CN112201770A - Electrode plate, preparation method thereof and lithium battery - Google Patents
Electrode plate, preparation method thereof and lithium battery Download PDFInfo
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- CN112201770A CN112201770A CN202011103675.0A CN202011103675A CN112201770A CN 112201770 A CN112201770 A CN 112201770A CN 202011103675 A CN202011103675 A CN 202011103675A CN 112201770 A CN112201770 A CN 112201770A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides an electrode plate, a preparation method thereof and a lithium battery. The electrode plate comprises an electrode current collector and an electrode active substance film layer positioned on the electrode current collector, wherein the electrode active substance film layer comprises at least 2 stacked electrode films; on the same surface of the electrode current collector, the mass fraction of the binder in each electrode membrane which is not attached to the electrode current collector is not lower than that of the binder in the electrode membrane which is closer to the electrode current collector than the mass fraction of the binder in each electrode membrane. The method comprises the following steps: 1) coating the electrode slurry on a current collector, and drying to obtain a layer of electrode diaphragm; 2) and repeating the operation of coating the electrode slurry on the electrode film obtained in the last operation and drying for at least 1 time to obtain the electrode film. The electrode plate provided by the invention can improve the overall bonding performance of the electrode, increase the loading capacity of active substances on the current collector in unit area and improve the energy density of the electrode plate.
Description
Technical Field
The invention belongs to the field of batteries, relates to an electrode plate, a preparation method thereof and a lithium battery, and particularly relates to a positive plate, a preparation method thereof and a lithium battery.
Background
The lithium/carbon fluoride battery is a lithium primary battery with the highest specific energy in a solid positive electrode series, the theoretical specific energy of the lithium/carbon fluoride battery is 2180Wh/kg, and the lithium/carbon fluoride battery has the advantages of wide working temperature range, high safety performance, high and stable working platform, low self-discharge rate and the like, and is widely concerned. With continuous progress of science and technology, the requirements of equipment which does not need power supply maintenance, such as computers, mobile phones, intelligent meters, communication equipment, equipment in special fields and the like, on the energy density of a power supply are higher and higher, and particularly, the lithium battery is required to have high energy density by the equipment in the special fields, such as unmanned aerial vehicles, underwater vehicles and the like. In view of the above, it is necessary to provide a high-capacity fluorocarbon electrode sheet and a method for preparing the same, which can improve the energy density of a lithium/fluorocarbon battery.
CN103594687A discloses a preparation method of a lithium fluorocarbon battery anode, wherein the process material comprises a substrate material, a conductive agent, a dispersing agent and a binder, and the preparation method comprises the following steps: adding a dispersant into a mixed solution of pure water and a binder and stirring; adding a conductive agent which is ground and passes through a 200-mesh molecular sieve into the mixed solution and stirring; adding a substrate material into the mixed solution and stirring; drying the slurry at a constant temperature for a certain time, and adding alcohol to demulsify; rolling the slurry into a film layer with the thickness of 0.2-1.0 mm by adopting a hot rolling mode; and pressing the film layer on a nickel mesh current collector. Although the capacity of the prepared thick electrode is high, continuous film making and film rolling are difficult to realize in the manufacturing process, and the density of the used nickel mesh current collector is high, so that the mass percentage of the structural member of the battery is increased, and the effective improvement of the energy density of the battery is not facilitated.
CN102903921A discloses an aqueous battery using carbon fluoride as a positive electrode, the battery provided by the scheme is provided with a positive electrode, a negative electrode and an electrolyte system, the positive electrode adopts a carbon fluoride material as an active substance, and the positive electrode is prepared by a coating mode.
CN104466107A discloses a carbon fluoride composite anode and a preparation method thereof, wherein the carbon fluoride composite anode takes an aluminum foil as a substrate, and a composite coating containing carbon fluoride, a carbon conductive agent and a binder and a nickel-containing coating are sequentially arranged on one surface of the substrate from bottom to top; the preparation method comprises the steps of adding carbon fluoride, a carbon conductive agent and a binder into an organic solvent, and uniformly stirring to obtain mixed slurry; coating the obtained mixed slurry on one surface of an aluminum foil, and forming a composite coating on the one surface of the aluminum foil after drying; and plating a nickel-containing plating layer on the surface of the composite coating by a chemical nickel plating method, performing heat treatment, rolling, and shearing to obtain the battery anode.
The CN102903921A and CN104466107A both adopt a coating mode to prepare electrodes, the thickness of each electrode is less than 300 mu m, the thickness of each electrode is influenced by the characteristics of low density, large specific surface area and the like of the carbon fluoride material, and carbon fluoride pole pieces manufactured by adopting a coating method are generally thin electrodes and are difficult to meet the requirement of batteries developing towards high energy density.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide an electrode sheet, a method for preparing the same, and a lithium battery. The electrode plate provided by the invention can improve the overall bonding performance, increase the active substance loading capacity on the current collector in unit area, and improve the energy density of the electrode plate.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an electrode sheet comprising an electrode current collector and an electrode active material film layer on the electrode current collector, the electrode active material film layer comprising at least 2 stacked electrode membrane sheets; on the same surface of the electrode current collector, the mass fraction of the binder in each electrode membrane which is not attached to the electrode current collector is not lower than that of the binder in the electrode membrane which is closer to the electrode current collector than the mass fraction of the binder in each electrode membrane.
In the electrode sheet provided by the invention, the electrode active material film layer comprises at least 2 stacked electrode film sheets, such as 2 layers, 3 layers or 4 layers. The electrode plate provided by the invention uses the multilayer membranes, and aims to solve the problems that the battery performance is poor due to slow solvent volatilization, floating of a conductive agent and cracking of the electrode plate caused by one-time coating of a thick electrode are avoided while the loading capacity of active substances is improved to increase the energy density by overlapping the multilayer electrode membranes.
In the present invention, since the current collector may be coated on one side or both sides, each of the electrode sheets may have one or two electrode active material film layers.
The electrode diaphragm not attached to the electrode current collector means that at least one electrode diaphragm is arranged between the diaphragm and the electrode current collector.
On the same surface of the electrode current collector, the mass fraction of the binder in each electrode membrane which is not attached to the electrode current collector is not lower than that of the binder in the electrode membrane which is closer to the electrode current collector than the mass fraction of the binder in each electrode membrane, namely the mass fraction of the binder of the electrode membrane far away from the electrode current collector is not lower than that of the binder of the electrode membrane close to the electrode current collector. Along the direction of keeping away from the electrode current collector, the mass fraction of binder tends to increase in the electrode diaphragm promptly, because along the electrode diaphragm is far away from the current collector, whole diaphragm thickness increases, and the diaphragm is easy atress fracture, and the design that electrode diaphragm binder mass fraction tends to increase has promoted the adhesion properties of place diaphragm and whole diaphragm effectively.
The following is a preferred technical solution of the present invention, but not a limitation to the technical solution provided by the present invention, and the technical objects and advantageous effects of the present invention can be better achieved and achieved by the following preferred technical solution.
As a preferable embodiment of the present invention, the electrode active material film layer is located on one or both surfaces of the electrode current collector.
Preferably, the electrode sheet is a positive electrode sheet. In this case, the electrode current collector is a positive electrode current collector, and the electrode active material is a positive electrode active material.
Preferably, the electrode current collector includes an aluminum foil and/or a carbon-coated aluminum foil.
Preferably, in each of the electrode membranes, the electrode active material independently comprises any one of carbon fluoride, a carbon fluoride/manganese dioxide composite or a carbon fluoride/sulfur composite.
The electrode plate provided by the invention is particularly beneficial to improving the loading capacity of active substances of the carbon fluoride electrode, and simultaneously avoids the problems of dry cracking, cracking and the like of the electrode plate. The carbon fluoride material has high specific surface characteristics, is favorable for the rapid transmission of lithium ions as an electrode material, eliminates the obstacle of long lithium ion transmission distance in a high-load electrode, and shows high working voltage and high energy density.
Preferably, the fluorinated carbon comprises any one or a combination of at least two of graphite fluoride, fluorinated graphene, fluorinated carbon nanotubes, fluorinated carbon microspheres, fluorinated carbon fibers, fluorinated hard carbon or fluorinated soft carbon.
Preferably, the thickness of the electrode active material film layer is 300 μm or more, for example, 300 μm, 310 μm, 320 μm, 350 μm, 380 μm, 400 μm, or the like. The thickness of the electrode active material film larger than 300 μm has the advantages of increasing the active material loading amount on the unit area current collector, reducing the proportion of the inactive materials of the battery, and improving the energy density of the lithium/carbon fluoride battery.
Preferably, the adhesive species of each of the electrode membranes are the same. The same adhesive is adopted, so that the compatibility between the membrane layers is better, and the adhesive property between the membrane layers is improved.
As a preferred embodiment of the present invention, the electrode membrane includes an electrode active material, a binder, and a conductive agent.
Preferably, the binder comprises any one or a combination of at least two of polyvinylidene fluoride, sodium carboxymethylcellulose, styrene butadiene rubber or acrylonitrile multipolymer.
Preferably, the conductive agent includes any one of conductive carbon black (Super P), graphite, carbon nanofibers, carbon nanotubes, graphene, ketjen black, or acetylene black, or a combination of at least two thereof.
In a preferred embodiment of the present invention, the electrode active material film layer includes 2 electrode films stacked one on another, wherein a first electrode film is disposed on the electrode current collector, and a second electrode film is stacked on the first electrode film. By adopting two layers of electrode diaphragms, the contradiction between the loading capacity of the active substances of the carbon fluoride electrode plate and the cracking of the electrode plate can be better solved.
Preferably, the thickness of the first electrode membrane is 10-80%, such as 10%, 20%, 30%, 40%, 50%, 60%, 70% or 80%, etc., of the thickness of the electrode active material membrane layer on which it is located, and the thickness of the second electrode membrane is 20-90%, such as 20%, 40%, 60%, 80% or 90%, etc., of the thickness of the electrode active material membrane layer on which it is located. In the invention, if the thickness of the first electrode diaphragm is too thick relative to the thickness of the second electrode diaphragm, the first electrode diaphragm and the whole electrode diaphragm are easy to crack; if the thickness of the first electrode membrane is too thin relative to the second electrode membrane, the manufacturing of the ultrathin membrane is difficult to realize by adopting a coating process, and the production cost is increased.
Preferably, the mass fraction of binder in the first electrode membrane is 5-10%, such as 5%, 6%, 7%, 8%, 9%, 10%, or the like.
Preferably, the mass fraction of the binder in the second electrode membrane is 5-15%, such as 5%, 7%, 9%, 10%, 12%, 14%, 15%, or the like.
In a second aspect, the present invention provides a method for preparing an electrode sheet according to the first aspect, the method comprising the steps of:
(1) coating the electrode slurry on an electrode current collector, and drying to obtain a layer of electrode diaphragm;
(2) repeatedly coating the electrode slurry on the electrode slice obtained in the last operation and drying for at least 1 time to obtain the electrode slice; the electrode plate comprises at least 2 layers of stacked electrode films, and the mass fraction of the binder in each electrode film which is not attached to the electrode current collector is not lower than that of the binder in the electrode film which is closer to the electrode current collector than the mass fraction of the binder in the electrode film on the same surface of the electrode current collector.
The preparation method provided by the invention can obtain the high-capacity electrode plate, and solves the problem that the electrode plate does not crack when the loading capacity of active substances is not improved by single-layer coating through multi-layer coating. And the mass fraction of the binder in each electrode membrane can be controlled by controlling the content of the binder in the solid-phase substance in the electrode slurry.
As a preferred embodiment of the present invention, the preparation method of the electrode slurry in the step (1) and the step (2) comprises: and mixing the binder and the solvent, adding the conductive agent, mixing to obtain conductive adhesive, adding the electrode active substance, and mixing to obtain the electrode slurry.
Preferably, the mixing is stirring mixing or/and ball milling mixing.
Preferably, the coating in the step (1) and the coating in the step (2) are independently one-time coating or multiple-time coating, and the number of times of the multiple-time coating is more than 2 times.
As a preferable technical scheme of the invention, the solid content of the electrode slurry in the step (1) and the solid content of the electrode slurry in the step (2) are 35-50%, such as 35%, 40%, 45% or 50%, and the like, and in the invention, the dry cracking of the pole piece caused by the volatilization of a large amount of solvent can be avoided by increasing the solid content of the slurry.
Preferably, the viscosity of the electrode slurry in step (1) and step (2) is greater than 6000 mPa.s, such as 6001 mPa.s, 8100 mPa.s, 8500 mPa.s, 9700 mPa.s or 11000 mPa.s.
Preferably, in the step (2), each time the operation of coating the electrode slurry on the electrode membrane obtained in the previous operation is repeated, the mass fraction of the binder in the solid-phase substance of the electrode slurry is not less than the mass fraction of the binder in the solid-phase substance of the electrode slurry used in the previous coating.
As a preferable technical scheme of the invention, the drying in the step (1) and the drying in the step (2) are both two-stage drying. By adopting two-stage drying, the pole piece can be dried at low temperature and then at high temperature, so that the pole piece is prevented from cracking due to too fast volatilization of the solvent.
Preferably, in the step (1) and the step (2), the temperature of the first stage drying is independently 60-100 ℃, such as 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃ and the like, and the temperature of the second stage drying is independently 100-140 ℃, such as 100 ℃, 110 ℃, 120 ℃, 130 ℃ or 140 ℃ and the like.
As a further preferable technical scheme of the preparation method, the method comprises the following steps:
(1) coating the electrode slurry on a current collector, and performing two-section drying to obtain a first electrode diaphragm;
(2) coating electrode slurry on the electrode membrane in the step (1), and drying in a two-section mode to obtain a second electrode membrane, namely the electrode plate; the electrode plate comprises 2 layers of laminated electrode membranes, and the mass fraction of the binder in the second electrode membrane is not less than that of the binder in the first electrode membrane;
the preparation method of the electrode slurry in the steps (1) and (2) comprises the following steps: mixing a binder and a solvent, adding a conductive agent, continuously mixing to obtain a conductive adhesive, adding an electrode active substance, and mixing to obtain the electrode slurry; the solid content of the electrode slurry obtained in the step (1) and the solid content of the electrode slurry obtained in the step (2) are respectively 35-50%, and the viscosity of the electrode slurry is greater than 6000mPa & s;
in the two-stage drying in the step (1) and the step (2), the temperature of the first stage drying is independently 60-100 ℃, and the temperature of the second stage drying is independently 100-140 ℃.
In a third aspect, the present invention provides a lithium battery comprising an electrode sheet as defined in the first aspect. The lithium battery provided by the invention is generally a primary battery.
Compared with the prior art, the invention has the following beneficial effects:
(1) the electrode slice provided by the invention comprises at least 2 layers of electrode diaphragms, and the mass fraction of the binder in the electrode diaphragm far away from the electrode current collector is not lower than that of the binder in the electrode diaphragm close to the electrode current collector, so that the overall bonding performance of the electrode slice is enhanced, and the problems of slow solvent volatilization, floating of a conductive agent and cracking of the electrode slice caused by too thick single-layer electrode diaphragm are solved; the electrode plate provided by the invention has the advantages that the active substance loading capacity on the current collector in unit area is increased, the proportion of the inactive substance current collector in the battery is reduced, the energy density of the battery is greatly improved, and the electrode plate is particularly suitable for high-capacity carbon fluoride electrode plates.
(2) The preparation method provided by the invention is simple to operate, short in flow, suitable for industrial large-scale production, and capable of avoiding pole piece drying crack caused by large-scale volatilization of the solvent by improving the solid content of the slurry.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1
In this example, a positive electrode sheet was prepared as follows:
(1) weighing the positive active material graphite fluoride, the conductive agent carbon black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 90:5:5, completely dissolving the adhesive PVDF in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, and stirring and dispersing uniformly to obtain a high-viscosity first-layer slurry (with a solid content of 35% and a viscosity of 7500mPa & s) to be coated. And uniformly coating the first layer of slurry on one surface of the carbon-coated aluminum foil, and drying by a low-temperature 90 ℃ and high-temperature 110 ℃ sectional oven to obtain a first anode membrane, wherein the thickness of the first anode membrane is 120 mu m.
(2) Weighing positive active material graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 85:5:10, completely dissolving the adhesive PVDF in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, stirring and dispersing uniformly to obtain high-viscosity second-layer slurry (the solid content is 40%, and the viscosity is 10000mPa & s), uniformly coating the second-layer slurry on the dried first positive membrane, and drying in a low-temperature 90 ℃ and high-temperature 110 ℃ segmented oven to obtain a second positive membrane, wherein the thickness of the second positive membrane is 180 mu m. The thus-produced electrode sheet having the first positive electrode diaphragm and the second positive electrode diaphragm was the positive electrode sheet (high-capacity fluorocarbon electrode sheet), and the thickness of the high-capacity fluorocarbon electrode sheet was 300 μm.
The positive plate provided by the embodiment comprises a positive current collector carbon-coated aluminum foil and a positive active material film layer positioned on one surface of the positive current collector carbon-coated aluminum foil, wherein the positive active material film layer comprises a first positive membrane attached to the positive current collector and a second positive membrane stacked on the first positive membrane. The first positive electrode diaphragm comprises positive electrode active substance graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 90:5:5, the second positive electrode diaphragm comprises graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 85:5:10, the thickness of the positive electrode active substance film layer is 300 mu m, the thickness of the first positive electrode diaphragm is 40% of that of the positive electrode active substance film layer where the first positive electrode diaphragm is located, and the thickness of the second positive electrode diaphragm is 60% of that of the positive electrode active substance film layer where the second positive electrode diaphragm is located.
Example 2
In this example, a positive electrode sheet was prepared as follows:
(1) preparing a first positive electrode membrane: weighing the positive active material carbon fluoride, the conductive agent carbon black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 89:5:6, completely dissolving the adhesive PVDF in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, and stirring and dispersing uniformly to obtain a high-viscosity first-layer slurry (with the solid content of 35% and the viscosity of 8100mPa & s) to be coated. And uniformly coating the first layer of slurry on one surface of the carbon-coated aluminum foil, and drying by a low-temperature 90 ℃ and high-temperature 110 ℃ sectional oven to obtain a first anode membrane, wherein the thickness of the first anode membrane is 150 mu m.
(2) Preparing a second anode membrane: weighing the positive active substance carbon fluoride fiber, the conductive agent carbon black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 85:5:10, completely dissolving the adhesive PVDF in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, stirring and dispersing uniformly to obtain a high-viscosity second-layer slurry (the solid content is 37% and the viscosity is 9000mPa & s) to be coated, uniformly coating the second-layer slurry on the dried first positive membrane, and drying in a segmented oven at a low temperature of 90 ℃ and a high temperature of 110 ℃ to obtain a second positive membrane, wherein the thickness of the second positive membrane is 170 mu m. The thus-produced electrode sheet having the first positive electrode diaphragm and the second positive electrode diaphragm was the positive electrode sheet (high-capacity fluorocarbon electrode sheet), and the high-capacity fluorocarbon electrode sheet had a thickness of 320 μm.
The positive plate provided by the embodiment comprises a positive current collector carbon-coated aluminum foil and a positive active material film layer positioned on one surface of the positive current collector carbon-coated aluminum foil, wherein the positive active material film layer comprises a first positive membrane attached to the positive current collector and a second positive membrane stacked on the first positive membrane. The first positive electrode diaphragm comprises positive electrode active substance graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 89:5:6, the second positive electrode diaphragm comprises graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 85:5:10, the thickness of the positive electrode active substance film layer is 320 mu m, the thickness of the first positive electrode diaphragm is 47% of that of the positive electrode active substance film layer where the first positive electrode diaphragm is located, and the thickness of the second positive electrode diaphragm is 53% of that of the positive electrode active substance film layer where the second positive electrode diaphragm is located.
Example 3
In this example, a positive electrode sheet was prepared as follows:
(1) the positive active material fluorinated graphene, the conductive agent Keqin black and the adhesive polyvinylidene fluoride (PVDF) are weighed according to the mass ratio of 90:4:6, the adhesive PVDF is completely dissolved in the solvent NMP, the conductive agent is added, stirring and dispersing are carried out to form conductive adhesive, the fluorinated graphite active material is added, and the high-viscosity first-layer slurry to be coated is obtained after stirring and dispersing are carried out uniformly (the solid content is 35%, and the viscosity is 8121mPa & s). And uniformly coating the first layer of slurry on one surface of the carbon-coated aluminum foil, and drying by a low-temperature 60 ℃ and high-temperature 100 ℃ sectional oven to obtain a first anode membrane, wherein the thickness of the first anode membrane is 60 mu m.
(2) Weighing the positive active material graphene fluoride, the conductive agent Keqin black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 89:5:6, completely dissolving the adhesive PVDF in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, stirring and dispersing uniformly to obtain a high-viscosity second-layer slurry to be coated (the solid content is 35%, and the viscosity is 8303mPa & s). And uniformly coating the second layer of slurry on the dried first positive diaphragm, and drying by a low-temperature 90 ℃ and high-temperature 120 ℃ sectional oven to obtain a second positive diaphragm, wherein the thickness of the second positive diaphragm is 240 micrometers. The thus-produced electrode sheet having the first positive electrode diaphragm and the second positive electrode diaphragm was the positive electrode sheet (high-capacity fluorocarbon electrode sheet), and the thickness of the high-capacity fluorocarbon electrode sheet was 300 μm.
The positive plate provided by the embodiment comprises a positive current collector carbon-coated aluminum foil and a positive active material film layer positioned on one surface of the positive current collector carbon-coated aluminum foil, wherein the positive active material film layer comprises a first positive membrane attached to the positive current collector and a second positive membrane stacked on the first positive membrane. The first positive electrode diaphragm comprises positive electrode active substance fluorinated graphene, conductive agent Keqin black and adhesive polyvinylidene fluoride in a mass ratio of 90:4:6, the second positive electrode diaphragm comprises fluorinated graphene, conductive agent Keqin black and adhesive polyvinylidene fluoride in a mass ratio of 89:5:6, the thickness of the positive electrode active substance film layer is 300 mu m, the thickness of the first positive electrode diaphragm is 20% of that of the positive electrode active substance film layer where the first positive electrode diaphragm is located, and the thickness of the second positive electrode diaphragm is 80% of that of the positive electrode active substance film layer where the second positive electrode diaphragm is located.
Example 4
In this example, a positive electrode sheet was prepared as follows:
(1) preparing a first positive electrode membrane: weighing the positive active material graphite fluoride, the conductive agent carbon black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 85:5:10, completely dissolving the adhesive styrene butadiene rubber in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, and stirring and dispersing uniformly to obtain a high-viscosity first layer slurry to be coated (the solid content is 45%, and the viscosity is 17000mPa & s). And uniformly coating the first layer of slurry on one surface of the carbon-coated aluminum foil, and drying by a low-temperature 100 ℃ and high-temperature 120 ℃ sectional oven to obtain a first anode membrane, wherein the thickness of the first anode membrane is 90 mu m.
(2) Preparing a second anode membrane: weighing the positive active material graphite fluoride, the conductive agent carbon black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 80:5:15, completely dissolving the adhesive styrene butadiene rubber in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, stirring and dispersing uniformly to obtain the high-viscosity second-layer slurry to be coated (the solid content is 45%, and the viscosity is 16000mPa & s). And uniformly coating the second layer of slurry on the dried first positive diaphragm, and drying the first positive diaphragm by a low-temperature 100 ℃ and high-temperature 140 ℃ sectional drying oven to obtain a second positive diaphragm, wherein the thickness of the second positive diaphragm is 210 um. The thus-produced electrode sheet having the first positive electrode diaphragm and the second positive electrode diaphragm was the positive electrode sheet (high-capacity fluorocarbon electrode sheet), and the thickness of the high-capacity fluorocarbon electrode sheet was 300 μm.
The positive plate provided by the embodiment comprises a positive current collector carbon-coated aluminum foil and a positive active material film layer positioned on one surface of the positive current collector carbon-coated aluminum foil, wherein the positive active material film layer comprises a first positive membrane attached to the positive current collector and a second positive membrane stacked on the first positive membrane. The first positive electrode diaphragm comprises positive electrode active substance graphite fluoride, conductive agent carbon black and adhesive styrene butadiene rubber in a mass ratio of 85:5:10, the second positive electrode diaphragm comprises the positive electrode active substance graphite fluoride, the conductive agent carbon black and the adhesive styrene butadiene rubber in a mass ratio of 80:5:15, the thickness of the positive electrode active substance film layer is 300 mu m, the thickness of the first positive electrode diaphragm is 30% of that of the positive electrode active substance film layer where the first positive electrode diaphragm is located, and the thickness of the second positive electrode diaphragm is 70% of that of the positive electrode active substance film layer where the second positive electrode diaphragm is located.
Example 5
This example prepared a positive electrode sheet comprising three positive electrode film sheets as follows:
(1) the first layer of slurry same as that in the embodiment 1 is evenly coated on one side of the carbon-coated aluminum foil, and is dried by a low-temperature 90 ℃ and high-temperature 110 ℃ sectional oven to obtain a first positive membrane, wherein the thickness of the first positive membrane is 100 mu m.
(2) And (3) uniformly coating the second layer of slurry which is the same as that in the embodiment 1 on the dried first positive membrane, and drying the first positive membrane by a low-temperature 90 ℃ and high-temperature 110 ℃ sectional oven to obtain a second positive membrane, wherein the thickness of the second positive membrane is 120 mu m.
(3) Weighing the positive active material graphite fluoride, the conductive agent carbon black and the adhesive polyvinylidene fluoride (PVDF) according to a mass ratio of 80:5:15, completely dissolving the adhesive PVDF in a solvent NMP, adding the conductive agent, stirring and dispersing to form a conductive adhesive, adding the graphite fluoride active material, and stirring and dispersing uniformly to obtain high-viscosity third-layer slurry (the solid content is 40% and the viscosity is 9800mPa & s) to be coated. And uniformly coating the third layer of slurry on the dried second positive membrane, and drying by a low-temperature 90 ℃ and high-temperature 110 ℃ sectional oven to obtain a third positive membrane, wherein the thickness of the third positive membrane is 130 mu m.
The thus-prepared electrode sheet having the first positive electrode diaphragm, the second positive electrode diaphragm and the third positive electrode diaphragm was the positive electrode sheet (high-capacity fluorocarbon electrode sheet) having a thickness of 350 μm.
The positive plate provided by the embodiment comprises a positive current collector carbon-coated aluminum foil and a positive active material film layer positioned on one surface of the positive current collector carbon-coated aluminum foil, wherein the positive active material film layer comprises a first positive membrane attached to the positive current collector, a second positive membrane stacked on the first positive membrane and a third positive membrane stacked on the second positive membrane. The first positive electrode diaphragm comprises positive electrode active substance graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 90:5:5, the second positive electrode diaphragm comprises graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 85:5:10, the third positive electrode diaphragm comprises graphite fluoride, conductive agent carbon black and adhesive polyvinylidene fluoride in a mass ratio of 80:5:15, the thickness of the positive electrode active substance film layer is 400 mu m, the thickness of the first positive electrode diaphragm is 28.6% of that of the positive electrode active substance film layer in which the first positive electrode diaphragm is arranged, the thickness of the second positive electrode diaphragm is 34.3% of that of the positive electrode active substance film layer in which the second positive electrode diaphragm is arranged, and the thickness of the third positive electrode diaphragm is 37.1% of that of the positive electrode active substance film layer in which the third positive electrode diaphragm is arranged.
Comparative example 1
The positive electrode sheet provided by this comparative example was identical in structure, size and composition to the positive electrode sheet of example 1, except that it contained only the first positive electrode sheet having a thickness of 300 μm without the second positive electrode sheet. The preparation method is different from that of the embodiment 1 in that a first positive electrode membrane is obtained by one-time coating, the coating thickness of the first positive electrode membrane is thicker, and the preparation of a second positive electrode membrane is not carried out.
Comparative example 2
The positive electrode sheet provided in this comparative example was the same as the positive electrode sheet of example 1 in terms of structure, size, and composition, except that the first positive electrode sheet included graphite fluoride, carbon black as a conductive agent, and polyvinylidene fluoride as a binder in a mass ratio of 90:5:5, and the second positive electrode sheet included graphite fluoride, carbon black as a conductive agent, and polyvinylidene fluoride as a binder in a mass ratio of 90:7: 3. The preparation method is different from that of the embodiment 1 in that the composition of the positive electrode active material graphite fluoride, the conductive agent carbon black and the adhesive polyvinylidene fluoride in the positive electrode slurry for preparing the second positive electrode diaphragm is 90:7: 3.
Test method
The positive electrode sheets of the respective examples and comparative examples were observed for the presence of cracks and dry cracks in appearance.
The test results are given in the following table:
TABLE 1
It can be known from the above examples and comparative examples that the positive plates provided in examples 1 to 5 enhance the overall adhesion performance of the electrode sheet, avoid the problems of slow solvent volatilization, floating of conductive agent and cracking of the electrode sheet due to too thick single-layer electrode membrane, reduce the proportion of inactive material current collectors in the battery, greatly improve the energy density of the battery, and are particularly suitable for high-capacity carbon fluoride electrode sheets.
Comparative example 1 only contains one layer of positive pole diaphragm, although the thickness of positive pole active material rete is the same with example 1, the diaphragm has only been carried out once coating and has been formed to the pole piece, and single coating electrode thickness is too thick, and electrode adhesive strength is not enough, and contains a large amount of solvent in the thick electrode, and the spill-over of a large amount of solvent also easily leads to the pole piece fracture when toasting.
In comparative example 2, the mass fraction of the binder of the positive electrode membrane far away from the positive electrode current collector is lower than that of the positive electrode membrane close to the positive electrode current collector, so that the adhesion strength of the positive electrode membrane far away from the positive electrode current collector is poor, and the pole piece is cracked.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. An electrode sheet, characterized in that the electrode sheet comprises an electrode current collector and an electrode active material film layer on the electrode current collector, wherein the electrode active material film layer comprises at least 2 stacked electrode membrane sheets; on the same surface of the electrode current collector, the mass fraction of the binder in each electrode membrane which is not attached to the electrode current collector is not lower than that of the binder in the electrode membrane which is closer to the electrode current collector than the mass fraction of the binder in each electrode membrane.
2. The electrode sheet according to claim 1, wherein the electrode active material film layer is located on one or both surfaces of an electrode current collector;
preferably, the electrode plate is a positive electrode plate;
preferably, the electrode current collector comprises an aluminum foil and/or a carbon-coated aluminum foil;
preferably, in each of the electrode membranes, the electrode active material independently comprises any one of carbon fluoride, a carbon fluoride/manganese dioxide composite material or a carbon fluoride/sulfur composite material;
preferably, the carbon fluoride comprises any one or a combination of at least two of graphite fluoride, graphene fluoride, carbon fluoride nanotubes, carbon fluoride microspheres, carbon fluoride fibers, fluorinated hard carbon or fluorinated soft carbon;
preferably, the thickness of the electrode active material film layer is 300 μm or more;
preferably, the adhesive species of each of the electrode membranes are the same.
3. An electrode sheet as defined in claim 1 or 2, wherein the electrode membrane includes an electrode active material, a binder, and a conductive agent;
preferably, the binder comprises any one or a combination of at least two of polyvinylidene fluoride, sodium carboxymethyl cellulose, styrene butadiene rubber or acrylonitrile multipolymer;
preferably, the conductive agent includes any one or a combination of at least two of conductive carbon black, graphite, carbon nanofibers, carbon nanotubes, graphene, ketjen black, or acetylene black.
4. The electrode sheet according to any one of claims 1 to 3, wherein the electrode active material film layer comprises 2 electrode film sheets stacked, wherein a first electrode film sheet is located on the electrode current collector, and a second electrode film sheet is stacked on the first electrode film sheet;
preferably, the thickness of the first electrode membrane is 10-80% of the thickness of the electrode active material membrane layer where the first electrode membrane is located, and the thickness of the second electrode membrane is 20-90% of the thickness of the electrode active material membrane layer where the second electrode membrane is located;
preferably, the mass fraction of the binder in the first electrode membrane is 5-10%;
preferably, the mass fraction of the binder in the second electrode membrane is 5-15%.
5. A method for preparing an electrode sheet as claimed in any one of claims 1 to 4, characterized in that the method comprises the steps of:
(1) coating the electrode slurry on an electrode current collector, and drying to obtain a layer of electrode diaphragm;
(2) repeatedly coating the electrode slurry on the electrode slice obtained in the last operation and drying for at least 1 time to obtain the electrode slice; the electrode plate comprises at least 2 layers of stacked electrode films, and the mass fraction of the binder in each electrode film which is not attached to the electrode current collector is not lower than that of the binder in the electrode film which is closer to the electrode current collector than the mass fraction of the binder in the electrode film on the same surface of the electrode current collector.
6. The method according to claim 5, wherein the method for preparing the electrode slurry of steps (1) and (2) comprises: mixing a binder and a solvent, adding a conductive agent, mixing to obtain a conductive adhesive, adding an electrode active substance, and mixing to obtain the electrode slurry;
preferably, the mixing is stirring mixing and/or ball milling mixing;
preferably, the coating in the step (1) and the coating in the step (2) are independently one-time coating or multiple-time coating, and the number of times of the multiple-time coating is more than 2 times.
7. The production method according to claim 5 or 6, characterized in that the solid content of the electrode slurry of step (1) and step (2) is independently 35 to 50%;
preferably, the viscosity of the electrode slurry obtained in the step (1) and the viscosity of the electrode slurry obtained in the step (2) are both greater than 6000mPa & s;
preferably, in the step (2), each time the operation of coating the electrode slurry on the electrode membrane obtained in the previous operation is repeated, the mass fraction of the binder in the solid-phase substance of the electrode slurry is not less than the mass fraction of the binder in the solid-phase substance of the electrode slurry used in the previous coating.
8. The method according to any one of claims 5 to 7, wherein the drying in step (1) and the drying in step (2) are both two-stage drying;
preferably, in the step (1) and the step (2), the temperature of the first stage drying is independently 60-100 ℃, and the temperature of the second stage drying is independently 100-140 ℃.
9. The method for preparing according to any one of claims 5 to 8, characterized in that it comprises the steps of:
(1) coating the electrode slurry on a current collector, and performing two-section drying to obtain a first electrode diaphragm;
(2) coating electrode slurry on the electrode membrane in the step (1), and drying in a two-section mode to obtain a second electrode membrane, namely the electrode plate; the electrode plate comprises 2 layers of laminated electrode membranes, and the mass fraction of the binder in the second electrode membrane is not less than that of the binder in the first electrode membrane;
the preparation method of the electrode slurry in the steps (1) and (2) comprises the following steps: mixing a binder and a solvent, adding a conductive agent, mixing to obtain a conductive adhesive, adding an electrode active substance, and mixing to obtain the electrode slurry; the solid content of the electrode slurry obtained in the step (1) and the solid content of the electrode slurry obtained in the step (2) are respectively 35-50%, and the viscosity of the electrode slurry is greater than 6000mPa & s;
in the two-stage drying in the step (1) and the step (2), the temperature of the first stage drying is independently 60-100 ℃, and the temperature of the second stage drying is independently 100-140 ℃.
10. A lithium battery comprising the electrode sheet according to any one of claims 1 to 4.
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