EP4690318A2 - Dispositifs de stockage d'énergie - Google Patents

Dispositifs de stockage d'énergie

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Publication number
EP4690318A2
EP4690318A2 EP24781793.5A EP24781793A EP4690318A2 EP 4690318 A2 EP4690318 A2 EP 4690318A2 EP 24781793 A EP24781793 A EP 24781793A EP 4690318 A2 EP4690318 A2 EP 4690318A2
Authority
EP
European Patent Office
Prior art keywords
blend
active material
anode
solvent
active layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP24781793.5A
Other languages
German (de)
English (en)
Inventor
Wanjun Ben Cao
Ji Chen
Nicolo Brambilla
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanoramic Inc
Original Assignee
Nanoramic Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanoramic Inc filed Critical Nanoramic Inc
Publication of EP4690318A2 publication Critical patent/EP4690318A2/fr
Pending legal-status Critical Current

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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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • 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
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/134—Electrodes based on metals, Si or alloys
    • 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
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

Definitions

  • FIGs. 3 - 5 depict various methods of mixing the ingredients to form the active material composition
  • FIG. 7 is a graph depiction the viscosity of the composition versus shear rate for compositions produced by the processes described herein;
  • FIGs. 8 - 9 are graphs showing the electrochemical performance of LFP half cells using NX LFP cathode paired with an Li metal counter electrode.
  • PVDF polyvinylidene fluoride
  • NMP N-methylpyrollidone
  • NX electrodes a 3D nanocarbon matrix works as a mechanical scaffold for the electrode active material and mimics the polymer chain entanglement.
  • the NX electrodes are made via a NX process and includes a novel high shear mixing process that is developed for blending and mixing electrode slurry homogenously in multiple stages or in a single stage (e.g., in one pot).
  • the composition made by this high shear process is devoid of polyvinylidene fluoride (PVDF) and N- methylpyrollidone (NMP) and is referred to a NX high shear mixing process.
  • PVDF polyvinylidene fluoride
  • NMP N- methylpyrollidone
  • the 3D nanocarbon matrix is highly electrically conductive, allowing for significantly thicker cathode active layer while improving the electrical conductivity of the electrode.
  • eco-friendly solvents that are easily evaporated the electrode throughput is higher, and, more importantly, the energy consumption from electrode drying process is reduced by 30% due to reduction of temperature from 150 °C-180 °C required by the NMP to 60-70 °C.
  • NX Si- dominant anode drastic increase the energy density and FC capability of EV battery cells can be achieved.
  • a method that includes high shear of a slurry for producing improved electrode active layers that may be used in the electrodes of batteries.
  • the high shear process produces high electrochemical performance electrodes by combining a number of different mixing tools and methods with a multistage mixing sequence.
  • LIBs lithium-ion batteries
  • Scalable LIB manufacturing involves mixing high solid-content slurries.
  • the electrode structure can be affected by the mixer type and mixing process parameters, particularly the order in which the materials are introduced (the "mixing sequence") and the intensity and duration of each step, which are crucial in determining the quality and electrochemical performance of the battery.
  • the mixing sequence the order in which the materials are introduced
  • the intensity and duration of each step which are crucial in determining the quality and electrochemical performance of the battery.
  • various mixing sequences have been researched. Kim et al. discovered that dry mixing the LiCoCL (LCO) and conductive agent, then adding the solution of polyvinylidene fluoride (PVDF) in N-methyl-2-pyrrolidone (NMP) to form a slurry, can yield the greatest capacity and stability of charge and discharge cycle.
  • LCO LiCoCL
  • NMP N-methyl-2-pyrrolidone
  • the configuration of the PVDF and carbon black (CB) dispersion can affect the stability and rheological characteristics of slurries utilizing NMP as the solvent.
  • the addition of CB to PVDF can aid in the formation of a stable coagulated gel system, giving it resistance to the LiNiMnCoO2 (NMC) particle’s quick sedimentation.
  • NMC LiNiMnCoO2
  • Bauer et al. discovered that a drying mixing process of NMC/CB powder mixes before adding PVDF solution can cause CB shells on NMC surfaces, lowering the viscosity and stability of the slurry. If PVDF was then coated on the CB shells after drying, the conductive contact with NMC would be inhibited. This issue was resolved by adding additional CB or graphite during the homogenization process.
  • the first step in the assembly of a battery is the deposition of a slurry containing the active material, conducting material and optional polymeric binder in a solvent on to a copper film or an aluminium film (the current collector). This is followed by drying, calendaring and sizing of the electrodes.
  • the multistep manufacturing process of energy storage device electrodes need to be closely controlled.
  • Viscosity of the polymeric binder solution affects coating performance. It influences the ease with which the powders are dispersed within it, the power used for mixing and the speed of application of uniform coating.
  • the Porous Electrode Theory (PET) suggests the relevance of positive electrode density on overall performance of lithium-ion battery cells, validated by experiments. Cells with high positive electrode density show a slightly higher discharge capacity at low current rates but at high current rates, cells with a low positive electrode density show a better performance.
  • a novel high shear mixing process was developed for blending and mixing electrode slurry homogenously in multiple stages or in a single stage (e.g., in one pot).
  • the composition made by this high shear process is devoid of polyvinylidene fluoride (PVDF) and N-methylpyrollidone (NMP) and is referred to a NX high shear mixing process.
  • PVDF polyvinylidene fluoride
  • NMP N-methylpyrollidone
  • a particle size approach employing a Hegman gauge was used to initially assess the performance of the mixing process. Following that, rheological analysis using shear viscosity and dynamic tests were conducted to determine how well anode and cathode materials were mixed. Electrical performance tests were performed on the batteries that were created from the slurries produced by various mixers and mixing schemes.
  • This one pot solution greatly reduces the cost to manufacture by limiting the infrastructure used in the coating process.
  • processes used for manufacturing active layers that contain carbonaceous materials use significant amounts of NMP to produce a slurry that is coated on a current collector.
  • solvents such as NMP to facilitate the coating involves significant venting, handling, safety, and recycling protocols, all of which are eliminated from the NX high shear mixing process.
  • the NX high shear mixing process uses water or alcohols that are miscible with water at all temperatures.
  • the water-based lithium ferro-phosphate (LFP) process combined with the NX high shear mixing process for manufacturing battery electrodes can be used on standard, high speed, high volume manufacturing equipment with no additional infrastructure updates.
  • the electrodes (manufactured from this process) are improved over current and future battery designs as well.
  • This NX manufacturing process for battery electrodes is relevant across Li- ion and solid-state battery markets, especially for the electric vehicle market.
  • FIG. 1 is a diagram of an electrode (an anode or a cathode) according to various embodiments.
  • electrode 100 is provided.
  • electrode 100 comprises current collector 102 and active layer 106.
  • Electrode 100 may optionally include an adhesion layer 104.
  • adhesion layer 104 comprises a material that promotes adhesion between current collector 102 and active layer 106.
  • the electrode (the anode or the cathode) comprises a current collector 102 that is an electrically conductive layer.
  • current collector 102 may be a metal, metal alloy, etc.
  • the current collector 102 is a metal foil.
  • current collector 102 is an aluminum foil or aluminum alloy foil.
  • current collector 102 is a copper foil or copper alloy foil.
  • the current collector 102 has a thickness of less than 30 pm, preferably less than 10 pm, preferably less than 8 pm, and more preferably less than 5 pm.
  • the current collector 102 has a thickness of 3 to 15 pm. In some preferred embodiments, current collector 102 has a thickness of between about 6 pm and about 8 pm. In some embodiments, current collector 102 is an aluminum foil or an aluminum alloy foil, and current collector 102 has a thickness of about 10 to about 15 pm.
  • the electrodes of lithium batteries comprise complex combinations of materials and mixtures.
  • the key component in the cathode is an active material such as lithium ferro-phosphate (LFP), LiCoO2, LiNiO2, or LiNi x Mn y Co z O2.
  • Other components in the formulation often include a binder, like polyvinylidene fluoride (PVDF), a solvent, such N-methyl-2-pyrrolidone (NMP), and a carbon additive, like carbon black (CB), to increase the conductivity of the battery.
  • PVDF polyvinylidene fluoride
  • NMP N-methyl-2-pyrrolidone
  • CB carbon black
  • the active constituents in the anode combination include silicon and graphite, while other components such as the binder, solvent, and conductive agents are often the same as those used in the cathode.
  • the solid compositions of the anode and cathode active materials range from 50% to 99.9%.
  • the binder's content ranges from 0.1% to 15%. Higher binder concentrations may improve adhesion, but they may increase resistivity.
  • the compositions for the cathode and the anode active layers are discussed in detail below.
  • the active layer slurry for the cathode (which is disposed on the current collector) includes an active material, a carbonaceous conductor, a solvent and an optional binder.
  • the active material, the carbonaceous conductor, the solvent and the optional binder are mixed together to form the slurry. The mixing will be described in detail later.
  • the slurry after the appropriate mixing is disposed on the current collector, followed by solvent evaporation to form the active layer.
  • the active material used in the cathode may include lithium cobalt oxide (LCO, sometimes called “lithium cobaltate” or “lithium cobaltite,”.
  • LCO lithium cobalt oxide
  • NMC lithium nickel manganese cobalt oxide
  • NCMA lithium nickel cobalt manganese aluminum oxide
  • LMO lithium manganese oxide
  • LiMn2O4, Li2MnOa or the like, or a combination thereof lithium titanate oxide (LTO, with one variant formula being Li ⁇ isOn); lithium iron phosphate (LFP, with one variant formula being LiFePO4); lithium manganese iron phosphate (LMFP); lithium nickel cobalt aluminum oxide (LiNixCoyAlzCL) as well as other
  • the active material can include lithium cobalt oxide (LiCoCL).
  • the LiCoCL material can be further doped with certain metal species to increase its high-voltage stability.
  • the batteries containing LiCoCL (with or without doping) as the cathode active material can be charged to a high-voltage (> 4.7 V vs. Li/Li + ) to increase cell energy density.
  • the active material can include lithium manganese iron phosphate (LMFP).
  • LMFP lithium manganese iron phosphate
  • the chemical formula of LMFP can be LiMn x Fei- x PO4, where x is in the range of 0.1 to 0.9, preferably 0.3 to 0.7. Increase of Mn content in the LMFP material is beneficial for increasing energy density.
  • the polymeric binder for LMFP and LCO can be water based polymers for high voltage applications for aqueous (where the solvent is water or a water-containing solvent) processing.
  • the binder can be polyacrylic acid combined with some polyamide and polyvinyl pyrollidone (PVP).
  • PVP polyvinyl pyrollidone
  • the polymeric binder may be a copolymer of polyacrylonitrile and a polyether.
  • the active material includes other forms of lithium nickel manganese cobalt oxide (LiNi x Mn y Coi- x-y O2).
  • Variants of this formula that may be used in the active material layer include NMC111 (detailed below), NMC532 (LiNio.5Mno.3Coo.2O2), NMC622 (LiNio.6Mno.2Coo.2O2), or a combination thereof.
  • the active material used in the cathode may include a combination of nickel, manganese, and cobalt.
  • Lithium-Nickel-Manganese-Cobalt-Oxide (LiNiMnCoO2), abbreviated as NMC delivers strong overall performance, excellent specific energy, and the lowest self-heating rate of all mainstream cathode powders.
  • the NMC powder may comprise nickel in an amount of 20 to 40 atomic percent, manganese in an amount of 20 to 40 atomic percent and cobalt in an amount of 20 to 40 atomic percent, based on a total weight of the NMC blend.
  • NMC powder can refer to a variety of blends
  • This blend sometimes referred to as 1-1-1 (NMC 111) is useful for applications that use frequent cycling (automotive, energy storage) due to the reduced material cost resulting from lower cobalt content.
  • the active material is contained in the active layer in an amount of 67 to 99 wt%, preferably 90 to 99 wt%, based on the total weight of the active layer (when it is devoid of solvent). Active Material for the Anode
  • the anode active material can comprise silicon (Si), germanium (Ge), tin (Sn), lead (Pb), antimony (Sb), bismuth (Bi), zinc (Zn), aluminum (Al), titanium (Ti), nickel (Ni) , cobalt (Co), cadmium (Cd); alloys or two or more thereof or alloys thereof with other elements; oxides, carbides, nitrides, sulfides, phosphides, selenides, and tellurides of those metals and their mixtures or lithium-containing composites; salts and hydroxides of Sn; lithium titanate, lithium manganate, lithium aluminate, lithium-containing titanium oxide, lithium transition metal oxide; pre-lithiated versions thereof; particles of Li, Li alloy, or surface stabilized Li having at least 60% by weight of lithium, or combinations thereof.
  • the active material can comprise graphite in lieu of or in addition to the anode active material.
  • the anode active material can comprise a silicon oxide and/or carbon silicon oxide.
  • Such anode active material comprising a silicon oxide or carbon silicon oxide can further comprise graphite.
  • the active material used in the anode is a lithium-based active material.
  • a lithium-based active material is Li x Si y O z , where x is 1 to 15, preferably 2 to 7, y is 0 to 4, preferably 1 or 2, and z is 0 to 9, preferably 1 to 5.
  • SiO is synthesized by mixing silicon and silica in a 1 : 1 molar ratio and then subliming the mixture to collect the amorphous SiO (a-SiO) material. Since the silicon atoms in a-SiO are randomly distributed, their valence numbers can be 0, 1+, 2+, 3+, and 4+ upon the bonding condition with different numbers of oxygen atoms.
  • Some silicon atoms agglomerate and form tiny silicon crystals surrounded by other amorphous substances, with Si-0 bonds that have different valence numbers of silicon.
  • these tiny silicon crystals in a-SiO react with Li + ions and form LiisSi4, serving as the active material to store energy. Owing to the nano scale of tiny silicon crystal, no pulverization occurs after lithiation; therefore, good reversibility can be obtained.
  • lithium based active materials include LiisSi4, Li2SiO3, Li2Si20s, LieSi2O7, Li4SiO4, Li2O, or a combination thereof.
  • the lithium based active materials may be blended with a carbonaceous material to form a Li-SiOx-C active material.
  • the active material may comprise lithium, silicate and carbon.
  • the carbon in the form of carbon black, carbon nanotubes or graphite may be blended and pulverized with the Li x Si y O z (where x, y and z values are detailed above) to form aggregates and agglomerates of Li-SiOx-C active material.
  • elemental silicon (Si) may first be reacted and blended with a silicate material (SiOx).
  • the combination of silicon with the silica is subjected to reaction and grinding processes in order to create a powder.
  • carbon in a carbon coating process
  • lithium in a lithium doping process.
  • the formed Li-SiOx-C material will be in a classification process to form the final usable anode active material called Li-SiO with carbon coatings.
  • the relative density of the formed material can be ⁇ 2.1 g/cm 3 at 25 °C.
  • an energy storage device may have an initial charge specific capacity of 1500 to 1600 mAh/g, preferably 1400 to 1500 mAh/g with an initial coulombic efficiency of 90 to 94%; preferably 1350 to 1400 mAh/g with an initial coulombic efficiency of 87 to 89%.
  • the lithium may be added in elemental form or in the form of a compound. Some of these lithium compounds are listed herein.
  • the D50 particle size for the Li-SiOx-C particles prepared in this manner is 6 to 9 micrometers.
  • the BET surface area of the formed Li-SiOx-C material can be 3 to 4 m 2 /g with a carbon content of 3 to 4 wt%, based on a total weight of the Li-SiOx-C active material.
  • the initial charge specific capacity to 5 mV vs. Li/Li + of the cell (also referred to as an energy storage device) with the Li-SiOx-C anode can be 1500 to 1600 mAh/g, and the initial discharge specific capacity to 2.0 V vs.
  • the electrically conducting material used in the anode and/or cathode may include graphite flakes. This is described later.
  • the high aspect ratio carbon elements can be single wall carbon nanotubes (SWCNTs), double wall carbon nanotubes (DWNTs), multiwall carbon nanotubes (MWNTs), thin walled nanotubes (TWNTs), carbon black, carbon nano-fiber, carbon nanotube fiber, porous carbons or a mixture of different types.
  • SWCNTs single wall carbon nanotubes
  • DWNTs double wall carbon nanotubes
  • MWNTs multiwall carbon nanotubes
  • TWNTs thin walled nanotubes
  • carbon black carbon nano-fiber
  • carbon nanotube fiber carbon nanotube fiber
  • porous carbons porous carbons or a mixture of different types.
  • the single wall carbon nanotubes can have an outer diameter of 0.5 to 5.0 nanometers, preferably 1.0 to 3.5 nanometers.
  • the single wall carbon nanotubes can have an aspect ratio (length to diameter ratio) greater than about 2.0, preferably greater than 5.0, preferably greater than 10.0, greater than 50 and more preferably greater than 100.
  • the single wall carbon nanotubes can have an average aspect ratio of 5 to 200.
  • the single wall carbon nanotubes can have a length greater than 6 nanometers, preferably greater than 10 nanometers, preferably greater than 15 nanometers, preferably greater than 30 nanometers, preferably greater than 50 nanometers, more preferably greater than 100 nanometers, preferably greater than 1 micrometer, preferably greater than 5 micrometers, preferably greater than 10 micrometers, and more preferably greater than 15 micrometers up to at least 200 micrometers.
  • the single wall carbon nanotubes can have an average length of 10 nanometers to 20 micrometers, preferably 20 nanometers to 15 micrometers.
  • the single wall carbon nanotubes can present in the mixture of electrically conductive material, binder material, electrode active material and solvent in an amount of 0.1 to 0.3 weight percent, preferably 0.15 to 0.25 weight percent based on the total weight of the mixture.
  • SWNTs used in the composition are metallic nanotubes in an amount of greater than or equal to about 1 wt %, preferably greater than or equal to about 20 wt %, more preferably greater than or equal to about 30 wt %, even more preferably greater than or equal to about 50 wt %, and most preferably greater than or equal to about 99.9 wt % of the total weight of the SWNTs.
  • the number of carbon walls in the multi-wall carbon nanotubes can be 2 or more, 5 or more, 10 or more, 50 or more.
  • the multi-wall carbon nanotubes can comprise an average of between 3 layers to 15 layers, 4 to 12 layer, 5 to 10 layers, 6 to 8 layers.
  • the active layer 106 can comprise multi-wall carbon nanotubes and single-wall carbon nanotubes.
  • the multi-wall carbon nanotubes swell more than singlewall carbon nanotubes when wetted with an electrolyte in an energy storage device in which electrode 100 is located.
  • the multi-wall carbon nanotubes can swell at least 15%, or at least 25% or at least 50% more than single-wall carbon nanotubes when wetted with an electrolyte in an energy storage device in which electrode 100 is located.
  • a length of the multi-wall carbon nanotubes can expand at least 15%, or at least 25% or at least 50% more than a length of the single-wall carbon nanotubes when wetted with the electrolyte.
  • the multi-wall carbon nanotubes swell up to 50% when wetted (e.g., a length of the multi-wall carbon nanotubes is 50% larger after wetting with an electrolyte, and/or a diameter of the multi-wall carbon nanotubes is 50% larger after wetting, etc.).
  • the multi-wall carbon nanotubes can have an outer diameter of 2.0 to 50 nanometers, 5.0 to 40 nanometers, or 6 to 10 nanometers.
  • the multi-wall carbon nanotubes can have a length greater than 10 nanometers, greater than 15 nanometers, greater than 30 nanometers, greater than 50 nanometers, greater than 100 nanometers, greater than 500 nanometers, greater than 1 micrometer, greater than 5 micrometers, greater than 10 micrometers, or greater than 15 micrometers.
  • the multi- wall carbo nanotubes can have an average length up to 25 micrometers or up to 20 micrometers.
  • the multi-wall carbon nanotubes have an average length of 10 nanometers to 20 micrometers, or 20 nanometers to 15 micrometers.
  • the multi- wall carbon nanotubes can have an aspect ratio (length to diameter ratio) greater than 5.0, greater than 10.0, greater than 50, greater than 100, or greater than 500.
  • the electrode comprises multi-wall carbon nanotubes can be relatively longer in comparison to multi-wall carbon nanotubes comprised in related art electrodes.
  • the use of relatively longer multi-wall carbon nanotubes in electrodes is found to have beneficial mechanical and/or electrical properties.
  • multi- wall carbon nanotubes provide relatively good power at low densities.
  • shorter multiwall carbon nanotubes generally do not swell (e.g., expand) as much as longer multiwall carbon nanotubes. As such use of shorter multi-wall carbon nanotubes loses (or reduces) some of the beneficial properties associated with swelling of the carbon nanotubes.
  • carbon black does not exhibit swelling because carbon black is merely particles of carbon without entanglement such as the entanglement exhibited by a set of multi-wall carbon nanotubes.
  • An indication that a length of a certain amount of multi- wall carbon nanotubes have a length exceeding a threshold length and thus have sufficient swelling properties is an observation during a calendering process - a relatively larger amount of pressure or effort to calendar the active layer in connection with applying to the foil is indicative that the collective swelling (e.g., an average swelling) of the multi-wall carbon nanotubes in the active layer will satisfy a certain performance threshold.
  • multiwall carbon nanotubes are generally difficult to process.
  • the processing of the multi-wall carbon nanotubes in connection with preparing/forming the active layer and/or electrode is gentler than processes for related art electrodes. As such, the processes according to various embodiments maintain longer multiwall carbon nanotubes (e.g., less multi-wall carbon nanotubes are crushed, fragmented, broken, etc.).
  • the active layer of the electrode comprises a set of multiwall carbon nanotubes having an average length that is more an average length of the multiwall carbon nanotubes in related art electrodes. According to various embodiments, a distribution of lengths of the set of multi-wall carbon nanotubes is skewed towards a nominal length a multi-wall carbon nanotube.
  • the nominal length of a multi-wall carbon nanotube is about 16 microns.
  • the multi- wall carbon nanotubes are processed and/or applied in a manner that reduces or minimizes fracturing or breaking of multi- wall carbon nanotubes.
  • the lengths of the multi- wall carbon nanotubes in the network of high aspect ratio carbon elements are generally the nominal length of the multi-wall carbon nanotubes, or a length of such the multi-wall carbon nanotubes tend to be more heavily skewed to the nominal length.
  • at least 75% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements are within 10% of the nominal length (e.g., between 13.4 microns to about 15 microns).
  • At least 75% of the multi- wall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 12 microns. In some embodiments, at least 75% of the multiwall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 13 microns. In some embodiments, at least 50% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements are within 10% of the nominal length (e.g., between 13.4 microns to about 15 microns). In some embodiments, at least 50% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 12 microns.
  • At least 50% of the multiwall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 8 microns. In some embodiments, at least 50% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 13 microns.
  • a distribution of lengths of the set of multi-wall carbon nanotubes is skewed towards a nominal length a multi-wall carbon nanotube.
  • the multi-wall carbon nanotubes are processed and/or applied in a manner that reduces or minimizes fracturing or breaking of multi- wall carbon nanotubes.
  • the lengths of the multi-wall carbon nanotubes in the network of high aspect ratio carbon elements are generally the nominal length of the multi-wall carbon nanotubes, or a length of such the multi-wall carbon nanotubes tend to be more heavily skewed to the nominal length.
  • At least 75% of the multiwall carbon nanotubes within the network of high aspect ratio carbon elements are within 10% of the nominal length (e.g., between 13.4 micrometers to about 15 micrometers). In some embodiments, at least 75% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 12 micrometers. In some embodiments, at least 75% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 13 micrometers. In some embodiments, at least 50% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements are within 10% of the nominal length (e.g., between 13.4 micrometers to about 15 micrometers).
  • At least 50% of the multi-wall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 12 micrometers. In some embodiments, at least 50% of the multiwall carbon nanotubes within the network of high aspect ratio carbon elements have a length of at least 13 micrometers.
  • the multi-wall carbon nanotubes can be present in the mixture (the mixture comprises the electrically conductive material, the electrode active material, the binder material and a solvent or a combination of solvents) in an amount of 0.3 to 1.0 weight percent, preferably 0.4 to 0.9 weight percent based on the total weight of the mixture.
  • the multi-wall carbon nanotubes are present in the solid anode active layer (the solid active layer comprises the electrically conductive material, the binder material, the electrode active material without the solvent) in an amount of 0.8 to 2.6 wt%, preferably 1.0 to 1.8 wt%, based on the entire weight of the solid anode active layer (when it is devoid of solvent).
  • the ratio of the weight of the multi-wall carbon nanotubes to the weight of the single wall carbon nanotubes in the mixture or in the solid active material layer can be at least 2:1.
  • three-dimensional network of high aspect ratio carbon elements 108 comprises carbon nanotubes, and the carbon nanotubes are only multi-wall carbon nanotubes and/or fragments of such carbon nanotubes.
  • the multiwall carbon nanotubes are present in the mixture or in the solid anode active material layer in an amount that is at least twice the amount of the single wall carbon nanotubes, based on the weight of the conductive materials.
  • the carbon nanotubes may comprise randomly dispersed carbon nanotubes in which are dispersed clumps of brush like oriented nanotubes.
  • the brush-lie oriented nanotubes are randomly dispersed in the randomly dispersed carbon nanotubes, but within each brush-like clump the nanotubes are aligned.
  • the aligned nanotubes in the brush-like clump may have a length that is greater than the thickness of the active layer (i.e., the cathode active layer or the anode active layer).
  • the network of three-dimensional network of high aspect ratio carbon elements 108 can comprise at least 99% carbon by weight.
  • the electrically conductive materials may optionally comprise graphite flakes, carbon black, or a combination thereof.
  • Carbon black, or porous carbon can also be used in addition to the carbon nanotubes.
  • These carbon materials are typically a high surface area carbon that has a surface area of greater than 50 square meters per gram (m 2 /gm), preferably greater than 200 m 2 /gm, and more preferably greater than 500 m 2 /gm.
  • An example of a high surface area carbon black is KELTJEN Black.
  • the carbon materials are optional and may be present in the solid anode active layer (the solid active layer comprises the electrically conductive material, the binder material, the electrode active material without the solvent) in an amount of 0.5 to 2.0 wt%, preferably 0.8 to 1.6 wt%, based on the entire weight of the solid anode active material. While the presence of high aspect ratio carbon nanotubes benefits the electrical conductivity and cell rate performance, the ID carbon materials (carbon black or porous carbons) are generally cheaper and can enable optimal slurry rheology properties at a high slurry solid content.
  • the three-dimensional network of high aspect ratio carbon elements 108 can comprise an electrically interconnected network of carbon elements exhibiting connectivity above a percolation threshold and wherein the network defines one or more highly electrically conductive pathways having a length greater than 100 pm.
  • the percolation threshold is one where the conducting elements contact one another to provide an electrically conducting network measured across any two points on any surface of the network.
  • the electrode active materials (the anode active material or the cathode active material) and the carbonaceous conductive material are held together by a binder.
  • the binder may include organic polymeric materials such as, for example, cellulose, polyacetals, polycarbonates, polyalkyds, polystyrenes, polyolefins, polyesters, polyamides, polyaramides, polyamideimides, polyarylates, polyurethanes, epoxies, phenolics, silicones, poly arylsulfones, polyethersulfones, polyphenylene sulfides, polysulfones, polyimides, poly acrylates, poly etherimides, polytetrafluoroethylenes, poly etherketones, polyether ether ketones, polyether ketone ketones, polybenzoxazoles, polyoxadiazoles, polybenzothiazinophenothiazines , polybenzothiazoles ,
  • the binder is present in the active layer in an amount of 0.1 to 15 wt%, preferably 1 to 10 wt%, and more preferably 1.5 to 5 wt%, based on the total weight of the active layer (when it is devoid of solvent).
  • the binder is present in the form of an emulsion prior to being mixed into the active material that is disposed on the current collector.
  • the binder is preferably water soluble or is made compatible with a water soluble polymer so that it can be dissolved in water. Water soluble solvents may also be used for dispersing the binder, the high aspect ratio carbon elements 108.
  • a solvent is used to facilitate blending of the active material (either the anode active material or the cathode active material), the carbonaceous conductive material, the binder, and any other additives if desired.
  • the solvent is preferably one that can dissolve the binder.
  • Suitable solvents are water, alcohol, or a combination thereof. Examples of alcohol are ethanol, methanol, propanol, butyl alcohol, ethylene glycol, propylene glycol, or a combination thereof.
  • other solvents may be added to facilitate solubilization and/or dispersion of the polymer.
  • Other solvents include polar solvents, non-polar solvents, and the like.
  • Liquid aprotic polar solvents such as propylene carbonate, ethylene carbonate, butyrolactone, acetonitrile, benzonitrile, nitromethane, nitrobenzene, sulfolane, dimethylformamide, N- methylpyrrolidone, or the like, or combinations thereof may be added to water or alcohol for dissolution of the polymer.
  • Polar protic solvents such acetonitrile, nitromethane, acetone, dimethyl sulfoxide, dimethylformamide, or the like, or a combination thereof may be used.
  • non-polar solvents such as a benzene, toluene, methylene chloride, carbon tetrachloride, hexane, diethyl ether, tetrahydrofuran, or the like, or a combination thereof may also be used.
  • Co- solvents comprising at least one aprotic polar solvent and at least one non-polar solvent may also be utilized to modify the solubilization power of the solvent.
  • the solvent only contains water and is ethanol-free. In another embodiment, the solvent only contains ethanol and is water-free. In another embodiment, the solvent can be a mixture of water and ethanol.
  • the ratio of water to alcohol is 80:20 to 95:5, preferably 88:12 to 92:8. In an exemplary embodiment, the ratio of water to alcohol is 90:10.
  • the choice of solvent system is dependent on the compatibility of active materials, availability of binders and slurry rheology properties.
  • the solvent is present in an amount of 30 to 60 wt%, preferably 40 to 55 wt%, based on the total weight of the first slurry.
  • the solvent is preferably removed from the active layer after it is disposed on the current collector.
  • the solid active layer preferably is free of solvent (water and alcohol).
  • FIGs. 3-5 shows a general mixing strategy of the cathode slurry w/ NX HS processing.
  • the NX mother slurry can be fully dispersed and homogenously mixed for downstream processing with additional polymer solution, carbon additives, and active materials.
  • the carbonaceous material and the polymeric binder are first mixed in step 1002 in a solvent or solvent mixture to form the mother slurry.
  • the solvent only contains water and is ethanol-free.
  • the solvent only contains ethanol and is water- free.
  • the solvent can be a mixture of water and ethanol.
  • the ratio of water to alcohol is 80:20 to 95:5, preferably 88:12 to 92:8. In an exemplary embodiment, the ratio of water to alcohol is 90:10.
  • the process to form the active material comprises first blending a portion of the ingredients in a NX high-shear (HS) process to form a uniform blend.
  • the machines used for such purposes can be a ball milling machine, magnetic stirrers, supersonic waves or a planetary dispersion (PD) mixer.
  • PD planetary dispersion
  • a commercial PD mixer from MTI Corporation can be used.
  • the stirring blade can be set at a stirring speed of 20 - 70 rpm, preferably at 30 - 60 rpm.
  • the dispersion blade can be set at a dispersion speed of 600 - 2000 rpm, preferably at 1000 - 1800 rpm.
  • This first blend may be a dry blend or may be conducted in a portion of the solvent that is used to facilitate the blending. If a dispersant is used to facilitate the blending of the conductive materials into the active material, then it is also added at this stage.
  • the mixing in step 1002 is conducted for 5 to 120 minutes, preferably 10 to 60 minutes.
  • steps 1004 to 1012 are all conducted using commercially available mixing machines, including ball milling machine, magnetic stirrers, supersonic waves or a PD mixer, blade and dispersion mixing.
  • a commercial PD mixer from MTI Corporation can be used.
  • the stirring blade can be set at a stirring speed of 20 - 70 rpm, preferably at 30 - 60 rpm.
  • the dispersion blade can be set at a dispersion speed of 600 - 2000 rpm, preferably at 1000 - 1800 rpm.
  • the mother slurry produced in step 1002 comprises the carbonaceous conductive material, the binder and any desirable optional dispersants, under a dry blending process or with a solvent.
  • the mother slurry is first mixed till the desired distribution of the carbonaceous conductive material in the binder (and the optional dispersant is achieved).
  • additional polymeric binder in a solvent is added to the mother slurry in several steps - notably steps 1004 - 1012.
  • additional binder may be added in one or more increments to the vessel. It is to be noted that the entire sequence of steps from 1002 to 1010 are conducted in a single vessel. More vessels that one may be used if desired. However, it is preferable to conduct the entire mixing in a single vessel.
  • steps 1004 and 1006 further mixing is conducted using blade and dispersion mixing.
  • the binder is added in the form of a solution.
  • a solvent may be added to the binder to solubilize the binder and the solution of the binder in the solvent is then added in increments in these steps.
  • the mixing in steps 1004 and 1006 may be conducted for 5 to 120 minutes, preferably 10 to 60 minutes.
  • the active material such as NCM/NCMA/LFP, LFMP, or the like, is then added to the same mixing vessel in step 1008. It may be added continuously or stepwise.
  • the mixing to add the active material is conducted for 5 to 120 minutes, preferably 10 to 60 minutes.
  • Step 1010 is optional and features the addition of additional solvent to the blend in the vessel.
  • the mixing in step 1010 may be conducted for 5 to 120 minutes, preferably 10 to 60 minutes to form the final cathode slurry (see step 1012).
  • the cathode slurry obtained in step 1012 is disposed on a film of metal (the current collector) and dried to form the active material layer.
  • the active material layer thus disposed on the current collector forms the electrode, which may be used in an energy storage device. While this process is detailed for manufacturing a cathode active layer, it can also be used to manufacture the anode active material and the anode active layer.
  • FIG. 4 depicts another process involving steps 2002 through 2012.
  • the manufacturing process of the FIG.4 is similar to that of the FIG. 3 except that the penultimate step 1010 of the FIG. 3 becomes the second step 2004 of the FIG. 4.
  • FIG. 4 depicts another manner of mixing the ingredients to form the cathode active layer.
  • the water and alcohol is added to the mother slurry (see step 2004) (of the FIG. 3) directly after it is formed (see step 2002).
  • the mother slurry together with the water and alcohol is subjected to additional blade and dispersion mixing (see step 2004).
  • Additional binder together with solvent is then added to the mixture of the mother slurry and water and alcohol in several steps with some mixing in between each step (see steps 2006 and 2008).
  • the active materials are added to the mixture of solvent, binder, carbonaceous conductive material to form the cathode (or anode) active material (see step 2010).
  • the cathode (or anode) active material is then disposed on a current collector and dried (by removing the solvent, water and alcohol) to form the active layer (see step 2012).
  • Tables 1 - 3 exemplify compositions that were manufactured using the processes described herein. Tables 1 - 3 detail the compositions with the respective ingredients.
  • a binder As noted above, there are typically four main components in both the cathode and anode slurries. These are a binder, a solvent, a carbonaceous conductive material and an active material.
  • the solid powders that make up the active and conductive materials range in size from nano to micro sizes. These solid powders are combined with a binder in an organic (ethanol) or aqueous solvent (H2O).
  • ethanol organic
  • H2O aqueous solvent
  • NMP N-methyl-2-pyrrolidone
  • PVDF poly vinylidene fluoride
  • FIG. 6 The viscosity for a blend of the mother slurry that is mixed with one or more binders / dispersant and LFP is shown on a graph in the FIG. 6.
  • FIG. 6 the viscosity of each of the blends decreases as the shear rate increases.
  • FIG. 7 depicts the viscosity of several blends that contain the mother slurry that is mixed with binders/dispersant and NCM, where each of the blends is mixed for increasing periods of time. From the FIG. 7, it may be seen that there is a decrease in the blend viscosity with increasing mixing time periods.
  • LFP cathode (16-35 mg/cm 3 ) can be coated without any cracking issues, good flexibility, and a pressed density of 2.4-2.7 g/cm 3 can be achieved (FIG. 9).
  • the electrochemical performance of LFP half cells using NX LFP cathode paired with an Li metal counter electrode is shown in FIG. 8 and FIG. 9. When the LFP cathodes are paired with NX Si/C anodes, LFP full Cell energy density of greater than 240 Wh/kg, preferably greater than or equal to 560 Wh/L were produced.
  • the LFP-SiGr battery cell energy density can be ranged from 200-250 Wh/kg and 490-570 Wh/L range for EV large-format battery cells depending on the battery cell design and electrode loadings. This represents a greater than 30% improvement in performance compared with LFP industry cell standard.
  • the cell cycle life is greater than or equal to 1000 cycles (70% nominal capacity).
  • Si-dominant anode may be pre-li thiated to achieve longer cycle life for NX LFP-Si cells to control the anode potential vs.
  • Li/Li+ to be in the range between 0.05V to 0.8 V during the full battery cell cycle life.
  • the anode electrodes can be not pre-lithiated too.
  • the anode electrodes are pre-lithiated in 10-20% lithiation degree based on the total anode areal capacity to control the anode potential vs. Li/Li+ to be in the range between 0.05V to 0.8 V during the full battery cell cycle life.
  • An anode potential 0.1V to 0.75V vs. Li/Li+ during the cycle life of the cell is preferred.
  • the electrolyte contains salt type and solvent type additives including LiFSI and FEC.
  • the separator is coated with PVDF material with 1- 2um thickness range.
  • the anode active layer areal capacity/cathode active layer areal capacity ratio is from 1.05-1.25.
  • the electrolyte used in the battery cells are disclosed in patent application WO2021226483 Al to Hyde, the entire contents of which are hereby incorporated in their entirety by reference.
  • the resulting energy storage device is a high mass loading PVDF-free NCMA/LMFP containing cathode electrodes with thin Si-dominant anodes.
  • the energy storage device enables a substantial jump in energy density for an EV battery cell (projected as >350-400Wh/kg, >900 Wh/L), while enabling fast charging (10 mins at 80% state of charge (SOC)).

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Abstract

L'abrégé est tel qu'il figure à la page 30 de la description.
EP24781793.5A 2023-03-27 2024-03-27 Dispositifs de stockage d'énergie Pending EP4690318A2 (fr)

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