CN113363666B - Preparation method of diaphragm, diaphragm and electrochemical device applying diaphragm - Google Patents
Preparation method of diaphragm, diaphragm and electrochemical device applying diaphragm Download PDFInfo
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- CN113363666B CN113363666B CN202110649648.1A CN202110649648A CN113363666B CN 113363666 B CN113363666 B CN 113363666B CN 202110649648 A CN202110649648 A CN 202110649648A CN 113363666 B CN113363666 B CN 113363666B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- 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
- 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
- H01M50/431—Inorganic 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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/443—Particulate 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
- H01M50/46—Separators, membranes or diaphragms characterised by their combination with electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
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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 discloses a preparation method of a diaphragm, the diaphragm and an electrochemical device using the diaphragm, wherein the method comprises the following steps: the method comprises the following steps: uniformly mixing inorganic particles, adhesive particles and a solvent to form a uniform mixed solution, wherein the adhesive particles are dissolved in the solvent; step two: drying the mixed solution to obtain particles coated with the adhesive; step three: and uniformly spreading the particles on the surface of the pole piece, heating the pole piece, and rolling by a hot roller to obtain the diaphragm. The invention also discloses an electrochemical device consisting of the cathode, the anode, the electrolyte and the diaphragm. Compared with the prior art, the preparation method has the advantages that the preparation process is simple, the preparation cost is low, the prepared diaphragm is thin, the energy density of the lithium ion battery can be greatly improved, in addition, the prepared diaphragm is in closer contact with a pole piece interface, the infiltration and the diffusion of electrolyte are facilitated, meanwhile, the transmission path of lithium ions is shortened, and the performance of the obtained lithium ion battery is better.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to a diaphragm preparation method, a diaphragm and an electrochemical device using the diaphragm.
Background
The country in 2021 clearly proposes specific targets for carbon peaking and carbon neutralization, and 65% of the global economy body also publishes a specific plan for carbon neutralization in own country. The lithium ion battery is used as a new energy carrier and plays an important role in reducing carbon emission.
From the nineties, significant progress has been made in battery technology, and each technology has entered a plateau, but the energy density and cost of batteries are still key factors that restrict their development. The diaphragm which is one of the main components of the battery is always a key component of the battery, the cost of the diaphragm accounts for about 20% of the cost of the battery cell, and meanwhile, because the diaphragm does not participate in the electrochemical reaction, but occupies the internal space volume of the battery, the thickness of the diaphragm directly influences the energy density of the battery, while the existing diaphragm preparation method has high manufacturing cost, approaches the limit to the reduction of the thickness and is difficult to meet the performance requirement of the market on the battery.
Disclosure of Invention
The invention aims to provide a preparation method of a diaphragm, the diaphragm and an electrochemical device applying the diaphragm, which can reduce the manufacturing cost and manufacture the diaphragm with thinner thickness, thereby improving the energy density of a battery and leading the performance of the battery to be better.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a preparation method of a diaphragm, which comprises the following steps:
the method comprises the following steps: uniformly mixing inorganic particles, adhesive particles and a solvent to form a uniform mixed solution, wherein the adhesive particles are dissolved in the solvent;
step two: drying the mixed solution to obtain particles coated with the adhesive;
step three: and uniformly paving the particles on the surface of a pole piece, heating the pole piece, and rolling by a hot roller to obtain the diaphragm.
The pole piece comprises a positive pole piece and a negative pole piece, wherein the active substance of the positive pole piece comprises but is not limited to one or a combination of two or more of lithium cobaltate, lithium manganate, lithium nickel cobalt manganese oxide and lithium iron phosphate, and the active substance of the negative pole piece comprises but is not limited to one or a combination of two or more of artificial graphite, silicon material, silicon carbon material and silicon protoxide material; the feeding sequence of the inorganic particles, the binder particles and the solvent is not limited during mixing; and finally, tightly bonding the diaphragm and the pole piece together to form a whole, thereby forming the composite diaphragm pole piece.
Further, in the first step, the inorganic particles are added into the container, and a solution formed by dissolving the binder particles in the solvent is slowly and uniformly sprayed while stirring. Therefore, the inorganic particles can be fully coated by the adhesive particles, the adhesive property of the inorganic particles is improved, and the inorganic particles can be tightly adhered to the pole piece after rolling; wherein the vessel for mixing comprises one of a stirred tank, a beaker, a double cone mixer, and a high speed particulate mixer.
Further, in the step one, the inorganic particles comprise one or a combination of more than two of silicon dioxide, aluminum oxide, boehmite, titanium dioxide, magnesium dioxide, barium sulfate and molybdenum disulfide;
the adhesive particles comprise one or the combination of more than two of polyolefin, polyacrylate, polybutylene-styrene block copolymer, polyisobutylene-styrene block copolymer, polybutylene terephthalate, polyvinylidene fluoride and hexafluoropropylene copolymer, and are used for adhering the inorganic particles and the pole pieces;
the solvent comprises one or a combination of more than two of alkane, cycloalkane, benzene homologue, ketone and ester, wherein the alkane comprises at least one of pentane, hexane, heptane or octane, the cycloalkane comprises at least one of cyclopentane, cyclohexane, cycloheptane or cyclooctane, the benzene homologue comprises at least one of benzene, toluene or xylene, the ketone comprises at least one of acetone or butanone, and the ester comprises at least one of methyl acetate or ethyl acetate, and is used for dissolving the adhesive particles.
Further, in the first step, the adhesive particles account for 1-15% of the microparticles by weight; the inorganic particles account for 85 to 99 percent of the weight of the particles; the solid content of the mixed solution is 5-50 wt%. The diaphragm prepared according to the weight percentage has the advantages of good cohesiveness and wettability and small internal resistance.
Further, in the second step, the drying temperature of the mixed solution is 80-90 ℃. Too high messenger of drying temperature the particle melting influences the even tiling of particle extremely the pole piece surface, the temperature is crossed lowly and is made liquid in the mixed liquid can not fully volatilize and lead to liquid to remain, can influence equally the even tiling of particle extremely the pole piece surface, consequently establishes drying temperature to above-mentioned scope, guarantees when guaranteeing the particle can not be molten liquid in the mixed liquid volatilizees completely.
Further, in the third step, the temperature for heating the pole piece is 80-110 ℃, the temperature of the hot roller is 70-140 ℃, and the rolling pressure is 500-2000 kgf.
The pole piece with the surface uniformly and flatly paved with the particles is heated, so that the particles are softened, and the particles are more easily extruded with each other during rolling to form a compact diaphragm; by using the hot roller, the extensibility of the pole piece can be enhanced, so that the extension of the pole piece is consistent with that of the diaphragm, and the problem of wrinkles caused by different extensibility of the pole piece and the diaphragm is avoided; when the rolling setting is within the above range, the particles can be well rolled into a dense diaphragm.
Furthermore, the heating mode of the pole piece is non-contact heating, and the non-contact heating mode comprises at least one of electromagnetic heating and infrared light heating. Through non-contact heating, the heating device can not contact the particles, the particles can be softened due to heating, and if contact heating is used, the softened particles can be adhered to the heating device, so that the particles are unevenly distributed on the pole piece, and the performance of the diaphragm is influenced.
The invention also discloses a diaphragm prepared by the preparation method of the diaphragm in any one of the schemes.
Further, the thickness of the diaphragm is 1-20 μm, the porosity is 30% -90%, the air permeability is 10-300S/100 cc, and the tortuosity is 1-10%.
In addition, the present invention also discloses an electrochemical device comprising: a positive electrode, a negative electrode, an electrolyte, and the separator of any of the above aspects, the separator being positioned between the positive electrode and the negative electrode.
Compared with the prior art, the invention at least comprises the following beneficial effects: the preparation method disclosed by the invention is simple in preparation process and low in preparation cost, the prepared diaphragm is thin, the energy density of the lithium ion battery can be greatly improved, in addition, the prepared diaphragm is in closer contact with a pole piece interface, the infiltration and the diffusion of electrolyte are facilitated, meanwhile, the transmission path of lithium ions is shortened, and the performance of the obtained lithium ion battery is better.
Drawings
FIG. 1 is a flow chart of a method of making a separator of the present invention;
FIG. 2 is a view of the surface structure of the separator of the present invention;
FIG. 3 is a schematic structural view of a composite separator plate of the present invention;
in the figure: 1-a separator; 2-pole piece; 201-an active substance; 202-current collector.
Detailed Description
The present invention will be further described below with reference to the accompanying drawings for easier understanding, but the present invention can be implemented in various forms, and is not limited to the embodiments described herein and does not constitute any limitation to the present invention.
As shown in fig. 1, this embodiment provides a method for preparing a separator, including the following steps:
the method comprises the following steps: uniformly mixing inorganic particles, adhesive particles and a solvent to form a uniform mixed solution, wherein the adhesive particles are dissolved in the solvent;
step two: drying the mixed solution to obtain particles coated with the adhesive;
step three: and uniformly paving the particles on the surface of the pole piece 2, heating the pole piece 2, and rolling by a hot roller to obtain the diaphragm 1.
The pole piece 2 comprises a positive pole piece and a negative pole piece, the active material 201 of the positive pole piece comprises but is not limited to one or the combination of more than two of lithium cobaltate, lithium manganate, lithium nickel cobalt manganese and lithium iron phosphate, and the active material 201 of the negative pole piece comprises but is not limited to one or the combination of more than two of artificial graphite, silicon material, silicon carbon material and silicon protoxide material; the inorganic particles, the binder particles and the solvent are mixed in an unlimited feeding sequence; and finally, the obtained diaphragm 1 and the pole piece 2 are mutually and tightly bonded together to form a whole, so that the composite diaphragm pole piece is formed.
Specifically, in the first step, the inorganic particles are added into the container, and a solution is slowly and uniformly sprayed while stirring, wherein the solution is formed by dissolving the binder particles in the solvent. Therefore, the inorganic particles can be fully coated by the adhesive particles, the adhesive property of the inorganic particles is improved, and the inorganic particles can be tightly adhered to the pole piece 2 after rolling; wherein the vessel for mixing comprises one of a stirred tank, a beaker, a double cone mixer, and a high speed particulate mixer.
Specifically, in the first step, the inorganic particles include one or a combination of two or more of silicon dioxide, aluminum oxide, boehmite, titanium dioxide, magnesium dioxide, barium sulfate and molybdenum disulfide;
the adhesive particles comprise one or the combination of more than two of polyolefin, polyacrylate, polybutylene-styrene block copolymer, polyisobutylene-styrene block copolymer, polybutylene terephthalate, polyvinylidene fluoride and hexafluoropropylene copolymer, and are used for adhering the inorganic particles and the pole piece 2;
the solvent comprises one or a combination of more than two of alkane, cycloalkane, benzene homologue, ketone and ester, wherein the alkane comprises at least one of pentane, hexane, heptane or octane, the cycloalkane comprises at least one of cyclopentane, cyclohexane, cycloheptane or cyclooctane, the benzene homologue comprises at least one of benzene, toluene or xylene, the ketone comprises at least one of acetone or butanone, and the ester comprises at least one of methyl acetate or ethyl acetate, and is used for dissolving the adhesive particles.
Specifically, in the first step, the adhesive particles account for 1-15% of the microparticles by weight; the inorganic particles account for 85 to 99 percent of the weight of the particles; the solid content of the mixed solution is 5-50 wt%. The diaphragm 1 prepared according to the weight percentage has the advantages of good cohesiveness and wettability and small internal resistance.
Specifically, in the second step, the drying temperature of the mixed solution is 80 ℃ to 90 ℃. Too high messenger of drying temperature the particle melting influences the particle evenly tile extremely 2 surfaces of pole piece, the temperature is crossed lowly and is made liquid in the mixed liquid can not fully volatilize and lead to liquid to remain, can influence equally the particle evenly tile extremely 2 surfaces of pole piece, consequently establish drying temperature to above-mentioned scope, guarantee when the particle can not be molten guarantee liquid in the mixed liquid volatilizees completely.
Specifically, in the third step, the temperature for heating the pole piece is 80-110 ℃, the temperature of the hot roller is 70-140 ℃, and the rolling pressure is 500-2000 kgf.
Wherein, the pole piece 2 with the particles evenly and flatly paved on the surface is heated to soften the particles, so that the particles are more easily extruded with each other during rolling to form the compact diaphragm 1; by using the hot roller, the extensibility of the pole piece 2 can be enhanced, so that the extensibility of the pole piece 2 is consistent with the extensibility of the diaphragm 1, and the problem of wrinkles caused by different extensibility of the pole piece 2 and the diaphragm 1 is avoided; setting the roll pressure within the above range enables the fine particles to be rolled into the dense diaphragm 1 well.
Specifically, the heating mode of the pole piece 2 is non-contact heating, and the heating mode includes at least one of electromagnetic heating and infrared light heating. By non-contact heating, the heating device does not contact the particles, the particles are softened due to heating, and if the contact heating is used, the softened particles are adhered to the heating device, so that the particles are unevenly distributed on the pole piece 2, and the performance of the diaphragm is affected.
As shown in fig. 2, this example also provides a separator, which is prepared by the method for preparing the separator 1 according to any one of the above embodiments.
Specifically, the thickness of the diaphragm 1 is 1-20 μm, the porosity is 30-90%, the air permeability is 10-300S/100 cc, and the tortuosity is 1-10%.
In addition, the present embodiment also provides an electrochemical device including: a positive electrode, a negative electrode, an electrolyte, and the separator 1 of any of the above aspects, the separator 1 being located between the positive electrode and the negative electrode.
Compared with the prior art, the invention at least comprises the following beneficial effects: the preparation method is simple in preparation process and low in preparation cost, the prepared diaphragm 1 is thin, the energy density of the lithium ion battery can be greatly improved, in addition, the prepared diaphragm 1 and the pole piece 2 are in closer interface contact, the infiltration and the diffusion of electrolyte are facilitated, meanwhile, the transmission path of lithium ions is shortened, and the performance of the obtained lithium ion battery is better.
The present invention will be specifically described below with reference to examples and comparative examples.
Example 1
Uniformly mixing inorganic particles and adhesive particles with a solvent according to the mixture ratio of 85% and 15% respectively by mass fraction to form a uniform mixed solution;
drying the obtained mixed solution at the temperature of 80-90 ℃ to obtain particles coated with the binder particles;
uniformly coating the obtained particles on a negative plate through an extruder to obtain the negative plate of the composite diaphragm 1;
preheating the pole piece by passing through an oven at 80-100 ℃ at the speed of 2m/min, and then rolling the negative pole piece of the composite diaphragm 1 at the temperature of 80-90 ℃ and under the pressure of 500kgf to obtain a diaphragm 1 with the thickness of 3 microns;
and rolling and splitting the rolled pole pieces to obtain the negative pole piece of the composite diaphragm 1, assembling the negative pole piece and the positive pole piece into a battery cell, and carrying out performance test.
Example 2
Different from the embodiment 1, in this embodiment, the inorganic particles and the adhesive particles are uniformly mixed with the solvent according to the mixture ratio of 90% and 10% by mass respectively to form a uniform mixed solution; the rest of the procedure was the same as in example 1.
Example 3
Different from the embodiment 1, in this embodiment, the inorganic particles and the adhesive particles are uniformly mixed with the solvent according to the mixture ratio of 95% and 5% by mass respectively to form a uniform mixed solution; the remaining procedure was the same as in example 1.
Example 4
Different from the embodiment 1, in this embodiment, the inorganic particles and the adhesive particles are uniformly mixed with the solvent according to the mixture ratio of 99% and 1% by mass respectively to form a uniform mixed solution; the rest of the procedure was the same as in example 1.
Comparative example 1
A PE diaphragm 1 with the thickness of 8 mu m and positive and negative pole pieces are wound or laminated to assemble a battery cell, and performance test is carried out.
The testing method of the membrane wettability comprises the following steps: the method is carried out by referring to a diaphragm national standard GB/T36363-2018, and specifically comprises the following steps: and (3) dropping a fixed amount (1 mu L) of electrolyte at a fixed height (conventionally 20cm), and recording the maximum diffusion distance d of the electrolyte after 1min, namely the wettability of the diaphragm.
The testing method of the membrane adhesiveness comprises the following steps: and (3) winding or laminating the obtained diaphragm 1 and the pole piece 2 to assemble the battery cell, and testing the capacity, the internal resistance and the cycle performance of the battery cell.
Specific performance indexes of the tests of examples 1-4 and comparative example 1 are shown in table 1:
TABLE 1
As can be seen from comparison among examples 1 to 4, the more the inorganic particles are, the better the wettability is; the more the binder particles, the better the binding force and the larger the internal resistance; when the binder particle content is less than 5%, the adhesion is remarkably deteriorated and the internal resistance is also increased. Compared with the diaphragm 1 obtained in the comparative example 1, the electric performance of the diaphragm 1 obtained in the embodiments 1-4 meets the requirement of the battery cell, wherein the inorganic particles account for 95% of the formula, and the performance of the diaphragm 1 is better than that of the diaphragm 1 in the comparative example 1.
To sum up: the thickness of the diaphragm 1 produced by the embodiment is less than or equal to 3 mu m, and the cost is reduced by about 50 percent compared with the diaphragm produced by the prior art. The diaphragm 1 and the battery cell prepared by the method have very outstanding advantages.
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. It will be apparent to those skilled in the art from this disclosure that many more simple derivations or substitutions can be made without departing from the inventive concepts herein.
Claims (7)
1. A method for preparing a separator, comprising the steps of:
the method comprises the following steps: uniformly mixing inorganic particles, adhesive particles and a solvent to form a uniform mixed solution, wherein the adhesive particles are dissolved in the solvent, and the solid content of the mixed solution is 5-50 wt%;
step two: drying the mixed solution to obtain particles coated with the adhesive, wherein the drying temperature of the mixed solution is 80-90 ℃, the adhesive particles account for 1-15 wt% of the particles, and the inorganic particles account for 85-99 wt% of the particles;
step three: and uniformly paving the particles on the surface of a pole piece, heating the pole piece, and rolling by using a hot roller to obtain the diaphragm, wherein the temperature for heating the pole piece is 80-110 ℃, the temperature of the hot roller is 70-140 ℃, and the rolling pressure is 500-2000 kgf.
2. The method for preparing a separator according to claim 1, wherein in the first step, the inorganic particles are added to a container, and a solution in which the binder particles are dissolved in the solvent is slowly and uniformly sprayed while stirring.
3. The method for manufacturing a separator according to claim 1, wherein in step one, the inorganic particles include one or a combination of two or more of silica, alumina, boehmite, titanium dioxide, magnesium dioxide, barium sulfate, and molybdenum disulfide;
the adhesive particles comprise one or the combination of more than two of polyolefin, polyacrylate, polybutylene styrene block copolymer, polyisobutylene-styrene block copolymer, polybutylene terephthalate, polyvinylidene fluoride and hexafluoropropylene copolymer;
the solvent comprises one or the combination of more than two of alkane, cyclane, benzene homologues, ketone and ester.
4. The method for preparing the separator according to claim 1, wherein the pole piece is heated by non-contact heating including at least one of electromagnetic heating and infrared heating.
5. A separator produced by the method for producing the separator according to any one of claims 1 to 4.
6. The separator according to claim 5, wherein the separator has a thickness of 1 to 20 μm, a porosity of 30 to 90%, an air permeability of 10 to 300S/100cc, and a tortuosity of 1 to 10%.
7. An electrochemical device, comprising: a positive electrode, a negative electrode, an electrolyte, and the separator according to any one of claims 5 to 6, the separator being located between the positive electrode and the negative electrode.
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