CN111033813B - Method for producing an electrode by fibrillation of a binder - Google Patents
Method for producing an electrode by fibrillation of a binder Download PDFInfo
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- CN111033813B CN111033813B CN201880050167.5A CN201880050167A CN111033813B CN 111033813 B CN111033813 B CN 111033813B CN 201880050167 A CN201880050167 A CN 201880050167A CN 111033813 B CN111033813 B CN 111033813B
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- electrode component
- electrode
- binder
- equal
- carbon
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- 239000011230 binding agent Substances 0.000 title claims abstract description 96
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 206010061592 cardiac fibrillation Diseases 0.000 title description 6
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- 238000000034 method Methods 0.000 claims abstract description 195
- 238000002156 mixing Methods 0.000 claims abstract description 119
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 28
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims description 195
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 96
- 229910002804 graphite Inorganic materials 0.000 claims description 40
- 239000010439 graphite Substances 0.000 claims description 40
- 229910052799 carbon Inorganic materials 0.000 claims description 37
- 239000000463 material Substances 0.000 claims description 34
- 239000002131 composite material Substances 0.000 claims description 33
- 239000006182 cathode active material Substances 0.000 claims description 29
- 239000006183 anode active material Substances 0.000 claims description 28
- 239000007772 electrode material Substances 0.000 claims description 23
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- 238000003860 storage Methods 0.000 claims description 21
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
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- 239000010941 cobalt Substances 0.000 description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 14
- 229910017052 cobalt Inorganic materials 0.000 description 13
- -1 for example Substances 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 11
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 9
- 229910052748 manganese Inorganic materials 0.000 description 9
- 239000011572 manganese Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 6
- 239000011258 core-shell material Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000010452 phosphate Substances 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 6
- 229920000573 polyethylene Polymers 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910000676 Si alloy Inorganic materials 0.000 description 5
- 229910001128 Sn alloy Inorganic materials 0.000 description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 5
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- 239000002904 solvent Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- 239000004793 Polystyrene Substances 0.000 description 4
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 description 4
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 4
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 4
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 4
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- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
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- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
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- 238000001035 drying Methods 0.000 description 3
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- 229910052742 iron Inorganic materials 0.000 description 3
- 230000002427 irreversible effect Effects 0.000 description 3
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 2
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
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- 229920000098 polyolefin Polymers 0.000 description 2
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- 238000010298 pulverizing process Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- PMVSDNDAUGGCCE-TYYBGVCCSA-L Ferrous fumarate Chemical compound [Fe+2].[O-]C(=O)\C=C\C([O-])=O PMVSDNDAUGGCCE-TYYBGVCCSA-L 0.000 description 1
- JHKXZYLNVJRAAJ-WDSKDSINSA-N Met-Ala Chemical class CSCC[C@H](N)C(=O)N[C@@H](C)C(O)=O JHKXZYLNVJRAAJ-WDSKDSINSA-N 0.000 description 1
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- 239000004570 mortar (masonry) Substances 0.000 description 1
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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
- H01M4/04—Processes of manufacture in general
-
- 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
-
- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
Abstract
The invention relates to a method for producing an electrode (E) for an electrochemical cell, in particular for a battery cell, for example for a lithium cell. In order to be able to produce, for example, a homogeneous mixture of electrodes (E) for motor vehicle batteries, in particular for electric and/or hybrid vehicles, with improved properties and/or a layer thickness of significantly more than 100 μm, for example, by dry coating, at least one binder (B) is mixed with at least one electrode component (E1) in a high-shear-load mixing process to form a mixture (fB+E1) containing fibrillated binder, and at least one further electrode component (E2) is then added to the mixture (fB+E1) containing fibrillated binder by a lower-shear-load mixing process. The invention also relates to an electrode (E) produced thereby and to a battery equipped with an electrode (E) of the type described.
Description
Technical Field
The present invention relates to a method of producing an electrode for an electrochemical cell, in particular for a battery cell; an electrode produced thereby; and an electrochemical cell equipped with an electrode of this type.
Background
When batteries based on, for example, lithium or sodium batteries (e.g., lithium or sodium batteries) are used in mobile and stationary applications, they offer great potential for energy conservation and local emission avoidance.
The electrodes of lithium batteries are typically produced by a wet coating process. The procedure generally used herein mixes the electrode components with at least one solvent to produce a (high viscosity) liquid slurry or slurry, which is then used to form a layer or coating, for example, by a slot coater, knife coater or roll coater.
In order to remove the at least one solvent again, a long drying channel must be used for slow and controlled drying of the layer or coating. However, this results in long production times and high production costs, for example in the form of energy costs for drying and for providing, recovering and/or catalytically burning the at least one solvent.
Furthermore, wet coating processes can only produce electrodes with a limited layer thickness, for example up to 100 μm. However, for large battery packs (such as those required for electric vehicles), thicker electrodes would be desirable.
Documents US 2015/03030681 A1, WO 2005/008807 A2 (EP 1 644 136 A2), WO 2005/049700 A1, US 4,556,618, US 4,379,772, US 4,354,958, US 3,898,099 and US 6,335,857 B1 relate to a method for producing an electrode.
Disclosure of Invention
The present invention provides a method of producing an electrode (e.g., anode and/or cathode) for an electrochemical cell. The method can be used in particular for producing electrodes (for example anodes and/or cathodes) for battery cells, in particular for lithium cells or sodium cells, or for metal-air cells, for example for lithium ion cells and/or lithium metal cells or for sodium ion cells. The method can be designed in particular for producing electrodes (e.g. anodes and/or cathodes) for lithium batteries, for example for lithium ion batteries and/or lithium metal batteries.
In the method, in particular in method step a), at least one binder, in particular a polymeric binder, is mixed with at least one electrode component by a high shear mixing procedure to obtain a mixture comprising fibrillated binder.
In the method (then), in particular in method step b), at least one further electrode component is admixed by a low-shear mixing procedure into the mixture comprising fibrillated binder, in particular from method step a).
By means of the high shear mixing procedure, in particular a higher shear load than is achieved by means of the low shear mixing procedure and a shear load which is capable of fibrillating the at least one binder can be achieved. Thus, the high shear mixing procedure may also be referred to as a higher shear mixing procedure, among other things.
By a low shear mixing procedure, in particular, lower shear loads than are achieved by a high shear mixing procedure can be achieved. Thus, the low shear mixing procedure may also be referred to as a lower shear mixing procedure, among other things.
The expression "high shear mixing procedure" may here particularly refer to mixing procedures in which the particles move relative to each other, in particular in the absence of a lubricant (e.g. liquid), in particular in which high shear loading occurs with a large velocity gradient between the particles themselves and/or between the particles and the mixer wall. Here, particles under high shear loading are particularly likely to experience breakage, e.g., clean breakage. The high shear mixing procedure may be carried out, for example, by a jet method (in particular by jet milling) and/or by a three-roll mill and/or by a twin-screw extruder.
The expression "low-shear mixing procedure" may particularly denote a mixing procedure in which the material flows fold over one another, in particular in which the velocity gradient occurring between the particles themselves and/or between the particles and the mixer wall is small, as a result of which a low-shear loading occurs. Here, the particles under low shear load may in particular retain their shape and/or be only subjected to wear. The low shear mixing procedure may be performed, for example, by a plow mixer and/or a paddle mixer and/or a static mixer (e.g., based on an elongated flow caused by, for example, a series of widening and narrowing in the channel system), and/or by a gravity mixer.
The at least one binder may be fibrillated, for example, by relative movement and/or impact/bombardment on particles of the at least one electrode component, by a high shear mixing procedure, for example, by jet milling. Here, the at least one binder may be shaped to obtain in particular long fibrils (binder filaments). Fibrils of the at least one fibrillated binder (binder filaments) may then be attached in a distributed form to the surface of the at least one electrode component. The resulting mixture can thus be made into an electrode by a dry production procedure, in other words a coating process which is operated without solvent, for example by dry coating. As a result, it is possible to produce, for example, a vehicle battery for an electric vehicle and/or a hybrid vehicle and/or a plug-in hybrid vehicle and/or an electrode for a stationary battery with a layer thickness of significantly more than 100 μm in a time-saving and inexpensive manner, and in particular without the use of flammable, toxic and/or carcinogenic solvents.
However, the high shear mixing procedure does impose a high mechanical load on the at least one electrode component.
For example, in high shear mixing procedures (e.g., by jet milling), soft, brittle and coated electrode components, such as relatively soft layered intercalated graphite used as the anode active material, can be affected and/or altered by mechanical forces acting thereon; and/or brittle storage alloys (storage alloys) such as silicon alloys and/or tin alloys for use as anode active materials; and/or as a coated electrode component of an anode active material or a cathode active material (e.g., in the form of particles having a particle core and a particle shell surrounding the particle core (core-shell particles) and/or in the form of gradient material particles).
The term "gradient material particles" may particularly refer to particles that exhibit varying properties within the particles and/or from the surface of the particles or from the periphery of the particles to the core of the particles and/or exhibit a gradient with respect to the material.
By means of a high shear mixing procedure, it is possible to pulverize and/or grind, for example, soft, brittle and/or fragile electrode components, which may reduce their average particle size and/or optionally alter their particle shape.
For example, in the case of intercalated graphite and/or storage alloys, this in turn may lead to a reduction in its reversible storage capacity and/or an increase in irreversible loss, for example, due to the formation (especially increased formation) of a coating layer by the incorporation of lithium at its surface when the battery is first operated.
Second, the properties of the electrode, such as morphology, e.g. its porosity, can be adversely affected by producing small particles and/or changing the particle shape, e.g. by converting spherical graphite particles into lamellar graphite particles via shearing along the sliding face of the graphite, thus adversely affecting its wettability, current carrying capacity and/or capacitance, as well as its surface structure and surface reactivity.
Furthermore, functional and/or protective particle top layers on the coated electrode component in the form of particles, for example, particles having a particle core and a particle shell surrounding the particle core (core-shell particles) and/or gradient material particles, can be destroyed by high shear mixing procedures, for example. This may also lead to a reduced reversible storage capacity and/or an increased irreversible loss of the battery, and may be detrimental to long-term stability, for example, due to formation (especially increased formation) of a coating layer by binding of lithium on its surface when the battery is first operated.
The subdivision into at least two separate mixing stages has the advantageous effect that individual electrode components can be used in the individual mixing stages depending on the nature and/or function of the components. For example, in a high shear mixing procedure, mechanically stable electrode components and/or electrode components that are used as conductive additives or agents and that retain their function even at low average particle sizes, in particular may still be advantageous; and/or in a low shear mixing procedure, mechanically sensitive electrode components and/or electrode components that are used as electrode active materials and whose function may be affected by comminution can be used.
Furthermore, by using at least one electrode component in a high shear mixing procedure, the at least one binder can advantageously be fibrillated by the material that functions in the electrode under production, and this can have a beneficial effect on the specific energy density.
Thus, it is possible to produce a homogeneous mixture, in particular a mixture in which the at least one binder is homogeneously attached to particles (e.g. all particles) of the at least one electrode component and the at least one further electrode component; and electrodes, such as anodes or cathodes, can be produced from the mixture in a time-and cost-effective manner, for example by a dry production procedure and/or by coating, for example by dry coating, for example by current collectors or carrier substrates, which have improved properties and/or (also) have a layer thickness of significantly more than 100 μm, for example for motor vehicle batteries, for example for electric and/or hybrid vehicles and/or plug-in hybrid vehicles, and/or for stationary battery packs.
The at least one electrode component and/or the at least one further electrode component may be formed from or comprise: for example at least one conductivity additive, in particular for improving conductivity; and/or at least one electrode active material, in particular an energy storage, for example for the storage of lithium and/or surface-coated particles and/or gradient material particles.
For example, the at least one electrode component and/or the at least one further electrode component may be formed from or comprise: at least one conductive carbon, for example conductive graphite and/or at least one amorphous conductive carbon, in particular in the form of non-porous carbon particles, such as conductive carbon black, and/or carbon fibers and/or Carbon Nanotubes (CNT) and/or graphene and/or expanded graphite; and/or at least one electrically conductive metal, such as silicon and/or tin and/or another metal and/or alloy, e.g. in the form of a metalA form of powder; and/or at least one anode active material and/or at least one cathode active material, for example at least one intercalation material and/or composite material (recombination material), in particular at least one intercalation material and/or composite material of lithium or sodium, for example intercalated graphite and/or at least one intercalated amorphous carbon and/or intercalated amorphous carbon, for example hard carbon and/or soft carbon; and/or at least one storage alloy, for example at least one lithium storage alloy, for example a silicon alloy and/or a tin alloy, in particular as anode active material; and/or at least one metal oxide and/or metal phosphate, such as silicon oxide, in particular for forming or as anode active material, and/or at least one metal oxide, such as at least one layered oxide and/or at least one spinel, such as at least one oxide of nickel and/or cobalt and/or manganese, such as an oxide of lithium nickel and/or cobalt and/or manganese, and/or at least one metal phosphate, such as at least one phosphate of iron and/or manganese and/or cobalt, such as at least one phosphate of lithium iron and/or manganese and/or cobalt, based on, for example, the formula: liMPO 4 Wherein m=fe, mn and/or Co, especially as cathode active material; and/or at least one conductive additive-electrode active material composite (composition), for example at least one conductive additive-anode active material composite or conductive additive-cathode active material composite, for example at least one carbon-electrode active material composite, for example at least one carbon-anode active material composite or at least one carbon-cathode active material composite, for example at least one carbon-metal phosphate composite, for example in the form of conductive additive-coated, for example carbon-coated, electrode active material particles, in particular anode active material particles or cathode active material particles, for example in the form of carbon-coated metal phosphate particles and/or surface-coated particles, for example particles having a particle core and a particle shell surrounding the particle core (referred to as core-shell particles) and/or gradient material particles.
Expanded graphite may particularly refer to materials produced by expansion of graphite and used to provide graphene and/or contain graphene.
The composite material may especially refer to an active material whose mode of action is based on a composite and/or phase inversion reaction, such as li+al→lial.
Hard carbon is understood to mean, in particular, carbon which is intercalated and/or intercalated, in particular relatively stable amorphous carbon, in particular carbon which is not graphitizable and which can be used as anode active material.
Soft carbon is understood to mean, in particular, carbon which can be intercalated and/or intercalated, in particular relatively stable amorphous carbon, in particular carbon which can be graphitized and which can be used as anode active material.
The high-shear mixing procedure, in particular in process step a), can take place or take place in particular by means of jet mills and/or three-roll mills and/or twin-screw extruders and/or opposed-jet fluidized-bed mills and/or ball mills and/or mortar mills and/or roller apparatuses (in an operation known as rolling out) and/or tablet presses. The high shear force can be formed here, for example, by a relative movement of the at least one electrode component with respect to at least one fibril-forming binder, in particular a polymer binder. The relative movement of the materials with respect to one another can be achieved in a particularly simple manner by means of a roller device and/or a tablet press.
In a high shear rate mixing procedure, in particular in method step a), it may be advantageous to use a suitable particle size distribution of the at least one binder and the individual electrode components. In particular, the at least one electrode component may have a larger average particle size than the at least one binder.
In a further embodiment, the high shear rate mixing procedure, in particular in method step a), takes place or is carried out by jet milling. By means of the jet mill, a uniform distribution of the at least one binder on the at least one electrode component can advantageously be achieved in a particularly simple and time-saving manner. With jet mills, the components are mixed using, in particular, a gas (e.g., air) at very high speeds (possibly up to the speed of sound). Here, the actual mixing procedure may advantageously last only about 1-2 seconds and may generate very high shear forces and thus very high shear loads. As a result, at least one binder can advantageously be fibrillated very efficiently and rapidly. The embodiments set forth above and below are of particular interest in connection with the use of at least one electrode component in a high-shear mixing procedure, for example having high mechanical stability and/or very functionality independent of comminution, and at least one further electrode component in a low-shear mixing procedure, for example having higher sensitivity and/or functionality dependent of comminution, based on very high mechanical loads, for example the damaging effects associated with very high shear loads, in the case of jet mills used in high-shear mixing procedures.
The jet mill is preferably operated such that at least one electrode material is not damaged or at least only minimally damaged, or where appropriate only controllably damaged. For example, to apply at least one adhesive, the jet mill may be operated at a minimum desired speed and/or residence time. For example, the operating conditions of the jet mill may be determined by a series of experiments. In this case, the properties of at least one electrode component can be studied, for example, by Scanning Electron Microscopy (SEM).
In the high-shear mixing procedure, the at least one binder may be fibrillated using in particular at least one electrode component which is more mechanically stable than at least one further electrode component (in particular the component to be mixed in the low-shear mixing procedure), in particular in the high-shear mixing procedure or under the conditions of the high-shear mixing procedure, and/or which has no or little adverse consequences on its mechanical load and the functional capacity of the electrode with which it is equipped, for example comminution, compared to the at least one further electrode component (in particular the component to be mixed in the low-shear mixing procedure). In this case, mechanical loading or comminution of the at least one electrode component in the high shear mixing procedure may in particular be tolerated and/or the at least one electrode component may be used as sacrificial material.
In a subsequent separate low-shear mixing procedure, the at least one further electrode component is mechanically less stable or more sensitive than the at least one electrode component mixed in the high-shear mixing procedure, for example based on its mechanical stability and/or sensitive coating, and can then be homogeneously incorporated into the mixture comprising fibrillated binder with lower mechanical loading.
In one embodiment, the at least one electrode component is more mechanically stable than at least one further electrode component, in particular in or under the conditions of a high shear mixing procedure, and/or the functionality of the at least one electrode component is less affected than the functionality of the at least one further electrode component, in particular by the high shear mixing procedure or under the conditions of a high shear mixing procedure and/or by mechanical loads such as crushing. Thus, the individual electrode components can be used advantageously according to their properties and/or their functionality.
The higher mechanical stability and/or lower impact on functionality of the at least one electrode component relative to the at least one further electrode component may be achieved in a variety of ways.
In another embodiment, for example, the at least one electrode component, for example in the case of spherical particles, has an average particle size, in particular a primary particle size, of less than 10 μm; and/or, for example in the case of fibrous and/or tubular particles, having an average particle length (e.g. average fiber length and/or tube length) of, for example, less than 10 μm; and/or, for example in the case of layered particles, having an average planar particle diameter (particle plane diameter) of less than 10 μm, or using such dimensions/lengths/diameters. For example, the at least one electrode component may have or use an average particle size, in particular a primary particle size, of less than or equal to 8 μm, in particular less than or equal to 6 μm; and/or an average grain length (e.g., average fiber length and/or tube length) of less than or equal to 8 μm, especially less than or equal to 6 μm; and/or an average planar particle diameter of less than or equal to 8 μm, in particular less than or equal to 6 μm.
Experimental studies have shown that: the high shear mixing procedure (e.g., by jet milling) produces a minimum achievable and thus stable average particle size or particle length (e.g., fiber length and/or tube length) or planar particle size, particularly in the range of greater than or equal to 4 μm to less than or equal to 6 μm; and in this case particles having a particle size or particle length (e.g. fiber length and/or tube length) or a planar particle size in this range will not be crushed further, especially from the physical boundary conditions of the mixer, e.g. mill, and the properties of the material.
Since the at least one electrode component has an average particle diameter or average particle length (e.g., average fiber length and/or tube length) or average planar particle diameter of less than 10 μm, such as less than or equal to 8 μm, especially less than or equal to 6 μm, the pulverizing effect acting thereon by the high shear mixing procedure can be reduced, since in this case the particles are mostly only pulverized to an average particle diameter or average particle length (e.g., average fiber length and/or tube length) or average planar particle diameter, such as in the range of greater than or equal to 4 μm to less than or equal to 6 μm. In this way, mechanical stability of the at least one electrode component can be obtained in a high shear mixing procedure.
In a particular configuration, the at least one electrode component has an average particle size in the range of greater than or equal to 0.01 μm to less than or equal to 6 μm, for example in the range of greater than or equal to 4 μm to less than or equal to 6 μm; and/or having an average grain length (e.g., average fiber length and/or tube length) in the range of greater than or equal to 0.01 μm to less than or equal to 6 μm, such as in the range of greater than or equal to 4 μm to less than or equal to 6 μm; and/or having an average planar particle diameter in the range of greater than or equal to 0.01 μm to less than or equal to 6 μm, for example in the range of greater than or equal to 4 μm to less than or equal to 6 μm; or such size/length/diameter may be used. Thus, the pulverizing effect acting thereon in the high-shear mixing procedure can be minimized, and high mechanical stability of the at least one electrode component can be achieved in the high-shear mixing procedure.
In another embodiment, the at least one further electrode component has a larger average particle diameter, in particular a primary particle diameter, than the at least one electrode component, for example in the case of spherical particles; and/or, for example, in the case of fibers and/or tubular particles, having a greater average particle length (e.g., a greater average fiber length and/or tube length); and/or, for example in the case of lamellar particles, a larger average planar particle diameter; or use such dimensions/length/diameter. Because the at least one electrode component has a smaller average particle size and/or smaller average particle length (e.g., smaller average fiber length and/or tube length), and/or smaller average planar particle size, as compared to the at least one other electrode component, the at least one electrode component may be more mechanically stable in a high shear rate mixing procedure as compared to the at least one other electrode component.
For example, the at least one other electrode component may have or use an average particle size, especially a primary particle size, of greater than or equal to 10 μm or greater than 8 μm or greater than 6 μm; and/or average particle length (e.g., average fiber length and/or tube length) and/or average planar particle size. For example, the at least one further electrode component may have or use an average particle diameter, in particular a primary particle diameter, of greater than or equal to 10 μm or greater than or equal to 12 μm or greater than or equal to 15 μm, for example in the range of greater than or equal to 10 μm to less than or equal to 20 μm; and/or greater than or equal to 10 μm or greater than or equal to 12 μm or greater than or equal to 15 μm, such as an average grain length (e.g., average fiber length and/or tube length) in the range of greater than or equal to 10 μm to less than or equal to 20 μm; and/or greater than or equal to 10 μm or greater than or equal to 12 μm or greater than or equal to 15 μm, such as an average planar particle size in the range of greater than or equal to 10 μm to less than or equal to 20 μm.
By using the at least one further electrode component in a low-shear mixing procedure, the at least one further electrode component can be protected from, for example, severe mechanical loading and/or comminution (especially due to high-shear mixing procedures), and can therefore be treated in such a way that the material is retained as much as possible even for relatively sensitive or mechanically less stable materials (such as relatively soft lamellar intercalated graphite) and/or coated particles (such as core-shell particles) and/or gradient material particles.
Alternatively or additionally, regarding the above-mentioned gradient between the at least one electrode component and the at least one further electrode component based on their mechanical stability of average particle size, particle length (e.g. fiber length and/or tube length) and/or planar particle size, it is possible to select that the at least one electrode component is less affected in its functionality due to the high shear mixing procedure compared to the at least one further electrode component.
In another embodiment, the at least one electrode component comprises or is formed from, for example: at least one conductivity additive, in particular for improving conductivity. More particularly, the at least one electrode component may comprise or be formed from: at least one conductive carbon and/or at least one conductive metal.
The functionality of conductive additives (e.g. conductive carbon, e.g. conductive graphite and/or amorphous conductive carbon, such as conductive carbon black, and/or carbon fibers and/or Carbon Nanotubes (CNT) and/or graphene and/or expanded graphite and/or conductive metals, especially for improving conductivity) is typically much less affected by high mechanical loads and/or comminution than the functionality of e.g. electrode active materials, especially for energy storage (e.g. for storage of lithium), e.g. anode active materials and/or cathode active materials, e.g. intercalated and/or composite materials, e.g. intercalated graphite and/or intercalated amorphous carbon, e.g. hard carbon and/or soft carbon and/or storage alloys. Furthermore, depolymerization and subsequent fibrillation of the at least one binder may be advantageously assisted by the application of conductive additives, such as conductive carbon, e.g. conductive graphite and/or conductive carbon black.
In one configuration of this embodiment, the at least one electrode component comprises or is formed from conductive graphite. The conductive graphite has a lower average particle diameter, for example, in the range of greater than or equal to 4 μm to less than or equal to 10 μm, and a lower reversible storage capacity and/or a higher reaction surface area, and thus has a higher irreversible capacity loss than, for example, intercalated graphite upon the first lithiation or first operation of the battery, and thus is not ideal for intercalation of lithium. The at least one electrode component used in the high mechanical loading process step, in particular in method step a), may be, for example, conductive graphite sold under the trade names KS4 and/or KS6 by Imerys (Timcal) or sold under different trade names by different manufacturers.
In another alternative or additional configuration of this embodiment, the at least one electrode component comprises or is formed from: amorphous conductive carbon, particularly in the form of non-porous carbon particles. The at least one electrode component may, for example, comprise or consist of conductive carbon black.
In another alternative or additional configuration of this embodiment, the at least one electrode component comprises or is formed from: carbon fibers and/or Carbon Nanotubes (CNTs).
The carbon fibers and/or carbon nanotubes are advantageously particularly suitable for fibrillation of the at least one binder. Furthermore, by using carbon fibers and/or carbon nanotubes in the high shear mixing procedure, the carbon fibers and/or carbon nanotubes may be dispersed particularly well, and problems that may occur with other mixing procedures (especially low shear mixing procedures) during dispersion or during uniform incorporation may be solved by dispersing the carbon fibers and/or carbon nanotubes. Jet milling enables the incorporation or dispersion of carbon fibers and/or carbon nanotubes by mixing in a particularly simple manner. For example, the at least one electrode component may comprise or be formed from: average diameters are much smaller than 1 μm, usually smaller than or equal to 200nm; and/or average grain length, e.g., fiber length and/or tube length, in the range of greater than or equal to 2 μm to less than or equal to 200 μm, e.g., carbon fibers in the range of greater than or equal to 2 μm to less than or equal to 20 μm; and/or an average diameter of less than or equal to 50nm, for example in the range of greater than or equal to 0.3nm to less than or equal to 50 nm; and/or average particle length, e.g., average fiber length and/or tube length, in the range of greater than or equal to 10nm to less than or equal to 50cm, e.g., greater than or equal to 10nm to less than or equal to 20 μm.
If the mechanical stabilization already described is to be achieved additionally by a low average particle length (e.g. fiber length and/or tube length), the at least one electrode component may comprise or use carbon fibers having an average particle length (e.g. average fiber length and/or tube length) e.g. in the range of more than or equal to 2 μm to less than 10 μm or less than or equal to 8 μm or less than or equal to 6 μm, and/or carbon nanotubes having an average particle length (e.g. average fiber length and/or tube length) e.g. in the range of more than or equal to 10nm to less than 10 μm or less than or equal to 8 μm or less than or equal to 6 μm.
In another alternative or additional configuration of this embodiment, the at least one electrode component comprises or is formed from: graphene and/or expanded graphite.
In another alternative or additional configuration of this embodiment, the at least one electrode component comprises: at least one conductive additive-electrode active material composite, for example at least one conductive additive-anode active material composite or at least one conductive additive-cathode active material composite, for example at least one carbon-electrode active material composite, such as at least one carbon-anode active material composite or at least one carbon-cathode active material composite, for example at least one carbon metal phosphate composite, in particular in the form of conductive additive-coated electrode active material particles, for example in the form of conductive additive-coated anode active material particles or in the form of conductive additive-coated cathode active material particles, for example in the form of carbon-coated electrode active material particles, for example in the form of carbon-coated anode active material particles or in the form of particles of carbon-coated cathode active material particles, for example particles of carbon-coated metal phosphate, in particular with an average particle diameter of less than 10 μm, for example less than or equal to 8 μm or less than or equal to 6 μm, for example less than or equal to 4 μm or less than or equal to 2 μm or less than or equal to 1 μm. This type of composite can be processed into conductive additives, used in part as active materials, and mechanically stable.
In another alternative or additional configuration of this embodiment, the at least one electrode component comprises or is formed from: at least one conductive metal, such as silicon and/or tin and/or another metal and/or alloy, for example in the form of a metal powder.
In a further alternative or additional embodiment, the at least one further electrode component comprises at least one electrode active material, in particular for energy storage, for example for lithium storage. For example, the at least one additional electrode component may comprise or be formed from: at least one anode active material and/or cathode active material, such as at least one intercalation material and/or composite material, such as at least one lithium or sodium intercalation and/or composite material.
In one configuration of this embodiment, the at least one additional electrode component may comprise or be formed from: intercalated graphite and/or intercalated amorphous carbon, such as hard carbon and/or soft carbon, particularly as anode active materials. By blending relatively soft lamellar intercalated graphite in the low shear mixing procedure and especially not in the high shear mixing procedure, a sharp decrease in the particle size of the intercalated graphite and/or severe damage to the intercalated graphite, e.g. due to its slip, can advantageously be prevented in the high shear mixing procedure, e.g. by jet milling.
In another alternative or additional configuration of this embodiment, the at least one additional electrode component comprises or is formed from: storing the alloy. In particular, the at least one further electrode component may comprise or be formed from: lithium storage alloys, such as silicon and/or tin alloys.
In another alternative or additional configuration of this embodiment, the at least one additional electrode component comprises or is formed from: at least one metal oxide and/or metal phosphate. For example, the at least one additional electrode component may comprise or be formed from: silicon oxide, in particular for forming or as anode active material; and/or at least one metal oxide, in particular at least one layered oxide and/or at least one spinel, for example at least one nickel and/or cobalt and/or manganeseFor example oxides of lithium nickel and/or cobalt and/or manganese; and/or at least one metal phosphate, for example at least one phosphate of iron and/or manganese and/or cobalt, for example at least one phosphate of lithium iron and/or manganese and/or cobalt based on the formula: liMPO 4 M=fe, mn and/or Co, especially as cathode active material.
In principle, the at least one electrode component and/or the at least one further electrode component may comprise or be formed from: spherical and/or non-spherical particles.
Alternatively or additionally to the above measures, it is possible to achieve a higher mechanical stability and/or less affected functionality of the at least one electrode component than the at least one further electrode component by means of a corresponding particle shape.
In another alternative or additional embodiment, the at least one electrode component comprises or is formed from spherical particles. For example, the at least one electrode component may comprise or be formed from: stable and/or compact spherical particles. Spherical particles, such as MCMB (mesophase carbon microbeads), may have a higher mechanical stability than non-spherical particles, such as lamellar graphite, e.g. intercalated graphite.
In a further alternative or additional embodiment, the at least one further electrode component accordingly comprises non-spherical particles, for example, if non-spherical particles are to be used in the method, in particular based on a lower mechanical load in a low shear mixing procedure (as already explained).
Alternatively or additionally to the above measures, it is possible to achieve a higher mechanical stability and/or less affected functionality of the at least one electrode component than the at least one further electrode component by means of a corresponding particle structure.
Thus, in another alternative or additional embodiment, the at least one electrode component is free of surface coated particles and/or gradient material particles. For example, the at least one electrode component may be free of particles having a particle core and a particle shell surrounding the particle core (referred to as core-shell particles), and/or free of particles of gradient material. This approach may be used, in particular, if surface-coated particles or gradient material particles are known to have relatively low mechanical stability. During the high shear mixing procedure, the surface coating of the particles and/or the gradient material particles may be damaged and/or destroyed. Thus, it may be advantageous to incorporate them by mixing in a low shear mixing procedure.
Thus, in another alternative or additional embodiment, the at least one further electrode component comprises surface-coated particles, such as particles having a particle core and a particle shell surrounding the particle core (referred to as core-shell particles), and/or gradient material particles.
In a further alternative or additional embodiment, the at least one electrode component is free of electrode active material, in particular for energy storage, for example for storage of lithium, for example free of anode active material and/or free of cathode active material. As already explained, the functionality of the electrode active material is generally more affected by mechanical loading and/or comminution than the functionality of the conductive additive.
However, as already stated, damage and/or destruction of surface coating and/or gradient material particles on the particles and/or the influence on the functionality of the electrode active material can optionally be counteracted by a low average particle diameter and/or a low average particle length (e.g. a low average fiber length and/or tube length) and/or a low average planar particle diameter of, in particular, less than 10 μm, such as less than or equal to 8 μm, such as less than or equal to 6 μm. Thus, for example, any conductive additive-electrode active material composite (especially in the form of conductive additive coated electrode active material particles) having an average particle size of less than 10 μm, such as less than or equal to 6 μm, especially less than or equal to 4 μm or less than or equal to 2 μm or less than or equal to 1 μm, such as a carbon-metal phosphate composite (e.g., in the form of carbon coated metal phosphate particles) may be mechanically stable in a high shear mixing procedure.
In addition to the effect that the gradient and/or functionality of the mechanical stability of at least one electrode component relative to at least one other electrode component is affected by the average particle size and/or average particle length (e.g. average fiber length and/or tube length) and/or average planar particle size, and/or by the use as a conductive additive or electrode active material, and/or by the particle shape and/or by the particle configuration, the gradient and/or functionality of the mechanical stability of different electrode components may be difficult, especially if the electrode components have one or more of the same characteristics as described above, and may for example be determined, especially on the basis of a series of experiments only: electrode compositions that are graded with respect to each other, as well as the particular type of high shear mixer to be used, such as a jet mill or other high shear mixer, and the mixtures produced under comparable mixing conditions are investigated, for example, by Scanning Electron Microscopy (SEM) and/or battery functional testing.
The at least one binder, in particular the polymeric binder, may comprise or be formed of: for example at least one lithium ion conducting or lithium ion conducting polymer, for example at least one polyalkylene oxide, for example polyethylene oxide (PEO), and/or at least one polyester and/or at least one polyacrylate and/or at least one polymethacrylate, for example polymethyl methacrylate (PMMA), and/or at least one polyacrylonitrile and/or at least one fluorinated and/or non-fluorinated polyolefin, for example polyvinylidene fluoride (PvdF) and/or polytetrafluoroethylene (PTFE, teflon) and/or Polyethylene (PE) and/or polypropylene (PP), and/or copolymers thereof, for example polyethylene oxide-polystyrene copolymers (PEO-PS copolymers) and/or acrylonitrile-butadiene-styrene copolymers (ABS).
In another alternative or additional embodiment, the at least one binder (in particular a polymeric binder) comprises or is formed from: at least one lithium ion conducting or lithium ion conducting polymer and/or copolymer thereof. Accordingly and advantageously, not only the adhesion but also the lithium ion conductivity can be provided within the electrode by means of the at least one binder. For example, the at least one binder (especially a polymeric binder) may comprise or be formed from: at least one polyalkylene oxide, such as polyethylene oxide; and/or at least one polyester and/or at least one polyacrylate and/or at least one polymethacrylate, for example polymethyl methacrylate, and/or at least one polyacrylonitrile; and/or copolymers thereof, such as polyethylene oxide-polystyrene (PEO-PS copolymer) and/or acrylonitrile-butadiene-styrene copolymer (ABS). For example, the at least one binder (especially a polymeric binder) can comprise or be formed from: at least one polyalkylene oxide, in particular polyethylene oxide, and/or copolymers thereof.
The at least one binder may be used in an amount that ensures that the at least one binder is equally attached to all particles of the at least one electrode component and the at least one further electrode component. In this case, a particle surface which covers the at least one electrode component and the at least one further electrode component in particular completely can be avoided. Preferably only point contacts are formed between the at least one binder and the particles of the at least one electrode component and the at least one further electrode component. In this way, the surface area available for the actual storage reaction can be maximized.
In another alternative or additional embodiment, greater than or equal to 0.1 wt% to less than or equal to 10 wt%, such as greater than or equal to 0.2 wt% to less than or equal to 5 wt% of the at least one binder is used, based on the total weight of the electrode components of the electrode. This has proven to be advantageous in achieving uniform attachment of the at least one binder in point contact to all particles of the electrode component and thus maximizing the surface area available for actual storage reactions.
In another alternative or additional embodiment, from greater than or equal to 0.1 wt% to less than or equal to 50 wt%, such as from greater than or equal to 0.1 wt% to less than or equal to 30 wt%, such as from greater than or equal to 0.25 wt% to less than or equal to 20 wt%, such as from greater than or equal to 0.5 wt% to less than or equal to 15 wt% or less than or equal to 10 wt% or less than or equal to 5 wt% of at least one electrode component is used, based on the total weight of the electrode components.
In another alternative or additional embodiment, from greater than or equal to 0.1 wt% to less than or equal to 98 wt%, such as from greater than or equal to 0.1 wt% to less than or equal to 90 wt%, such as from greater than or equal to 0.1 wt% to less than or equal to 80 wt% of at least one additional electrode component is used, based on the total weight of the electrode components of the electrode.
In this method, for example, the at least one binder (e.g., if two or more different binders are to be used) and/or the at least one electrode component (e.g., if two or more electrode components are to be used) can be added in multiple stages in a high shear mixing procedure. For example, in a high shear mixing procedure, in particular in method step a), it is possible to first add a first binder, then one or more further binders, and mix them with the at least one electrode component; and/or first blending the at least one binder with a first electrode component of the at least one electrode component and then with a second electrode component of the at least one electrode component and mixing.
However, in another embodiment, especially in method step a), a first high shear mixing procedure is used to mix at least one first binder with at least one electrode component to obtain a first mixture comprising fibrillated binder; and at least one second high shear mixing procedure is used to mix at least one second binder with at least one electrode component (which may be, for example, the same as or different from the at least one electrode component used in the first mixing procedure) to obtain at least one second mixture comprising fibrillated binder. This may facilitate binder fibrillation and/or mixing of the binder with the electrode components.
In another alternative or additional embodiment, in particular in method step a), a first high shear mixing procedure is used to mix at least one binder, optionally at least one first binder, with a first electrode component of the at least one electrode component to obtain a first mixture comprising fibrillated binder; and at least one second high shear mixing procedure is used to mix at least one binder (which may be, for example, the same as or different from the at least one binder used in the first mixing procedure; for example, at least one second binder) with the second electrode component of the at least one electrode component to obtain at least one second mixture comprising fibrillated binder. This may facilitate mixing of the binder with the electrode components and/or binder fibrillation.
In the above embodiment, in particular in method step b), the first mixture comprising fibrillated binder and the second mixture comprising fibrillated binder may then be mixed with at least one further electrode component by a low shear mixing procedure.
In another embodiment, the method is designed for producing an anode. In this case, the at least one further electrode component may comprise or be formed from: in particular at least one anode active material, such as intercalated graphite and/or intercalated amorphous carbon, such as hard carbon and/or soft carbon, and/or a storage alloy, such as a lithium storage alloy, such as a silicon alloy and/or a tin alloy, and/or a metal oxide, in particular a silicon oxide. For example, greater than or equal to 80 wt%, alternatively greater than or equal to 90 wt% of at least one anode active material can be used, based on the total weight of the electrode components of the anode.
In one configuration of this embodiment, greater than or equal to 5 wt.% to less than or equal to 10 wt.% of at least one conductive carbon, such as amorphous conductive carbon, especially conductive carbon black, and/or conductive graphite and/or carbon fibers and/or carbon nanotubes and/or graphene and/or expanded graphite, and/or greater than or equal to 5 wt.% to less than or equal to 10 wt.% of at least one conductive metal, based on the total weight of the electrode components of the anode (especially in the form of at least one electrode component), is used.
In this case, a first high shear mixing procedure may be used to mix the at least one binder with the at least one conductive carbon (e.g., in the form of conductive carbon black) to obtain a first mixture comprising fibrillated binder; and a second high shear mixing procedure may be used to mix the at least one binder with the at least one conductive metal to obtain a second mixture comprising fibrillated binder.
The first mixture comprising the fibrillated binder and the second mixture comprising the fibrillated binder may then be mixed with the at least one anode active material, such as intercalated graphite and/or intercalated amorphous carbon, such as hard and/or soft carbon, and/or a storage alloy, such as a lithium storage alloy, such as a silicon alloy and/or a tin alloy, and/or a metal oxide, in particular a silicon oxide, by a low shear mixing procedure.
In another embodiment, the method is designed for producing a cathode. In this case, the at least one further electrode component may comprise or be formed from: in particular at least one cathode active material, such as at least one metal oxide and/or metal phosphate, such as at least one metal oxide, in particular at least one layered oxide and/or at least one spinel, such as at least one oxide of nickel and/or cobalt and/or manganese, such as an oxide of lithium nickel and/or cobalt and/or manganese, and/or at least one metal phosphate, such as at least one phosphate of iron and/or manganese and/or cobalt, such as at least one phosphate of lithium iron and/or manganese and/or cobalt, such as based on the formula: liMPO 4 Where m=fe, mn, and/or Co. The at least one further electrode component, in particular the at least one cathode active material, may be used, for example, in an amount of greater than or equal to 80 wt%, optionally greater than or equal to 90 wt%, based on the total weight of the electrode components of the cathode. Here, the at least one additional electrode component, particularly the at least one cathode active material, may have an average particle diameter, for example, a primary particle diameter, in the range of greater than or equal to 10 μm to less than or equal to 20 μm.
Here, the at least one electrode component may be or comprise, for example, at least one electrically conductive carbon, such as electrically conductive graphite and/or electrically conductive carbon black.
In one configuration of this embodiment, greater than or equal to 0.25 wt% to less than or equal to 20 wt%, such as greater than or equal to 0.5 wt% to less than or equal to 10 wt%, and especially greater than or equal to 0.5 wt% to less than or equal to 5 wt% of the at least one electrode component, such as at least one conductive carbon, such as conductive graphite and/or conductive carbon black, is used based on the total weight of the electrode components of the cathode.
In another particular configuration of this embodiment, the at least one other electrode component, in particular the at least one cathode active material, comprises or is formed from: at least one metal oxide, for example at least one layered oxide and/or at least one spinel, for example at least one oxide of nickel and/or cobalt and/or manganese, for example lithium nickel and/or cobalt and/or manganese oxide. In this case, the at least one additional electrode component, in particular the at least one cathode active material, may also have an average particle diameter, for example, a primary particle diameter, in the range of greater than or equal to 10 μm to less than or equal to 20 μm. The at least one further electrode component, for example at least one metal oxide, may be used, for example, in an amount of greater than or equal to 50 wt%, for example greater than or equal to 70 wt% or greater than or equal to 80 wt% or greater than or equal to 85 wt%, optionally greater than or equal to 90 wt%, based on the total weight of the electrode components of the cathode.
In another alternative or additional specific configuration of this embodiment, the at least one electrode component comprises or is formed from: at least one conductive additive, such as at least one conductive carbon, such as conductive graphite and/or conductive carbon black, and/or at least one metal phosphate, such as at least one iron and/or manganese and/or cobalt phosphate, such as at least one lithium iron and/or manganese and/or cobalt phosphate based on, for example, the formula: liMPO 4 Wherein m=fe, mn and/or Co, e.g. an average particle size, e.g. a primary particle size of less than 10 μm or less than or equal to 8 μm or less than or equal to 6 μm, e.g. less than or equal to 4 μm, e.g. less than or equal to 2 μm or less than or equal to 1 μm, and/or at least one conductive additive-cathode active material composite, e.g. at least one carbon-cathode active material composite, e.g.At least one carbon-metal phosphate composite, for example in the form of conductive additive coated (e.g., carbon coated) cathode active material particles, for example in the form of carbon coated metal phosphate particles, having an average particle size of less than 10 μm or less than or equal to 8 μm or less than or equal to 6 μm, for example less than or equal to 4 μm or less than or equal to 2 μm or less than or equal to 1 μm.
The at least one electrode component, such as at least one conductive additive, such as conductive carbon, such as conductive graphite and/or conductive carbon black, and/or the at least one metal phosphate and/or combinations thereof, such as the at least one carbon-cathode active material composite, such as at least one carbon-metal phosphate composite, such as in the form of conductive additive coated cathode active material particles, such as in the form of carbon coated metal phosphate particles having an average particle size of less than 10 μm or less than 8 μm or less than 6 μm, such as less than or equal to 4 μm, and/or especially 2 μm or less than 1 μm, may be used, such as in the range of from greater than or equal to 0.1 wt% to less than 50 wt%, such as in the range of greater than or equal to 0.1 wt% to less than 30 wt%, especially in the range of greater than or equal to 0.5 wt% to less than or equal to 15 wt%, based on the total weight of the electrode component of the cathode.
In another embodiment, the at least one binder is mixed with the at least one electrode component in a low shear pre-mixing procedure upstream of the high shear mixing procedure to obtain a pre-mixture, which is then mixed in the high shear mixing procedure, in particular in method step a), to obtain a mixture comprising fibrillated binder. The premixing procedure may be carried out in particular in a process step a 0) upstream of process step a).
In another embodiment, the low-shear mixing procedure and/or the low-shear premixing procedure is carried out by means of a gravity mixer and/or a mixer based on the principle of turbulence, for example produced by means of an elongated flow and/or a tube widening and/or by means of a kneader and/or an extruder and/or by means of a plow mixer and/or a paddle mixer and/or by means of a drum mixer, or with such a device. This type of mixing assembly may advantageously impart a low shear load to the electrode components, for example a lower shear load than jet mills and/or three-roll mills and/or by twin screw extruders, especially a lower shear load than jet mills. Especially in the case of mixers based on the turbulent flow principle, for example, only low material loads may advantageously occur because no internals are required and/or no "contact mixing" is present.
In a further embodiment, for example in method step c) downstream of method step b), the electrode (in particular the anode and/or the cathode) is formed, for example by dry production and/or by coating, for example by dry coating of the current collector or the carrier substrate, in particular a mixture comprising at least one fibrillated binder, at least one electrode component and at least one further electrode component from method step b). From this mixture, for example, electrodes having a defined porosity and/or a defined thickness (for example in the form of a film) can be formed. The current collector may for example be a metal current collector foil or a different kind of current collector, such as expanded metal, mesh, metal braid, metallized braid and/or foil perforated or punched or otherwise suitably prepared.
For further technical features and advantages of the method of the invention, reference is explicitly made here to the description relating to the electrode of the invention and the battery of the invention, and also to the figures and the description of the figures.
The invention also provides an electrode (e.g., anode and/or cathode) produced by the method of the invention.
The electrodes (e.g., anode and/or cathode) produced by the methods of the invention may be studied, for example, by Scanning Electron Microscopy (SEM), and demonstrated, for example, based on damage to individual components.
For further technical features and advantages of the electrode according to the invention, reference is explicitly made here to the description relating to the method according to the invention and to the battery according to the invention, and also to the figures and the description of the figures.
The invention also relates to an electrochemical cell, in particular a battery cell, such as a lithium cell or a sodium cell or a metal-air cell, such as a lithium ion cell and/or a lithium metal cell or a sodium ion cell, in particular a lithium cell, such as a lithium ion cell and/or a lithium metal cell, comprising at least one electrode according to the invention or an electrode produced according to the invention.
For further technical features and advantages of the battery of the invention, reference is explicitly made here to the description relating to the method of the invention and to the electrode of the invention, and also to the figures and the description of the figures.
Drawings
Additional advantages and advantageous configurations of the inventive subject matter are set forth in the accompanying drawings and are set forth in the description that follows. Here, it should be kept in mind that: the drawings are merely illustrative in nature and are not intended to limit the invention in any way. In the drawings of which there are shown,
fig. 1 shows a schematic flow chart illustrating one embodiment of the production method of the present invention.
Detailed Description
Fig. 1 shows an embodiment of the method according to the invention for producing an electrode, in particular an anode or a cathode, for an electrochemical cell, in particular for a battery cell, for example a lithium cell.
Fig. 1 shows: optionally, first, in a low shear premixing procedure, in an optional upstream method step a 0), at least one binder B is mixed with at least one electrode component E1 to obtain a premix b+e1. The at least one binder B may for example comprise at least one lithium ion conducting polymer or lithium ion conducting polymer, such as polyethylene oxide (PEO) and/or polymethyl methacrylate (PMMA), and/or at least one fluorinated and/or non-fluorinated polyolefin, such as polyvinylidene fluoride (PVDF) and/or Polytetrafluoroethylene (PTFE) and/or Polyethylene (PE) and/or polypropylene (PP), and/or copolymers thereof.
Fig. 1 also shows: in the high shear mixing procedure, in process step a), the at least one binder B is mixed with the at least one electrode component E1, optionally in the form of a premix from optional upstream process step a0, to obtain a mixture fb+e1 comprising fibrillated binder. The high shear rate mixing procedure may be performed, for example, by jet milling.
Further, fig. 1 shows: in process step b), at least one further electrode component E2 is incorporated into the mixture fb+e1 comprising fibrillated binder from process step a) by means of a low-shear mixing procedure.
In particular, in the high-shear mixing procedure, the at least one electrode component E1 may be more mechanically stable than the at least one further electrode component E2 and/or the functionality of the at least one electrode component E1 may be less affected by the high-shear mixing procedure and/or comminution than the functionality of the at least one further electrode component E2.
For example, the at least one electrode component E1 may have an average particle diameter or average particle length or average planar particle diameter of less than 10 μm, for example in the range of greater than or equal to 4 μm to less than or equal to 6 μm. Such small sized particles have been shown to undergo little or no further comminution during high shear mixing procedures (e.g., in jet mills) and are therefore mechanically quasi-stable during such procedures. Conversely, the at least one further electrode component E2 may have, for example, a larger average particle diameter or a larger average particle length or a larger average planar particle diameter of greater than or equal to 10 μm to less than or equal to 20 μm, and thus may be mechanically sensitive or unstable in a high shear mixing procedure (e.g. in a jet mill) from a comparison point of view.
Alternatively, for example, the at least one electrode component E1 may comprise at least one conductive additive, such as at least one conductive carbon, such as conductive graphite and/or amorphous conductive carbon, such as conductive carbon black, and/or carbon fibers and/or carbon nanotubes and/or graphene and/or expanded graphite, and/or at least one conductive metal; and the at least one further electrode component E2 may comprise at least one electrode active material, such as at least one anode active material or cathode active material, such as at least one intercalation material and/or composite material. The functionality of the conductive additive is significantly less affected by comminution during the high shear mixing procedure than the functionality of the electrode active material (e.g., anode active material or cathode active material, such as intercalation material and/or composite material).
Alternatively, the at least one electrode component E1 may for example be free of surface-coated particles and/or free of gradient material particles, while the at least one further electrode component E2 may comprise surface-coated particles and/or gradient material particles. In high shear mixing procedures, such as in jet mills, the surface coating of the gradient material particles and/or surface coated particles may be damaged and/or destroyed, and thus their function may be affected.
Further, fig. 1 shows: in method step c), the electrode E is formed, for example, by a dry production procedure and/or by coating, for example by dry coating, from the mixture fb+e1+e2 comprising at least one fibrillating binder fB, at least one electrode component E1 and at least one further electrode component E2 from method step b).
Claims (41)
1. A method for producing an electrode (E) for an electrochemical cell, wherein,
-mixing at least one binder (B) and at least one electrode component (E1) by a high shear mixing procedure to obtain a mixture (fb+e1) comprising fibrillated binder, and
incorporating at least one further electrode component (E2) into the mixture (fB+E1) comprising fibrillated binder by a low shear mixing procedure,
wherein the at least one electrode component (E1) is mechanically more stable than the at least one further electrode component (E2); and/or wherein the functionality of the at least one electrode component (E1) is less affected by the high shear mixing procedure and/or comminution than the functionality of the at least one further electrode component (E2),
wherein the at least one electrode component (E1) is selected from:
-conductive graphite, and/or
Amorphous conductive carbon in the form of non-porous carbon particles, and/or
-carbon fibers, and/or
-carbon nanotubes, and/or
-graphene and/or expanded graphite, and/or
At least one electrically conductive metal, and/or
At least one conductive additive-electrode active material composite,
wherein the at least one further electrode component (E2) is at least one electrode active material.
2. The method of claim 1, wherein the electrochemical cell is a battery cell.
3. The method of claim 2, wherein the battery cell is a lithium battery cell.
4. The method according to claim 1 or 2, wherein the at least one electrode component (E1) having an average particle size or average particle length or average planar particle size of less than 10 μm is used.
5. The method according to claim 1 or 2, wherein the at least one electrode component (E1) having an average particle size or average particle length or average planar particle size of less than or equal to 6 μm is used.
6. The method according to claim 1 or 2, wherein the at least one electrode component (E1) having an average particle diameter or average particle length or average planar particle diameter in the range of greater than or equal to 0.01 μm to less than or equal to 6 μm is used.
7. The method according to claim 1 or 2, wherein the at least one electrode component (E1) having an average particle size or average particle length or average planar particle size in the range of greater than or equal to 4 μm to less than or equal to 6 μm is used.
8. The method according to claim 1 or 2, wherein the at least one further electrode component (E2) is used which has a larger average particle size or has a larger average particle length or has a larger average planar particle size than the at least one electrode component (E1).
9. The method according to claim 1 or 2, wherein the at least one further electrode component (E2) having an average particle size or average particle length or average planar particle size of greater than or equal to 10 μm or greater than 6 μm is used.
10. The method according to claim 1 or 2, wherein the at least one electrode component (E1) is formed from or comprises at least one conductive additive.
11. The method according to claim 1 or 2, wherein the at least one electrode component (E1) is formed of and/or comprises at least one conductive carbon and/or at least one conductive metal.
12. The method according to claim 1 or 2, wherein the at least one electrode component (E1) comprises:
-conductive carbon black, and/or
-at least one carbon-metal phosphate complex.
13. The method according to claim 1 or 2, wherein the at least one further electrode component (E2) comprises at least one anode active material or at least one cathode active material.
14. Method according to claim 1 or 2, wherein the at least one further electrode component (E2) comprises at least one intercalation material and/or composite material.
15. The method according to claim 1 or 2, wherein the at least one further electrode component (E2) comprises:
intercalated graphite and/or intercalated amorphous carbon, and/or
At least one memory alloy, and/or
-at least one metal oxide and/or metal phosphate.
16. The method according to claim 1 or 2, wherein the at least one further electrode component (E2) comprises:
hard carbon and/or soft carbon, and/or
-silicon oxide and/or at least one layered oxide and/or at least one spinel and/or at least one metal phosphate.
17. The method according to claim 1 or 2, wherein the at least one electrode component (E1) comprises spherical particles.
18. The method according to claim 1 or 2,
wherein the at least one electrode component (E1) is free of electrode active material and/or free of surface-coated particles and/or free of gradient material particles and/or
Wherein the at least one further electrode component (E2) comprises surface-coated particles and/or gradient material particles.
19. The method according to claim 1 or 2, wherein the at least one electrode component (E1) is free of anode active material or free of cathode active material.
20. The method of claim 1 or 2, wherein the high shear rate mixing procedure is performed by jet milling.
21. The method according to claim 1 or 2, wherein the at least one binder (B) comprises at least one lithium ion conducting polymer or lithium ion conducting polymer and/or copolymers thereof.
22. The method according to claim 1 or 2, wherein the at least one binder (B) comprises polyethylene oxide and/or copolymers thereof.
23. The method according to claim 1 or 2, wherein the electrode components (E1, E2) of the electrode are used based on the total weight of the electrode
-from greater than or equal to 0.1% to less than or equal to 10% by weight of said at least one binder (B), and/or
-from greater than or equal to 0.1% to less than or equal to 50% by weight of said at least one electrode component (E1), and/or
-from greater than or equal to 0.1% to less than or equal to 98% by weight of said at least one further electrode component (E2).
24. The method according to claim 1 or 2, wherein,
-mixing at least one first binder and at least one electrode component by a first high shear mixing procedure to obtain a first mixture comprising fibrillated binder; and
-mixing at least one second binder and at least one electrode component by at least one second high shear mixing procedure to obtain at least one second mixture comprising fibrillated binder; and/or
-mixing at least one binder and a first electrode component of said at least one electrode component by a first high shear mixing procedure to obtain a first mixture comprising fibrillated binder; and
-mixing at least one binder and a second electrode component of said at least one electrode component by at least one second high shear mixing procedure to obtain at least one second mixture comprising fibrillated binder; and
-mixing the first mixture comprising fibrillated binder and the second mixture comprising fibrillated binder with the at least one further electrode component by the low shear mixing procedure.
25. The method according to claim 1 or 2, wherein the method is designed for producing an anode, wherein the at least one further electrode component (E2) comprises at least one anode active material.
26. Method according to claim 1 or 2, wherein the method is designed for producing an anode, wherein the at least one further electrode component (E2) comprises intercalated graphite and/or intercalated amorphous carbon, and/or a storage alloy and/or a metal oxide.
27. The method according to claim 1 or 2, wherein the method is designed for producing an anode, wherein the at least one further electrode component (E2) comprises hard carbon and/or soft carbon.
28. The method according to claim 1 or 2, wherein the method is designed for producing an anode, wherein the at least one further electrode component (E2) comprises silicon oxide.
29. The method according to claim 1 or 2, wherein the method is designed for producing a cathode, wherein the at least one further electrode component (E2) comprises at least one cathode active material.
30. The method according to claim 1 or 2, wherein the method is designed for producing a cathode, wherein the at least one further electrode component (E2) comprises at least one metal oxide and/or metal phosphate.
31. The method according to claim 1 or 2, wherein the method is designed for producing a cathode, wherein the at least one further electrode component (E2) comprises at least one layered oxide and/or at least one spinel and/or at least one metal phosphate.
32. The method according to claim 1 or 2, wherein the at least one binder (B) and the at least one electrode component (E1) are mixed in a low-shear pre-mixing procedure upstream of the high-shear mixing procedure to obtain a pre-mixture (b+e1), and the pre-mixture (b+e1) is then mixed in the high-shear mixing procedure to obtain a mixture (fb+e1) comprising fibrillated binder.
33. The method according to claim 32, wherein the low-shear mixing procedure and/or the low-shear premixing procedure is performed by a gravity mixer and/or by a mixer based on the principle of turbulence and/or by a kneader and/or by an extruder and/or by a coulter mixer and/or a paddle mixer and/or by a drum mixer.
34. The method according to claim 1 or 2, wherein the electrode (E) is formed from a mixture (fb+e1+e2) comprising the at least one fibrillating binder, the at least one electrode component (E1) and the at least one further electrode component (E2).
35. The method according to claim 34, wherein the electrode (E) is formed by a dry production procedure and/or by coating.
36. The method according to claim 34, wherein the electrode (E) is formed by dry coating.
37. An electrode produced by the method of any one of claims 1 to 36.
38. The electrode of claim 37, wherein the electrode is an anode or a cathode.
39. Electrochemical cell comprising at least one electrode according to claim 37 or 38.
40. The electrochemical cell of claim 39, wherein the electrochemical cell is a battery cell.
41. The electrochemical cell of claim 40, wherein said battery cell is a lithium cell.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102017213403.8A DE102017213403A1 (en) | 2017-08-02 | 2017-08-02 | Electrode production process by binder fibrillation |
| DE102017213403.8 | 2017-08-02 | ||
| PCT/EP2018/070536 WO2019025336A1 (en) | 2017-08-02 | 2018-07-30 | Method for producing electrodes by means of binder fibrillation |
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| Publication Number | Publication Date |
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| CN111033813A CN111033813A (en) | 2020-04-17 |
| CN111033813B true CN111033813B (en) | 2023-10-24 |
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| EP (1) | EP3642894A1 (en) |
| CN (1) | CN111033813B (en) |
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| DE102020210614A1 (en) | 2020-08-20 | 2022-02-24 | Robert Bosch Gesellschaft mit beschränkter Haftung | Method for producing an electrode of a battery cell, battery cell and use of the same |
| CN112038579A (en) * | 2020-09-28 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Metal lithium composite electrode, preparation method thereof and electrochemical energy storage device |
| CN112420975B (en) * | 2020-10-20 | 2022-02-22 | 浙江南都电源动力股份有限公司 | Production method of electrode plate in battery |
| KR20220065124A (en) * | 2020-11-12 | 2022-05-20 | 에스케이온 주식회사 | Anode active material including core-shell composite and method for manufacturing same |
| DE102022105656A1 (en) | 2022-03-10 | 2023-09-14 | Volkswagen Aktiengesellschaft | Process for the continuous production of a battery electrode |
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| JP2000149954A (en) * | 1998-11-11 | 2000-05-30 | Sanyo Electric Co Ltd | Nonaqueous electrolyte battery, and its manufacture |
| CN1838999A (en) * | 2003-07-09 | 2006-09-27 | 麦斯韦尔技术股份有限公司 | Dry particle based electrochemical apparatus and methods of making same |
| CN106463267A (en) * | 2014-04-18 | 2017-02-22 | 麦斯韦尔技术股份有限公司 | Dry energy storage device electrode and methods of making the same |
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| US3898099A (en) | 1974-03-18 | 1975-08-05 | Energy Res Corp | Hydrophilic electrode and method for making the same |
| US4379772A (en) | 1980-10-31 | 1983-04-12 | Diamond Shamrock Corporation | Method for forming an electrode active layer or sheet |
| US4354958A (en) | 1980-10-31 | 1982-10-19 | Diamond Shamrock Corporation | Fibrillated matrix active layer for an electrode |
| US4556618A (en) | 1983-12-01 | 1985-12-03 | Allied Corporation | Battery electrode and method of making |
| US5393617A (en) * | 1993-10-08 | 1995-02-28 | Electro Energy, Inc. | Bipolar electrochmeical battery of stacked wafer cells |
| CN1107090C (en) * | 1994-10-19 | 2003-04-30 | 大金工业株式会社 | Binder for cell and composition for electrodes and cell prepared therefrom |
| JP2000049055A (en) | 1998-07-27 | 2000-02-18 | Asahi Glass Co Ltd | Electric double layer capacitor and electrode for it |
| EP1687360A1 (en) | 2003-11-20 | 2006-08-09 | Bayerische Julius-Maximilians-Universität Würzburg | Polymer bonded functional materials |
-
2017
- 2017-08-02 DE DE102017213403.8A patent/DE102017213403A1/en active Pending
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2018
- 2018-07-30 CN CN201880050167.5A patent/CN111033813B/en active Active
- 2018-07-30 WO PCT/EP2018/070536 patent/WO2019025336A1/en unknown
- 2018-07-30 EP EP18756376.2A patent/EP3642894A1/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000149954A (en) * | 1998-11-11 | 2000-05-30 | Sanyo Electric Co Ltd | Nonaqueous electrolyte battery, and its manufacture |
| CN1838999A (en) * | 2003-07-09 | 2006-09-27 | 麦斯韦尔技术股份有限公司 | Dry particle based electrochemical apparatus and methods of making same |
| CN106463267A (en) * | 2014-04-18 | 2017-02-22 | 麦斯韦尔技术股份有限公司 | Dry energy storage device electrode and methods of making the same |
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| EP3642894A1 (en) | 2020-04-29 |
| CN111033813A (en) | 2020-04-17 |
| WO2019025336A1 (en) | 2019-02-07 |
| DE102017213403A1 (en) | 2019-02-07 |
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