WO2021237846A1 - Solution électrolytique et dispositif électrochimique faisant appel à une solution électrolytique - Google Patents

Solution électrolytique et dispositif électrochimique faisant appel à une solution électrolytique Download PDF

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WO2021237846A1
WO2021237846A1 PCT/CN2020/097759 CN2020097759W WO2021237846A1 WO 2021237846 A1 WO2021237846 A1 WO 2021237846A1 CN 2020097759 W CN2020097759 W CN 2020097759W WO 2021237846 A1 WO2021237846 A1 WO 2021237846A1
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electrolyte
carbon atoms
silicon
compound
active material
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PCT/CN2020/097759
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English (en)
Chinese (zh)
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文倩
唐超
刘俊飞
郑建明
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宁德新能源科技有限公司
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Publication of WO2021237846A1 publication Critical patent/WO2021237846A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M10/0568—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
    • H01M4/13—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
    • H01M4/1395—Processes of manufacture of 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
    • H01M4/36—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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

  • This application relates to the technical field of electrochemical devices, and more specifically to an electrolyte and an electrochemical device using the electrolyte.
  • lithium-ion batteries have higher working voltage, greater energy density, faster charging speed and longer working life.
  • high-energy density secondary batteries have become an inevitable trend in the development of lithium-ion batteries.
  • Silicon has a reversible capacity of up to 4200mAh/g, making it the most promising negative electrode material for improving the energy density of lithium-ion batteries.
  • the use of silicon-containing anodes also faces many challenges. For example, the large volume expansion of silicon during the charge and discharge process destroys the solid electrolyte interface (SEI) film on the silicon surface, and the side reactions between the silicon anode material and the electrolyte intensify, resulting in battery production. Gas and capacity decay rapidly, and increase the cycle expansion rate.
  • SEI solid electrolyte interface
  • the embodiments of the present application provide an electrolyte and an electrochemical device using the electrolyte, in an attempt to solve at least one problem existing in the related field at least to some extent.
  • the embodiments of the present application also provide electrochemical devices and electronic devices using the electrolyte.
  • the present application provides an electrolyte solution comprising a fluorosiloxane compound and a trinitrile compound, wherein the fluorosiloxane compound includes a compound of formula I:
  • R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 are each independently selected from hydrogen, fluorine atoms, alkyl groups of 1-12 carbon atoms, fluoroalkyl groups of 1-12 carbon atoms, Cycloalkyl with 3-12 carbon atoms, fluorocycloalkyl with 3-12 carbon atoms, alkenyl with 2-12 carbon atoms, fluoroalkenyl with 2-12 carbon atoms, 3-12 A heterocyclic group of carbon atoms or a fluorinated heterocyclic group of 3-12 carbon atoms, and wherein at least one of R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 is a fluorine atom, Fluorinated alkyl groups with 1-12 carbon atoms, fluorinated cycloalkyl groups with 3-12 carbon atoms, fluoroalkenyl groups with 2-12 carbon atoms, or fluorinated heterocyclic groups with 3-12
  • trinitrile compound includes at least one of a compound of formula II or a compound of formula III:
  • a, b, c, d, e, f, g, h and i are integers of 0-5.
  • the fluorosiloxane compound includes at least one of the following compounds:
  • the trinitrile compound includes at least one of the following compounds:
  • the weight percentage of the fluorosiloxane compound is 0.01 wt% to 6 wt%, and the weight percentage of the trinitrile compound is 0.01 wt% to 8 wt%.
  • the electrolyte further includes an additive
  • the additive includes at least one of the following compounds: vinylene carbonate, 1,3-propane sultone, vinyl sulfate, succinonitrile, hexamethylene The dinitrile or fluoroethylene carbonate, wherein based on the total weight of the electrolyte, the weight percentage of the additive is 0.01 wt% to 20 wt%.
  • the present application provides an electrochemical device, which includes a positive electrode, a negative electrode, and the electrolyte according to the embodiment of the present application.
  • the anode includes a silicon-based anode active material
  • the silicon-based anode active material includes a silicon-containing matrix
  • the silicon-containing matrix includes at least one of Si, silicon oxide SiO x, or Si-M alloy.
  • the silicon-based negative electrode active material further includes an oxide Me a O b layer, the oxide Me a O b layer is located on at least a part of the surface of the silicon-containing matrix, wherein Me includes Al, Si At least one of Ti, Mn, V, Cr, Co or Zr, a is 1-3, b is 1-4, and wherein the thickness of the oxide Me a O b layer is 1 nm-500 nm.
  • the negative electrode further includes a conductive agent
  • the conductive agent includes at least one of carbon nanotubes, graphene, or carbon black, wherein the carbon nanotubes have a diameter of 1-100 nm and a length of 1-50 ⁇ m.
  • the silicon-based negative active material further includes a carbon layer located on at least a part of the surface of the silicon-containing substrate, and the thickness of the carbon layer is 1-500 nm.
  • the application provides an electronic device, which includes the electrochemical device according to the embodiment of the application.
  • the electrolyte provided by the application can form a stable solid electrolyte interface (SEI) protective layer on the surface of the positive and negative electrodes, and can significantly improve the normal temperature and high temperature cycle performance of the lithium ion secondary battery. Especially when applied to a battery with a silicon-based active material in the negative electrode, it can ensure the good stability of the negative electrode SEI protective layer after the battery is cycled, thereby improving the cycle performance of the battery.
  • SEI solid electrolyte interface
  • a list of items connected by the terms “one of”, “one of”, “one of” or other similar terms can mean any of the listed items.
  • Project A can contain a single element or multiple elements.
  • Project B can contain a single element or multiple elements.
  • Project C can contain a single element or multiple elements.
  • a list of items connected by the terms “at least one of”, “at least one of”, “at least one of” or other similar terms may mean the listed items Any combination of. For example, if items A and B are listed, then the phrase “at least one of A and B” means only A; only B; or A and B. In another example, if items A, B, and C are listed, then the phrase "at least one of A, B, and C” means only A; or only B; only C; A and B (excluding C); A and C (exclude B); B and C (exclude A); or all of A, B, and C.
  • Project A can contain a single element or multiple elements.
  • Project B can contain a single element or multiple elements.
  • Item C can contain a single element or multiple elements.
  • alkyl is expected to be a linear saturated hydrocarbon structure having 1 to 20 carbon atoms.
  • Alkyl is also expected to be a branched or cyclic hydrocarbon structure having 3 to 20 carbon atoms.
  • the alkyl group may be an alkyl group of 1-20 carbon atoms, an alkyl group of 1-10 carbon atoms, an alkyl group of 1-5 carbon atoms, an alkyl group of 5-20 carbon atoms, and an alkyl group of 5-15 carbon atoms. Carbon atom alkyl group or 5-10 carbon atom alkyl group.
  • butyl means to include n-butyl, sec-butyl, isobutyl, and tert-butyl And cyclobutyl
  • propyl includes n-propyl, isopropyl and cyclopropyl.
  • alkyl groups include, but are not limited to, methyl, ethyl, n-propyl, isopropyl, cyclopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, cyclobutyl, n-pentyl, Isopentyl, neopentyl, cyclopentyl, methylcyclopentyl, ethylcyclopentyl, n-hexyl, isohexyl, cyclohexyl, n-heptyl, octyl, cyclopropyl, cyclobutyl, norbornyl Base etc.
  • the alkyl group may be optionally substituted.
  • cycloalkyl encompasses cyclic alkyl groups.
  • the cycloalkyl group may be a cycloalkyl group of 3-20 carbon atoms, a cycloalkyl group of 6-20 carbon atoms, a cycloalkyl group of 3-12 carbon atoms, or a cycloalkyl group of 3-6 carbon atoms.
  • the cycloalkyl group may be cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, and the like.
  • cycloalkyl groups may be optionally substituted.
  • alkenyl refers to a monovalent unsaturated hydrocarbon group that can be straight or branched and has at least one and usually 1, 2, or 3 carbon-carbon double bonds. Unless otherwise defined, the alkenyl group usually contains 2-20 carbon atoms, for example, it can be an alkenyl group with 2-20 carbon atoms, an alkenyl group with 6-20 carbon atoms, or an alkenyl group with 2-12 carbon atoms. Group or alkenyl of 2-6 carbon atoms.
  • alkenyl groups include, for example, vinyl, n-propenyl, isopropenyl, n-but-2-enyl, but-3-enyl, n-hex-3-enyl, and the like. In addition, alkenyl groups may be optionally substituted.
  • heterocyclic group encompasses aromatic and non-aromatic cyclic groups. Heteroaromatic cyclic group also means heteroaryl.
  • the heteroaromatic ring group and the heteronon-aromatic ring group are C 3 -C 20 heterocyclic groups including at least one heteroatom, C 3 -C 150 heterocyclic groups, C 3 -C 10 Heterocyclic group, C 5 -C 20 heterocyclic group, C 5 -C 10 heterocyclic group, C 3 -C 6 heterocyclic group.
  • morpholinyl for example, morpholinyl, piperidinyl, pyrrolidinyl, etc., and cyclic ethers, such as tetrahydrofuran, tetrahydropyran, and the like.
  • the heterocyclic group may be optionally substituted.
  • trinitrile compound refers to a compound containing three -CN functional groups.
  • heteroatom encompasses O, S, P, N, B or isosteres thereof.
  • halogen encompasses F, Cl, Br, I.
  • substituents When the above-mentioned substituents are substituted, their substituents may be independently selected from the group consisting of halogen, alkyl, alkenyl, and aryl.
  • each component is based on the total weight of the electrolyte.
  • substituted or “substituted” means that it can be substituted with 1 or more (eg, 2, 3) substituents.
  • fluoro means that it can be substituted with one or more (for example, two, three) F.
  • the present application provides an electrolyte solution comprising a fluorosiloxane compound and a trinitrile compound, wherein the fluorosiloxane compound includes a compound of formula I:
  • R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 are each independently selected from hydrogen, fluorine atoms, alkyl groups of 1-12 carbon atoms, fluoroalkyl groups of 1-12 carbon atoms, Cycloalkyl with 3-12 carbon atoms, fluorocycloalkyl with 3-12 carbon atoms, alkenyl with 2-12 carbon atoms, fluoroalkenyl with 2-12 carbon atoms, 3-12 A heterocyclic group of carbon atoms or a fluorinated heterocyclic group of 3-12 carbon atoms, and wherein at least one of R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 is a fluorine atom, Fluorinated alkyl groups with 1-12 carbon atoms, fluorinated cycloalkyl groups with 3-12 carbon atoms, fluoroalkenyl groups with 2-12 carbon atoms, or fluorinated heterocyclic groups with 3-12
  • trinitrile compound includes or is selected from at least one compound of formula II or formula III:
  • a, b, c, d, e, f, g, h and i are integers of 0-5.
  • the fluorosiloxane compound includes or is selected from at least one of the following compounds:
  • the trinitrile compound includes or is selected from at least one of the following compounds:
  • the weight percentage of the fluorosiloxane compound is 0.01 wt% to 6 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the fluorosiloxane compound is 0.01 wt%, 0.05 wt%, 0.1 wt%, 0.5 wt%, 0.8 wt%, 1 wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 6wt%, or a range composed of any two of these values.
  • the weight percentage of the trinitrile compound is 0.01 wt% to 8 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the trinitrile compound is 0.01 wt%, 0.05 wt%, 0.1 wt%, 0.2 wt%, 0.5 wt%, 1 wt%, 1.5 wt% , 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 8wt%, or any two of these values.
  • the electrolyte further includes an additive, and the additive includes at least one of the following compounds: vinylene carbonate, 1,3-propane sultone, vinyl sulfate, succinonitrile, and adiponitrile. Nitrile or fluoroethylene carbonate.
  • the weight percentage of the additive is 0.01 wt% to 20 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the additive is 0.01 wt%, 0.05 wt%, 0.1 wt%, 0.5 wt%, 1 wt%, 5 wt%, 6 wt%, 6.5 wt% , 7wt%, 10wt%, 11wt%, 15wt%, 18wt%, 20wt% or any two of these values.
  • the electrolyte further includes a cyclic ether.
  • the cyclic ether can form a film on the anode and the cathode at the same time to reduce the reaction between the electrolyte and the active material.
  • the cyclic ether includes, but is not limited to: tetrahydrofuran, 2-methyltetrahydrofuran, 1,3-dioxolane, 2-methyl 1,3-dioxolane, 4-methyl Base 1,3-dioxolane, 1,3-dioxane, 1,4-dioxane, dimethoxypropane.
  • the weight percentage of the cyclic ether is 0.1 wt% to 10 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the cyclic ether is not less than 0.1 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the cyclic ether is not less than 0.5 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the cyclic ether is not more than 2 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the cyclic ether is not more than 5 wt%.
  • the electrolyte further includes chain ether.
  • chain ethers include, but are not limited to: dimethoxymethane, 1,1-dimethoxyethane, 1,2-dimethoxyethane, diethoxymethane, 1 ,1-diethoxyethane, 1,2-diethoxyethane, ethoxymethoxymethane, 1,1-ethoxymethoxyethane, 1,2-ethoxymethyl Oxyethane.
  • the weight percentage of the chain ether is 0.1 wt% to 10 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the chain ether is not less than 0.5 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the chain ether is not less than 2 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the chain ether is not less than 3 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the chain ether is not more than 10 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the chain ether is not more than 5 wt%.
  • the electrolyte further includes a phosphorus-containing organic solvent.
  • Phosphorus-containing organic solvents can enhance the safety performance of the electrolyte.
  • the phosphorus-containing organic solvent includes, but is not limited to: trimethyl phosphate, triethyl phosphate, dimethyl ethyl phosphate, methyl diethyl phosphate, ethylene methyl phosphate, phosphoric acid Ethylene ethyl, triphenyl phosphate, trimethyl phosphite, triethyl phosphite, triphenyl phosphite, tris(2,2,2-trifluoroethyl) phosphate, tris(2, 2,3,3,3-pentafluoropropyl) ester.
  • the weight percentage of the phosphorus-containing organic solvent is 0.1 wt% to 10 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the phosphorus-containing organic solvent is not less than 0.1 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the phosphorus-containing organic solvent is not less than 0.5 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the phosphorus-containing organic solvent is not more than 2 wt%.
  • the weight percentage of the phosphorus-containing organic solvent is not more than 3 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the phosphorus-containing organic solvent is not more than 5 wt%.
  • the electrolyte further includes an aromatic fluorine-containing solvent.
  • the aromatic fluorine-containing solvent can quickly form a film to protect the active material, and the fluorine-containing substance can improve the infiltration performance of the electrolyte to the active material.
  • the aromatic fluorine-containing solvent includes, but is not limited to: fluorobenzene, difluorobenzene, trifluorobenzene, tetrafluorobenzene, pentafluorobenzene, hexafluorobenzene, and trifluoromethylbenzene.
  • the weight percentage of the aromatic fluorine-containing solvent is about 0.1 wt% to 10 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the aromatic fluorine-containing solvent is not less than 0.5 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the aromatic fluorine-containing solvent is not less than 2 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the aromatic fluorine-containing solvent is not more than 4 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the aromatic fluorine-containing solvent is not more than 8 wt%.
  • the electrolyte further includes a lithium salt additive.
  • the lithium salt additives include, but are not limited to, lithium trifluoromethanesulfonimide LiN(CF 3 SO 2 ) 2 (LiTFSI for short), lithium bis(fluorosulfonyl)imide Li(N (SO 2 F) 2 ) (LiFSI for short), Lithium bisoxalate borate LiB (C 2 O 4 ) 2 (LiBOB for short), lithium tetrafluorophosphate oxalate (LiPF4C2O2), lithium difluorooxalate borate LiBF 2 (C 2 O 4 ) (abbreviated as LiDFOB), lithium hexafluorocesium oxide (LiCsF 6 ).
  • the weight percentage of the lithium salt additive is 0.01 wt% to 10 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the lithium salt additive is 0.1 wt% to 5 wt%. In some embodiments, based on the total weight of the electrolyte, the weight percentage of the lithium salt additive is 0.1wt%, 1wt%, 3wt%, 5wt%, 7wt%, 9wt%, 10wt% or any of these values. The range of the two.
  • This application provides an electrolyte containing a fluorosiloxane compound and a trinitrile compound.
  • the electrolyte can form a stable SEI protective layer on the surface of the positive and negative electrodes, and can significantly improve the normal temperature and high temperature cycle performance of the secondary battery.
  • it can ensure the good stability of the negative electrode SEI protective layer after the battery is cycled, thereby improving the cycle performance of the battery.
  • the electrolyte used in the electrolyte of the embodiment of the present application may be an electrolyte known in the prior art.
  • the electrolyte includes, but is not limited to: inorganic lithium salts, such as LiClO 4 , LiAsF 6 , LiPF 6 , LiBF 4 , LiSbF 6 , LiSO 3 F, LiN(FSO 2 ) 2 etc.; fluorine-containing organic lithium salts, such as LiCF 3 SO 3 , LiN(FSO 2 )(CF 3 SO 2 ), LiN(CF 3 SO 2 ) 2 , LiN(C 2 F 5 SO 2 ) 2.
  • inorganic lithium salts such as LiClO 4 , LiAsF 6 , LiPF 6 , LiBF 4 , LiSbF 6 , LiSO 3 F, LiN(FSO 2 ) 2 etc.
  • fluorine-containing organic lithium salts such as LiCF 3 SO 3 , LiN(FSO 2 )(CF 3 SO 2 ),
  • LiBF 2 (CF 3 ) 2 LiBF 2 (C 2 F 5 ) 2 , LiBF 2 (CF 3 SO 2 ) 2 , LiBF 2 (C 2 F 5 SO 2 ) 2 ; lithium salt containing dicarboxylic acid complex
  • the above-mentioned electrolytes may be used singly, or two or more of them may be used at the same time.
  • the electrolyte includes a combination of LiPF 6 and LiBF 4.
  • the electrolyte includes a combination of an inorganic lithium salt such as LiPF 6 or LiBF 4 and a fluorine-containing organic lithium salt such as LiCF 3 SO 3 , LiN(CF 3 SO 2 ) 2 , and LiN(C 2 F 5 SO 2 ) 2 .
  • the concentration of the electrolyte is in the range of 0.8-3 mol/L, for example, in the range of 0.8-2.5 mol/L, in the range of 0.8-2 mol/L, in the range of 1-2 mol/L, 0.5- 1.5mol/L, 0.8-1.3mol/L, 0.5-1.2mol/L, for example, 1mol/L, 1.15mol/L, 1.2mol/L, 1.5mol/L, 2mol/L or 2.5mol/L.
  • the present application provides a negative electrode including a current collector and a coating layer on the current collector, and the coating layer includes a silicon-based negative electrode active material.
  • the silicon-based negative active material include silicon-containing body, said body comprising a silicon-containing Si, silicon oxide SiO x, Si-M alloy is at least one, wherein, 0.6 ⁇ x ⁇ 2, M is selected from at least one of Al, Ti, Fe, or Ni.
  • the silicon-containing matrix includes at least one of Si, SiO 2 , SiO, or SiC.
  • the silicon-based negative electrode active material further includes an oxide Me a O b layer, the oxide Me a O b layer is located on at least a part of the surface of the silicon-containing matrix, wherein Me includes Al, Si At least one of, Ti, Mn, V, Cr, Co, or Zr, and a is 1-3, and b is 1-4.
  • the thickness of the oxide Me a O b layer is 1 nm-500 nm. In some embodiments, the thickness of the oxide Me a O b layer is 1 nm, 5 nm, 10 nm, 20 nm, 30 nm, 50 nm, 80 nm, 120 nm, 150 nm, 200 nm, 300 nm, 400 nm, 450 nm, 500 nm, or any of these values. The range of the two.
  • the oxide Me a O b includes at least one of Al 2 O 3 , TiO 2 , CoO, and ZrO 2.
  • the negative electrode further includes a conductive agent, and the conductive agent includes at least one of carbon nanotubes, graphene, or carbon black.
  • the diameter of the carbon nanotubes is 1-100 nm. In some embodiments, the diameter of the carbon nanotube is 1nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 70nm, 80nm, 90nm, 100nm or these values The range of any two of them.
  • the length of the carbon nanotubes is 1-50 ⁇ m. In some embodiments, the length of the carbon nanotubes is 1 ⁇ m, 5 ⁇ m, 10 ⁇ m, 15 ⁇ m, 20 ⁇ m, 25 ⁇ m, 30 ⁇ m, 35 ⁇ m, 45 ⁇ m, 50 ⁇ m, or a range composed of any two of these values.
  • the aspect ratio of the carbon nanotubes is 0.1-5000. In some embodiments, the aspect ratio of the carbon nanotubes is 0.1, 7, 10, 50, 100, 200, 500, 1000, 2000, 2500, 2800, 3000, 3500, 4000, 4500, 5000 or these values The range of any two of them.
  • the silicon-based negative electrode active material further includes a carbon layer located on at least a part of the surface of the silicon-containing substrate.
  • the thickness of the carbon layer is 1-500 nm. In some embodiments, the thickness of the carbon layer is 1nm, 5nm, 10nm, 30nm, 40nm, 50nm, 80nm, 100nm, 150nm, 200nm, 250nm, 300nm, 400nm, 500nm or any two of these values. Scope.
  • the carbon layer includes at least one of amorphous carbon, graphite, hard carbon, soft carbon, carbon black, acetylene black, or carbon nanotubes.
  • the coating further includes graphite particles.
  • the weight ratio of the silicon-based negative active material to the graphite particles is 1:30-1:10. In some embodiments, the weight ratio of the silicon-based negative electrode active material to the graphite particles is 1:30, 1:25, 1:20, 1:15, 1:10 or any two of these values. Scope.
  • the coating further includes a thickener.
  • the thickener includes at least one of sodium carboxymethyl cellulose (CMC-Na), lithium carboxymethyl cellulose (CMC-Li), and cellulose.
  • the coating further includes a binder, the binder including polyacrylate, polyimide, polyamide, polyamideimide, polyvinylidene fluoride, styrene butadiene rubber, seaweed Sodium, polyvinyl alcohol, polytetrafluoroethylene, polyacrylonitrile or any combination thereof.
  • a binder including polyacrylate, polyimide, polyamide, polyamideimide, polyvinylidene fluoride, styrene butadiene rubber, seaweed Sodium, polyvinyl alcohol, polytetrafluoroethylene, polyacrylonitrile or any combination thereof.
  • the current collector includes copper, aluminum, nickel, copper alloy, aluminum alloy, nickel alloy, or a combination thereof.
  • the preparation method of the silicon-based negative electrode active material (which includes a silicon-containing substrate and an oxide Me a O b layer on at least a part of the surface of the silicon-containing substrate) includes:
  • the silicon-containing matrix and the oxide precursor MeT n are formed into a mixed solution in the presence of an organic solvent and deionized water;
  • Me includes at least one of Al, Si, Ti, Mn, Cr, V, Co or Zr,
  • T includes at least one of methoxy, ethoxy, isopropoxy or halogen
  • n 1, 2, 3, or 4.
  • the oxide precursor MeT n includes isopropyl titanate, aluminum isopropoxide, or a combination thereof.
  • the silicon-containing matrix is as defined above.
  • the sintering temperature is 250-900°C. In some embodiments, the sintering temperature is 300-850°C. In some embodiments, the sintering temperature is 350-650°C. In some embodiments, the sintering temperature is 400°C, 500°C, 600°C, or 700°C.
  • the sintering time is 1-25h. In some embodiments, the sintering time is 1-119h. In some embodiments, the sintering time is 1-14h. In some embodiments, the sintering time is 1.5-5h. In some embodiments, the sintering time is 2h, 3h, 4h, 5h, 6h, 8h, or 10h.
  • the organic solvent includes at least one of the following solvents: ethanol, methanol, n-hexane, N,N-dimethylformamide, pyrrolidone, acetone, toluene, isopropanol, or n-propanol. In some embodiments, the organic solvent is ethanol.
  • the halogen includes F, Cl, Br, or a combination thereof.
  • sintering is performed under the protection of inert gas.
  • the inert gas includes nitrogen, argon, or a combination thereof.
  • the drying is spray drying, and the drying temperature is 100-300°C.
  • the negative electrode can be obtained by mixing the negative electrode active material, conductive agent, thickener, and binder in a solvent to prepare an active material composition slurry, and coating the slurry on On the current collector.
  • the thickness of the oxide Me a O b layer is controlled by controlling the weight of the oxide precursor.
  • the solvent may include, but is not limited to: N-methylpyrrolidone, deionized water.
  • the electrolyte according to the present application can generate a stable SEI protective layer on the surface of the silicon-based negative electrode active material.
  • the SEI protective layer is circulating During the process, it is not easy to peel off from the silicon-based negative electrode active material, which can effectively improve the cycle capacity retention rate of lithium-ion batteries (silicon negative electrode lithium-ion batteries) using silicon-based negative electrode active materials, and alleviate battery swelling during cycling , And can improve the high temperature resistance of the battery after cycling, and avoid thermal runaway of the silicon anode lithium ion battery.
  • the electrolyte of the present application can effectively improve the stability of the SEI protective layer, due to the huge volume expansion of the silicon-based negative electrode active material particles, the SEI protective layer needs to continuously consume additives for repair, which accelerates the consumption of additives rate.
  • the present application provides an oxide Me a O b layer and/or a carbon layer on the surface of the silicon-containing substrate of a part of the silicon-based negative electrode active material .
  • the oxide Me a O b layer or the carbon layer has a certain mechanical strength. It can effectively suppress the volume expansion of the silicon-based negative electrode active material, and can also inhibit the etching of the surface of the silicon-based negative electrode active material by HF in the electrolyte.
  • the combined use of the electrolyte containing the SEI film-forming additive of fluorosiloxane and trinitrile compound and the silicon-based negative electrode active material with oxide Me a O b layer or carbon layer on the surface can effectively improve the performance of lithium ion batteries. Cycle stability and cycle capacity retention rate, and reduce the cycle thickness expansion rate of lithium ion batteries.
  • the conductivity of the silicon-based negative electrode active material is usually not very ideal, and it not only cannot support the high-rate charging performance during the full battery cycle, but also has a certain impact on the cycle performance.
  • Carbon materials have good electrical conductivity, mechanical strength and ductility. Therefore, in order to improve the conductivity of the negative electrode containing silicon-based negative electrode active material, this application provides a carbon layer on the surface of the silicon-containing substrate of part of the silicon-based negative electrode active material. And the carbon nanotube conductive agent is doped into the negative electrode active material to effectively improve the cycle performance of the battery.
  • the electrochemical device of the present application includes any device that undergoes an electrochemical reaction, and specific examples thereof include all kinds of primary batteries, secondary batteries, fuel cells, solar cells, or capacitors.
  • the electrochemical device is a lithium secondary battery, including a lithium metal secondary battery, a lithium ion secondary battery, a lithium polymer secondary battery, or a lithium ion polymer secondary battery.
  • the electrochemical device of the present application is an electrochemical device having a positive electrode having a positive electrode active material capable of occluding and releasing metal ions, and a negative electrode having a negative electrode active material capable of occluding and releasing metal ions. Its characteristics are It includes the electrolyte in any of the above-mentioned embodiments of the present application.
  • the electrolyte used in the electrochemical device of the present application is the electrolyte of any of the above-mentioned embodiments in the present application.
  • the electrolytic solution used in the electrochemical device of the present application may also include other electrolytic solutions within the scope not departing from the gist of the present application.
  • the negative electrode used in the electrochemical device of the present application is a conventional negative electrode in the prior art, or the negative electrode of any of the above-mentioned embodiments in this application.
  • the negative electrode used in the electrochemical device of the present application may also include other negative electrodes within the scope not departing from the gist of the present application.
  • the material of the positive electrode used in the electrochemical device of the present application can be prepared using materials, structures, and manufacturing methods known in the art.
  • the technology described in US9812739B can be used to prepare the positive electrode of the present application, which is incorporated into the present application by reference in its entirety.
  • the positive electrode includes a current collector and a positive electrode active material layer on the current collector.
  • the positive electrode active material includes at least one lithiated intercalation compound that reversibly intercalates and deintercalates lithium ions.
  • the positive active material includes a composite oxide.
  • the composite oxide contains lithium and at least one element selected from cobalt, manganese, and nickel.
  • the positive electrode active material is selected from lithium cobalt oxide (LiCoO 2 ), lithium nickel cobalt manganese (NCM) ternary material, lithium iron phosphate (LiFePO 4 ), lithium manganese oxide (LiMn 2 O 4 ), or their Any combination of.
  • the positive active material may have a coating on its surface, or may be mixed with another compound having a coating.
  • the coating may include at least one selected from the oxide of the coating element, the hydroxide of the coating element, the oxyhydroxide of the coating element, the oxycarbonate of the coating element, and the hydroxycarbonate of the coating element.
  • the compound used for the coating may be amorphous or crystalline.
  • the coating element contained in the coating may include Mg, Al, Co, K, Na, Ca, Si, Ti, V, Sn, Ge, Ga, B, As, Zr, F, or these Any combination of.
  • the coating can be applied by any method as long as the method does not adversely affect the performance of the positive electrode active material.
  • the method may include any coating method known in the art, such as spraying, dipping, and the like.
  • the positive active material layer further includes a binder, and optionally a conductive material.
  • the binder improves the bonding of the positive electrode active material particles to each other, and also improves the bonding of the positive electrode active material to the current collector.
  • the binder includes, but is not limited to: polyvinyl alcohol, hydroxypropyl cellulose, diacetyl cellulose, polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene-containing Oxygen polymers, polyvinylpyrrolidone, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, polypropylene, styrene butadiene rubber, acrylic (ester) styrene butadiene rubber, epoxy resin, Nylon etc.
  • conductive materials include, but are not limited to: carbon-based materials, metal-based materials, conductive polymers, and mixtures thereof.
  • the carbon-based material is selected from natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, carbon fiber, or any combination thereof.
  • the metal-based material is selected from metal powder, metal fiber, copper, nickel, aluminum, silver.
  • the conductive polymer is a polyphenylene derivative.
  • the current collector may be aluminum, but is not limited thereto.
  • the positive electrode can be prepared by a preparation method known in the art.
  • the positive electrode can be obtained by mixing the active material, the conductive material, and the binder in a solvent to prepare an active material composition, and coating the active material composition on a current collector.
  • the solvent may include N-methylpyrrolidone and the like, but is not limited thereto.
  • the positive electrode is made by forming a positive electrode material using a positive electrode active material layer including lithium transition metal-based compound powder and a binder on a current collector.
  • the positive active material layer can generally be made by the following operations: dry mixing the positive electrode material and the binder (conducting material and thickener used as needed) to form a sheet, The obtained sheet is press-bonded to the positive electrode current collector, or these materials are dissolved or dispersed in a liquid medium to form a slurry, which is coated on the positive electrode current collector and dried.
  • the material of the positive active material layer includes any material known in the art.
  • the electrochemical device of the present application is provided with a separator between the positive electrode and the negative electrode to prevent short circuits.
  • the material and shape of the isolation membrane used in the electrochemical device of the present application are not particularly limited, and it may be any technology disclosed in the prior art.
  • the isolation membrane includes a polymer or an inorganic substance formed of a material that is stable to the electrolyte of the present application.
  • the isolation film may include a substrate layer and a surface treatment layer.
  • the substrate layer is a non-woven fabric, film or composite film with a porous structure, and the material of the substrate layer is selected from at least one of polyethylene, polypropylene, polyethylene terephthalate and polyimide.
  • a polypropylene porous film, a polyethylene porous film, a polypropylene non-woven fabric, a polyethylene non-woven fabric, or a polypropylene-polyethylene-polypropylene porous composite film can be selected.
  • a surface treatment layer is provided on at least one surface of the substrate layer, and the surface treatment layer may be a polymer layer or an inorganic substance layer, or a layer formed by a mixed polymer and an inorganic substance.
  • the inorganic layer includes inorganic particles and a binder.
  • the inorganic particles are selected from alumina, silica, magnesium oxide, titanium oxide, hafnium dioxide, tin oxide, ceria, nickel oxide, zinc oxide, calcium oxide, zirconium oxide, One or a combination of yttrium oxide, silicon carbide, boehmite, aluminum hydroxide, magnesium hydroxide, calcium hydroxide, and barium sulfate.
  • the binder is selected from polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, polyamide, polyacrylonitrile, polyacrylate, polyacrylic acid, polyacrylate, polyvinylpyrrolidone, polyvinyl ether, One or a combination of polymethyl methacrylate, polytetrafluoroethylene and polyhexafluoropropylene.
  • the polymer layer contains a polymer, and the material of the polymer includes polyamide, polyacrylonitrile, acrylate polymer, polyacrylic acid, polyacrylate, polyvinylpyrrolidone, polyvinyl ether, polyvinylidene fluoride or poly( At least one of vinylidene fluoride-hexafluoropropylene).
  • the electrolyte according to the embodiments of the present application can be used to improve the rate performance, storage capacity retention rate at room temperature, and cycle and high temperature storage performance of the battery, and is suitable for use in electronic equipment including electrochemical devices.
  • the use of the electrochemical device of the present application is not particularly limited, and it can be used for various well-known uses.
  • notebook computers pen-input computers, mobile computers, e-book players, portable phones, portable fax machines, portable copiers, portable printers, stereo headsets, video recorders, LCD TVs, portable cleaners, portable CD players, Mini discs, transceivers, electronic notebooks, calculators, memory cards, portable recorders, radios, backup power supplies, motors, cars, motorcycles, assisted bicycles, bicycles, lighting equipment, toys, game consoles, clocks, power tools, flashlights , Cameras, large household storage batteries or lithium-ion capacitors, etc.
  • a lithium ion battery is taken as an example and combined with specific examples of preparing the electrolyte of the present application and the measurement method of the electrochemical device to illustrate the preparation and performance of the lithium ion battery of the present application.
  • the preparation methods described in this application are only examples, and any other suitable preparation methods are within the scope of this application.
  • the cathode material of this application can be used in other suitable electrochemical devices.
  • Such an electrochemical device includes any device that undergoes an electrochemical reaction, and specific examples thereof include all kinds of primary batteries, secondary batteries, fuel cells, solar cells, or capacitors.
  • the electrochemical device is a lithium secondary battery, including a lithium metal secondary battery, a lithium ion secondary battery, a lithium polymer secondary battery, or a lithium ion polymer secondary battery.
  • ethylene carbonate (EC), propylene carbonate (PC) and diethyl carbonate (DEC) are mixed uniformly in a weight ratio of 20:10:70, and then fully dried lithium salt LiPF 6 is dissolved in The mixed solvents above obtain a basic electrolyte, wherein the concentration of LiPF 6 in the basic electrolyte is 1 mol/L.
  • the different contents of fluorosiloxane, trinitrile compound and fluoroethylene carbonate (FEC) shown in Table 1 were added to the basic electrolyte to obtain electrolytes of different examples and comparative examples.
  • the content of each substance in the electrolyte described below is calculated based on the total weight of the electrolyte.
  • Isolation membrane Polyethylene (PE) porous polymer film is used as the isolation membrane.
  • the negative electrode slurry is evenly coated on the copper foil of the negative electrode current collector with a thickness of 8 ⁇ m, and the negative electrode film is obtained by baking at 120° C. for 1 hour, and the negative electrode is obtained by compaction and slitting.
  • Table 1 shows the types and contents of related substances in the electrolyte in Examples 1-65 and Comparative Examples 1-4 and the substances used in steps 1)-5) in Examples 1-65 and Comparative Examples 1-4
  • the type and dosage and related parameters The order of the types and contents of additives in Table 1 is the same.
  • the types and contents of additives in Example 22 are FEC: 5 wt% + PS: 0.5 wt% + SN: 1.5 wt%.
  • the thickness of the oxide Me a O b layer is controlled by controlling the weight of the oxide precursor.
  • the "—” means that the substance does not exist.
  • FEC Fluorinated Ethylene Carbonate
  • the lithium ion secondary battery stand for 30 minutes, charge at a constant current of 0.5C to a voltage of 4.45V, charge at a constant voltage of 4.45V to a current of 0.05C, and stand for 5 minutes at a constant current of 0.5C Discharge to a voltage of 3.0V as a charge-discharge cycle process.
  • the discharge capacity this time is the first discharge capacity of the lithium-ion secondary battery.
  • the lithium-ion secondary battery is subjected to a cyclic charge and discharge test in the above manner until the capacity retention rate is less than 80%, and the test is stopped, and the number of cycles of different groups is recorded.
  • the capacity retention rate (%) of the lithium ion secondary battery after N cycles discharge capacity at the Nth cycle/first discharge capacity ⁇ 100%.
  • the lithium ion secondary battery stand for 30 minutes, charge at a constant current of 0.5C to a voltage of 4.45V, charge at a constant voltage of 4.45V to a current of 0.05C, and stand for 5 minutes at a constant current of 0.5C Discharge to a voltage of 3.0V as a charge-discharge cycle process.
  • the discharge capacity this time is the first discharge capacity of the lithium-ion secondary battery.
  • the lithium-ion secondary battery is subjected to a cyclic charge and discharge test in the above manner until the capacity retention rate is less than 80%, and the test is stopped, and the number of cycles of different groups is recorded.
  • the capacity retention rate (%) of the lithium ion secondary battery after N cycles discharge capacity at the Nth cycle/first discharge capacity ⁇ 100%.
  • Table 2 shows the performance test results of the lithium ion secondary batteries of Examples 1-65 and Comparative Examples 1-4.
  • Example 1 Serial number Number of cycles at 25°C 45°C cycle number
  • Example 2 668 362
  • Example 3 670 369
  • Example 4 674 375
  • Example 5 675 379
  • Example 6 674 376
  • Example 8 671 372
  • Example 9 673 374
  • Example 10 673 375
  • Example 11 658 355
  • Example 12 665 367
  • Example 13 674 374
  • Example 14 673 372
  • Example 15 670 371
  • Example 16 668 368
  • Example 17 664 352
  • Example 18 673 374
  • Example 19 675 376
  • Example 20 674 376
  • Example 21 680 381
  • Example 22 678 392
  • Example 23 677 392
  • Example 24 681 390
  • Example 25 670 374
  • Example 26 677 376 Example 27 679 380 Example 28 681 386 Example 29 680 397 Example 30 678 398 Example 31 669 400 Example 32 653 350 Example 33 675 388 Example 34 672 380 Example 35 675 380 Example 36 678 381 Example 37 681 381 Example 38 685 380 Example 39 688 379 Example 40 688 378 Example 41 685 375 Example 42 662 380 Example 43 677 392 Example 44 649 348 Example 45 662 376 Example 46 663 376 Example 47 663 376 Example 48 664 378 Example 49 664 378 Example 50 670 380 Example 51 675 381 Example 52 681 382 Example 53 682 382 Example 54 682 382 Example 55 683 382 Example 56 660 381 Example 57 659 373 Example 58 630 371 Example 59 657 345 Example 60 628 341 Example 61 681 380 Example 62 680 381 Example 63 675 390 Example 64 674 390 Example 65 674 389 Comparative example 1 642 339 Comparative
  • references to “some embodiments”, “partial embodiments”, “one embodiment”, “another example”, “examples”, “specific examples” or “partial examples” throughout the specification mean At least one embodiment or example in this application includes the specific feature, structure, material, or characteristic described in the embodiment or example. Therefore, the descriptions appearing in various places throughout the specification, such as: “in some embodiments”, “in embodiments”, “in one embodiment”, “in another example”, “in an example “In”, “in a specific example” or “exemplified”, which are not necessarily quoting the same embodiment or example in this application.
  • the specific features, structures, materials, or characteristics herein can be combined in one or more embodiments or examples in any suitable manner.

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Abstract

L'invention concerne une solution électrolytique et un dispositif électrochimique faisant appel à la solution électrolytique. La solution électrolytique contient un composé fluorosiloxane et un composé trinitrile, le composé fluorosiloxane comprenant un composé de formule I, et le composé trinitrile comprenant un composé de formule II et/ou un composé de formule III, a, b, c, d, e, f, g, h et i étant des nombres entiers de 0 à 5. Une batterie au lithium-ion préparée à partir de la solution électrolytique possède des performances améliorées en termes de cycle à température ambiante et à haute température.
PCT/CN2020/097759 2020-05-27 2020-06-23 Solution électrolytique et dispositif électrochimique faisant appel à une solution électrolytique WO2021237846A1 (fr)

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