CN113644273A - Ionic-electronic co-conductive material and preparation method and device thereof - Google Patents
Ionic-electronic co-conductive material and preparation method and device thereof Download PDFInfo
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- CN113644273A CN113644273A CN202110930607.XA CN202110930607A CN113644273A CN 113644273 A CN113644273 A CN 113644273A CN 202110930607 A CN202110930607 A CN 202110930607A CN 113644273 A CN113644273 A CN 113644273A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- H—ELECTRICITY
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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Abstract
The invention relates to the technical field of lithium batteries, in particular to an ionic-electronic co-conductive material and a preparation method and a device thereof; using Li2S、MS2、P2S5And LiX is used for preparing a conductive polymer, a composite binder is prepared from polyacrylamide, polyvinyl alcohol and lithium carboxymethyl cellulose, the prepared conductive polymer, the composite binder and a solid filler are fully mixed to obtain slurry, the obtained slurry is coated by a scraper, a single-sided aluminum foil with the thickness of 20 microns is used as a current collector, the coating thickness is 400 microns, and the ionic-electronic co-conductive material is obtained after natural drying.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to an ionic-electronic co-conductive material and a preparation method and a device thereof.
Background
Lithium ion batteries are used as the leading army in the current battery industry, and are mainly applied to rechargeable batteries of portable electronic products, electric tools, electric vehicles and the like. The market of domestic and foreign electric vehicles is expanding, and the demand of lithium ion batteries is increasing. The preparation of lithium ion batteries requires auxiliary material binders, which are also important factors affecting the battery composition and its overall performance.
The charge and discharge process of the lithium ion battery is a cycle process in which lithium ions and electrons participate together, and in order to guarantee a larger charge and discharge current and cycle life, the electrode material of the lithium ion battery must be a good mixed conductor of the ions and the electrons, but the ion conductive channel and the electron conductive network in the composite anode of the conventional lithium ion battery are usually realized by mechanically mixing a solid electrolyte material and an electronic conductive additive such as conductive carbon and the like at present, so that the mixing effect is poor, and the distribution of the electron conductive network and the ion conductive network is not uniform enough.
Disclosure of Invention
The invention aims to provide an ionic-electronic co-conductive material, and a preparation method and a device thereof, and solves the problem that ionic conductive channels and electronic conductive networks in a composite anode of a lithium ion battery in the prior art are not uniformly distributed.
In order to achieve the purpose, the invention provides an ionic-electronic co-conductive material which comprises a conductive polymer, a composite binder and 2-12 parts of solid filler, wherein the conductive polymer comprises 12-16 parts of Li2S, 22-24 parts of MS28 to 12 parts of P2S5And 12-18 parts of LiX, wherein the composite binder comprises 0.5-5 parts of a flexibilizer, 2-10 parts of a water-soluble polymer and 1-5 parts of an ionic binder.
Preferably, the MS is2Wherein M is at least one element selected from the group consisting of Si, Ge and Sn, and X in the LiX is at least one element selected from the group consisting of F, Cl, Br and I.
Preferably, the flexibilizer is partially hydrolyzed polyacrylamide, the water-soluble polymer is polyvinyl alcohol, the ionic binder is lithium carboxymethyl cellulose, and the solid filler is any one or more selected from acetylene black, graphite, graphene, carbon black, carbon nanotubes and the like.
The invention also provides a preparation method of the ionic-electronic co-conductive material, which comprises the following steps:
provision of Li2S、MS2、P2S5And LiX powder, and mixing the powder to obtain a powder mixture;
grinding the resulting powder mixture under an inert atmosphere to obtain a ground mixture;
heating the obtained grinding mixture at the temperature of 450-550 ℃ and under the pressure of 1-100 Pa, cooling the heated grinding mixture to room temperature, and grinding for the second time to obtain conductive polymer powder;
dissolving a flexibilizer solvent in water to obtain a first solution, adding a water-soluble polymer into the first solution, stirring until the water-soluble polymer is dissolved to obtain a second solution, adding an ionic binder into the second solution, and stirring until the ionic binder is dissolved to obtain a polymer matrix;
adding the obtained polymer matrix into the grinding mixture, adding a solid filler, and fully mixing to obtain slurry;
coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the ionic-electronic co-conductive material, wherein the coating thickness is 400 um.
Preferably, Li is provided in step (ii)2S、MS2、P2S5And LiX powder, and mixing the powders to obtain a powder mixture in which:
first Li2S、MS2、P2S5And evenly spreading LiX powder on a drying table, and utilizing a hot air blower to carry out Li treatment2S、MS2、P2S5And LiX powder, and then mixing the dried powder to obtain a powder mixture.
The invention also provides a preparation device adopting the preparation method of the ion-electron co-conductive material,
the preparation facilities includes agitator tank, magnetic stirrers, magnetism son and electric heating wire, be provided with on the magnetic stirrers the agitator tank, the magnetism son is located the inside of agitator tank, the inside of agitator tank still is provided with the intermediate layer, be provided with in the intermediate layer electric heating wire.
The invention relates to an ion-electron co-conductive material, a preparation method and a device thereof, which utilize Li2S、MS2、P2S5And LiX is used for preparing a conductive polymer, a composite binder is prepared from polyacrylamide, polyvinyl alcohol and lithium carboxymethyl cellulose, the prepared conductive polymer, the composite binder and a solid filler are fully mixed to obtain slurry, the obtained slurry is coated by a scraper, a single-sided aluminum foil with the thickness of 20 microns is used as a current collector, the coating thickness is 400 microns, and the ionic-electronic co-conductive material is obtained after natural drying.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the steps of a method for preparing an ionic-electronic co-conductive material according to the present invention.
FIG. 2 is a flow chart of the steps of example 1 provided by the present invention.
FIG. 3 is a flow chart of the steps of example 2 provided by the present invention.
FIG. 4 is a flow chart of the steps of example 3 provided by the present invention.
FIG. 5 is a schematic structural view of a manufacturing apparatus provided in the present invention.
1-stirring tank, 2-magnetic stirrer, 3-magneton, 4-electric heating wire and 5-interlayer.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The invention provides an ionic-electronic co-conductive material which comprises a conductive polymer, a composite binder and 2-12 parts of solid filler, wherein the conductive polymer comprises 12-16 parts of Li2S, 22-24 parts of MS28 to 12 parts of P2S5And 12 to 18 parts of LiX, said MS2The composite binder comprises 0.5-5 parts of a flexibilizer, 2-10 parts of a water-soluble polymer and 1-5 parts of an ionic binder, wherein the flexibilizer is partially hydrolyzed polyacrylamide, the water-soluble polymer is polyvinyl alcohol, the ionic binder is lithium carboxymethyl cellulose, and the solid filler is any one or more selected from acetylene black, graphite, graphene, carbon black, carbon nanotubes and the like.
Referring to fig. 1, the present invention further provides a method for preparing the ion-electron co-conductive material, comprising the following steps:
s1: provision of Li2S、MS2、P2S5And LiX powder, and mixing the powder to obtain a powder mixture;
s2: grinding the resulting powder mixture under an inert atmosphere to obtain a ground mixture;
s3: heating the obtained grinding mixture at the temperature of 450-550 ℃ and under the pressure of 1-100 Pa, cooling the heated grinding mixture to room temperature, and grinding for the second time to obtain conductive polymer powder;
s4: dissolving a flexibilizer solvent in water to obtain a first solution, adding a water-soluble polymer into the first solution, stirring until the water-soluble polymer is dissolved to obtain a second solution, adding an ionic binder into the second solution, and stirring until the ionic binder is dissolved to obtain a polymer matrix;
s5: adding the obtained polymer matrix into the grinding mixture, adding a solid filler, and fully mixing to obtain slurry;
s6: coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the ionic-electronic co-conductive material, wherein the coating thickness is 400 um.
Preferably, in step S1, Li is first introduced2S、MS2、P2S5And evenly spreading LiX powder on a drying table, and utilizing a hot air blower to carry out Li treatment2S、MS2、P2S5And LiX powder, and then mixing the dried powder to obtain a powder mixture.
Preferably, in step S4, the polyacrylamide is dissolved in water, lithium hydroxide is added, the mixture is heated to 40-90 ℃, stirred for 2-8 hours, cooled to room temperature, an organic solvent such as ethanol is added until a solid is precipitated, and the mixture is allowed to stand, filtered, washed and dried at a drying temperature of 50-80 ℃ to obtain the flexibilizer.
Preferably, in step S4, the first solution is heated to 50 to 80 ℃, polyvinyl alcohol is added while stirring, then the solution is stirred until the polyvinyl alcohol is completely dissolved, heating is stopped, and the solution is cooled to room temperature while stirring to obtain a second solution.
Preferably, in step S4, sodium carboxymethyl cellulose is dispersed in ethanol, acid is added to dissolve while stirring until insoluble substances are separated out, 90% ethanol is added, and carboxymethyl cellulose is obtained by precipitation, filtration, washing and drying; dispersing carboxymethyl cellulose in ethanol, adding a lithium hydroxide solution, stirring until the carboxymethyl cellulose is completely dissolved, adding 90% ethanol, precipitating, filtering, washing, and drying to obtain the ionic binder.
Example 1, referring to fig. 1, the present invention further provides a method for preparing the ion-electron co-conductive material, which comprises the following steps:
s1: supply of 12 parts of Li2S, 12 parts of MS28 parts of P2S5And 12 parts of LiX powder, and mixing the powders to obtain a powder mixture;
s2: grinding the resulting powder mixture under an inert atmosphere to obtain a ground mixture;
s3: heating the obtained grinding mixture at the temperature of 450 ℃ and under the pressure of 1Pa, cooling the heated grinding mixture to room temperature, and grinding for the second time to obtain conductive polymer powder;
s4: dissolving a flexibilizer solvent in water to obtain a first solution, adding a water-soluble polymer into the first solution, stirring until the water-soluble polymer is dissolved to obtain a second solution, adding an ionic binder into the second solution, and stirring until the ionic binder is dissolved to obtain a polymer matrix;
s5: adding the obtained polymer matrix into the grinding mixture, adding a solid filler, and fully mixing to obtain slurry;
s6: coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the ionic-electronic co-conductive material, wherein the coating thickness is 400 um.
In the present embodiment, first, 12 parts by mass of Li2S, 22 portions of MS28 parts of P2S5And 12 parts of LiX powder are uniformly paved on a drying table, and the Li in parts by mass is treated by a hot air blower2S、MS2、P2S5Drying LiX powder, mixing the dried powder to obtain a powder mixture, grinding the obtained powder mixture in an inert atmosphere to obtain a ground mixture, heating the ground mixture at the temperature of 450 ℃ under the pressure of 1Pa, cooling the heated ground mixture to room temperature, grinding for the second time to obtain conductive polymer powder, dissolving polyacrylamide in water, adding lithium hydroxide, heating to 40 ℃, stirring for 2 hours, cooling to room temperature, adding an organic solvent such as ethanol until solids are precipitated, standing, performing suction filtration, washing, drying at the temperature of 50 ℃ to obtain 0.5 part of a flexibilizer, dissolving 0.5 part of the flexibilizer in water to obtain a first solution, heating the first solution to 50 ℃, adding 2 parts of polyvinyl alcohol while stirring, stirring until the polyvinyl alcohol is completely dissolved, stopping heating, cooling to room temperature while stirring, dispersing sodium carboxymethylcellulose in ethanol, dissolving with acid under stirring, adding 90% ethanol when insoluble substances are separated out, precipitating, filtering, washing, and drying to obtain carboxymethyl cellulose; dispersing carboxymethyl cellulose in ethanol, adding a lithium hydroxide solution, stirring until the carboxymethyl cellulose is completely dissolved, adding 90% ethanol, precipitating, filtering, washing, drying to obtain 1 part of ionic binder, adding 1 part of ionic binder into the obtained second solution, stirring until the ionic binder is dissolved to obtain a polymer matrix, adding the obtained polymer matrix into a grinding mixture, adding 2 parts of solid filler, fully mixing to obtain a slurry, coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20 micrometers as a current collector, and obtaining the ionic-electronic co-conductive material after natural drying.
In embodiment 2, referring to fig. 2, the present invention further provides a method for preparing the ion-electron co-conductive material, which comprises the following steps:
s1: supply of 16 parts of Li2S, 24 parts of MS212 parts of P2S5And 18 parts of LiX powder, and mixing the powders to obtain a powder mixture;
s2: grinding the resulting powder mixture under an inert atmosphere to obtain a ground mixture;
s3: heating the obtained ground mixture at 550 ℃ under the pressure of 100Pa, cooling the heated ground mixture to room temperature, and secondarily grinding to obtain conductive polymer powder;
s4: dissolving a flexibilizer solvent in water to obtain a first solution, adding a water-soluble polymer into the first solution, stirring until the water-soluble polymer is dissolved to obtain a second solution, adding an ionic binder into the second solution, and stirring until the ionic binder is dissolved to obtain a polymer matrix;
s5: adding the obtained polymer matrix into the grinding mixture, adding a solid filler, and fully mixing to obtain slurry;
s6: coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the ionic-electronic co-conductive material, wherein the coating thickness is 400 um.
In the present embodiment, first, 16 parts by mass of Li is measured2S, 24 parts of MS212 parts of P2S5And evenly spreading 18 parts of LiX powder on a drying table, and using a hot air blower to mix the Li in parts by mass2S、MS2、P2S5Drying LiX powder, mixing the dried powder to obtain a powder mixture, grinding the obtained powder mixture in an inert atmosphere to obtain a ground mixture, heating the ground mixture at the temperature of 550 ℃ under the pressure of 100Pa, cooling the heated ground mixture to room temperature, grinding for the second time to obtain conductive polymer powder, dissolving polyacrylamide in water, adding lithium hydroxide, heating to 90 ℃, stirring for 8 hours, cooling to room temperature, adding an organic solvent such as ethanol until solids are precipitated, standing, performing suction filtration, washing, drying at the temperature of 80 ℃ to obtain 5 parts of a flexibilizer, dissolving 5 parts of the flexibilizer in water to obtain a first solution, heating the first solution to 80 ℃, adding 10 parts of polyvinyl alcohol while stirring, stirring until the polyvinyl alcohol is completely dissolved, stopping heating, cooling to room temperature while stirring, dispersing sodium carboxymethylcellulose in ethanol, stirring, adding acid, dissolving, and separating insoluble substancesAdding 90% ethanol, precipitating, filtering, washing, and drying to obtain carboxymethyl cellulose; dispersing carboxymethyl cellulose in ethanol, adding a lithium hydroxide solution, stirring until the carboxymethyl cellulose is completely dissolved, adding 90% ethanol, precipitating, filtering, washing, drying to obtain 5 parts of ionic binder, adding 5 parts of ionic binder into the obtained second solution, stirring until the ionic binder is dissolved to obtain a polymer matrix, adding the obtained polymer matrix into a grinding mixture, adding 12 parts of solid filler, fully mixing to obtain a slurry, coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20 micrometers as a current collector, and obtaining the ionic-electronic co-conductive material after natural drying.
In embodiment 3, referring to fig. 3, the present invention further provides a method for preparing the ion-electron co-conductive material, comprising the following steps:
s1: supply of 14 parts of Li2S, 23 parts of MS210 parts of P2S5And 15 parts of LiX powder, and mixing the powders to obtain a powder mixture;
s2: grinding the resulting powder mixture under an inert atmosphere to obtain a ground mixture;
s3: heating the obtained ground mixture at the temperature of 500 ℃ and under the pressure of 50Pa, cooling the heated ground mixture to room temperature, and secondarily grinding to obtain conductive polymer powder;
s4: dissolving a flexibilizer solvent in water to obtain a first solution, adding a water-soluble polymer into the first solution, stirring until the water-soluble polymer is dissolved to obtain a second solution, adding an ionic binder into the second solution, and stirring until the ionic binder is dissolved to obtain a polymer matrix;
s5: adding the obtained polymer matrix into the grinding mixture, adding a solid filler, and fully mixing to obtain slurry;
s6: coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the ionic-electronic co-conductive material, wherein the coating thickness is 400 um.
In the present embodiment, the quality is determinedMeasured in parts by weight, first 14 parts of Li2S, 23 parts of MS210 parts of P2S5And 15 parts of LiX powder are uniformly paved on a drying table, and the Li in parts by mass is treated by a hot air blower2S、MS2、P2S5Drying LiX powder, mixing the dried powder to obtain a powder mixture, grinding the obtained powder mixture in an inert atmosphere to obtain a ground mixture, heating the ground mixture at the temperature of 500 ℃ under the pressure of 50Pa, cooling the heated ground mixture to room temperature, grinding for the second time to obtain conductive polymer powder, dissolving polyacrylamide in water, adding lithium hydroxide, heating to 65 ℃, stirring for 5 hours, cooling to room temperature, adding an organic solvent such as ethanol until solids are precipitated, standing, performing suction filtration, washing, drying at the temperature of 65 ℃ to obtain 2.5 parts of a flexibilizer, dissolving 2.5 parts of the flexibilizer in water to obtain a first solution, heating the first solution to 65 ℃, adding 6 parts of polyvinyl alcohol while stirring, stirring until the polyvinyl alcohol is completely dissolved, stopping heating, cooling to room temperature while stirring, dispersing sodium carboxymethylcellulose in ethanol, dissolving with acid under stirring, adding 90% ethanol when insoluble substances are separated out, precipitating, filtering, washing, and drying to obtain carboxymethyl cellulose; dispersing carboxymethyl cellulose in ethanol, adding a lithium hydroxide solution, stirring until the carboxymethyl cellulose is completely dissolved, adding 90% ethanol, precipitating, filtering, washing, drying to obtain 2.5 parts of ionic binder, adding 2.5 parts of ionic binder into the obtained second solution, stirring until the ionic binder is dissolved to obtain a polymer matrix, adding the obtained polymer matrix into a grinding mixture, adding 2 parts of solid filler, fully mixing to obtain a slurry, coating the obtained slurry by using a scraper, using a single-sided aluminum foil with the thickness of 20 micrometers as a current collector, and obtaining the ionic-electronic co-conductive material after natural drying.
Referring to fig. 4, the present invention further provides a manufacturing apparatus using the method for manufacturing an ion-electron co-conductive material as described above,
the preparation facilities includes agitator tank 1, magnetic stirrers 2, magnon 3 and electric heating wire 4, be provided with on the magnetic stirrers 2 agitator tank 1, magnon 3 is located agitator tank 1's inside, agitator tank 1's inside still is provided with intermediate layer 5, be provided with in the intermediate layer 5 electric heating wire 4.
In the embodiment, the magnetic stirrer 2 drives the magnetons 3 to rotate in the stirring tank 1, so that the mixing of the raw materials in the stirring tank 1 is accelerated, and the solution in the stirring tank 1 is heated by the electric heating wire 4.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. An ion-electron co-conductive material, characterized in that,
the ionic-electronic co-conductive material comprises a conductive polymer, a composite binder and 2-12 parts of solid filler, wherein the conductive polymer comprises 12-16 parts of Li2S, 22-24 parts of MS28 to 12 parts of P2S5And 12-18 parts of LiX, wherein the composite binder comprises 0.5-5 parts of a flexibilizer, 2-10 parts of a water-soluble polymer and 1-5 parts of an ionic binder.
2. The ionic-electronic co-conductive material of claim 1,
the MS2Wherein M is at least one element selected from the group consisting of Si, Ge and Sn, and X in the LiX is at least one element selected from the group consisting of F, Cl, Br and I.
3. The ionic-electronic co-conductive material of claim 2,
the flexible agent is partially hydrolyzed polyacrylamide, the water-soluble polymer is polyvinyl alcohol, the ionic binder is lithium carboxymethyl cellulose, and the solid filler is one or more selected from acetylene black, graphite, graphene, carbon black, carbon nanotubes and the like.
4. A method for preparing the ionic-electronic co-conductive material according to claim 3, comprising the steps of:
provision of Li2S、MS2、P2S5And LiX powder, and mixing the powder to obtain a powder mixture;
grinding the resulting powder mixture under an inert atmosphere to obtain a ground mixture;
heating the obtained grinding mixture at the temperature of 450-550 ℃ and under the pressure of 1-100 Pa, cooling the heated grinding mixture to room temperature, and grinding for the second time to obtain conductive polymer powder;
dissolving a flexibilizer solvent in water to obtain a first solution, adding a water-soluble polymer into the first solution, stirring until the water-soluble polymer is dissolved to obtain a second solution, adding an ionic binder into the second solution, and stirring until the ionic binder is dissolved to obtain a polymer matrix;
adding the obtained polymer matrix into the grinding mixture, adding a solid filler, and fully mixing to obtain slurry;
coating the obtained slurry by using a scraper, taking a single-sided aluminum foil with the thickness of 20um as a current collector, and naturally airing to obtain the ionic-electronic co-conductive material, wherein the coating thickness is 400 um.
5. The method of preparing an ionic-electronic co-conductive material according to claim 4, wherein Li is provided in step (hi)2S、MS2、P2S5And LiX powder, and mixing the powders to obtain a powder mixture in which:
mixing Li2S、MS2、P2S5And evenly spreading LiX powder on a drying table, and utilizing a hot air blower to carry out Li treatment2S、MS2、P2S5And LiX powder, and then mixing the dried powder to obtain a powder mixture.
6. A production apparatus using the production method of an ionic-electronic co-conductive material according to claim 5,
the preparation facilities includes agitator tank, magnetic stirrers, magnetism son and electric heating wire, be provided with on the magnetic stirrers the agitator tank, the magnetism son is located the inside of agitator tank, the inside of agitator tank still is provided with the intermediate layer, be provided with in the intermediate layer electric heating wire.
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