CN110752348A - Method for preparing self-supporting flexible electrode by solvent-nonsolvent method and self-supporting flexible electrode - Google Patents
Method for preparing self-supporting flexible electrode by solvent-nonsolvent method and self-supporting flexible electrode Download PDFInfo
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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Abstract
The invention relates to a method for preparing a self-supporting flexible electrode by a solvent-nonsolvent method, which comprises the following steps: preparing active substances, a conductive agent, a binder and a solvent into slurry; coating the slurry on a substrate, transferring the substrate to water and standing; and (3) after the substrate coated with the slurry is placed in water, drying the substrate, and tearing the film to obtain the self-supporting flexible electrode. A self-supporting flexible electrode is prepared by adopting the method. The invention has the beneficial effects that: the preparation method is simple, the manufacturing equipment is cheap and easy to obtain, the electrode can meet good flexibility without a current collector, the prepared self-supporting flexible electrode can be prepared without using a pore-forming agent and additional complex post-treatment work, the prepared self-supporting flexible electrode has a microporous structure and is more beneficial to lithium ion conduction, so that the electrochemical performance is greatly improved on the premise of not reducing the mechanical performance and the flexibility, and the method is suitable for preparing the self-supporting flexible electrode on a large scale.
Description
Technical Field
The invention relates to the field of batteries, in particular to a method for preparing a self-supporting flexible electrode by a solvent-non-solvent method and the self-supporting flexible electrode.
Background
Lithium Ion Batteries (LiBs) have the advantages of high energy density, high cycle stability, environmental friendliness and the like, and have been widely used in various electronic devices, and meanwhile, along with the rapid development of flexible wearable electronic devices such as portable phones and implantable sensors, the design concept of flexible lithium ion batteries is more and more emphasized by people to meet the requirements of future advanced applications. In addition to high energy and high power density, flexible batteries are required to have good bending properties and mechanical properties, and in order to develop flexible batteries that meet the requirements. Developers have focused their goals primarily on flexible electrodes, current collectors, and solid-state electrolytes, however, flexible electrodes, and in particular, a simple and easy method of fabrication suitable for large-scale fabrication, is the most challenging.
Among the numerous studies on flexible electrodes, researchers mostly prepare flexible electrodes by two ways:
1) mixing an active substance with a super-strong binder and a conductive additive, and then coating the mixture on a current collector to obtain a flexible electrode;
2) and blending the active material and the nano carbon material to obtain the self-supporting flexible electrode.
2) Compared with the electrode prepared by the method 1), due to the lack of a binder and a current collector, the self-supporting electrode prepared by the method 2) has higher specific mass capacity and energy density, and at present, a great number of self-supporting flexible electrodes based on carbon nanotubes, carbon fibers and carbon cloth are reported to be used in the development of flexible lithium ion batteries.
In the prior art, the self-supporting flexible electrode is usually prepared by Chemical Vapor Deposition (CVD), magnetron sputtering and other complicated nano-preparation techniques, however, the manufacturing methods have low efficiency and high cost, and are not suitable for mass production of the self-supporting flexible electrode.
Disclosure of Invention
The invention aims to provide a method for preparing a self-supporting flexible electrode by a solvent-non-solvent method and the self-supporting flexible electrode, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a method for preparing a self-supporting flexible electrode by a solvent-nonsolvent method comprises the following steps:
s100: preparing active substances, a conductive agent, a binder and a solvent into slurry;
s200: coating the slurry on a substrate, transferring the substrate to water and standing;
s300: and (3) after the substrate coated with the slurry is placed in water, drying the substrate, and tearing the film to obtain the self-supporting flexible electrode.
Further, the active substance is one of lithium iron phosphate, ternary materials, lithium cobaltate, lithium titanate, graphite and silicon carbon;
the conductive agent is one or two of carbon nano tube, graphene, carbon fiber, acetylene black, carbon black and Ketjen black;
the binder is one or two of PU, PAN, PEDOT and PSS;
the solvent is one of DMSO, acetone and DMF.
Furthermore, the mass ratio of the active substance to the conductive agent is (7.5-9): 1-0.5, the mass ratio of the active substance to the binder is (5-9): 1, and the solid content of the slurry is 227 mg/mL-380 mg/mL.
Further, in S100, the slurry preparation method specifically includes:
the active substance, the conductive agent and the binder are placed in a ball milling tank, the solvent is added into the ball milling tank, and then high-speed ball milling is carried out, wherein the rotating speed of the ball mill is 250-350 r/min, and the ball milling time is 1-3 h.
Further, in S100, the slurry preparation method specifically includes:
the active substance, the conductive agent and the binder are placed in a glass container, the solvent is added into the glass container, magnetic stirring is carried out, the rotating speed of the magnetic stirring is 500-1000 r/min, and the magnetic stirring time is 4-10 h.
In S200, the substrate is made of one of glass, a PET sheet, a PP sheet, and polytetrafluoroethylene.
Further, in S200, after the slurry is coated on the substrate, the substrate is left to stand for 1 to 3 minutes, and then transferred to water to stand.
Further, in S200, the substrate coated with the slurry is left to stand in water for 2 to 6 hours.
Further, in S300, the drying temperature is 40-80 ℃, and the drying time is 2-24 h.
The invention has the beneficial effects that: compared with the traditional preparation method of the self-supporting flexible electrode, the self-supporting flexible electrode prepared by the method has a microporous structure and is more beneficial to lithium ion conduction, so that the electrochemical performance is greatly improved on the premise of not reducing the mechanical performance and the flexibility, and the method is suitable for preparing the self-supporting flexible electrode on a large scale.
A self-supporting flexible electrode is prepared by adopting the method.
The adoption of the further beneficial effects is as follows: the porous structure is more beneficial to lithium ion conduction, so that the electrochemical performance is greatly improved on the premise of not reducing the mechanical performance and flexibility.
Drawings
FIG. 1 is a flow chart of a method for preparing a self-supporting flexible electrode according to the solvent-nonsolvent method of the present invention;
FIG. 2 is a SEM picture of a self-supporting flexible electrode provided in example 1 of the present invention;
FIG. 3 is a SEM picture of a self-supporting flexible electrode provided in example 2 of the present invention;
fig. 4 is an SEM picture of the self-supporting flexible electrode provided in example 3 of the present invention.
Detailed Description
The embodiment of the application realizes the preparation of the porous self-supporting flexible electrode by the phase separation technology by providing the solvent-nonsolvent method, the preparation method is simple, the manufacturing equipment is cheap and easy to obtain, the prepared electrode can meet good flexibility without a current collector, and the prepared self-supporting flexible electrode can be used for preparing the micro-porous self-supporting flexible electrode without using a pore-forming agent or extra complex post-treatment work.
In order to better understand the technical solutions, the technical solutions will be described in detail below with reference to the drawings and the specific embodiments of the specification, and it should be understood that the embodiments and specific features of the embodiments of the present invention are detailed descriptions of the technical solutions of the present application, and are not limitations of the technical solutions of the present application, and the technical features of the embodiments and examples of the present application may be combined with each other without conflict.
As shown in fig. 1, a method for preparing a self-supporting flexible electrode by a solvent-nonsolvent method comprises the following steps:
s100: preparing active substances, a conductive agent, a binder and a solvent into slurry;
s200: coating the slurry on a substrate, transferring the substrate to water and standing;
s300: and (3) drying the substrate coated with the slurry after standing in water, and tearing the film, wherein the torn film is the self-supporting flexible electrode.
More preferably, in S100, the active material is one of lithium iron phosphate, a ternary material, lithium cobaltate, lithium titanate, graphite, and silicon carbon;
the conductive agent is one or two of carbon nano tube, graphene, carbon fiber, acetylene black, carbon black and Ketjen black;
the binder is one or two of PU (polyurethane for short), PAN (polyacrylonitrile for PAN), PEDOT (polymer of EDOT (3, 4-ethylene dioxythiophene monomer)) and PSS (sodium polystyrene sulfonate for PSS);
the solvent is one of DMSO, acetone and DMF.
In addition, the mass ratio of the active substance to the conductive agent is (7.5-9): 1-0.5, the mass ratio of the active substance to the binder is (5-9): 1, and the solid content of the slurry is 227 mg/mL-380 mg/mL.
There are various methods for formulating the slurry, and the following two are preferred in the present invention:
the method comprises the following steps of 1: in S100, the slurry preparation method specifically comprises the following steps:
the active substance, the conductive agent and the binder are placed in a ball milling tank, the solvent is added into the ball milling tank, and then high-speed ball milling is carried out, wherein the rotating speed of the ball mill is 250-350 r/min, and the ball milling time is 1-3 h.
The method comprises the following steps of 2: in S100, the slurry preparation method specifically comprises the following steps:
the active substance, the conductive agent and the binder are placed in a glass container, the solvent is added into the glass container, magnetic stirring is carried out, the rotating speed of the magnetic stirring is 500-1000 r/min, and the magnetic stirring time is 4-10 h.
More preferably, in S200, the substrate material is one of glass, a PET sheet, a PP sheet, and polytetrafluoroethylene;
and after the slurry is coated on a substrate, standing for 1-3 minutes, and then transferring to water for standing, wherein the standing time in the water is 2-6 hours.
More preferably, in S300, the drying treatment is carried out at a temperature of 40 to 80 ℃ for a drying time of 2 to 24 hours.
The self-supporting flexible electrode is prepared by the method, wherein the prepared self-supporting flexible electrode is a flexible negative electrode or a flexible positive electrode.
Example 1
Putting 1.5g of lithium cobaltate, 0.3g of PU and 0.2g of carbon nano tube into a ball milling tank, adding 7.5mL of DMF into the ball milling tank, passing through a ball mill at the rotating speed of 300 revolutions per minute for 2 hours, and carrying out ball milling dispersion treatment;
after the treatment, transferring the slurry into a polytetrafluoroethylene mold by using a dropper or a medicine spoon, uniformly coating the slurry by using a 500-micrometer scraper, standing for 1-3 minutes, placing the polytetrafluoroethylene mold coated with the slurry into a water tank, and standing for 6 hours when the water level is higher than that of the polytetrafluoroethylene mold;
and after standing, placing the polytetrafluoroethylene mold in a forced air drying oven, drying at 80 ℃ for 2h, cutting the edge of the self-supporting flexible electrode with a knife after drying, and winding and tearing the film to obtain the self-supporting porous self-supporting flexible electrode film.
Referring to fig. 2, a Scanning Electron Microscope (SEM) photograph of the solution shows that the self-supporting flexible electrode prepared by the solution has a porous surface and uniform distribution of voids, as shown in fig. 2.
Example 2
1.8g of graphite, 0.05g of PEDOT, 0.05g of PSS, 0.05g of graphene and 0.05g of carbon black are taken to be placed in a ball milling tank, 5mL of DMSO is added into the ball milling tank, magnetic stirring is carried out, the rotating speed is 800 revolutions per minute, the duration is 6 hours, and dispersion treatment is carried out;
after treatment, transferring the slurry on glass by using a dropper or a medicine spoon, uniformly coating the slurry by using a 200-micrometer scraper, standing for 1-3 minutes, placing the glass coated with the slurry in a water tank, and standing for 4 hours, wherein the water level is higher than that of the glass sheet;
and after standing, placing the glass sheet in a forced air drying oven, drying at 50 ℃ for 18h, cutting the edge of the self-supporting flexible electrode with a knife after drying, and winding and tearing the film to obtain the self-supporting porous self-supporting flexible electrode film.
Referring to fig. 3, a Scanning Electron Microscope (SEM) photograph of the solution shows that the self-supporting flexible electrode prepared by the solution is porous and uniformly dispersed, as is apparent from fig. 3.
Example 3
Putting 1.6g of lithium iron phosphate, 0.1g of PU, 0.1g of carbon nano tube and 0.1g of carbon fiber into a ball milling tank, adding 5mL of acetone into the ball milling tank, and carrying out ball milling dispersion treatment by a ball mill at the rotating speed of 250 revolutions per minute for 6 hours;
after the treatment, transferring the slurry on the PET sheet by using a dropper or a medicine spoon, uniformly coating the slurry by using a 250-micrometer scraper, standing for 1-3 minutes, placing the PET sheet coated with the slurry in a water tank, and standing for 2 hours, wherein the water level is higher than that of the PET sheet;
and after standing, placing the PET sheet in a forced air drying oven, drying for 24h at 40 ℃, cutting the edge of the self-supporting flexible electrode with a knife after drying, and winding and tearing the film to obtain the self-supporting porous self-supporting flexible electrode film.
Referring to fig. 4, a Scanning Electron Microscope (SEM) photograph of the solution shows that the self-supporting flexible electrode of the solution has a porous surface as can be clearly observed from fig. 4.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
the embodiment of the application provides a solvent-nonsolvent method for preparing a self-supporting flexible electrode, which realizes the preparation of a porous self-supporting flexible electrode by a phase separation technology, has simple preparation method and cheap and easily-obtained manufacturing equipment, can meet good flexibility without a current collector, can prepare a micro-porous self-supporting flexible electrode without using a pore-forming agent and additional complex post-treatment work, compared with the traditional preparation method of the self-supporting flexible electrode, the self-supporting flexible electrode prepared by the method has a microporous structure and is more beneficial to lithium ion conduction, thereby the electrochemical performance is greatly improved on the premise of not reducing the mechanical performance and the flexibility, in addition, the method has cheap equipment and materials, simple and efficient manufacturing process, and is particularly suitable for preparing the self-supporting flexible electrode on a large scale, the method has important significance for the development and popularization of the preparation of the self-supporting flexible electrode towards industrialization.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for preparing a self-supporting flexible electrode by a solvent-nonsolvent method is characterized by comprising the following steps:
s100: preparing active substances, a conductive agent, a binder and a solvent into slurry;
s200: coating the slurry on a substrate, transferring the substrate to water and standing;
s300: and (3) after the substrate coated with the slurry is placed in water, drying the substrate, and tearing the film to obtain the self-supporting flexible electrode.
2. The method for preparing the self-supporting flexible electrode according to the claim 1, wherein the active material is one of lithium iron phosphate, ternary material, lithium cobaltate, lithium titanate, graphite and silicon carbon;
the conductive agent is one or two of carbon nano tube, graphene, carbon fiber, acetylene black, carbon black and Ketjen black;
the binder is one or two of PU, PAN, PEDOT and PSS;
the solvent is one of DMSO, acetone and DMF.
3. The method for preparing the self-supporting flexible electrode by the solvent-nonsolvent method according to claim 1 or 2, wherein the mass ratio of the active substance to the conductive agent is (7.5-9): 1-0.5, the mass ratio of the active substance to the binder is (5-9): 1, and the solid content of the slurry is 227 mg/mL-380 mg/mL.
4. The method for preparing the self-supporting flexible electrode according to claim 1, wherein in S100, the slurry preparation method specifically comprises the following steps:
the active substance, the conductive agent and the binder are placed in a ball milling tank, the solvent is added into the ball milling tank, and then high-speed ball milling is carried out, wherein the rotating speed of the ball mill is 250-350 r/min, and the ball milling time is 1-3 h.
5. The method for preparing the self-supporting flexible electrode according to claim 1, wherein in S100, the slurry preparation method specifically comprises the following steps:
the active substance, the conductive agent and the binder are placed in a glass container, the solvent is added into the glass container, magnetic stirring is carried out, the rotating speed of the magnetic stirring is 500-1000 r/min, and the magnetic stirring time is 4-10 h.
6. The method of claim 1, wherein in the step S200, the substrate is made of one of glass, PET sheet, PP sheet, and teflon.
7. The method for preparing a self-supporting flexible electrode according to claim 1, wherein in step S200, after the slurry is coated on the substrate, the substrate is allowed to stand for 1 to 3 minutes, and then the substrate is transferred to water for standing.
8. The method for preparing the self-supporting flexible electrode according to claim 1, wherein the substrate coated with the slurry is allowed to stand in water for 2 to 6 hours in S200.
9. The method for preparing the self-supporting flexible electrode according to the claim 1, wherein in the step S300, the temperature of the drying treatment is 40-80 ℃, and the drying time is 2-24 h.
10. A self-supporting flexible electrode, produced by the method of any one of claims 1 to 9.
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