CN111952519B - Ceramic diaphragm and preparation method thereof - Google Patents
Ceramic diaphragm and preparation method thereof Download PDFInfo
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- CN111952519B CN111952519B CN202010806327.3A CN202010806327A CN111952519B CN 111952519 B CN111952519 B CN 111952519B CN 202010806327 A CN202010806327 A CN 202010806327A CN 111952519 B CN111952519 B CN 111952519B
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M2200/00—Safety devices for primary or secondary batteries
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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
- 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
Abstract
The invention relates to the field of film materials, and particularly discloses a novel ceramic diaphragm which is characterized in that: the preparation method comprises the steps of adding a binder and a plasticizer into inorganic nano powder serving as a raw material, and then carrying out hot press molding. The invention can prepare the novel ceramic diaphragm with different product shapes, sizes, complex shapes and precisions by a hot press molding method, has higher porosity and extremely high heat resistance so as to improve the electrochemistry and heat-resistant shrinkage performance of the diaphragm, can greatly improve the safety use performance of the lithium ion battery, has simple process, is easy to be applied to a production line for mass production and manufacture, and has huge application prospect.
Description
Technical Field
The invention relates to the field of membrane materials, in particular to a ceramic diaphragm and a preparation method thereof.
Background
In recent years, with the increase of the environmental pollution control strength of the country, new energy vehicles are more and more encouraged by government departments and favored by consumers. Therefore, new energy automobiles powered by lithium batteries are receiving wide attention from scientific researchers and automobile manufacturers.
Four major materials of lithium batteries include positive electrodes, negative electrodes, separators, and electrolytes. The lithium battery diaphragm is one of the four materials, and the diaphragm has the main function of separating the positive electrode from the negative electrode of the battery, preventing the two electrodes from contacting and short-circuiting, and has the function of enabling electrolyte ions to pass through. In addition, the diaphragm of the lithium battery can block the conduction of ions in the battery through the closed pore function when the battery is overheated, so that potential safety hazards such as ignition and explosion caused by short circuit of the anode and the cathode are avoided. The performance of the diaphragm determines the interface structure, internal resistance and the like of the battery, directly influences the capacity, circulation, safety performance and other characteristics of the battery, and the diaphragm with excellent performance plays an important role in improving the comprehensive performance of the battery.
The development and the start of lithium battery diaphragms in China are late, the difference is still small compared with international same lines, in the prior art, the lithium battery diaphragms are prepared by taking high polymer materials such as polyethylene, polypropylene and the like as raw materials, however, the diaphragms have the defects of low surface energy, inertia and no high temperature resistance, and most accidents of lithium battery automobiles are caused by the fact that the diaphragms have poor heat-resistant shrinkage performance and the short circuit of positive and negative electrodes is caused by heat shrinkage at high temperature. Therefore, the development of a high-temperature-resistant lithium battery separator is more and more urgent.
Disclosure of Invention
In view of the above, the present invention is intended to provide a high temperature resistant lithium battery separator, so as to solve a series of safety accidents, such as explosion and combustion, caused by short circuit caused by contact between the positive electrode and the negative electrode of the lithium battery due to contraction of the existing separator in a high temperature working environment.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention aims to provide a ceramic diaphragm which is prepared by adopting inorganic nano powder as a raw material, adding a binder and a plasticizer and then carrying out hot press molding.
Further, the binder accounts for 10-30% of the inorganic nano powder by mass.
Further, the plasticizer accounts for 1-10% of the inorganic nano powder by mass.
Furthermore, the particle size of the inorganic nano powder is 1-100 nm.
Further, the inorganic nano powder is aluminum oxide (Al)2O3) Zirconium oxide (ZrO)2) Titanium oxide (TiO)2) Silicon dioxide (SiO)2) Barium sulfate (BaSO)4) Boehmite, and the like.
Further, the binder is thermoplastic or resin.
Further, the thermoplastic or resin is one or more of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polymethyl methacrylate, polyester, polyoxymethylene, polyamide, and polyphenylene oxide.
Further, the plasticizer is one or more of lignosulfonate, naphthalene sulfonic acid condensate and sulfonated melamine formaldehyde.
Another object of the present invention is to provide a method for preparing the above ceramic separator, comprising the steps of:
(1) adding a binder and a plasticizer into the inorganic nano powder, and uniformly mixing under a heating condition;
(2) filling the mixture into a mould;
(3) the mixture in the die is extruded and formed by setting the pressure and the temperature of a punch;
(4) and cutting the punch-formed film into specific sizes and polishing the surface of the film to obtain the lithium battery ceramic diaphragm with the required size.
Further, the heating condition in the step (1) is 150-200 ℃.
Further, the pressure of the punch is set to be 10-50 Mpa, and the temperature is set to be 150-200 ℃.
Further, the surface polishing needs to be carried out by grinding and polishing materials, wherein the grinding and polishing materials are SIC and B4C or diamond.
It is still another object of the present invention to provide an electrochemical device using the above ceramic separator to coat a pole piece assembled battery.
The invention has the following beneficial effects:
1) according to the invention, the ceramic diaphragm with different product shapes, sizes, complex shapes and precisions can be prepared by a hot press molding method, and the ceramic diaphragm has higher porosity and extremely high heat resistance, so that the electrochemistry and heat-resistant shrinkage performances of the diaphragm are improved;
2) the ceramic diaphragm prepared by the invention has no potential safety hazard of shrinkage and combustion at high temperature, and can greatly improve the safety use performance of the lithium ion battery;
3) the invention has simple process and is easy to be applied to a production line for mass production and manufacture.
Drawings
FIG. 1 is a scanning electron micrograph of a surface of a ceramic diaphragm according to an embodiment of the present invention;
FIG. 2 is a cross-sectional scanning electron micrograph of a ceramic diaphragm according to one embodiment of the present invention;
FIG. 3 is a scanning electron micrograph of a surface of a ceramic diaphragm according to an embodiment of the present invention;
FIG. 4 is a scanning electron microscope image of a cross section of a ceramic diaphragm according to an embodiment of the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The specific embodiment of the invention provides a ceramic diaphragm which is prepared by adopting inorganic nano powder as a raw material, adding a binder and a plasticizer and then carrying out hot press molding.
Preferably, the binder accounts for 10-30% of the inorganic nano powder by mass.
Preferably, the plasticizer accounts for 1-10% of the inorganic nano powder by mass.
Preferably, the particle size of the inorganic nano powder is 1-100 nm.
Preferably, the inorganic nanopowder is alumina (Al)2O3) Zirconium oxide (ZrO)2) Titanium oxide (TiO)2) Silicon dioxide (SiO)2) Barium sulfate (BaSO)4) Boehmite, and the like.
Preferably, the binder is a thermoplastic or resin.
Specifically, the thermoplastic plastic or resin is one or more of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polymethyl methacrylate, polyester, polyformaldehyde, polyamide and polyphenyl ether.
Preferably, the plasticizer is one or more of lignosulfonate, naphthalene sulfonic acid condensate and sulfonated melamine formaldehyde.
The specific embodiment of the invention also provides a method for preparing the ceramic diaphragm, which comprises the following steps:
(1) adding a binder into the inorganic nano powder, and uniformly mixing the binder and the plasticizer at 150-200 ℃ to facilitate molding;
(2) filling the mixture into a mold with a specified size, so that the mold is filled with the alumina powder completely as far as possible;
(3) the mixture in the die is extruded and formed by setting the pressure and the temperature of a punch;
(4) the aluminum oxide film formed by stamping is cut into specific size and surface polished, because the aluminum oxide ceramic material has higher hardness, the aluminum oxide ceramic material needs to be finely polished by harder grinding and polishing materials, and the aluminum oxide ceramic material is usually ground step by coarse to fine grinding materials and finally surface polished.
Preferably, the pressure of the punch is set to be 10-50 Mpa, and the temperature is set to be 150-200 ℃.
Preferably, the surface polishing needs a grinding and polishing material, and the grinding and polishing material is SIC and B4C or diamond.
The invention also provides an electrochemical device, which adopts the ceramic diaphragm to coat a pole piece assembled battery.
The present invention will be described in detail below by way of examples.
In the following examples and comparative examples, the film property test was performed as follows:
the test method of the air permeability of the lithium battery diaphragm comprises the following steps: the air permeability tester of the lithium battery diaphragm is a Wang-grinding type air permeability tester, fixes the battery diaphragm, and applies 0.05Mpa air pressure to one side of the diaphragm, and the air pressure can be gradually reduced due to micropores in the diaphragm, and when 100mL of air completely passes through the diaphragm, the air pressure is equal to atmospheric pressure. The air permeability (s/100cc) of the separator was determined by recording the time taken for 100ml of air to pass through the separator under a pressure of 0.05 MPa. By comparing the pressure drop times of different membranes, their air permeability performance can be compared. The smaller the pressure drop time, the better the air permeability.
The thermal shrinkage test method of the lithium battery separator includes the steps of cutting three 10cm by 10cm separators, testing the lengths in the MD and TD directions, pressing three sheets of A4 paper on the separators, placing the separators in an oven for 1 hour at 150 ℃, measuring the change of the lengths, wherein the thermal shrinkage is (the length before the test-the length after the test)/the length before the test is 100%, and averaging the three measurement data and filling the average data into the table 1.
Example 1
A lithium battery ceramic diaphragm is a lithium battery diaphragm which is manufactured by taking nano alumina powder as a raw material through a hot press molding method and comprises the following specific steps:
1) preparation of raw materials: drying powdery nano alumina, adding 10 parts of polyamide and 1 part of lignosulfonate per 100 parts by mass, and stirring for 5 hours in a sealed stirring tank at 150 ℃ to thoroughly and uniformly mix alumina nano powder, a binder and a plasticizer;
2) stamping: filling the uniformly mixed slurry into a mold to enable the slurry to fill the whole cavity of the mold, and then pressing the slurry into a diaphragm sheet with a specific specification by using a punching machine at 10MPa and 150 ℃;
3) cutting and trimming: cutting the punched and formed aluminum oxide sheet into specific sizes and polishing the surface, wherein the aluminum oxide ceramic material has higher hardness, the aluminum oxide ceramic material needs to be finely processed by a diamond drill which is a harder grinding and polishing material, the aluminum oxide ceramic material is ground step by coarse-fine grinding materials and finally polished to obtain the lithium battery ceramic diaphragm, the batch of diaphragms are subjected to air permeability and heat shrinkage performance tests, the results are recorded in a table 1, the surface and the cross section of the diaphragms are subjected to a scanning electron microscope (as shown in figures 1 and 2), and the compact microporous diaphragm is formed by a hot press forming method after a binder and a plasticizer are added into the aluminum oxide powder body.
Example 2
A lithium battery ceramic diaphragm is a lithium battery diaphragm which is manufactured by taking nano barium sulfate powder as a raw material through a hot press molding method and comprises the following specific steps:
1) preparation of raw materials: drying powdery nano barium sulfate, and then adding 20 parts of polyamide and 2 parts of lignosulfonate per 100 parts by mass, stirring for 5 hours in a sealed stirring tank at 160 ℃ to thoroughly and uniformly mix barium sulfate nano powder, a binder and a plasticizer;
2) stamping: filling the uniformly mixed slurry into a mold to enable the slurry to fill the whole cavity of the mold, and then pressing the slurry into a diaphragm sheet with a specific specification by using a punching machine under the pressure of 20MPa and at the temperature of 160 ℃;
3) cutting and trimming: cutting the punched barium sulfate sheet into specific size and polishing the surface, wherein the barium sulfate material has high hardness, a harder grinding and polishing material SiC is required to finish the barium sulfate material, coarse grinding and fine grinding are adopted to grind the barium sulfate material step by step, and the surface is polished finally to obtain the lithium battery ceramic diaphragm, the batch of diaphragms are subjected to air permeability and heat shrinkage performance tests, the results are recorded in a table 1, the surface and the cross section of the diaphragms are subjected to a scanning electron microscope (as shown in figures 3 and 4), and the compact microporous diaphragm is formed by a hot press molding method after the binder and the plasticizer are added into the barium sulfate powder.
Example 3
A lithium battery ceramic diaphragm is prepared by taking nano titanium oxide powder as a raw material and adopting a hot press molding method, and comprises the following specific steps:
1) preparation of raw materials: drying the powdery nano titanium oxide, adding 30 parts of polyamide and 8 parts of lignosulfonate per 100 parts by mass, and stirring for 5 hours in a sealed stirring tank at 170 ℃ to thoroughly and uniformly mix the titanium oxide nano powder, the binder and the plasticizer;
2) stamping: filling the uniformly mixed slurry into a mold to enable the slurry to fill the whole cavity of the mold, and then pressing the slurry into a diaphragm sheet with a specific specification by using a punching machine under the pressure of 30MPa and at the temperature of 170 ℃;
3) cutting and trimming: the press-formed titanium oxide sheet is cut into a specific size and subjected to surface polishing because the titanium oxide material is hardHigher degree of grinding and polishing, and need harder grinding and polishing material B4And C, performing finish machining on the lithium battery ceramic diaphragm, grinding the lithium battery ceramic diaphragm step by adopting coarse-to-fine grinding materials, polishing the surface finally to obtain the lithium battery ceramic diaphragm, testing the air permeability and the heat shrinkage performance of the diaphragm batch, and recording the result in the table 1.
Example 4
A lithium battery ceramic diaphragm is prepared by taking nano zirconia powder as a raw material and adopting a hot press molding method, and comprises the following specific steps:
1) preparation of raw materials: drying the powdery nano zirconia, adding 25 parts of polyamide and 10 parts of lignosulfonate per 100 parts by mass, and stirring for 5 hours in a sealed stirring tank at 180 ℃ to thoroughly and uniformly mix the zirconia nano powder, the binder and the plasticizer;
2) stamping: filling the uniformly mixed slurry into a mold to enable the slurry to fill the whole cavity of the mold, and then pressing the slurry into a diaphragm sheet with a specific specification by using a punching machine under 40MPa and at 180 ℃;
3) cutting and trimming: cutting the punched zirconia sheets into specific sizes and polishing the surfaces of the zirconia sheets, wherein the zirconia materials have higher hardness, the zirconia sheets are subjected to finish machining by using a diamond drill which is a harder grinding and polishing material, are subjected to gradual grinding by adopting coarse-fine grinding materials and are finally polished to obtain the lithium battery ceramic membranes, and the membranes are subjected to air permeability and heat shrinkage performance tests, and the results are recorded in table 1.
Example 5
A lithium battery ceramic diaphragm is prepared by taking nano silicon dioxide powder as a raw material and adopting a hot press molding method, and comprises the following specific steps:
1) preparation of raw materials: drying powdery nano silicon dioxide, adding 20 parts of polyamide and 5 parts of lignosulfonate per 100 parts by mass, and stirring for 6 hours in a sealed stirring tank at 190 ℃ to thoroughly and uniformly mix silicon dioxide nano powder, a binder and a plasticizer;
2) stamping: filling the uniformly mixed slurry into a mold to enable the slurry to fill the whole cavity of the mold, and then pressing the slurry into a diaphragm sheet with a specific specification by using a punching machine under 50MPa and 190 ℃;
3) cutting and trimming: cutting the punched silicon dioxide slices into specific sizes and polishing the surfaces of the silicon dioxide slices, wherein the silicon dioxide material has higher hardness, the silicon dioxide slices are subjected to finish machining by using a diamond drill which is a harder grinding and polishing material, are subjected to gradual grinding by adopting coarse-to-fine grinding materials and are finally polished on the surfaces to obtain the lithium battery ceramic membranes, and the membranes are subjected to air permeability and heat shrinkage performance tests, and the results are recorded in table 1.
Example 6
A lithium battery ceramic diaphragm is a lithium battery diaphragm which is manufactured by taking nano boehmite powder as a raw material through a hot press molding method and comprises the following specific steps:
1) preparation of raw materials: drying powdery nano boehmite, adding 30 parts of polyamide and 8 parts of lignosulfonate per 100 parts by mass, and stirring for 5 hours in a sealed stirring tank at 200 ℃ to thoroughly and uniformly mix boehmite nano powder, a binder and a plasticizer;
2) stamping: filling the uniformly mixed slurry into a mold to enable the slurry to fill the whole cavity of the mold, and then pressing the slurry into a diaphragm sheet with a specific specification by using a punching machine under the pressure of 50MPa and at the temperature of 200 ℃;
3) cutting and trimming: cutting the punch formed boehmite slices into specific sizes and polishing the surfaces of the boehmite slices, wherein the boehmite material has higher hardness, a harder grinding and polishing material diamond is required to finish the boehmite slices, coarse grinding and fine grinding are adopted to grind the boehmite slices step by step, the surfaces of the boehmite slices are polished finally to obtain the lithium battery ceramic membranes, and the membranes are subjected to air permeability and heat shrinkage performance tests, and the results are recorded in table 1.
Comparative example 1 is a commercially available ceramic coated wet process polyethylene separator coated in a double layer coating with a thickness of 3 microns. Comparative example 2 is a commercially available ceramic-coated dry polyethylene separator coated in a double layer manner, each having a thickness of 3 μm.
TABLE 1 test tables for air permeability and heat shrinkage properties of examples 1 to 4 and comparative examples 1 to 3
As can be seen from the data in Table 1, the examples of the present invention are effectively secured in terms of air permeability, and are qualitatively fly-through in terms of heat shrinkability. Therefore, the lithium battery ceramic diaphragm prepared by the inorganic nano powder greatly improves the current technical situation in the aspect of heat shrinkage under the condition of ensuring air permeability.
In addition, the method has simple process, is easy to be applied to production lines for mass production and manufacture, and has huge application prospect.
The above matters related to the common general knowledge are not described in detail and can be understood by those skilled in the art.
The above-described embodiments are merely illustrative of the principles of the present invention and its efficacy, and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (4)
1. A ceramic diaphragm, characterized by: the MD and TD shrinkage rate of the ceramic diaphragm at 150 ℃ for 1 hour is 0%, and the preparation method comprises the following steps:
(1) adding a binder and a plasticizer into inorganic nano powder, and uniformly mixing under a heating condition to form slurry, wherein the inorganic nano powder is aluminum oxide (Al)2O3) Zirconium dioxide (ZrO)2) Titanium dioxide (TiO)2) Silicon dioxide (SiO)2) Barium sulfate (BaSO)4) The adhesive is polyamide, the plasticizer is lignosulfonate, and the heating condition is 150-200 ℃;
(2) filling the mixed slurry into a mold;
(3) the method comprises the following steps of (1) carrying out extrusion forming on mixed slurry in a die by setting the pressure and temperature of a punching machine, wherein the pressure is set to be 10-50 Mpa, and the temperature is set to be 150-200 ℃;
(4) cutting the punch-formed film into a specific size and polishing the surface of the film to prepare the ceramic diaphragm with the required size;
the binder accounts for 10-30% of the inorganic nano powder by mass;
the plasticizer accounts for 1-10% of the inorganic nano powder by mass.
2. A method of making a ceramic diaphragm, comprising the steps of:
(1) adding a binder and a plasticizer into inorganic nano powder, and uniformly mixing under a heating condition to form slurry, wherein the inorganic nano powder is aluminum oxide (Al)2O3) Zirconium dioxide (ZrO)2) Titanium dioxide (TiO)2) Silicon dioxide (SiO)2) Barium sulfate (BaSO)4) The adhesive is polyamide, the plasticizer is lignosulfonate, and the heating condition is 150-200 ℃;
(2) filling the mixed slurry into a mold;
(3) the method comprises the following steps of (1) carrying out extrusion forming on mixed slurry in a die by setting the pressure and temperature of a punching machine, wherein the pressure is set to be 10-50 Mpa, and the temperature is set to be 150-200 ℃;
(4) cutting the punch-formed film into a specific size and polishing the surface of the film to obtain a ceramic diaphragm with a required size, wherein the MD and TD shrinkage of the ceramic diaphragm at 150 ℃ for 1 hour is 0%;
the binder accounts for 10-30% of the inorganic nano powder by mass;
the plasticizer accounts for 1-10% of the inorganic nano powder by mass.
3. The method of claim 2, wherein: the surface polishing needs to be carried out by grinding and polishing materials, wherein the grinding and polishing materials are SIC and B4C or diamond.
4. An electrochemical device, characterized in that: the ceramic separator according to claim 1 is used.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007095440A (en) * | 2005-09-28 | 2007-04-12 | Nippon Sheet Glass Co Ltd | Separator for electric storage device, and electric storage device |
| CN109037549A (en) * | 2018-06-28 | 2018-12-18 | 中国电力科学研究院有限公司 | A kind of preparation process of electrode-supported anodic aluminium oxide membrane |
| CN110379986A (en) * | 2019-07-11 | 2019-10-25 | 郭建中 | A kind of lithium-sulfur rechargeable battery new types of diaphragm material and preparation method |
| CN111477818A (en) * | 2020-04-24 | 2020-07-31 | 吉林大学 | Full-ceramic lithium ion battery diaphragm and preparation method thereof |
| CN111477819A (en) * | 2020-04-24 | 2020-07-31 | 吉林大学 | Full-ceramic diaphragm for lithium ion battery and preparation method thereof |
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- 2020-08-12 CN CN202010806327.3A patent/CN111952519B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007095440A (en) * | 2005-09-28 | 2007-04-12 | Nippon Sheet Glass Co Ltd | Separator for electric storage device, and electric storage device |
| CN109037549A (en) * | 2018-06-28 | 2018-12-18 | 中国电力科学研究院有限公司 | A kind of preparation process of electrode-supported anodic aluminium oxide membrane |
| CN110379986A (en) * | 2019-07-11 | 2019-10-25 | 郭建中 | A kind of lithium-sulfur rechargeable battery new types of diaphragm material and preparation method |
| CN111477818A (en) * | 2020-04-24 | 2020-07-31 | 吉林大学 | Full-ceramic lithium ion battery diaphragm and preparation method thereof |
| CN111477819A (en) * | 2020-04-24 | 2020-07-31 | 吉林大学 | Full-ceramic diaphragm for lithium ion battery and preparation method thereof |
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