WO2017202693A1 - Suspensions de matières inorganiques pour former des structures solides - Google Patents

Suspensions de matières inorganiques pour former des structures solides Download PDF

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Publication number
WO2017202693A1
WO2017202693A1 PCT/EP2017/062016 EP2017062016W WO2017202693A1 WO 2017202693 A1 WO2017202693 A1 WO 2017202693A1 EP 2017062016 W EP2017062016 W EP 2017062016W WO 2017202693 A1 WO2017202693 A1 WO 2017202693A1
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WO
WIPO (PCT)
Prior art keywords
slurry
slurry according
binder
organic solvent
formula
Prior art date
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PCT/EP2017/062016
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English (en)
Inventor
Pascal HARTMANN
Christoph ERK
Hannes Wolf
Ulrich Karl
Nicolas Marion
Thomas Reissner
Ulrich Abel
Original Assignee
Basf Se
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Publication of WO2017202693A1 publication Critical patent/WO2017202693A1/fr

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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • 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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0568—Liquid materials characterised by the solutes
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • 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

  • the present invention relates to a slurry comprising i) an inorganic material,
  • R 1 is H, d-Ce-Alkyl
  • R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 are independently from each other either H or Me, and
  • n O oM .
  • the present invention further relates to the use of such slurries as a component for producing a solid structure, to a process for preparing a solid structure and to a process for preparing a cathode for a rechargeable electrochemical cell.
  • Slurries of solid materials for the production of electrodes for rechargeable batteries in particular slurries of electroactive inorganic materials for the production of cathodes for lithium- ion batteries are well known to the person skilled in the art. These known slurries usually comprise, beside the inorganic, electroactive material and binders, a solvent such as N- methylpyrrolidone (NMP).
  • NMP N- methylpyrrolidone
  • Desirable properties of the slurries are, for example, easy handling including environmentally relevant aspects, and desirable properties of the produced electrochemical cells are maintenance of cathode capacity, reduced self-discharge of the electrochemical cells during storage, an increase in the lifetime of the electrochemical cell, an improvement in the mechanical stability of the cathode.
  • the desired properties mentioned also make a crucial contribution to improving the economic viability of the electrochemical cell, which, as well as the aspect of the desired technical performance profile of an electrochemical cell, is of crucial significance to the producer and the user.
  • R 1 is H, d-Ce-Alkyl
  • R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 are independently from each other either H or Me, and
  • n 0 or 1.
  • the electrode where during discharging a net negative charge occurs is called the anode and the electrode where during discharging a net positive charge occurs is called the cathode.
  • the inventive slurry comprises as a first component an inorganic material, also referred to hereinafter as inorganic material (i), for short, as a second component a binder, also referred to hereinafter as binder (ii) and as a third component an organic solvent of formula (I), also referred to hereinafter as solvent (iii).
  • the slurry can also be described as a suspension of at least one solid material, an inorganic material in the present case, in a liquid phase, which comprises at least one organic solvent.
  • the inorganic material (i) is usually an electroactive material, which is the essential material of an electrode, either an anode or a cathode, preferably a cathode, of an electrochemical cell, in particular a rechargeable electrochemical cell.
  • electroactive material which is the essential material of an electrode, either an anode or a cathode, preferably a cathode, of an electrochemical cell, in particular a rechargeable electrochemical cell.
  • Inorganic materials, which are used as electroactive materials for the production of electrochemical cells, in particular of rechargeable electrochemical cells are well known. Suitable cathode materials and suitable anode materials are described in appropriate monographs and reference works: e.g. Wakihara et al.
  • Preferred inorganic materials are electroactive chalcogen-containing materials, such as transition metal oxides, metal sulfides or transition metal phosphates. Further preferred inorganic materials (i) are electroactive halogen-containing, preferably fluorine-containing materials.
  • the inventive slurry is characterized in that the inorganic material is an electroactive chalcogen-containing material, preferably an electroactive chalcogen-containing material, that is selected from the group consisting of lithium- containing transition metal oxides and lithium-containing transition metal phosphates.
  • electroactive chalcogen-containing material preferably an electroactive chalcogen-containing material, that is selected from the group consisting of lithium- containing transition metal oxides and lithium-containing transition metal phosphates.
  • Lithium-containing transition metal oxides and lithium-containing transition metal phosphates are described in detail in WO 2015/189094 on page 1 1 , line 15 to page 13, line 14 wherein said reference is incorporated by reference in its entirety for all useful purposes.
  • the inventive slurry further comprises a binder (ii).
  • Suitable binders can be selected from organic (co)polymers. Suitable organic (co)polymers may be halogenated or halogen-free.
  • Examples are polyethylene oxide (PEO), cellulose, carboxyme- thyl cellulose, polyvinyl alcohol, polyethylene, polypropylene, polytetrafluoroethylene, polyac- rylonitrile-methyl methacrylate, styrene-butadiene copolymers, tetrafluoroethylene- hexafluoropropylene copolymers, vinylidene fluoride-hexafluoropropylene copolymers (PVdF-HFP), vinylidene fluoride-tetrafluoroethylene copolymers, perfluoroalkyl vinyl ether copolymers, ethylene-tetrafluoroethylene copolymers, vinylidene fluoride- chlorotrifluoroethylene copolymers, ethylene-chlorofluoroethylene copolymers, ethylene- acrylic acid copolymers, optionally at least partially neutralized with alkali metal salt or ammonia, ethylene-methacrylic acid cop
  • Preferred binders (ii) comprise a fluoropolymer, such as fluorinated (co)polymers such as polyvinyl fluoride and especially polyvinylidene fluoride.
  • the inventive slurry is characterized in that the binder comprises a fluoropolymer, preferably a fluoropolymer, that comprises -CH2-CF2- units.
  • fluoropolymers are polyvinylidene difluoride or copolymers comprising -CH2-CF2-units, in particular polyvinylidene difluoride.
  • the average molecular weight M w of the binder, in particular of the fluoropolymer may be selected within wide limits, suitable examples being 1000 g/mol or higher, preferably 10000 g/mol or higher, in particular 20,000 g/mol to 2,000,000 g/mol.
  • R 1 is H, d-Ce-Alkyl
  • R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 are independently from each other either H or Me, and
  • n 0 or 1 , are known as such.
  • R 1 is H, methyl, ethyl, n-propyl, i-propyl, n-butyl, sec. -butyl, tert-butyl, n-pentyl or n-hexyl, preferably H or methyl, in particular H,
  • R2, R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 are H,
  • n is 0 or 1 , in particular 0.
  • Particularly preferred organic solvents are N-formylpyrrolidine, N-acetylpyrrolidine, N- formylpiperidine or N-acetylpiperidine, in particular N-formylpyrrolidine.
  • the inventive slurry is characterized in that the organic solvent of formula (I) is N-formylpyrrolidine.
  • the inventive slurry further comprises, as well as inorganic material (i), binder (ii) and solvent (iii) as a fourth component a conductive material, also referred to hereinafter as conductive material (iv).
  • the inventive slurry is characterized in that the slurry further comprises a conductive material as component (iv).
  • conductive materials can show electronic conductiv- ity or ionic conductivity or both.
  • the conductive materials (iv) are preferably solid materials, that are either insoluble in solvent (iii) or at least partly soluble in solvent (iii).
  • the inventive slurry is characterized in that the slurry further comprises a conductive material as component iv), which is solid material that shows electronic and/or ionic conductivity, in particular an electron conductive material.
  • lithium ion conductive materials or materials showing ionic conductivity are preferably lithium ion conductive materials such as lithium ion conductive ceramics, sintered ceramics, glass-ceramics, glasses, and polymers more preferably well-known Li ion conducting inor- ganic solid lithium ion conductors as described by P. Knauth in Solid State Ionics 180 (2009) 91 1 -916 or by A. Hayashi and M. Tatsumisago in Electronic Materials Letters 8 (2012) 199- 207.
  • ceramic materials with perovskite, Nasicon, Thio-Lisicon, argyrodite or garnet related crystal structure offer good conductivities, but also inorganic phosphorous and sulfur containing materials are good candidates.
  • Preferred lithium ion conductive materials show a conductivity for lithium ions of higher than 10 "7 S/cm at 25 °C, preferably in the range of M O- 6 S/cm - 5 ⁇ 10-2 S/cm at 25 °C.
  • electron conductive materials or materials showing electronic conductivity are in particular metals, carbons in a conductive polymorph, conductive organic polymer and cer- tain metal oxides, metal sulfides, metal carbides or metal nitrides.
  • Preferred electron conductive materials are carbons in a conductive polymorph, such as graphite, activated carbon, carbon black, carbon fibers, carbon nanotubes, graphene or mixtures of at least two of the aforementioned substances.
  • the inventive slurry is characterized in that the slurry further comprises a conductive material as component (iv), which is carbon in a conductive polymorph
  • the inventive slurry comprises as a first component an inorganic material, also referred to hereinafter as inorganic material (i), for short, as a second component a binder, also referred to hereinafter as binder (ii) and as a third component an organic solvent of formula (I), also referred to hereinafter as solvent (iii).
  • the ratio of the mass fractions of the different components of the slurry can be varied in a wide range.
  • the inventive slurry is characterized in that the slurry comprises i) 20 to 90 wt.-%, preferably 40 to 80 wt.-% of the inorganic material, preferably of the electroactive chalcogen-containing material,
  • the inventive slurry is characterized in that the inorganic material is an electroactive chalcogen-containing material, in particular selected from the group consisting of lithium-containing transition metal oxides and lithium-containing transition metal phosphates, the binder is a fluoropolymer, in particular a fluoropolymer comprising -CH2-CF2- units, the organic solvent of formula (I) is N-formylpyrrolidine and the conductive material is carbon in a conductive polymorph.
  • the inorganic material is an electroactive chalcogen-containing material, in particular selected from the group consisting of lithium-containing transition metal oxides and lithium-containing transition metal phosphates
  • the binder is a fluoropolymer, in particular a fluoropolymer comprising -CH2-CF2- units
  • the organic solvent of formula (I) is N-formylpyrrolidine
  • the conductive material is carbon in a conductive polymorph.
  • the inventive slurry is characterized in that the slurry comprises i) 40 to 80 wt.-% of the electroactive chalcogen-containing material, in particular selected from the group consisting of lithium-containing transition metal oxides and lithium- containing transition metal phosphates,
  • a solid structure has a three- dimensional geometric shape.
  • three-dimensional geometric shapes are films or layers, wherein one of the three dimensions is at least by a factor 10 smaller than the two other dimensions, or bodies, wherein the smallest of the three spatial dimensions (extents) is or is not recognizable to the naked eye.
  • three-dimensional geometric shapes in form of bodies are polyhedrons, like cubes, pyramids or toroids, cylinders, ellipsoids or spheres.
  • the present invention further provides the use of the inventive slurry as described above as a component for producing a solid structure, preferably wherein the solid structure is a layer, in particular wherein the solid structure is part of an electrode, in particular a cathode, for a rechargeable electrochemical cell.
  • a solid structure is usually obtained from the inventive slurry by first forming a liquid three- dimensional geometric shape of the slurry, for example a layer or a film of the slurry on at least one surface of a solid body by known deposition methods, or a liquid body in a correspondingly shaped mold, and secondly solidifying the initially formed body by removing the liquid medium, that means the organic solvent.
  • the present invention further provides a process for preparing a solid structure, comprising the process steps of a) forming a body by depositing of the slurry according to any of claims 1 to 7 on or in a substrate, and
  • the substrate on which or in which the slurry is deposited by known methods, like spin coating, casting, slot die coating, doctor blading, dip coating, spray coating, screen printing, inkjet printing or molding, can be varied in a wide range, depending on the desired solid structure.
  • Suitable substrates range from grids, meshs, sheets or foils of metal or non-metallic materials, in particular aluminum, nickel or copper foils, to specially designed molds.
  • the organic solvent of formula (I) is removed by heating the body, which was formed in process step a) and which was initially liquid, at a temperature in the range from 0 °C to 200 °C, preferably in the range from 50 °C to 180 °C, preferably for a period in the range from 0.001 h to 24 h, more preferably 0.01 h to 10 h.
  • the inventive slurry allows the preparation of electrodes for rechargeable electrochemical cells, preferably cathodes, wherein the cathodes comprise an electroactive chalcogen- containing material, a binder and optionally a conductive material, wherein the process steps of the preparation correspond to above-described process steps a) and b) for preparing a solid structure.
  • the present invention further provides a process for preparing a cathode for a rechargeable electrochemical cell, wherein the cathode comprises, v) a layer, which comprises an electroactive chalcogen-containing material, a binder and optionally a conductive material, comprising the process steps of a) forming a layer by depositing of the slurry according to any of claims 1 to 8 on a sub- strate, and
  • the inventive slurry allows the production of cathodes for electrochemical cell with advanta- geous properties, in particular with respect to the specific capacity of the electroactive material in the finally assembled electrochemical cell, which show an improved capacity.
  • the invention is illustrated by the examples which follow, but these do not restrict the invention.
  • PVDF material HSV900, Arkema
  • THINKY Planetary Centrifugal Mixer
  • Carbon materials SFG6L, C65, both from Timcal
  • solvent NFP
  • PVDF material HSV900, Arkema
  • THINKY Planetary Centrifugal Mixer
  • Carbon materials SFG6L, C65, both from Timcal
  • solvent NMP
  • NCM622 cathode active material
  • Electrodes were coated using continuous coating system (Mathis KTF-S, Switzerland). Drying conditions were 80°C and 135°C in the first and second drying zone, respectively. Electrodes were calendered using a lab-scale calender (Sumet, Germany) to a density of 3.1 g/cm 3 . For thickness measurements a micrometer gauge (Mitutoyo, Japan) was used.
  • Electrodes were coated using a table coater and quadruple film applicators (Erichsen, Ger- many). Electrodes were dried at 120 °C over-night in a vacuum drying chamber (BINDER, Germany). Electrodes were calendered using a lab-scale calender (Sumet, Germany) to a density of 3.1 g/cm 3 . For thickness measurements a micrometer gauge (Mitutoyo, Japan) was used. 1.4 Preparation of cathode CC4 from slurry CS4
  • Electrodes were coated using a table coater and quadruple film applicators (Erichsen, Germany). Electrodes were dried at 120 °C over-night in a vacuum drying chamber (BINDER, Germany). Electrodes were calendered using a lab-scale calender (Sumet, Germany) to a density of 3.1 g/cm 3 . For thickness measurements a micrometer gauge (Mitutoyo, Japan) was used.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

La présente invention concerne une bouillie comprenant i) un matériau inorganique, ii) un liant, et iii) un solvant organique de formule (I), L'invention concerne une suspension comprenant: i) un matériau inorganique, ii) un liant, et iii) un solvant organique de formule (I), dans laquelle R1 est H; d-Ce-Alkyl, R2, R3, R4, R5, R6, R7, R8, R9, R10, R11 sont indépendamment les uns des autres H ou Me; et n est O ou M. L'invention concerne en outre l'utilisation de telles suspensions comme constituant pour la production d'une structure solide, un procédé de préparation d'une structure solide, et un procédé de préparation d'une cathode pour cellule électrochimique rechargeable.
PCT/EP2017/062016 2016-05-25 2017-05-18 Suspensions de matières inorganiques pour former des structures solides WO2017202693A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP16171212 2016-05-25
EP16171212.0 2016-05-25

Publications (1)

Publication Number Publication Date
WO2017202693A1 true WO2017202693A1 (fr) 2017-11-30

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008113570A1 (fr) * 2007-03-19 2008-09-25 Umicore Matière d'insertion/extraction de li à une seule phase à température ambiante pour une utilisation dans une batterie à base de li
EP2383828A2 (fr) * 2010-04-30 2011-11-02 Samsung SDI Co., Ltd. Agent conducteur, composition de suspension d'électrode positive pour batterie secondaire au lithium incluant l'agent conducteur et batterie secondaire au lithium incluant l'agent conducteur
US20150104716A1 (en) 2013-10-10 2015-04-16 Samsung Electronics Co., Ltd. Electrolyte solution for secondary lithium battery and secondary lithium battery using the same
WO2015189094A1 (fr) 2014-06-12 2015-12-17 Basf Se Procédé de production de membranes de polyester microporeuses pour des applications électroniques

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008113570A1 (fr) * 2007-03-19 2008-09-25 Umicore Matière d'insertion/extraction de li à une seule phase à température ambiante pour une utilisation dans une batterie à base de li
EP2383828A2 (fr) * 2010-04-30 2011-11-02 Samsung SDI Co., Ltd. Agent conducteur, composition de suspension d'électrode positive pour batterie secondaire au lithium incluant l'agent conducteur et batterie secondaire au lithium incluant l'agent conducteur
US20150104716A1 (en) 2013-10-10 2015-04-16 Samsung Electronics Co., Ltd. Electrolyte solution for secondary lithium battery and secondary lithium battery using the same
WO2015189094A1 (fr) 2014-06-12 2015-12-17 Basf Se Procédé de production de membranes de polyester microporeuses pour des applications électroniques

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
"Lithium ion Batteries", 1998, WILEY VCH
A. HAYASHI; M. TATSUMISAGO, ELECTRONIC MATERIALS LETTERS, vol. 8, 2012, pages 199 - 207
C. JULIEN ET AL.: "Lithium Batteries: Science and Technology", 2016, SPRINGER INTERNATIONAL PUBLISHING
DAVID LINDEN: "Handbook of Batteries", 2010, MCGRAW-HILL PROFESSIONAL
J. O. BESENHARD: "Handbook of Battery Materials", 2011, WILEY-VCH
P. KNAUTH, SOLID STATE IONICS, vol. 180, 2009, pages 911 - 916

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