polyethylene materials are co-extruded into a film by adopting twin-screw casting to prepare a double-layer casting film consisting of a PP layer and a PE layer with the thickness of 17 microns;
(2) annealing the prepared double-layer casting film at the high temperature of 120 ℃ to form regular platelets;
(3) laminating and compounding 16 annealed double-layer casting films, and stretching and forming holes together, wherein the stretching ratio is 3 times;
(4) layering the multi-layer diaphragm after the stretching and hole forming, and stripping a double-layer film consisting of a PP layer and a PE layer;
(5) and forming an aramid coating on the surface of the PE layer of the double-layer film consisting of the PP layer and the PE layer to obtain a three-layer composite diaphragm consisting of the PP layer, the PE layer and the high-temperature-resistant layer, namely the multi-stage safety protection lithium battery diaphragm.
In the step (5), the preparation method of the aramid fiber coating comprises the following steps:
dissolving aramid fiber to prepare a dispersion liquid, and then coating the dispersion liquid by using a roll coating or dip coating mode.
The multi-stage safety protection lithium battery diaphragm of the embodiment is observed by a scanning electron microscope, wherein the thickness of the PP layer is 7 microns, the thickness of the PE layer is 7 microns, and the thickness of the high-temperature resistant layer is 2 microns.
The air permeability values at normal temperature, MD heat shrinkage, TD heat shrinkage, and air permeability values after heat treatment at 130 ℃, 150 ℃, and 170 ℃ respectively of the multi-stage safety protection lithium battery separator of this example were tested, and the test results are shown in table 1. Wherein, the ventilation values after heat treatment at 130 ℃, 150 ℃ and 170 ℃ are used for representing the safety of open circuit, and the larger the ventilation value is, the lower the lithium ion passing rate in the battery is, and the more obvious the open circuit effect is.
Comparative example 1
The tests were carried out directly on a single-layer polyethylene membrane having a porosity of 55% and a thickness of 16 μm, the polyethylene membrane being tested in the same manner as in example one. The test results are shown in table 1.
Comparative example No. two
The test was carried out directly on this example using a single layer polypropylene membrane having a porosity of 45% and a thickness of 16 μm, the polypropylene membrane being tested in the same manner as in example one. The test results are shown in table 1.
The separators of example one, example two, comparative example one, and comparative example two were subjected to a room temperature air permeability test, a MD heat shrinkage test at 130 ℃ for 1 hour, a TD heat shrinkage test at 130 ℃ for 1 hour, an air permeability test after 130 ℃ for 30min, an air permeability test after 150 ℃ for 30min, and an air permeability test after 170 ℃ for 30 min.
Wherein the permeability test employs the Gurley method, i.e., the time required for 100mL of gas to pass through the membrane is in units of s/100 mL.
The heat shrinkage performance test included:
(1) cutting the diaphragm prepared in each example and each comparative example into samples of 10cm multiplied by 10cm, cutting five samples in each example and each comparative example, and averaging the test results;
(2) respectively testing the thermal shrinkage condition of the membrane after being baked for 1 hour at the temperature of 130 ℃;
this example was tested for heat shrinkage in the transverse and longitudinal directions, respectively.
Table 1 test results of various properties of the separator
The results in table 1 show that examples 1 and 2 of the present application have a significant gradient closed cell function and significantly less thermal shrinkage compared to comparative examples 1 and 2. The composite lithium battery diaphragm has the multistage safety protection performance of gradually closing the pores under the condition that the temperature is gradually increased, and the lithium battery diaphragm prepared by the method has the advantages of small heat shrinkage rate and high safety performance, so that the safety performance of the battery is further improved.
The foregoing is a more detailed description of the present application in connection with specific embodiments thereof, and it is not intended that the present application be limited to the specific embodiments thereof. For those skilled in the art to which the present application pertains, several simple deductions or substitutions may be made without departing from the concept of the present application, and all should be considered as belonging to the protection scope of the present application.
Claims (12)
1. A preparation method of a multi-stage safety protection lithium battery diaphragm is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(1) carrying out double-screw or single-screw casting coextrusion on polypropylene and polyethylene materials to form a film, and preparing a double-layer casting film consisting of a PP layer and a PE layer;
(2) annealing the prepared double-layer casting film at the high temperature of 100-135 ℃ to form regular platelets;
(3) laminating and compounding 4-32 annealed double-layer casting films, and stretching and forming holes together, wherein the stretching ratio is 1.5-3.0 times;
(4) layering the multi-layer diaphragm after the stretching and hole forming, and stripping a double-layer film consisting of a PP layer and a PE layer;
(5) and forming a high-temperature resistant layer on the surface of the PE layer of the double-layer film consisting of the PP layer and the PE layer to obtain a three-layer composite diaphragm consisting of the PP layer, the PE layer and the high-temperature resistant layer, namely the multi-stage safety protection lithium battery diaphragm.
2. The method of claim 1, wherein: the high temperature resistant layer is a ceramic coating and/or an aramid coating.
3. The method of claim 2, wherein: the ceramic coating is formed by coating at least one of alumina, silicon oxide, titanium oxide, zirconium oxide, barium titanate and barium sulfate serving as a main component.
4. The method of claim 1, wherein: in the step (5), the high temperature resistant layer is formed on the surface of the PE layer of the double-layer film by at least one of gravure printing, roll coating, dip coating, doctor blade, and spray coating.
5. The production method according to any one of claims 1 to 4, characterized in that: the polypropylene has an isotacticity of more than or equal to 96 percent and a melt index of 0.3-5g/10 min; the polyethylene is high-density polyethylene with the melt index of 0.05-5g/10 min.
6. A lithium battery separator prepared by the preparation method of any one of claims 1 to 5, which is a three-layer composite separator consisting of a PP layer, a PE layer and a high temperature resistant layer.
7. The lithium battery separator according to claim 6, wherein: the PE layer is a first fused closed pore layer, and the fusing temperature of the PE layer is 125-145 ℃; the PP layer is a second fused closed-pore layer, and the fusing temperature of the PP layer is 155-175 ℃; the heat-resistant temperature of the high-temperature resistant layer is higher than 200 ℃.
8. The lithium battery separator according to claim 6 or 7, wherein: the raw material of the PE layer is high-density polyethylene with the melt index of 0.05-5g/10 min.
9. The lithium battery separator according to claim 8, wherein: the porosity of the PE layer is 20% -60%.
10. The lithium battery separator according to claim 6 or 7, wherein: the PP layer is made of polypropylene with the melt index of 0.3-5g/10min and the isotacticity of more than or equal to 96%.
11. The lithium battery separator as claimed in claim 10, wherein: the porosity of the PP layer is 20-60%.
12. The lithium battery separator according to claim 6 or 7, wherein: the thickness of the lithium battery diaphragm is 10-40 microns;
wherein the thickness of the PP layer is 4-20 microns, and the thickness of the PE layer is 4-20 microns;
the thickness of the high-temperature resistant layer is 1-8 microns, and the porosity of the high-temperature resistant layer is 10% -70%.
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| CN110071247A (en) * | 2019-04-22 | 2019-07-30 | 深圳中兴新材技术股份有限公司 | A kind of gradient low temperature closed pore composite diaphragm and preparation method thereof that adhesive property improves |
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| CN115954612A (en) * | 2023-03-15 | 2023-04-11 | 河南新太行电源股份有限公司 | High-temperature-resistant safety lithium ion battery diaphragm and preparation method thereof |
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| CN104157819A (en) * | 2014-09-02 | 2014-11-19 | 深圳市星源材质科技股份有限公司 | Ceramic-gel polymer multilayer composite lithium battery diaphragm and preparation method thereof |
| CN108025539A (en) * | 2015-07-15 | 2018-05-11 | 三菱化学株式会社 | Laminated porous film, separator for nonaqueous electrolyte secondary battery, the manufacture method of rechargeable nonaqueous electrolytic battery and laminated porous film |
| CN107316964A (en) * | 2017-06-02 | 2017-11-03 | 武汉惠强新能源材料科技有限公司 | A kind of modified HOPP/high density polyethylene (HDPE)/three-layer co-extruded lithium battery diaphragm of modification HOPP and preparation method thereof |
| CN108189499A (en) * | 2017-12-14 | 2018-06-22 | 深圳市星源材质科技股份有限公司 | A kind of multilayer complex films and preparation method thereof |
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