CN114243206A - Preparation method of lithium battery quick-charging diaphragm based on polymer semi-interpenetrating structure - Google Patents
Preparation method of lithium battery quick-charging diaphragm based on polymer semi-interpenetrating structure Download PDFInfo
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- CN114243206A CN114243206A CN202111376671.4A CN202111376671A CN114243206A CN 114243206 A CN114243206 A CN 114243206A CN 202111376671 A CN202111376671 A CN 202111376671A CN 114243206 A CN114243206 A CN 114243206A
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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
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
- H01M50/423—Polyamide resins
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Abstract
The invention discloses a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure, which comprises the steps of dispersing a prepolymer with functional groups, a linear macromolecule and a photoinitiator into a solvent to prepare a sol, coating the sol on the surface of a lithium battery diaphragm matrix, irradiating by ultraviolet light to finish curing, heating in an oven to evaporate the solvent in the modified diaphragm to form a modified diaphragm, combining the advantages of two polymers of thermoplastic polyurethane and polyurethane acrylate by using an ultraviolet curing technology to form a semi-interpenetrating network containing a polymer network structure and the linear macromolecule which are wound together, coating the semi-interpenetrating network on the diaphragm matrix, ensuring that the semi-interpenetrating network has higher adhesiveness with the diaphragm matrix and higher electrolyte retention rate, and greatly improving long-time circulation capacity attenuation rate when being applied to the lithium battery quick-charging technology, the preparation method has the advantages of mild preparation conditions, simple process, excellent liquid retention performance and good chemical stability.
Description
Technical Field
The invention relates to a preparation method of a lithium battery quick-charging diaphragm, in particular to a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure, and belongs to the application fields of new energy, lithium batteries and the like.
Background
In recent years, with the rapid development of portable electronic products and electric vehicles, higher requirements are put on the performance of lithium ion batteries, but the performance of rapid charging and discharging and short-time high-power output is poorer, so that the development of high-rate and rapid-charging lithium ion batteries is required. The diaphragm is one of the important components of the lithium ion battery, not only plays a role in isolating the positive and negative pole pieces in the battery and preventing the positive and negative poles from being in direct contact with each other to generate short circuit, but also provides a diffusion channel for the migration of lithium ions through a tortuous and through pore channel inside the diaphragm, so that the performance of the diaphragm influences the diffusion speed of the lithium ions, the retentivity of electrolyte, the internal resistance of a system, the interface of the battery and the like.
At present, a diaphragm in a lithium battery is usually a ceramic diaphragm, a layer of polyvinylidene fluoride (PVDF) covers the surface of the ceramic, and lithium analysis behaviors often occur in a high-rate charging process of the lithium battery using the diaphragm, and the reason is that electrolyte is consumed too fast in a quick charging process, so that the electrolyte content is insufficient in the later period to form lithium analysis. Therefore, there is an urgent need to develop a method for preparing a separator having mild preparation conditions, simple process, excellent liquid retention properties, and good chemical stability.
The thermoplastic polyurethane has extremely excellent swelling performance in the electrolyte, has high liquid retention rate when being sprayed on the diaphragm, but has weaker adhesion with ceramics, and the polyurethane acrylate has stronger viscosity, but has poorer swelling performance in the electrolyte and lower liquid retention rate. The advantages of the two polymers are combined by using an ultraviolet curing technology to form a polymer semi-interpenetrating structure and the polymer semi-interpenetrating structure is coated on the diaphragm, so that the polymer semi-interpenetrating structure has high adhesiveness with ceramic and high electrolyte retention rate, and when the polymer semi-interpenetrating structure is applied to a lithium battery quick-charging technology, the long-time circulating capacity attenuation rate is greatly improved. The preparation method has the advantages of mild preparation conditions, simple process, excellent liquid retention performance and good chemical stability.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure, which disperses a prepolymer with functional groups, a linear macromolecule and a photoinitiator into a solvent to prepare a sol, coats the sol on the surface of a lithium battery diaphragm matrix, irradiates with ultraviolet light to finish curing, heats and evaporates the solvent in the modified diaphragm in an oven to form a modified diaphragm, combines the advantages of two polymers of thermoplastic polyurethane and polyurethane acrylate by using an ultraviolet curing technology to form a semi-interpenetrating network containing a polymer network structure and the linear macromolecule which are wound together and coats the semi-interpenetrating network on the diaphragm matrix, so that the semi-interpenetrating network has higher adhesion with the diaphragm matrix and higher electrolyte liquid retention rate, and the long-time circulating capacity decay rate is greatly improved when the semi-interpenetrating network is applied to the lithium battery quick-charging technology, the preparation method has the advantages of mild preparation conditions, simple process, excellent liquid retention performance and good chemical stability.
In order to realize the technical effects, the following technical scheme is adopted:
a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure comprises the following steps:
step S1: dispersing the prepolymer with functional groups, linear macromolecules and a photoinitiator in a solvent according to a mass ratio to prepare uniform sol;
step S2: coating the sol prepared in the step S1 on the surface of a diaphragm substrate, and irradiating by using ultraviolet light to finish curing modification;
step S3: and heating the modified diaphragm solidified and modified in the step S2 in an oven to evaporate the solvent in the modified diaphragm to form the modified diaphragm.
Further, the prepolymer with functional groups in step S1 is urethane acrylate with a functionality of 2-4.
Further, in the step S1, the linear polymer is thermoplastic polyurethane with a molecular weight greater than 2 × 105。
Further, in the step S1, the photoinitiator is one or more of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl phenyl ketone, 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide, and 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-propanone; the solvent in the step S1 is one or more of ethanol, acetone, ethyl acetate, cyclohexane and n-hexane.
Further, in the step S1, the mass ratio of the prepolymer with functional groups in the sol is 15-25%, the content of linear polymers in the sol is 15-40%, and the mass of the photoinitiator in the sol is 0.01-0.2% of the mass of the prepolymer with functional groups.
Further, the dispersion mode of the sol prepared in the step S1 is stirring or ultrasonic; the method for coating the sol on the surface of the diaphragm substrate in the step S2 comprises one or more of spin coating, spray coating, roll coating and brush coating.
Further, in the step S2, the separator is a PP separator, a PE separator, or a PP/PE separator, and the substrate is aluminum oxide (Al)2O3) Or magnesium hydroxide (Mg (HO)2)。
Further, in the step S2, after the sol is coated, the ultraviolet light irradiation is rapidly carried out, the interval time between the two is less than 20S, and the ultraviolet light exposure of the sol is more than 1000mJ/cm2The ultraviolet light irradiation time is 5-30 s.
Further, the temperature of the solvent in the membrane after the heating evaporation modification in the oven in the step S3 is not more than 60 ℃.
An application method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure, which is applied to the field of lithium battery preparation by the lithium battery quick-charging diaphragm based on the polymer semi-interpenetrating structure prepared by any one of claims 1 to 9.
The invention has the beneficial effects that:
the invention discloses a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure, which comprises the steps of dispersing a prepolymer with functional groups, a linear macromolecule and a photoinitiator into a solvent to prepare a sol, coating the sol on the surface of a lithium battery diaphragm matrix, irradiating by using ultraviolet light to finish curing, heating in an oven to evaporate the solvent in the modified diaphragm to form a modified diaphragm, combining the advantages of thermoplastic polyurethane and polyurethane acrylate by using an ultraviolet light curing technology, and adopting the basic principle that the ultraviolet light curing reaction usually only needs a few seconds to realize the conversion from liquid state to solid state, the conversion of the prepolymer to a high polymer forms a semi-interpenetrating network containing a polymer network structure and the linear macromolecule which are wound together and is coated on the diaphragm matrix, so that the preparation method can have higher adhesiveness with the diaphragm matrix and also has higher electrolyte liquid retention rate, the quick-charging lithium battery diaphragm has simple process and excellent performance. The preparation method has the advantages of mild preparation conditions, simple process, excellent liquid retention performance and good chemical stability.
Drawings
FIG. 1 is a schematic diagram comparing a membrane containing a polymer semi-interpenetrating network of example 1 of the present invention with a conventional membrane;
FIG. 2 is a graph comparing the infrared spectra of the semi-interpenetrating network membrane containing polymer and the conventional membrane in the present invention;
FIG. 3 is a graph comparing the capacity retention of a battery after cycling with a conventional separator, in accordance with an embodiment of the present invention;
Detailed Description
The invention will be further described with reference to the accompanying drawings, without limiting the scope of the invention to the following:
example 1:
a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure comprises the following steps:
step S1: mixing polyurethane acrylate with functionality of 4, thermoplastic polyurethane and molecular weight of 2.5 x 105Dispersing a 2-hydroxy-2-methyl-1-phenyl acetone photoinitiator in an acetone solvent according to a mass ratio, and ultrasonically preparing into uniform sol;
the mass ratio of the prepolymer with functional groups in the sol is 15%, the linear polymer content in the sol is 15%, the mass of the photoinitiator in the sol is 0.01% of that of the prepolymer with functional groups, and the balance is solvent.
Step S2: coating the sol prepared in the step S1 on the surface of a PP/PE diaphragm alumina matrix by adopting a spin coating process, and irradiating by using ultraviolet light to finish curing modification; after the sol is coated, the ultraviolet irradiation is rapidly carried out, the interval between the two is 10s, and the ultraviolet exposure of the sol is 1500mJ/cm2The ultraviolet irradiation time was 20 seconds.
Step S3: and heating the modified diaphragm solidified and modified in the step S2 in an oven to evaporate the solvent in the modified diaphragm to form the modified diaphragm, wherein the temperature is 50 ℃.
And preparing the lithium battery quick-charging diaphragm 1 based on the polymer semi-interpenetrating structure according to the steps.
Example 2:
a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure comprises the following steps:
step S1: mixing polyurethane acrylate with 2 functionality, thermoplastic polyurethane and 3-10 molecular weight5Dispersing the 1-hydroxycyclohexyl phenyl ketone photoinitiator in a normal hexane solvent according to a mass ratio, and stirring to prepare uniform sol;
the mass ratio of the prepolymer with functional groups in the sol is 25%, the linear polymer content in the sol is 40%, the mass of the photoinitiator in the sol is 0.2% of that of the prepolymer with functional groups, and the balance is solvent.
Step S2: coating the sol prepared in the step S1 on the surface of the PP membrane magnesium hydroxide matrix by adopting a spraying process, and irradiating by using ultraviolet light to finish curing modification; after the sol is coated, the sol is quickly irradiated by ultraviolet light, the interval between the sol and the sol is 15s, and the ultraviolet light exposure of the sol is 1800mJ/cm2The ultraviolet irradiation time was 30 seconds.
Step S3: and heating the modified diaphragm solidified and modified in the step S2 in an oven to evaporate the solvent in the modified diaphragm to form the modified diaphragm, wherein the temperature is 55 ℃.
And preparing the lithium battery quick-charging diaphragm 2 based on the polymer semi-interpenetrating structure according to the steps.
Example 3:
a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure comprises the following steps:
step S1: mixing polyurethane acrylate with functionality of 3, thermoplastic polyurethane and molecular weight of 3 x 105Dispersing 2, 4, 6-trimethylbenzoyl-diphenylphosphine oxide photoinitiator in ethyl acetate solvent according to mass ratio, and stirring to prepare uniform sol;
the mass percentage of the prepolymer with functional groups in the sol is 20%, the linear polymer content in the sol is 30%, the mass of the photoinitiator in the sol is 0.1% of that of the prepolymer with functional groups, and the balance is solvent.
Step S2: coating the sol prepared in the step S1 on the surface of the PE diaphragm magnesium hydroxide matrix by adopting a roll coating process, and irradiating by using ultraviolet light to finish curing modification; after the sol is coated, the sol is quickly irradiated by ultraviolet light, the interval between the sol and the sol is 15s, and the ultraviolet light exposure of the sol is 1800mJ/cm2The ultraviolet irradiation time was 30 seconds.
Step S3: and heating the modified diaphragm solidified and modified in the step S2 in an oven to evaporate the solvent in the modified diaphragm to form the modified diaphragm, wherein the temperature is 45 ℃.
And preparing the lithium battery quick-charging diaphragm 3 based on the polymer semi-interpenetrating structure according to the steps.
Example 4:
a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure comprises the following steps:
step S1: mixing polyurethane acrylate with functionality of 3, thermoplastic polyurethane and molecular weight of 3 x 1052-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl]Dispersing a-1-acetone photoinitiator in an ethanol solvent according to a mass ratio, and stirring to prepare uniform sol;
the mass percentage of the prepolymer with functional groups in the sol is 20%, the linear polymer content in the sol is 30%, the mass of the photoinitiator in the sol is 0.1% of that of the prepolymer with functional groups, and the balance is solvent.
Step S2: will step S1The sol prepared in the step (1) is coated on the surface of the PE diaphragm magnesium hydroxide matrix by adopting a brushing coating process, and is irradiated by ultraviolet light to finish curing modification; after the sol is coated, the sol is quickly irradiated by ultraviolet light, the interval between the sol and the sol is 15s, and the ultraviolet light exposure of the sol is 1800mJ/cm2The ultraviolet irradiation time was 30 seconds.
Step S3: and heating the modified diaphragm solidified and modified in the step S2 in an oven to evaporate the solvent in the modified diaphragm to form the modified diaphragm, wherein the temperature is 45 ℃.
And preparing the lithium battery quick-charging diaphragm 4 based on the polymer semi-interpenetrating structure according to the steps.
Example 5:
a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure comprises the following steps:
step S1: mixing polyurethane acrylate with functionality of 3, thermoplastic polyurethane and molecular weight of 3 x 1052-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl]-1-acetone photoinitiator is dispersed in cyclohexane according to mass ratio
Stirring the mixture in a solvent to prepare uniform sol;
the mass percentage of the prepolymer with functional groups in the sol is 20%, the linear polymer content in the sol is 30%, the mass of the photoinitiator in the sol is 0.1% of that of the prepolymer with functional groups, and the balance is solvent.
Step S2: coating the sol prepared in the step S1 on the surface of the PE diaphragm magnesium hydroxide matrix by adopting a brush coating process, and irradiating by using ultraviolet light to finish curing modification; after the sol is coated, the sol is quickly irradiated by ultraviolet light, the interval between the sol and the sol is 15s, and the ultraviolet light exposure of the sol is 1800mJ/cm2The ultraviolet irradiation time was 30 seconds.
Step S3: and heating the modified diaphragm solidified and modified in the step S2 in an oven to evaporate the solvent in the modified diaphragm to form the modified diaphragm, wherein the temperature is 45 ℃.
The lithium battery quick-charging diaphragm 5 based on the polymer semi-interpenetrating structure is prepared according to the steps.
Example 6:
1) structural characterization
In summary, as shown in fig. 1, a schematic diagram comparing the polymer-containing semi-interpenetrating network membrane in example 1 of the present invention with a conventional membrane shows that the polymer-containing semi-interpenetrating network membrane in example 1 of the present invention forms a layer of semi-interpenetrating network structure on the surface of the membrane substrate, which not only has high adhesion with the substrate, but also has high electrolyte retention rate, and when applied to the lithium battery fast charging technology, the long-time cycle capacity decay rate is greatly improved.
The method is characterized by utilizing Fourier infrared spectroscopy (FTIR), and a potassium bromide tabletting method is adopted, wherein polyurethane acrylate and thermoplastic polyurethane are uniformly mixed and then coated on transparent potassium bromide, and then the mixture is placed in FTIR equipment to be tested to obtain a spectrum before curing; the potassium bromide was then rapidly cured under uv light and tested in FTIR to give another spectrum.
As shown in fig. 2, after the urethane acrylate and the thermoplastic polyurethane are cured, double bonds of the urethane acrylate substantially disappear to form a network structure, the thermoplastic polyurethane can form a semi-interpenetrating structure therein, and infrared spectroscopy also proves that the technical scheme can form a polymer-containing semi-interpenetrating network membrane.
2) Performance testing
The lithium battery fast-charging diaphragm 1 based on the polymer semi-interpenetrating structure prepared in the embodiment 1 and the traditional diaphragm are selected, the two diaphragms are respectively arranged in a lithium cobaltate/lithium titanate laminated soft-package battery (with the capacity of 1200mAh), charge and discharge are carried out at the rate of 1.5C in the environment of 25 ℃, the capacity retention rates of the two batteries are obtained by taking the first discharge capacity as the reference, as shown in figure 3, the capacity retention rate of the diaphragm containing the polymer semi-interpenetrating network is much higher than that of the traditional diaphragm under the same condition, and the fact that the diaphragm containing the polymer semi-interpenetrating network can greatly improve the long-time cycle capacity attenuation of the battery is proved to have better chemical stability.
The invention discloses a preparation method of a lithium battery quick-charging diaphragm based on a polymer semi-interpenetrating structure, which comprises the steps of dispersing a prepolymer with functional groups, a linear macromolecule and a photoinitiator into a solvent to prepare a sol, coating the sol on the surface of a lithium battery diaphragm matrix, irradiating by using ultraviolet light to finish curing, heating in an oven to evaporate the solvent in the modified diaphragm to form a modified diaphragm, combining the advantages of thermoplastic polyurethane and polyurethane acrylate by using an ultraviolet light curing technology, and adopting the basic principle that the ultraviolet light curing reaction usually only needs a few seconds to realize the conversion from liquid state to solid state, the conversion of the prepolymer to a high polymer forms a semi-interpenetrating network containing a polymer network structure and the linear macromolecule which are wound together and is coated on the diaphragm matrix, so that the preparation method can have higher adhesiveness with the diaphragm matrix and also has higher electrolyte liquid retention rate, the quick-charging lithium battery diaphragm has simple process and excellent performance. The preparation method has the advantages of mild preparation conditions, simple process, excellent liquid retention performance and good chemical stability.
Thus, it will be appreciated by those skilled in the art that while embodiments of the invention have been illustrated and described in detail herein, many other variations or modifications can be made which conform to the principles of the invention, as may be directly determined or derived from the disclosure herein, without departing from the spirit and scope of the invention. Accordingly, the scope of the invention should be understood and interpreted to cover all such other variations or modifications.
Claims (10)
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| US20210119195A1 (en) * | 2019-10-16 | 2021-04-22 | Samsung Sdi Co., Ltd. | Separator for rechargeable lithium battery and rechargeable lithium battery including the same |
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| US20020061449A1 (en) * | 2000-09-19 | 2002-05-23 | Tatsuya Maruo | Ion-conductive composition, gel electrolyte, non-aqueous electrolyte battery, and electrical double-layer capacitor |
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Application publication date: 20220325 |