CN115332539A - Composite material for preparing electrode, preparation method of composite material, electrode and preparation method of electrode - Google Patents
Composite material for preparing electrode, preparation method of composite material, electrode and preparation method of electrode Download PDFInfo
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- CN115332539A CN115332539A CN202211264664.XA CN202211264664A CN115332539A CN 115332539 A CN115332539 A CN 115332539A CN 202211264664 A CN202211264664 A CN 202211264664A CN 115332539 A CN115332539 A CN 115332539A
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- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 24
- 239000006258 conductive agent Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000011149 active material Substances 0.000 claims abstract description 27
- 230000001070 adhesive effect Effects 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000000853 adhesive Substances 0.000 claims abstract description 18
- 238000005096 rolling process Methods 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 239000000839 emulsion Substances 0.000 claims description 21
- 239000011888 foil Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
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- 239000000843 powder Substances 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000013329 compounding Methods 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 229910001415 sodium ion Inorganic materials 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 229910021385 hard carbon Inorganic materials 0.000 claims description 2
- 229910021432 inorganic complex Inorganic materials 0.000 claims description 2
- 238000009830 intercalation Methods 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000010450 olivine Substances 0.000 claims description 2
- 229910052609 olivine Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical group [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 239000002210 silicon-based material Substances 0.000 claims description 2
- 239000011029 spinel Chemical group 0.000 claims description 2
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- 239000003990 capacitor Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000007731 hot pressing Methods 0.000 description 4
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- CYKMNKXPYXUVPR-UHFFFAOYSA-N [C].[Ti] Chemical compound [C].[Ti] CYKMNKXPYXUVPR-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007765 extrusion coating Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000002048 multi walled nanotube Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Classifications
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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
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
- H01M4/0435—Rolling or calendering
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
-
- 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
- H01M4/623—Binders being polymers fluorinated polymers
-
- 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
- H01M4/624—Electric conductive fillers
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of electrode preparation, and particularly relates to a composite material for preparing an electrode, a preparation method of the composite material, the electrode and a preparation method of the electrode. The composite material for preparing the electrode comprises the following components in percentage by weight: 40-99% of active material, 0-15% of conductive agent, 0.1-20% of adhesive and 0-25% of solvent, wherein the adhesive is an adhesive material with adhesive effect at the temperature of 120 ℃ or higher. The electrode prepared by the process omits large-scale homogenizing, coating, drying and rolling processes, and can realize the electrode with high compaction density, high surface density, high conductivity and strong bonding force only by 2 to 3 simple processes.
Description
Technical Field
The invention belongs to the technical field of electrode preparation, and particularly relates to a composite material for preparing an electrode, a preparation method of the composite material, the electrode and a preparation method of the electrode.
Background
The traditional preparation process of the battery is that raw materials including an active material, a binder, a conductive agent, a solvent and the like are gradually added into a homogenate tank body according to a certain process flow, the raw materials are uniformly mixed into slurry with certain fluidity and viscosity after being stirred at a high speed for about 12 hours, the slurry is respectively coated on the single side and the double sides of a current collector, and then the slurry is dried and rolled and cut into required pole pieces.
In addition, the electrode preparation of the battery can also be used for preparing the electrode of the capacitor. Therefore, the improvement of the electrode preparation method is significant for the production of batteries and capacitors.
Disclosure of Invention
Based on the defects of the prior art, the invention adopts the steps of prefabricating the raw materials into the composite material, and then preparing the composite material into the electrode through the one-step forming technology, the electrode prepared by the process omits the large-scale homogenizing, coating, drying and rolling processes, and the electrode with high compaction density, high surface density, high conductivity and strong bonding force can be realized only through 2 to 3 simple processes.
The technical scheme provided by the invention is as follows:
a composite material for preparing an electrode comprises the following components in percentage by weight: 40-99% of active material, 0-15% of conductive agent (excluding zero), 0.1-20% of adhesive and 0-25% of solvent (excluding zero), wherein the adhesive is adhesive material with adhesive effect at temperature of 120 ℃ or higher.
In the above technical scheme:
the particle surface in the composite material is covered with a layer of binder, the binder has no bonding effect at normal temperature, has strong bonding property at the temperature higher than 120 ℃, bulk powder materials can not be bonded together in the transfer process at normal temperature to influence the film forming effect, and a self-supporting film with a three-dimensional structure is easily formed under the hot pressing condition, so that the large homogenizing, coating, drying and rolling procedures required by a liquid phase coating process can be avoided.
In the above technical scheme:
the content of the solvent is less than or equal to 25 percent, the content of the solvent exceeds 25 percent, and the powder is easy to agglomerate and is not beneficial to the film-forming dispersion uniformity of the next working procedure; the granularity D50 of the powder is less than or equal to 20 mu m, and the granularity of the powder exceeds 20 mu m, so that the film forming uniformity of the next working procedure can be influenced; the tap density of the powder is between 0.3 and 2.0g/cm < 3 >.
In the above technical scheme:
the electrode is a battery electrode, or a capacitor electrode.
Specifically, the composite material for preparing the electrode is full-dry or semi-dry powder.
Specifically, the binder is a fluorine-containing binder, a styrene-butadiene rubber binder, a polyacrylic binder or a polyurethane binder.
Preferably, the binder includes, but is not limited to: polyvinylidene fluoride emulsions or particles; polytetrafluoroethylene emulsions or particles; polyacrylamide emulsions or granules; polyacrylonitrile emulsion or particles; polymethyl methacrylate or particles; a poly (styrene-butadiene rubber) emulsion.
Specifically, the active material is selected from any one or more of lithium titanate, hard carbon, graphite, activated carbon, si-based materials, sn-based materials, sb-based materials, pb-based materials, phosphorus materials or phosphide materials which can embed lithium ions or sodium ions; alternatively, the active material is selected from any one or more of layered structure oxides capable of intercalating lithium ions or sodium ions, olivine phosphate, spinel structure, inorganic complex or organic sodium salt compounds.
Specifically, the conductive agent is selected from any one or more of a 0-dimensional conductive agent, a 1-dimensional conductive agent, a 2-dimensional conductive agent, or a 3-dimensional conductive agent.
The 0-dimensional conductive agent may be, for example, carbon black, acetylene black, ketjen black, or the like.
The 1-dimensional conductive agent may be, for example, a carbon nanofiber, a single-walled nanotube, etc., a multi-walled nanotube, etc.
The 2-dimensional conductive agent is mainly MXene, and can be graphene, a carbon titanium compound, a titanium nitrogen compound and the like.
The 3-dimensional conductive agent may be, for example, a flake graphite conductive agent, spherical conductive graphite, or the like.
Specifically, the solvent is selected from one or more of deionized water, N-methyl pyrrolidone, ethanol or acetone.
The invention also provides a preparation method of the composite material for preparing the electrode, which is characterized by comprising the following steps of: adding the active material, the conductive agent, the binder and the solvent into a dispersing container according to the amount of the formula, dispersing at 50-70 ℃ to allow the binder to coat the surfaces of the particles, volatilizing the solvent from the uniformly dispersed slurry in a spray drying mode to leave dispersed powder, namely the uniformly dispersed composite material for preparing the electrode.
In the above technical solution, the structures of the formed composite materials have different situations and advantages according to different adding sequences of the active material, the conductive agent, the binder and the solvent.
Specifically, the active material, a part of the binder, the conductive agent, and the remaining binder are mixed in this order.
Based on the technical scheme, the composite material with a layered structure coated layer by layer can be formed, and the maximum utilization of the conductive network is facilitated under the condition of ensuring bonding.
Specifically, a first mixture is obtained by mixing a part of the binder with the active material, a second mixture is obtained by mixing the remaining binder with the conductive agent, and the first mixture and the second mixture are mixed in this order.
Based on the technical scheme, the conductivity is ensured, meanwhile, the structural stability among particles is enhanced, and the film forming is facilitated.
The invention also provides a preparation method of the electrode, which at least comprises the following steps:
1) The composite material for preparing the electrode is formed into a three-dimensional self-supporting film by rolling double rollers at the temperature of 120-180 ℃;
2) And compounding the three-dimensional self-supporting film on at least one surface of the current collector foil to obtain the electrode.
Specifically, the method comprises the following steps:
1) Respectively adopting rolling double rollers with the temperature of 120-180 ℃ to form the composite material for preparing the electrode into a three-dimensional self-supporting film to obtain a first self-supporting film and a second self-supporting film;
2) And respectively compounding the first self-supporting film and the second self-supporting film onto two surfaces of a current collector foil by adopting rolling double rollers at the temperature of 150-170 ℃ to obtain the electrode.
Based on the technical scheme, the electrode preparation process flow is from spraying to finished electrode production, and the process flow is compact, so that the electrode preparation process flow is suitable for a small production line and can also be applied to a large production line.
Specifically, the method comprises the following steps:
1) Forming the composite material for preparing the electrode on one surface of a current collector foil by using rolling double rollers at the temperature of 150-180 ℃, and forming a three-dimensional self-supporting film on one surface of the current collector foil;
2) And (3) forming the composite material for preparing the electrode on the other surface of the current collector foil by using rolling double rollers at the temperature of 150-180 ℃, and forming a three-dimensional self-supporting film on the other surface of the current collector foil to obtain the electrode.
The invention also provides the electrode prepared by the preparation method.
Drawings
Fig. 1 is a schematic diagram of a mixing process provided by the present invention.
FIG. 2 is a flow chart of an electrode preparation process provided by the present invention.
Fig. 3 is a flow chart of another electrode preparation process provided by the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
As a compounding process 1 shown in part a of fig. 1, an active material, a part of a binder, a conductive agent, and the remaining binder are sequentially compounded in this order. The structure of the formed composite material is that the middle is provided with an active material 20, a layer of granular 10 (formed by polyacrylic emulsion for example) or chain structure 11 (formed by PVDF emulsion) binder is coated around the active material 20, then the conductive agent 30 is coated on the outer layer of the binder 10 or 11, and finally the binder 12 or 13 is coated on the outer layer of the conductive agent 30, wherein the binder 10 is the same as the binder 13, and the binder 11 is the same as the binder 12; the composite material which is formed by adopting the material mixing process 1 and has a layered structure coated layer by layer is beneficial to the maximum utilization of a conductive network under the condition of ensuring bonding.
Example 2
As shown in a mixing process 2 of part b of fig. 1, a first mixture is obtained by mixing a part of the binder with the active material, a second mixture is obtained by mixing the remaining binder with the conductive agent, and the first mixture and the second mixture are mixed in this order. The structure of the formed composite material is that the chain-shaped binder 11 and the granular binder 13 are respectively coated on the surface of the active material 20, the chain-shaped binder 12 and the granular binder 10 are respectively coated on the surface of the conductive agent 30, and then the conductive agent with complete binder coating is coated on the surface of the active material with complete binder coating.
Example 3
As shown in fig. 2, the composite material after spray drying is stored in a material tank C41 through a pipeline C48, then the composite material in the material tank C41 is uniformly transferred to a platform C46, and then transferred to a rolling pair roller C42 with the temperature of 120-180 ℃ to form a three-dimensional self-supporting film C48, the upper and lower 2 independent self-supporting films enter a pair roller C47 with the temperature of 150-170 ℃ and are respectively compounded on the a/B surfaces of a current collector foil C43 to prepare an electrode C44, the electrode C44 is dried through a high-temperature tunnel furnace, and after the residual solvent is baked out, the electrode can enter the assembly process; the preparation process flow of the electrode is from spraying to finishing of the finished electrode, and the process flow is compact, so that the electrode can be suitable for a small production line and can also be applied to a large production line.
Example 4
As shown in fig. 3, the spray-dried composite material is stored in a material tank C41 through a pipeline C48, then the composite material in the material tank C41 is uniformly sprayed onto a current collector foil C43, then the composite material C40 is compounded onto the current collector foil C43 through a pair roller C42 at 150-180 ℃ to form a single-side coated electrode C49, the single-side coated electrode C49 enters a second material tank C41 through 2 guide rollers C45, the composite material C40 sprayed from the spray pipe tank C48 is sprayed onto the single-side electrode C49, the single-side coated electrode C44 is formed through a pair roller C47 at 150-180 ℃ again, and the double-side electrode C44 is baked in an infrared high-temperature tunnel furnace and then enters an assembly process.
Example 5
Raw materials of active material active carbon, adhesive spherical polyacrylonitrile emulsion, conductive agent carbon black and solvent deionized water are mixed according to the formula: adhesive: the formula of the conductive agent =80, 10 is uniformly dispersed, the solid content is 40%, and the dispersion process is as follows: adding activated carbon into a grinding machine by using a grinding dispersion machine, adding 85% by weight of a binder, heating to 55 ℃, grinding for 2 hours, adding a conductive agent Super _ P Li at one time, grinding for 1 hour, adding the rest 15% of binder emulsion, grinding for 2 hours, adding a solvent to adjust the solid content to 40%, spray-drying, and drying to obtain the composite material which is bulk particles and has no adhesiveness at normal temperature; at this time, the solvent content of the bulk particles was 5.3%, and the tap density was 0.46g/cm 3 D50 is 8.3 μm; directly compounding the bulk composite material on an aluminum foil by adopting an electrode preparation process flow 2 (figure 3) under the condition of hot pressing of 160 +/-2 ℃, and then obtaining an activated carbon electrode after passing through an infrared oven with the length of 5 meters, wherein the double-sided surface density of the electrode is 230g/m 2 The carbon film has a thickness of 0.280mm and a compacted density of 0.82 g/cm 3 The peel strength of the electrode sheet tested at the same time was 0.08kgf/cm, and the conductivity of the electrode was 0.004S/cm.
The same electric capacity of 3000F electric capacity structure is assembled into with above-mentioned pole piece, and the roll core diameter is 56.0 +/-0.1 mm, and after the liquid was annotated in the stoving, test capacity, ESR and durability test, test data are seen in table 1.
Example 6
Raw materials, namely active material, namely active carbon, a binder spherical polyacrylonitrile emulsion, a conductive agent, namely carbon black, and solvent deionized water are mixed according to a formula, wherein the active material comprises the following components in parts by weight: adhesive: the formula of the conductive agent =80, 10 is uniformly dispersed, the solid content is 40%, and the dispersion process is as follows: adding active materials into 85% adhesive emulsion by using a planetary mixer, heating to 55 ℃, stirring at high speed for 5h, adding the required conductive agent, stirring for 3h, adding 15% of the rest adhesive emulsion, stirring for 4h, adding a solvent to adjust the solid content to 40%, coating by using an extrusion coating machine, wherein the density of the coated double-sided surface is 140g/m 2 (ii) a Then rolling the carbon film by a hot pressing mode, wherein the thickness of the rolled carbon film is 0.233mm, and the compaction density is 0.6 g/cm 3 (ii) a The peel strength of the electrode sheet was measured to be 0.03 kgf/cm, and the conductivity of the electrode was measured to be 0.001S/cm.
The electrode plates are assembled into a capacitor with the same 3000F capacitor structure, the diameter of a winding core is 56.0 +/-0.1 mm, after baking and liquid injection, the capacity, ESR and durability tests are carried out, and the test data are shown in table 1.
Example 7
Raw materials of active material active carbon, adhesive chain polytetrafluoroethylene emulsion, conductive agent Super-P Li and solvent deionized water are mixed according to the formula: adhesive: the formula of the conductive agent =80, 10 is uniformly dispersed, the solid content is 40%, and the dispersion process is as follows:
adding activated carbon into 85% of polytetrafluoroethylene emulsion at one time by using a grinding dispersion machine 1, grinding for 2h, adding a required conductive agent Super _ P Li into the rest 15% of polytetrafluoroethylene emulsion in a second grinding dispersion machine 2, heating to 55 ℃, dispersing for 2h, and adding the conductive agent and the polytetrafluoroethylene emulsion into the grindingGrinding the mixture in a dispersion machine 1, dispersing for 2 hours to form uniformly dispersed mixed liquor, and adjusting the solid content of the mixed liquor to 40% and then carrying out spray drying to form a composite material; the solvent content of the composite material is 8.6 percent, and the array density is 0.48g/cm 3 D50 is 8.2 μm; adopting electrode preparation process flow 1 (figure 2) to form a three-dimensional self-supporting film at the temperature of 150 +/-2 ℃ by a pair roller C42, enabling the upper and lower 2 self-supporting films to run through the pair roller C47 to prepare an electrode C44 at the temperature of 155 +/-2 ℃, and testing the density of the coated double-sided surface to be 256g/m after the electrode C44 is baked by an infrared tunnel 2 The carbon film has a thickness of 0.301mm and a compacted density of 0.85 g/cm 3 The peel strength of the electrode sheet was 0.086kgf/cm, and the conductivity was 0.0036S/cm.
Assemble into 3000F electric capacity that the capacitor structure is the same with above-mentioned pole piece, roll up the core diameter and be 56.0 +/-0.1 mm, annotate the liquid back through toasting, test capacity, ESR and durability test, test data see table 1:
TABLE 1
Dispersing the active material, the conductive agent, the binder and the solvent in two different mixing modes in the figure 1, and discovering from the mixing process 1 (part a in the figure 1) and the mixing process 2 (part b in the figure 1) that different material adding sequences and contact modes among the components are different, but the material of the outermost layer is the binder, and the reason that the outermost layer is the binder is the film forming of the following process; the dispersion mode can adopt grinding, planetary stirring and airflow modes for dispersion; in the preparation method of a composite material and an electrode thereof, the electrode is a flexible membrane which forms a three-dimensional structure by a semi-dry or full-dry composite material under a hot-pressing environment, and the process flow of membrane forming is shown in figures 2 and 3; the pole piece after film forming can be assembled by adopting the assembly process of the existing lithium ion battery or sodium ion battery, or the assembly process of the existing capacitor.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The composite material for preparing the electrode is characterized by comprising the following components in percentage by weight: 40-99% of active material, 0-15% of conductive agent, 0.1-20% of adhesive and 0-25% of solvent, wherein the adhesive is an adhesive material with adhesive effect at the temperature of 120 ℃ or higher.
2. The composite material for preparing an electrode according to claim 1, wherein: the binder is fluorine-containing binder, styrene-butadiene rubber binder, polyacrylic binder or polyurethane binder.
3. The composite material for preparing an electrode according to claim 2, wherein: the binder includes, but is not limited to: polyvinylidene fluoride emulsions or particles; polytetrafluoroethylene emulsions or particles; polyacrylamide emulsions or granules; polyacrylonitrile emulsion or particles; polymethyl methacrylate or particles; a poly (styrene-butadiene rubber) emulsion.
4. The composite material for preparing an electrode according to claim 1, wherein:
the active material is selected from any one or more of lithium titanate, hard carbon, graphite, activated carbon, si-based material, sn-based material, sb-based material, pb-based material, phosphorus or phosphide material which can embed lithium ions or sodium ions;
or the active material is selected from any one or more of layered structure oxides capable of intercalating lithium ions or sodium ions, olivine phosphate, spinel structure, inorganic complex or organic sodium salt compound;
the conductive agent is selected from any one or more of a 0-dimensional conductive agent, a 1-dimensional conductive agent, a 2-dimensional conductive agent or conductive graphite;
the solvent is selected from any one or more of deionized water, N-methyl pyrrolidone, ethanol or acetone.
5. The composite material for preparing an electrode according to claim 1, wherein: the composite material for preparing the electrode is full-dry or semi-dry powder.
6. A method for preparing a composite material for preparing an electrode is characterized by comprising the following steps: adding the active material, the conductive agent, the binder and the solvent into a dispersing container according to the amount of the formula, dispersing at 50-70 ℃ to allow the binder to coat the surfaces of the particles, volatilizing the solvent from the uniformly dispersed slurry in a spray drying mode to leave dispersed powder, namely the uniformly dispersed composite material for preparing the electrode.
7. The method for preparing a composite material for an electrode according to claim 6, comprising the steps of:
mixing the active material, part of the adhesive, the conductive agent and the rest of the adhesive in sequence;
or mixing a part of the binder and the active material to obtain a first mixture, mixing the rest of the binder and the conductive agent to obtain a second mixture, and mixing the first mixture and the second mixture in sequence.
8. A method for preparing an electrode, characterized by comprising at least the following steps:
1) Forming the composite material for preparing the electrode, which is described in any one of claims 1 to 5, into a three-dimensional self-supporting film by using rolling double rollers with the temperature of 120-180 ℃;
2) And compounding the three-dimensional self-supporting film on at least one surface of the current collector foil to obtain the electrode.
9. The method for preparing an electrode according to claim 8, comprising the steps of:
1) Forming the composite material for preparing the electrode, which is described in any one of claims 1 to 5, into a three-dimensional self-supporting film by respectively adopting rolling double rollers with the temperature of 120-180 ℃ to obtain a first self-supporting film and a second self-supporting film;
2) Respectively compounding the first self-supporting film and the second self-supporting film on two surfaces of a current collector foil by using a rolling pair roller with the temperature of 150-170 ℃ to obtain the electrode;
or:
1) Forming the composite material for preparing the electrode according to any one of claims 1 to 5 on one surface of a current collector foil by using a rolling double roller with the temperature of 150-180 ℃, and forming a three-dimensional self-supporting film on one surface of the current collector foil;
2) Forming the composite material for preparing the electrode according to any one of claims 1 to 5 on the other side of the current collector foil by using rolling double rollers at the temperature of 150-180 ℃, and forming a three-dimensional self-supporting film on the other side of the current collector foil to obtain the electrode.
10. An electrode produced by the production method according to claim 8 or 9.
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