CN117476880A - Quick-charge negative electrode plate and preparation method thereof - Google Patents
Quick-charge negative electrode plate and preparation method thereof Download PDFInfo
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- CN117476880A CN117476880A CN202311600756.5A CN202311600756A CN117476880A CN 117476880 A CN117476880 A CN 117476880A CN 202311600756 A CN202311600756 A CN 202311600756A CN 117476880 A CN117476880 A CN 117476880A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000010410 layer Substances 0.000 claims abstract description 97
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000011889 copper foil Substances 0.000 claims abstract description 76
- 238000005096 rolling process Methods 0.000 claims abstract description 55
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- 239000006258 conductive agent Substances 0.000 claims description 42
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- 238000005507 spraying Methods 0.000 claims description 26
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- 239000002041 carbon nanotube Substances 0.000 claims description 13
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- 238000007590 electrostatic spraying Methods 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 11
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000007773 negative electrode material Substances 0.000 claims description 6
- 238000009832 plasma treatment Methods 0.000 claims description 6
- 238000003851 corona treatment Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 229910000733 Li alloy Inorganic materials 0.000 claims description 3
- 239000002033 PVDF binder Substances 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 3
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- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000001989 lithium alloy Substances 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 229910021382 natural graphite Inorganic materials 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 229920009441 perflouroethylene propylene Polymers 0.000 claims description 3
- 239000002006 petroleum coke Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 229910021332 silicide Inorganic materials 0.000 claims description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- -1 transition metal nitride Chemical class 0.000 claims description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 2
- 239000003973 paint Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229940098458 powder spray Drugs 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 17
- 238000001035 drying Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000007787 electrohydrodynamic spraying Methods 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 5
- 239000010949 copper Substances 0.000 abstract description 5
- 238000013329 compounding Methods 0.000 abstract description 3
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- 238000010438 heat treatment Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 13
- 239000011888 foil Substances 0.000 description 11
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 10
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- 239000006255 coating slurry Substances 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
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- 239000011149 active material Substances 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M4/0402—Methods of deposition of the material
- H01M4/0419—Methods of deposition of the material involving spraying
-
- 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
- H01M4/0433—Molding
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- 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)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A fast-charging negative electrode plate and a preparation method thereof are used for solving the problems that the surface density and the size of each layer cannot be accurately controlled, a large amount of energy consumption is caused by solvent drying, the process threshold is high and the like in the existing negative electrode wet double-layer coating. The preparation method mainly comprises the steps of primary powder mixing, secondary powder mixing, bottom layer fibrillation, copper foil surface treatment, copper foil-bottom layer compounding, electrospraying of a surface layer, multistage rolling and the like. The dry route preparation process is simplified, and no solvent participates, so that the complicated pole piece baking process is avoided. The preparation route of the double-layer electrode adopts a mode of firstly forming the bottom layer and then forming the layer, thereby being beneficial to accurately controlling the surface density and the size of each layer and being beneficial to realizing different structural requirements of the double-layer electrode. The method of the invention can be popularized and adapted to a plurality of lithium battery application fields, such as solid-state batteries and electrode pre-lithium, and the pole piece manufacturing process can realize complete drying, thereby reducing the process difficulty and the production cost in the corresponding fields.
Description
Technical Field
The invention relates to the technical field of lithium ion battery production, in particular to a fast-charging negative electrode plate and a preparation method thereof.
Background
With the increasing expansion of the market size of new energy automobiles, the development of lithium ion batteries with more excellent performance and safety has received a great deal of attention. At present, more attention is focused on the aspects of continuous mileage, quick charge and the like of an electric automobile, which provides new challenges for a lithium ion battery, so that a novel lithium ion battery with high capacity and excellent quick charge performance needs to be developed.
In the production and manufacture of lithium ion batteries, the preparation of the pole piece is of great importance, and the manufacturing process of the pole piece determines the final performance of the lithium ion batteries to a great extent. In order to improve the quick charge performance of the lithium ion battery and ensure the advantage of high capacity of the lithium ion battery, the prior art adopts double-layer coating to design the negative electrode of the lithium ion battery, the bottom layer often adopts a design with lower porosity and higher surface density to ensure high specific energy, and the surface layer adopts a design with higher porosity to ensure the quick charge performance of the battery cell.
However, the preparation of the cathode is basically carried out by adopting a wet double-layer coating mode in the prior art, the surface density and the size of each layer cannot be accurately controlled in the process, the process is complicated, the parameters are difficult to control, the process window range is small, and the drying process is required to be dried, so that higher requirements are put forward for the drying process, a large amount of extra energy is consumed, and the popularization and the implementation of the electrode design scheme are not facilitated.
Disclosure of Invention
The technical problems to be solved are as follows: aiming at the problems that the surface density and the size of each layer cannot be accurately controlled by the wet double-layer coating of the negative electrode, a large amount of energy consumption caused by solvent drying, a higher process threshold and the like in the prior art, the invention provides the quick-charge negative electrode plate and the preparation method thereof, the preparation process is simplified, the active material is compacted by improving the energy density by 20% through a dry process, the cycle performance, the durability and the impedance of a dry process battery are better, the participation of solvents is avoided, the complicated electrode plate baking process is avoided, the preparation route of the double-layer electrode adopts a mode of firstly and secondly layers, the surface density and the size of each layer are accurately controlled, and the different structural requirements of the double-layer electrode are realized.
The technical scheme is as follows: the preparation method of the fast-charging negative electrode plate comprises the following steps:
mixing the negative electrode dry powder with dry powder;
carrying out high-speed shearing and mixing on the mixed powder;
rolling the mixture obtained by high-speed shearing to obtain an electrode film;
at least one measure of plasma treatment and surface electrostatic spraying conductive agent surface treatment is adopted for the copper foil;
cutting the electrode film according to a target size (the width of the copper foil is larger than that of the electrode film, the electrode film is arranged in the middle of the copper foil, the two sides of the copper foil are left with a margin of 20-40 mm and used as electrode lugs), and rolling the copper foil and the electrode film on at least one surface of the copper foil to form an electrode for loading the electrode film;
preparing negative electrode dry powder, spraying the negative electrode dry powder onto an electrode of the load electrode film, and rolling to obtain the quick-charging negative electrode plate.
Preferably, the negative electrode dry powder is a mixture of negative electrode active material, conductive agent and binder powder with the mass ratio of 95 (1-5) to 1-5.
Preferably, the negative electrode active material is a carbon material or a non-carbon material, wherein the carbon material comprises artificial graphite, natural graphite, mesophase carbon microspheres, petroleum coke, carbon fibers or pyrolytic resin carbon, and the non-carbon material comprises transition metal oxide, multi-element lithium alloy, lithium metal nitride, transition metal nitride, phosphide, sulfide or silicide; the conductive agent is a carbon conductive agent and at least comprises one of a granular conductive agent, a fibrous conductive agent and a sheet conductive agent, wherein the granular conductive agent is conductive graphite or conductive carbon black, and the fibrous conductive agent is carbon nano tube or VGCF; the flaky conductive agent is graphene; the binder is at least one of a fibrillated binder and a non-fibrillated binder, and the fibrillated binder is PTFE, ETFE or FEP; the non-fibrillated binder is PVDF, CMC or SBR.
Further, the dry powder can be mixed and added simultaneously or in steps, and the mixing equipment comprises, but is not limited to, a double planetary vacuum power mixer, a double spiral conical mixer, a horizontal gravity-free mixer, a horizontal coulter mixer, a horizontal ribbon mixer and the like.
Further, the high-speed shearing mixing equipment includes, but is not limited to, high-speed shearing dispersing machines, jet mills, screw extruders, open mills, and the like.
Preferably, when the electrode film is obtained by rolling the mixture obtained by high-speed shearing, the rolling is performed in a fibrillation film forming machine under a working pressure of 5-50T, and the film thickness after rolling is 50-500 μm.
Preferably, the thickness of the copper foil is 5-15 μm, and the plasma treatment is specifically: carrying out surface treatment on the copper foil by adopting a corona treatment machine, wherein the surface tension of the treated copper foil is not lower than 34 dyne/cm; the surface electrostatic spraying conductive agent surface treatment specifically comprises the following steps: and spraying the conductive agent to the two surfaces of the copper foil by adopting an electrostatic spraying method, wherein the spraying thickness of the conductive agent is 0.1-1 mu m.
Preferably, when the copper foil and the electrode film on at least one side thereof are rolled, the rolling pressure is 5 to 20T.
Preferably, the electrode film is cut to a desired size, and then the surface-treated copper foil and the electrode films on both sides thereof are rolled to form a double-sided single-layer electrode carrying the electrode film.
Preferably, the preparation of the negative electrode dry powder and the spraying of the negative electrode dry powder onto the electrode of the load electrode film are as follows: and mixing the cathode dry powder to obtain pre-mixed powder, spraying the pre-mixed powder on two sides of a double-sided single-layer electrode by utilizing electrostatic spraying, controlling the distance between a spray head and a receiving surface to adjust the size of the surface coating, and obtaining a structure with two layers of electrodes on both sides, wherein the load mass ratio of electrode film raw materials to surface layer raw materials is 3:7-7:3.
Preferably, the electrostatic spraying specifically adopts an electrostatic powder spraying method, and the steps are as follows: by using a backThe roller is grounded, the spray gun is high in voltage, a stable electric field is formed between the spray gun and the back roller, the paint sprayed by the electrostatic powder spray gun is negatively charged while dispersing, the charged powder particles are coated on a grounded object to be coated under the action of airflow or centrifugal force and electrostatic attraction, and then the object to be coated is heated, melted and solidified into a film, wherein the high voltage is 30kV-50kV, the distance from a spray gun opening to a receiving surface is 100-300mm, and the powder spraying speed is 0.1-10g/m 2 /min。
Preferably, in the fast-charging negative electrode plate obtained after rolling, the rolling process is that the fast-charging negative electrode plate with target thickness is obtained after rolling for 2-5 times and the rolling pressure is 5-50T, and the compression ratio of each stage of rolling can be determined by pre-experiment according to different systems.
Preferably, the rolling is performed by using a hot roll, and the temperature of the hot roll is 60-80 ℃.
The fast-charging negative electrode plate prepared based on the method.
The beneficial effects are that: compared with the existing wet double-layer coating technology, the invention has the beneficial effects that:
the dry route preparation process provided by the invention is simplified, and no solvent participates, so that a complicated pole piece baking process is avoided, different components of the electrode material can be uniformly distributed, electrode layering caused by solvent evaporation is avoided, and meanwhile, the electrode preparation cost is effectively reduced;
the preparation route of the double-layer electrode provided by the invention adopts a mode of firstly carrying out bottom layer and then carrying out layer, thereby being beneficial to accurately controlling the area density and the size of each layer and being beneficial to realizing different structural requirements of the double-layer electrode: the bottom layer adopts a fibrillation dry electrode method, the accurate control of the electrode thickness is realized and the porosity is effectively reduced by optimizing the molecular weight and the processing temperature of the binder, so that the requirement of the bottom layer electrode on high capacity is met; the surface layer adopts an electrostatic spraying method to effectively reduce the tortuosity of the pores of the surface layer, improve the diffusion efficiency of lithium ions in the surface layer and meet the requirement of the surface layer electrode on high multiplying power.
The surface treatment measures such as plasma treatment and conductive adhesive spraying are carried out on the copper foil before the electrode film and the copper foil are pressed, the surface of the copper foil is activated, and part of organic matters, grease, oil stains and other microscopic organic dirt and oxide layers are removed, so that the conductive path between the bottom electrode and the copper foil is increased, the internal resistance of the electrode is effectively reduced, the bonding force between the copper foil and the material layer is also increased, the processability of the electrode in subsequent procedures (such as slitting, die cutting and the like) is improved, and the yield and the cycle life of the battery cell manufacturing process are improved.
The dry electrode mode provided by the invention can be popularized and adapted to a plurality of lithium battery application fields, such as solid-state batteries and electrode pre-lithium, and the pole piece manufacturing process can realize complete drying, so that the process difficulty and the production cost in the corresponding fields are reduced, and the production efficiency is improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a schematic diagram of a production line according to an embodiment of the present invention.
The numerical designations in fig. 2 are as follows: 1. a double-planetary vacuum power mixer; 2. a high-speed shearing and dispersing machine; 3. a bottom layer fibrillation unit; 31. discharging a hopper; 32. a fibrillating press roll; 33. an electrode film; 4. a copper foil surface treatment unit; 41. copper foil; 42. a corona treater; 43. a conductive film spray gun; 44. a conductive film backing roll; 5. a copper foil-base layer composite unit; 51. an electrode composite roller; 52. double-sided single-layer electrodes; 6. an electrospraying surface layer unit; 61. a surface layer spray gun; 62. a facing back roller; 63. double-sided double-layer electrodes; 7. a multi-stage rolling unit; 71. a multistage roller; 81. a copper foil heating system; 82. a surface layer heating and curing system a; 83. the surface layer is heated and cured to form the system b.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
Accordingly, the detailed description of the embodiments of the invention provided in the drawings below is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention.
The preparation method of the fast-charging negative electrode plate comprises the following steps:
mixing the negative electrode dry powder with dry powder;
carrying out high-speed shearing and mixing on the mixed powder;
rolling the mixture obtained by high-speed shearing to obtain an electrode film;
at least one measure of plasma treatment and surface electrostatic spraying conductive agent surface treatment is adopted for the copper foil;
cutting the electrode film according to a target size (the width of the copper foil is larger than that of the electrode film, the electrode film is arranged in the middle of the copper foil, the two sides of the copper foil are left with a margin of 20-40 mm and used as electrode lugs), and rolling the copper foil and the electrode film on at least one surface of the copper foil to form an electrode for loading the electrode film;
preparing negative electrode dry powder, spraying the negative electrode dry powder onto an electrode of the load electrode film, and rolling to obtain the quick-charging negative electrode plate.
The materials and equipment used in the examples of the present invention, unless otherwise specified, were all from ordinary commercial products.
The negative electrode dry powder in the embodiment of the present specification is a mixture of a negative electrode active material, a conductive agent, and a binder powder. The negative electrode active material is a carbon material or a non-carbon material, wherein the carbon material comprises artificial graphite, natural graphite, mesophase carbon microspheres, petroleum coke, carbon fibers or pyrolytic resin carbon, and the non-carbon material comprises transition metal oxide, multi-element lithium alloy, lithium metal nitride, transition metal nitride, phosphide, sulfide or silicide; the conductive agent is a carbon conductive agent and at least comprises one of a granular conductive agent, a fibrous conductive agent and a sheet conductive agent, wherein the granular conductive agent is conductive graphite or conductive carbon black, and the fibrous conductive agent is carbon nano tube or VGCF; the flaky conductive agent is graphene; the binder is at least one of a fibrillated binder and a non-fibrillated binder, and the fibrillated binder is PTFE, ETFE or FEP; the non-fibrillated binder is PVDF, CMC or SBR.
The apparatus used in the examples of this specification is shown in fig. 2, and comprises a double planetary vacuum power mixer 1, a high-speed shearing and dispersing machine 2, a bottom layer fibrillation unit 3, a copper foil surface treatment unit 4, a copper foil-bottom layer composite unit 5, an electrospraying surface layer unit 6, a multi-stage rolling unit 7 and a heating unit, wherein the heating unit comprises a copper foil heating system 81, a surface layer heating and curing system a 82 and a surface layer heating and curing system b (the heating unit in this specification is a section of heating oven which can structurally pass through a foil or an electrode tape), and the units are connected through the electrode tape. The double planetary vacuum power mixer 1 is connected with the high-speed shearing dispersing machine 2 through pipelines, a discharging pipe of the high-speed shearing dispersing machine 2 is divided into two parts, the two parts are respectively connected with the pipeline of a feed inlet of the two bottom layer fibrillation units 3, the bottom layer fibrillation units 3 comprise a discharging hopper 31 and a fibrillation press roller 32 connected with the discharging hopper, electrode films 33 obtained after materials are rolled by the fibrillation press roller 32, a copper foil surface treatment unit 4 is connected between the two bottom layer fibrillation units 3, the copper foil surface treatment unit 4 comprises a copper foil 41, a corona processor 42, two conductive film spray guns 43 and two conductive film back rollers 44, the copper foil 41 is processed by the corona processor 42 and then is fed into the conductive film back rollers 44, two sides of the processed copper foil correspond to one conductive film back roller 44 and one conductive film spray gun 43 respectively, the copper foil processed by the conductive film spray guns 43 is fed into the next process after the conductive film is solidified, and is heated by the copper foil heating system 81 in order to speed up the solidification time; then rolling the treated copper foil and the self-supporting electrode films on two sides of the copper foil in a copper foil-bottom layer composite unit 5, wherein the copper foil-bottom layer composite unit 5 comprises an electrode composite roller 51 and a double-sided single-layer electrode 52 compounded by the electrode composite roller 51, the double-sided single-layer electrode 52 is sent to an electrospraying surface layer unit 6, the electrospraying surface layer unit 6 comprises two groups of opposite surface layer spray guns 61 and a surface layer back roller 62, two sides of the double-sided single-layer electrode 52 respectively correspond to one surface layer spray gun and one surface layer back roller, the electrode treated by the first surface layer spray gun is cured by a surface layer heating curing system a 82 and then sent to a second surface layer spray gun for treatment, then cured by a surface layer heating curing system b 83, finally a double-sided double-layer electrode 63 is obtained, and then the double-sided double-layer electrode 63 is sent to a multistage roller 71 in a multistage rolling unit 7 for multistage rolling, and finally a fast-charge anode pole piece is obtained.
Example 1
As shown in fig. 1, a flowchart of a preparation method of a fast-charging negative electrode plate provided by the invention is further described below with reference to fig. 2 (in this embodiment, the size of the electrode plate only gives a thickness, and the target thickness is 170 μm):
s1, mixing primary powder: adding artificial graphite, conductive carbon black, carbon nano tubes and PTFE into a double-planetary vacuum power mixer 1 according to the weight ratio of 95:1:1:3, and then mixing powder for 1-5 h according to the revolution speed of 200rpm and the high-speed dispersion speed of 1500 rpm;
s2, mixing secondary powder: transferring the obtained mixed powder into a high-speed shearing and dispersing machine 2 (a transfer route is indicated by a dotted arrow in fig. 2, a transfer pipeline facility is not indicated in fig. 2), fibrillating PTFE in the mixed powder for 0.5-2 h under the high-speed shearing action of 3000rpm, uniformly dispersing and forming a dough-shaped mixture;
s3, bottom layer fibrillation: transferring the above dough-like mixture into a discharging hopper 31, and rolling in a fibrillating press roll 32 under a pressure of 20T at a roll temperature of 80 ℃ to obtain a self-supporting electrode film 33 having a thickness of 100 μm;
s4, copper foil surface treatment: the copper foil 41 has a thickness of 12 μm and a width of 500mm (generally 200-2000 mm), is wound into a corona treatment machine 42, and is respectively passed through two conductive film back rollers 44 on both sides of the treated copper foil, a conductive film with a thickness of 0.5 μm is sprayed on the corresponding position by a conductive film spray gun 43, the mixture ratio of the conductive agent is 1:1 as that of the conductive carbon black and the carbon nano tube, the mixing mode of the conductive agent is the same as that of the primary powder, and the sprayed copper foil is passed through a copper foil heating system 81, and the conductive film is cured therein;
s5, compounding copper foil and bottom layer: cutting the electrode film obtained by fibrillation of the bottom layer according to the target size (cutting equipment is not identified in fig. 2), wherein the cutting width is 460mm, each 20mm optical foil area is left on two sides of a foil material (copper foil) to serve as a tab, and then the copper foil 41 subjected to surface treatment and the self-supporting electrode film 33 positioned on two sides of the copper foil are rolled at the rolling pressure of 5T and the rolling temperature of 80 ℃ to form a double-sided single-layer electrode 52 carrying the bottom layer, and the total thickness is 172 mu m;
s6, electric spraying of a surface layer: adding artificial graphite, conductive carbon black, carbon nano tube and PTFE into a double-planetary vacuum power mixer 1 according to the weight ratio of 96:1:1:2, mixing powder according to revolution speed of 200rpm and high-speed dispersion speed of 1500rpm, spraying the mixed surface powder onto two sides of a double-sided single-layer electrode 52 through a surface layer spray gun 61 when the double-sided single-layer electrode 52 passes through two surface layer back rollers 62 respectively, controlling the distance between a spray head and a receiving surface to adjust the size of the surface coating, enabling the surface coating to cover a bottom layer and the width difference to be within a tolerance, entering a surface layer heating and curing system a 82 and a surface layer heating and curing system b 83 after each surface coating is sprayed, and finally obtaining a double-sided double-layer electrode 63 with two layers of electrodes, wherein the thickness is 220 mu m, and the loading amount is 50g/m of the bottom layer 2 Single-layer top coat 50g/m 2 ；
S7, multistage rolling: the double-sided double-layer electrode 63 obtained in the electrospraying surface layer process 6 is rolled for a plurality of times, in this embodiment, 3 times, the pressures of the multistage roller 71 are respectively 15T, 20T and 30T according to the sequence of rolling, and the thicknesses after the rolling are respectively 200 μm, 180 μm and 170 μm, so as to obtain the final fast-charge negative electrode sheet.
Comparative example 1: wet double layer coating
Adding artificial graphite, conductive carbon black, carbon nano tube and PTFE (emulsion, powder in example 1) into a double planetary vacuum power mixer according to the weight ratio of 95:1:1:3, and adding a proper amount of water to control the solid content to be 5Mixing 5% of the mixed slurry to obtain a primary coating slurry, and preparing a top coating slurry from artificial graphite, conductive carbon black, carbon nano tubes and PTFE according to the weight ratio of 95:1:1:3; the extrusion coater was used at the same loading as in example 1 (remark: example 1 loading was 50g/m for single layer primer) 2 Single-layer top coat 50g/m 2 ) Double-layer coating is carried out, rolling is carried out after drying, and the thickness of the final pole piece is controlled to be 170 mu m after rolling is carried out twice, wherein the compression amounts are respectively 70% and 30%.
Comparative example 2: fibril bottom layer and fibril surface layer
The difference from example 1 is that the process parameters of the individual steps are kept unchanged, and the preparation process S6 of the surface layer is changed to fibrillation, i.e. step S3.
The method comprises the following steps:
s1, mixing primary powder: adding artificial graphite, conductive carbon black, carbon nano tubes and PTFE into a double-planetary vacuum power mixer 1 according to the weight ratio of 95:1:1:3, and then mixing powder for 1-5 h according to the revolution speed of 200rpm and the high-speed dispersion speed of 1500 rpm;
s2, mixing secondary powder: transferring the obtained mixed powder into a high-speed shearing and dispersing machine 2 (a transfer route is indicated by a dotted arrow in fig. 2, a transfer pipeline facility is not indicated in fig. 2), fibrillating PTFE in the mixed powder for 0.5-2 h under the high-speed shearing action of 3000rpm, uniformly dispersing and forming a dough-shaped mixture;
s3, bottom layer fibrillation: transferring the above dough-like mixture into a discharging hopper 31, and rolling in a fibrillating press roll 32 under a pressure of 20T at a roll temperature of 80 ℃ to obtain a self-supporting electrode film 33 having a thickness of 100 μm;
s4, copper foil surface treatment: the copper foil 41 has a thickness of 12 μm and a width of 500mm (generally 200-2000 mm), is wound into a corona treatment machine 42, and is respectively passed through two conductive film back rollers 44 on both sides of the treated copper foil, a conductive film with a thickness of 0.5 μm is sprayed on the corresponding position by a conductive film spray gun 43, the mixture ratio of the conductive agent is 1:1 as that of the conductive carbon black and the carbon nano tube, the mixing mode of the conductive agent is the same as that of the primary powder, and the sprayed copper foil is passed through a copper foil heating system 81, and the conductive film is cured therein;
s5, compounding copper foil and bottom layer: cutting the electrode film obtained by fibrillation of the bottom layer according to the target size (cutting equipment is not identified in fig. 2), wherein the cutting width is 460mm, each 20mm optical foil area is left on two sides of a foil material (copper foil) to serve as a tab, and then the copper foil 41 subjected to surface treatment and the self-supporting electrode film 33 positioned on two sides of the copper foil are rolled at the rolling pressure of 5T and the rolling temperature of 80 ℃ to form a double-sided single-layer electrode 52 carrying the bottom layer, and the total thickness is 172 mu m;
s6, cutting the film prepared in the step S3 according to a target size, wherein the cutting width is 460mm, leaving 20mm optical foil areas on two sides of a foil (copper foil) as electrode lugs, rolling the double-sided single-layer electrode 52 carrying the bottom layer and the film on two sides of the double-sided single-layer electrode 52, wherein the rolling pressure is 5T, the rolling temperature is 80 ℃, and forming a double-sided double-layer electrode with two layers of electrodes on two sides, the total thickness is 220 mu m, and the loading capacity is 50g/m of the bottom layer 2 Single-layer top coat 50g/m 2 ；
S7, multistage rolling: the double-sided double-layer electrode 63 obtained in the electrospraying surface layer process 6 is rolled for a plurality of times, in this embodiment, 3 times, the pressures of the multistage roller 71 are respectively 15T, 20T and 30T according to the sequence of rolling, and the thicknesses after the rolling are respectively 200 μm, 180 μm and 170 μm, so as to obtain the final fast-charge negative electrode sheet.
Comparative example 3: spraying bottom layer and spraying surface layer
The difference from example 1 is that the process parameters of each step are kept unchanged, and the preparation method S3 of the bottom layer is changed to electrospraying (i.e., step S6).
The method comprises the following steps:
copper foil surface treatment: the copper foil 41 has a thickness of 12 μm and a width of 500mm (generally 200-2000 mm), is wound into a corona treatment machine 42, and is respectively passed through two conductive film back rollers 44 on both sides of the treated copper foil, a conductive film with a thickness of 0.5 μm is sprayed on the corresponding position by a conductive film spray gun 43, the mixture ratio of the conductive agent is 1:1 as that of the conductive carbon black and the carbon nano tube, the mixing mode of the conductive agent is the same as that of the primary powder, and the sprayed copper foil is passed through a copper foil heating system 81, and the conductive film is cured therein;
spraying a bottom layer: adding artificial graphite, conductive carbon black, carbon nano tube and PTFE into a double-planetary vacuum power mixer 1 according to the weight ratio of 95:1:1:3, mixing powder for 1-5 h according to revolution speed of 200rpm and high-speed dispersion speed of 1500rpm, spraying the mixed surface powder onto two surfaces of a double-surface single-layer electrode through a surface layer spray gun when two surfaces of copper foil (each 20mm of photo foil area is left on two sides of a foil material (copper foil) to serve as a polar lug) respectively pass through two surface layer back rollers, controlling the distance between a spray head and a receiving surface to adjust the size of the surface coating, enabling the surface coating to cover the bottom layer and the width difference to be within a tolerance, entering a surface layer heating and curing system a and a surface layer heating and curing system b after each surface coating is sprayed, and finally obtaining the double-surface double-layer electrode with two layers of electrodes on two surfaces, wherein the thickness is 220 mu m and the loading amount is 50g/m of the bottom layer 2 ；
Spraying a surface layer: adding artificial graphite, conductive carbon black, carbon nano tubes and PTFE into a double-planetary vacuum power mixer 1 according to the weight ratio of 96:1:1:2, mixing powder according to revolution speed of 200rpm and high-speed dispersion speed of 1500rpm, spraying the mixed surface layer powder onto two surfaces of the double-surface single-layer electrode through a surface layer spray gun when the double-surface single-layer electrode passes through two surface layer back rollers respectively, controlling the distance between a spray head and a receiving surface to adjust the size of the surface coating, enabling the surface coating to cover the bottom layer and the width difference to be within a tolerance, entering a surface layer heating and curing system a and a surface layer heating and curing system b after each surface coating is sprayed, and finally obtaining the double-surface double-layer electrode with two layers of electrodes, wherein the thickness is 220 mu m, and the loading capacity is 50g/m of the bottom layer 2 Single-layer top coat 50g/m 2 ；
Multistage rolling: and rolling the double-sided double-layer electrode obtained in the surface layer electric spraying process for multiple times, wherein in the embodiment, the multi-stage roller is respectively pressed for 15T, 20T and 30T according to the sequence of rolling, and the thicknesses after the rolling are respectively 200 mu m, 180 mu m and 170 mu m, so that the final fast-charging negative electrode plate is obtained.
Comparative example 4: the copper foil is not subjected to surface treatment
The difference from example 1 is that the process parameters of the respective steps are kept unchanged, but the copper foil is not subjected to surface treatment (i.e., step S4 is not employed).
The anode pole piece obtained in the above examples and comparative examples is cut into pole pieces with a material area length of 230mm and a width of 100mm by laser cutting and die cutting, the height of the pole ear is 20mm and the width is 30mm, an anode with an N/p=1.08 (the ratio of the anode capacity to the cathode capacity is denoted by N/P), a diaphragm with a width of 232mm and a thickness of 15 μm is selected to prepare a stacked core of an anode 20 layer and an anode 19 layer in a lamination manner, and then the soft package battery core is tested by steps of baking, pre-packaging, liquid injection, sealing and the like, and the quick charging performance of the battery core under a 1C multiplying power (national standard) is tested, so that the obtained result is as follows:
note that: the method is characterized in that: in the embodiment 1, the bottom layer and the surface layer are prepared sequentially, and each layer structure meets the design requirement;
in comparative example 1, the bottom layer and the surface layer are coated simultaneously, the two layers of electrodes are mutually influenced, the ideal design requirement is hardly met, and the parameter adjustment difficulty is high;
comparative example 2, bottom layer and top layer were prepared sequentially, the top layer porosity was less than example 1;
comparative example 3, bottom layer and top layer were prepared sequentially, the compaction density of the bottom layer being less than example 1;
in comparative example 4, the bottom layer and the surface layer were prepared sequentially, each layer structure satisfied the design requirement, and the foil was not subjected to surface treatment.
From the table it can be seen that:
the comparison of the example 1 and the comparative example 1 shows that the traditional wet double-layer coating has higher cost, a considerable part of the cost is energy consumption caused by solvent drying, and the utilization rate of the cathode material is lower due to higher debugging difficulty of the wet double-layer coating, so that the cost is further increased; meanwhile, the adhesive floats upwards in the solvent drying process in the wet coating process, so that the final pole piece peeling strength is lower than that of a dry method, and although the wet double-layer coating also reaches the national standard of 1200 cycles, the cycle numbers of double-layer electrodes prepared by the dry method have larger difference, and the DCR is higher.
Comparison of example 1 and comparative example 2 shows that the lack of electrospraying of the facing layer reduces the porosity, and the fast charge performance of the cell is greatly reduced, as can be seen by the significant increase in DCR.
The comparison of example 1 and comparative example 3 shows that the quick charge performance is reduced due to the fact that the required compaction density is not achieved when the bottom layer is subjected to electric spraying, but the comparison of example 2 shows that a large amount of lithium precipitation does not occur in the battery cell due to the large porosity, and the 1200 circles of circulating standard of national standard is achieved.
The comparison of example 1 and comparative example 4 shows that the surface treatment of the copper foil is very important in the preparation process of the dry double-layer electrode provided by the invention, on one hand, the peeling strength of the electrode sheet can be improved, and on the other hand, the DCR of the battery cell can be effectively reduced by reducing the contact resistance between the active substance and the foil.
Finally, it should be noted that: in the embodiment of the specification, the dry powder can be mixed and added simultaneously or in steps, and the mixing equipment comprises, but is not limited to, a double planetary vacuum power mixer, a double spiral conical mixer, a horizontal gravity-free mixer, a horizontal coulter mixer, a horizontal ribbon mixer and the like.
Such high-speed shear mixing equipment includes, but is not limited to, high-speed shear dispersers, jet mills, screw extruders, open mills, and the like.
The above embodiments are merely for illustrating the technical solution of the present invention, and are not limiting thereof; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced with equivalents; such modifications and substitutions do not depart from the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present invention.
Claims (12)
1. The preparation method of the fast-charging negative electrode plate is characterized by comprising the following steps:
mixing the negative electrode dry powder with dry powder;
carrying out high-speed shearing and mixing on the mixed powder;
rolling the mixture obtained by high-speed shearing to obtain an electrode film;
at least one measure of plasma treatment and surface electrostatic spraying conductive agent surface treatment is adopted for the copper foil;
cutting the electrode film according to the target size, and rolling the copper foil and the electrode film positioned on at least one side of the copper foil to form an electrode carrying the electrode film;
preparing negative electrode dry powder, spraying the negative electrode dry powder onto an electrode of the load electrode film, and rolling to obtain the quick-charging negative electrode plate.
2. The preparation method of the quick-charging negative electrode plate according to claim 1 is characterized in that the negative electrode dry powder is a mixture of negative electrode active material, conductive agent and binder powder with a mass ratio of 95 (1-5).
3. The method for preparing a fast-charging negative electrode sheet according to claim 2, wherein the negative electrode active material is a carbon material or a non-carbon material, the carbon material comprises artificial graphite, natural graphite, mesophase carbon microspheres, petroleum coke, carbon fibers or pyrolytic resin carbon, and the non-carbon material comprises transition metal oxide, multi-element lithium alloy, lithium metal nitride, transition metal nitride, phosphide, sulfide or silicide; the conductive agent is a carbon conductive agent and at least comprises one of a granular conductive agent, a fibrous conductive agent and a sheet conductive agent, wherein the granular conductive agent is conductive graphite or conductive carbon black, and the fibrous conductive agent is carbon nano tube or VGCF; the flaky conductive agent is graphene; the binder is at least one of a fibrillated binder and a non-fibrillated binder, and the fibrillated binder is PTFE, ETFE or FEP; the non-fibrillated binder is PVDF, CMC or SBR.
4. The method for preparing the fast-charging negative electrode plate according to claim 1, wherein when the electrode film is obtained by rolling the mixture obtained by high-speed shearing, the rolling is carried out in a fibrillation film forming machine, the working pressure is 5-50T, and the film thickness after rolling is 50-500 μm.
5. The preparation method of the fast-charging negative electrode plate according to claim 1, wherein the thickness of the copper foil is 5-15 μm, and the plasma treatment is specifically as follows: carrying out surface treatment on the copper foil by adopting a corona treatment machine, wherein the surface tension of the treated copper foil is not lower than 34 dyne/cm; the surface electrostatic spraying conductive agent surface treatment specifically comprises the following steps: and spraying the conductive agent to the two surfaces of the copper foil by adopting an electrostatic spraying method, wherein the spraying thickness of the conductive agent is 0.1-1 mu m.
6. The method for preparing a fast-charging negative electrode sheet according to claim 1, wherein the rolling pressure is 5-20T when the copper foil and the electrode film on at least one side thereof are rolled.
7. The method for preparing a fast-charging negative electrode sheet according to claim 1, wherein the electrode film is cut according to a target size, and then the surface-treated copper foil and the electrode films on both sides thereof are rolled to form a double-sided single-layer electrode carrying the electrode film.
8. The method for preparing a fast-charging negative electrode sheet according to claim 7, wherein the preparation of the negative electrode dry powder and the spraying of the negative electrode dry powder onto the electrode of the load electrode film comprises the following specific steps: and mixing the cathode dry powder to obtain pre-mixed powder, spraying the pre-mixed powder to two sides of a double-sided single-layer electrode by utilizing electrostatic spraying, controlling the distance between a spray head and a receiving surface to adjust the size of the surface coating, and obtaining a structure with two layers of electrodes on both sides, wherein the load mass ratio of electrode film raw materials to surface layer raw materials is 3:7-7:3.
9. The method for preparing the fast-charging negative electrode plate according to claim 1, wherein the electrostatic spraying specifically adopts an electrostatic powder spraying method, and comprises the following steps: the back roller is adopted to be grounded,the spray gun is high in voltage, a stable electric field is formed between the spray gun and the back roller, the paint sprayed by the electrostatic powder spray gun is negatively charged while dispersing, the charged powder particles are coated on a grounded object to be coated under the action of airflow or centrifugal force and electrostatic attraction, and then the object to be coated is heated, melted, solidified and formed into a film, wherein the high voltage is 30kV-50kV, the distance from a spray gun opening to a receiving surface is 100-300mm, and the powder spraying speed is 0.1-10g/m 2 /min。
10. The method for preparing the fast-charging negative electrode plate according to claim 1, wherein the fast-charging negative electrode plate is obtained after rolling, the rolling process is that the fast-charging negative electrode plate with the target thickness is obtained after rolling for 2-5 times and the rolling pressure is 5-50T.
11. The method for preparing the fast-charging negative electrode plate according to claim 1, wherein the rolling is performed by a hot roller, and the temperature of the hot roller is 60-80 ℃.
12. A fast-charging negative electrode sheet prepared based on the method of any one of claims 1-11.
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