CN112563669A - High-wettability diaphragm and preparation method thereof - Google Patents
High-wettability diaphragm and preparation method thereof Download PDFInfo
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- CN112563669A CN112563669A CN201910914402.5A CN201910914402A CN112563669A CN 112563669 A CN112563669 A CN 112563669A CN 201910914402 A CN201910914402 A CN 201910914402A CN 112563669 A CN112563669 A CN 112563669A
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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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- 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 a high-wettability diaphragm and a preparation method thereof.A mixed slurry coating containing inorganic ceramic and cellulose acetate is arranged on at least one side of a diaphragm base film of a lithium ion battery. The application utilizes the excellent liquid permeability and the adsorptivity of the cellulose acetate to enable the coating diaphragm to adsorb more electrolyte, thereby achieving the purpose of improving the wettability of the coating diaphragm and further improving the electrochemical performance of the battery.
Description
Technical Field
The invention relates to the technical field of diaphragm production, in particular to a high-wettability diaphragm and a preparation method thereof.
Background
With the continuous deterioration of ecological environment, human beings are gradually aware of the importance of environmental protection and develop various new green clean energy sources to improve our living environment. Among various new energy sources, lithium ion batteries are widely used in the fields of portable electronic devices, new energy vehicles and the like due to the advantages of high power, high energy density, high working voltage, wide working temperature range, long cycle life, low self-discharge rate, no memory effect, no pollution and the like.
The separator, one of the key materials in the lithium ion battery, plays an indispensable role in the operation of the lithium ion battery. The diaphragm isolates the direct contact of the positive pole and the negative pole in the lithium ion battery to cause the short circuit of the battery, and isolates electrons at the same time, and only allows lithium ions to pass through the diaphragm to move to and from the positive pole and the negative pole. The performance of the separator directly affects the performance of the lithium ion battery. The traditional single-layer polyolefin diaphragm has difficulty in meeting the performance requirements of the battery, so that the inorganic ceramic coating diaphragm is developed to improve the thermal stability and puncture strength of the diaphragm, thereby improving the working temperature of the battery and improving the safety performance of the battery. However, the inorganic ceramic coating diaphragm has a low liquid absorption rate, and cannot allow more lithium ions to come and go between the positive electrode and the negative electrode, so that the full specific capacity of the material cannot be exerted.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-wettability diaphragm and a preparation method thereof. The defect that the wettability of the existing inorganic ceramic coating diaphragm is poor can be improved, and the scheme that inorganic ceramic and acetate fiber mixed slurry is coated on the surface of the base film is provided, so that the wettability of the inorganic ceramic coating diaphragm is improved, and the electrochemical performance of the battery is improved.
The purpose of the invention is realized by the following technical scheme:
a high-wettability diaphragm is characterized in that at least one side of a diaphragm base film of a lithium ion battery is coated with a mixed slurry layer containing inorganic ceramic and cellulose acetate. The coating diaphragm absorbs more electrolyte by utilizing the excellent liquid permeability and adsorbability of the cellulose acetate, so that the purpose of improving the wettability of the coating diaphragm is achieved, and the electrochemical performance of the battery is further improved.
The base film is at least one of a polyethylene film, a polypropylene-polyethylene-polypropylene composite film, an aramid film and a polyamide film.
The thickness of the base film is 5-60 micrometers, the porosity is 10-60%, and the pore diameter is 0.01-0.5 micrometers.
The thickness of the diaphragm coating is 1-10 microns.
The inorganic ceramic and cellulose acetate mixed slurry layer comprises the following components in parts by mass:
deionized water: 40 to 60 parts by mass of a stabilizer,
inorganic ceramic powder: 20 to 50 parts by mass of a water-soluble polymer,
cellulose acetate: 5 to 30 parts by mass of a stabilizer,
adhesive agent: 2 to 10 parts by mass of a stabilizer,
auxiliary agent: 5 to 20 parts by mass.
The inorganic ceramic powder is at least one of aluminum oxide, silicon oxide, titanium oxide, calcium oxide, magnesium oxide and boehmite.
The particle size of the inorganic ceramic powder particles is 0.01-10 microns.
The cellulose acetate is 0.05-5 microns in length and 0.05-2 microns in diameter.
The melting point of the cellulose acetate is 230-300 ℃.
The adhesive is at least one of acrylic acid, methacrylic acid, acrylate and methacrylate.
The adhesive is at least one of polymers obtained by copolymerizing at least one of acrylic acid, methacrylic acid, acrylate and methacrylate with olefin or ester.
The auxiliary agent is at least one of sodium polyacrylate, polyoxyethylene, polyvinyl alcohol, methyl cellulose, hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyether organic silicon copolymer and polyoxyethylene alkanolamide.
A preparation method of a high-wettability diaphragm comprises the following specific steps:
firstly), preparing mixed slurry of inorganic ceramic and cellulose acetate;
secondly), providing a base film, and coating the base film on at least one surface in the step one);
thirdly), placing the coating film obtained in the second step in a drying oven for drying; to obtain a high wettability membrane.
The first step) comprises the following steps:
1-1) mixing inorganic ceramic powder, cellulose acetate and deionized water according to a preset proportion, uniformly stirring and then uniformly grinding to obtain inorganic powder slurry;
1-2) adding an auxiliary agent into the inorganic powder slurry obtained in the step 1-1), uniformly mixing, adding a binder, and uniformly mixing again to obtain inorganic ceramic and cellulose acetate mixed slurry;
the second step) comprises the following steps:
2-1) coating the mixed slurry of the inorganic ceramic and the cellulose acetate obtained in the step one) on at least one surface of a base film to obtain a mixed coating of the inorganic ceramic and the cellulose acetate;
2-2) the coating method used in the step 2-1) is at least one of a blade coating method, a meyer rod coating method, a reverse roll coating method, a gravure roll coating method, a dip coating method and a brush coating method.
And (3) placing the coating film obtained in the step three) at a drying temperature of 30-60 ℃ for 20-120S to obtain the diaphragm for the lithium ion battery.
Compared with the prior art, the invention has the beneficial effects that:
(1) the prepared slurry has good stability and is not easy to lose efficacy after being placed for a long time;
(2) the coating on the surface of the coating film is uniformly dispersed;
(3) the separator maintains good thermal stability while increasing the wettability of the separator;
(4) the electrochemical performance of the battery is improved;
(5) the manufacturing cost is saved.
Detailed Description
The following provides a specific embodiment of a high-wettability separator and a method for producing the same.
Example 1:
a: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 7 parts by mass of cellulose acetate powder and 35 parts by mass of alumina powder into 50 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic mixed slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the prepared inorganic ceramic and cellulose acetate mixed slurry on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven for drying for 100s to obtain the lithium ion battery mixed coating membrane.
Example 2:
a: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 8 parts by mass of cellulose acetate powder and 33 parts by mass of alumina powder into 51 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic mixed slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the prepared inorganic ceramic and cellulose acetate mixed slurry on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven for drying for 110s to obtain the lithium ion battery mixed coating membrane.
Example 3
A: preparing inorganic ceramic mixed slurry: adding 3 parts by mass of a dispersing auxiliary agent, 8 parts by mass of cellulose acetate powder and 33 parts by mass of alumina powder into 52 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of a thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of an adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain a water-based ceramic mixed slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the prepared inorganic ceramic and cellulose acetate mixed slurry on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven for drying for 110s to obtain the lithium ion battery mixed coating membrane.
Example 4
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 8 parts by mass of cellulose acetate powder and 33 parts by mass of alumina powder into 51 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic mixed slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: and immersing the lithium ion battery base membrane into the mixed slurry of the inorganic ceramic and the cellulose acetate, keeping for 5min to obtain a double-sided coating membrane, and then placing the membrane in a 50 ℃ drying oven to dry for 120s to obtain the lithium ion battery mixed coating membrane.
Example 5
Preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 7 parts by mass of cellulose acetate powder and 35 parts by mass of boehmite powder into 50 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic mixed slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the prepared inorganic ceramic and cellulose acetate mixed slurry on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven for drying for 100s to obtain the lithium ion battery mixed coating membrane.
Example 6
Preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 7 parts by mass of cellulose acetate powder and 35 parts by mass of boehmite powder into 50 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic mixed slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: and immersing the lithium ion battery base membrane into the mixed slurry of the inorganic ceramic and the cellulose acetate, keeping for 5min to obtain a double-sided coating membrane, and then placing the membrane in a 50 ℃ drying oven to dry for 120s to obtain the lithium ion battery mixed coating membrane.
Comparative example 1
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent and 35 parts by mass of alumina powder into 57 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the prepared inorganic ceramic slurry on one side of a lithium ion battery base membrane on a small-sized coating machine, and then drying the membrane in a 50 ℃ drying oven for 100s to obtain the lithium ion battery ceramic coating membrane.
Comparative example 2
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 7 parts by mass of cellulose nitrate and 33 parts by mass of alumina powder into 52 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the mixed slurry of inorganic ceramic and cellulose nitrate on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven to be dried for 120s to obtain the lithium ion battery ceramic coating membrane.
Comparative example 3
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing type auxiliary agent, 7 parts by mass of ethyl cellulose and 32 parts by mass of alumina powder into 53 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the mixed slurry of inorganic ceramic and ethyl cellulose on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing a diaphragm in a 50 ℃ drying oven for drying for 120s to obtain the lithium ion battery mixed ceramic coating diaphragm.
Comparative example 4
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of a dispersing auxiliary agent, 7 parts by mass of lignocellulose and 32 parts by mass of boehmite powder into 53 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of a thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of an adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain a water-based ceramic slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the mixed slurry of the ceramic and the lignocellulose on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven for drying for 120s to obtain the lithium ion battery ceramic coating membrane.
Comparative example 5
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of a dispersing auxiliary agent, 7 parts by mass of microcrystalline cellulose and 32 parts by mass of boehmite powder into 53 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of a thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of an adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain a water-based ceramic slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the mixed slurry of the ceramic and the microcrystalline cellulose on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing a diaphragm in a 50 ℃ drying oven for drying for 120s to obtain the lithium ion battery ceramic coating diaphragm.
Comparative example 6
A: preparing inorganic ceramic mixed slurry: adding 4 parts by mass of dispersing auxiliary agent, 7 parts by mass of hydroxypropyl cellulose and 32 parts by mass of boehmite powder into 53 parts by mass of deionized water, uniformly stirring, grinding and uniformly dispersing, then adding 2 parts by mass of thickening wetting auxiliary agent aqueous solution, continuously uniformly stirring, and finally adding 2 parts by mass of adhesive, and continuously stirring until the mixture is completely and uniformly mixed to obtain water-based ceramic slurry;
b: the preparation process of the lithium ion battery mixed coating diaphragm comprises the following steps: coating the mixed slurry of the ceramic and the hydroxypropyl cellulose on one side of a lithium ion battery base membrane on a small-sized coating machine, and then placing the membrane in a 50 ℃ drying oven for drying for 120s to obtain the lithium ion battery ceramic coating membrane.
Test examples 1 to 6
And (3) wettability testing: mu.L of the electrolyte was dropped on the surface of the mixed coating separator prepared in test examples one to six, respectively, and the diameter lengths in the MD and TD directions were recorded just after dropping the electrolyte on the surface of the separator, and the diameter lengths in the MD and TD directions were measured again after 5 minutes, and the extension lengths of the electrolyte in the MD and TD directions of the surface of the separator ((length after wetting-length before wetting)/2) were calculated, respectively.
Electrochemical testing: prepared with LiCoO using electrolyte membrane or electrolyte2As a positive electrode material, a separator, and LiPF61.0mol/L organic solvent of EC/DEC/DMC 1/1/1 as electrolyte, lithium sheet as negative electrode material, CR2032 half cell prepared at 25 deg.C for the following test
1) Charging at 0.2C, and cutting off voltage 4.2V; 2) charging at constant voltage for 4.2V, and cutting off current for 0.05C; 3) discharge at 0.2C, cut-off voltage 3V; repeating the steps 1) to 3), and recording the specific capacity after 300 cycles and the corresponding capacity retention rate.
Comparative test examples 1 to 6
The wettability and electrochemical properties of the electrolyte were tested according to the methods of test examples one to six.
The test results were as follows:
electrochemical performance test
Cellulose acetate has superior liquid permeability and adsorptivity compared with other celluloses. After the mixed slurry of the cellulose acetate and the ceramic is coated on the surface of the lithium battery diaphragm, the diffusion length of electrolyte is longer than that of other mixed slurry of the cellulose and the ceramic when the electrolyte is dripped into the coating, so that the diaphragm can be wetted by the electrolyte, and the wettability of the diaphragm is improved.
The comparative test results show that: the high-wettability diaphragm provided by the invention can improve the wettability of the diaphragm to a certain extent, and the electrochemical performance is improved. The diaphragm not only can improve the wettability of the diaphragm and improve the electrochemical performance, but also can save the manufacturing cost because the cellulose acetate contained in the diaphragm coating is rich in the natural world.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations should also be regarded as being within the protection scope of the present invention.
Claims (15)
1. The high-wettability diaphragm is characterized in that at least one side of a diaphragm base film of a lithium ion battery is coated with a mixed slurry layer containing inorganic ceramic and cellulose acetate.
2. The high-wettability membrane according to claim 1, wherein the base film is at least one of a polyethylene film, a polypropylene-polyethylene-polypropylene composite film, an aramid film and a polyamide film.
3. The high-wettability membrane as claimed in claim 1, wherein the thickness of the membrane coating is 1 to 10 μm.
4. The high-wettability membrane as claimed in claim 1, wherein the mixed slurry layer of the inorganic ceramic and the cellulose acetate comprises the following components in parts by mass:
deionized water: 40 to 60 parts by mass of a stabilizer,
inorganic ceramic powder: 20 to 50 parts by mass of a water-soluble polymer,
cellulose acetate: 5 to 30 parts by mass of a stabilizer,
adhesive agent: 2 to 10 parts by mass of a stabilizer,
auxiliary agent: 5 to 20 parts by mass.
5. The high-wettability separator according to claim 4, wherein the inorganic ceramic powder is at least one of alumina, silica, titania, calcium oxide, magnesium oxide, and boehmite.
6. The high-wettability membrane as claimed in claim 4, wherein the particle size of the inorganic ceramic powder particles is 0.01 to 10 μm.
7. The high-wettability membrane according to claim 4, wherein the cellulose acetate has a length of 0.05 to 5 μm and a diameter of 0.05 to 2 μm.
8. The high-wettability membrane according to claim 4, wherein the melting point of the cellulose acetate is 230 to 300 ℃.
9. The high-wettability membrane according to claim 4, wherein the adhesive is at least one of acrylic acid, methacrylic acid, acrylate and methacrylate.
10. The high-wettability membrane according to claim 4, wherein the binder is at least one of polymers obtained by copolymerizing at least one of acrylic acid, methacrylic acid, acrylic esters and methacrylic esters with olefins or esters.
11. The high-wettability membrane according to claim 4, wherein the auxiliary agent is at least one of sodium polyacrylate, polyethylene oxide, polyvinyl alcohol, methyl cellulose, hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyether silicone copolymer and polyoxyethylene alkanolamide.
12. The preparation method of the high-wettability diaphragm is characterized by comprising the following specific steps of:
firstly), preparing mixed slurry of inorganic ceramic and cellulose acetate;
secondly), providing a base film, and coating the base film on at least one surface in the step one);
thirdly), placing the coating film obtained in the second step in a drying oven for drying; to obtain a high wettability membrane.
13. The method as claimed in claim 12, wherein the step one) comprises the steps of:
1-1) mixing inorganic ceramic powder, cellulose acetate and deionized water according to a preset proportion, uniformly stirring and then uniformly grinding to obtain inorganic powder slurry;
1-2) adding an auxiliary agent into the inorganic powder slurry obtained in the step 1-1), uniformly mixing, then adding a binder, and uniformly mixing again to obtain the inorganic ceramic and cellulose acetate mixed slurry.
14. The method as claimed in claim 12, wherein the step two) comprises the steps of:
2-1) coating the mixed slurry of the inorganic ceramic and the cellulose acetate obtained in the step one) on at least one surface of a base film to obtain a mixed coating of the inorganic ceramic and the cellulose acetate;
2-2) the coating method used in the step 2-1) is at least one of a blade coating method, a meyer rod coating method, a reverse roll coating method, a gravure roll coating method, a dip coating method and a brush coating method.
15. The method for preparing the high-wettability membrane according to claim 12, wherein the coating film obtained in the step three) is dried at a drying temperature of 30-60 ℃ for 20-120S to obtain the membrane for the lithium ion battery.
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| CN115506180A (en) * | 2022-10-10 | 2022-12-23 | 浙江理工大学 | Preparation method of nano cellulose-based lithium ion battery diaphragm |
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