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WO2004093099A1 - Procede de production d'un electrolyte solide conducteur de ion lithium et pile secondaire de type entierement solide au moyen dudit electrolyte - Google Patents

Procede de production d'un electrolyte solide conducteur de ion lithium et pile secondaire de type entierement solide au moyen dudit electrolyte Download PDF

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Publication number
WO2004093099A1
WO2004093099A1 PCT/JP2004/005248 JP2004005248W WO2004093099A1 WO 2004093099 A1 WO2004093099 A1 WO 2004093099A1 JP 2004005248 W JP2004005248 W JP 2004005248W WO 2004093099 A1 WO2004093099 A1 WO 2004093099A1
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WO
WIPO (PCT)
Prior art keywords
lithium
solid electrolyte
ion conductive
conductive solid
sulfide
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.)
Ceased
Application number
PCT/JP2004/005248
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English (en)
Japanese (ja)
Inventor
Minoru Senga
Yoshikatsu Seino
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Idemitsu Kosan Co Ltd
Original Assignee
Idemitsu Kosan Co Ltd
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 Idemitsu Kosan Co Ltd filed Critical Idemitsu Kosan Co Ltd
Priority to JP2005505406A priority Critical patent/JP4621139B2/ja
Publication of WO2004093099A1 publication Critical patent/WO2004093099A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • 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 method for producing a lithium ion conductive solid electrolyte and an all-solid-state secondary battery using the same. More specifically, the present invention provides a method for industrially advantageously producing a lithium ion conductive solid electrolyte by applying a reaction in an organic solvent at a relatively low temperature without requiring special equipment, and The present invention relates to an all-solid-state secondary battery using the same. Background art
  • Lithium batteries are being actively studied in various fields as batteries that can obtain high energy density, but most solid electrolytes currently used in lithium batteries contain flammable organic substances. Therefore, if an abnormality occurs in the battery, there is a risk of fire, etc., and it is desired to ensure the safety of the battery.
  • solid electrolytes composed of non-combustible solid materials have been developed due to the strong social demands for improved reliability against shock and vibration, higher energy density, and a clean and highly efficient energy conversion system for the global environment. The development of an all-solid-state lithium secondary pond using methane is desired.
  • a method is also known in which a raw material is put in a carbon-coated silica tube, vacuum-sealed, and reacted at 700 ° C. for 8 hours (Japanese Patent Laid-Open No. 11-176326). I have. However, this method is also unsuitable for mass production because it requires special equipment for performing high-temperature reactions under vacuum.
  • the present invention has been made in view of the above problems, and can easily mass-produce a lithium-ion conductive solid electrolyte at a relatively low reaction temperature without requiring special equipment.
  • the purpose is to provide an industrially advantageous method.
  • Another object is to provide an all-solid-state lithium secondary battery using the same. Disclosure of the invention
  • the present inventors have conducted intensive studies to achieve the above object, and as a result, have found that the object can be achieved by applying an organic solvent reaction, thereby completing the present invention.
  • the present invention (1) Reacting a lithium component, a sulfur component, and one or more components selected from the group consisting of a simple phosphorus, a simple silicon, a single boron, and a simple germane in an organic solvent.
  • a method for producing a lithium ion conductive solid electrolyte A method for producing a lithium ion conductive solid electrolyte,
  • the sulfur component and one or two or more components selected from the group consisting of a simple phosphorus, a simple silicon, a simple boron and a simple germanium are selected from the group consisting of sulfur nitride, silicon sulfide,
  • a method for producing a lithium ion conductive solid electrolyte characterized by reacting one or more compounds selected from the group consisting of:
  • the lithium compound having basicity is one or more compounds selected from the group consisting of n-butyllithium, sec-butyllithium, tert-butyllithium, hexyllithium, and lithium alkoxide.
  • the raw material is a lithium component, a sulfur component, and one selected from the group consisting of a simple phosphorus, a simple silicon, a simple boron, and a simple germanium.
  • a lithium component a sulfur component
  • two or more types of 'components are used, and these components are reacted in an organic solvent to produce a lithium ion conductive solid electrolyte.
  • lithium hydrosulfide is used as the first component, and elemental sulfur, phosphorus, silicon, boron, germanium, phosphorus sulfide, silicon sulfide, silicon sulfide, and boron sulfide are used as the second component.
  • a lithium ion conductive solid electrolyte is produced by reacting one or two or more compounds selected from the group consisting of manganese and germanium sulfide in an organic solvent.
  • the lithium component used as a raw material in the method of the present invention is not particularly limited, but it is preferable to use a high-purity product. Particularly preferred are lithium sulfide and lithium hydrosulfide.
  • lithium hydrosulfide As a method for producing lithium hydrosulfide, a method in which hydrogen sulfide is blown into lithium hydroxide in a non-protonic organic solvent to cause a reaction (Japanese Patent Application Laid-Open No. 7-33012) can be employed. Specifically, in N-methyl-2-pyrrolidone, lithium hydroxide / hydrogen sulfide (molar ratio) is supplied in the range of 1.8 to 3.00, preferably 1.95 to 3.00, 0 to 150 ° C, Preferably, the reaction can be carried out at 120 to 140 ° C.
  • the sulfur component as a raw material of the method of the present invention and one or more components selected from the group consisting of simple phosphorus, simple silicon, single boron, and simple germanium may be used as separate components, respectively. It may be used as one or more compounds selected from the group consisting of phosphorus sulfide, silicon sulfide, boron sulfide and germanium sulfide. Commercial products can be used for these separate components or compounds as long as they are highly pure.
  • the method of the present invention is characterized in that the raw materials are reacted in an organic solvent.
  • the organic solvent is not particularly limited, but a non-protonic organic solvent is particularly preferred.
  • Non-protonic organic solvents generally include non-protonic polar organic compounds (for example, amide compounds, lactam compounds, urea compounds, organic compounds, cyclic organic phosphorus compounds, etc.). It can be suitably used as a single solvent or as a mixed solvent.
  • non-protonic polar organic compounds for example, amide compounds, lactam compounds, urea compounds, organic compounds, cyclic organic phosphorus compounds, etc.
  • examples of the amide compound include N, N-dimethylformamide, N, N-dimethylaminoformamide, N, N-dimethylacetamide , N, N-diethylacetamide, N, N-dipropylacetamide, N, N-dimethylbenzoic acid amide and the like.
  • lactam compound examples include hydrprolactam, N-methylol lactam, N-ethylcaprolactam, N-isopropylcap latatum, N-soptylcaprolactam, N-n-propyl lactam, N-alkyl prolactams such as normal butylcaprolactam and N-cyclohexylcaprolactam, N-methyl-1-pyrrolidone (NMP), N-ethyl-12-pyrrolidone, N-isopropyl-12-pyrrolidone Ridone, N-isobutyl-2-pyrrolidone, N-norma Norepropynole 2-N-pyrrolin, N-Noremalbutyl-2-pyrrolidone, N-cyclohexyl 2-pyrrolidone, N-methyl-3-methyl 2-pyrrolidone, N-ethyl 3- Methyl-2-pyrrolidone, N-methyl-34,5—tri
  • urea compound examples include tetramethylurea, N, N'-dimethylethyleneurea, N, N'-dimethylpropyleneurea and the like.
  • organic compound examples include dimethyl sulfoxide, ethynolenolesoxide, diphenylsnolephone, 1-methinole-one-oxo-snoleforane, 1-ethinole-one-oxo-snole-holan, and one-feno-nore-one. 1 oxosulfolane and the like.
  • Examples of the cyclic organic phosphorus compound include 1-methyl-11-oxophosphorane, 1-n-propyl-11-oxophosphorane, and 1-phenyl-1-oxophosphorane.
  • Each of these various non-protonic polar organic compounds can be used alone or in combination of two or more, and further mixed with other solvent components which do not interfere with the object of the present invention. They can be mixed and used as the non-protonic organic solvent.
  • N-alkylcaprolactam and N-alkylpyrrolidone preferred are N-alkylcaprolactam and N-alkylpyrrolidone, and particularly preferred is N-methyl_2-pyrrolidone.
  • the first component is lithium hydrosulfide
  • the second component is elementary sulfur, elemental phosphorus, elemental silicon, elemental boron, elemental germanium.
  • One or more compounds selected from the group consisting of luma, phosphorus sulfide, silicon sulfide, boron sulfide, and germanium sulfide are an organic solvent, preferably the above-mentioned non-protonic organic solvent, more preferably Is to react in N-methyl-2-pyrrolidone.
  • a lithium compound exhibiting basicity can be further present as a third component.
  • the lithium compound is not particularly limited, but preferably does not produce water as a by-product during the reaction.
  • Particularly preferred compounds include n-butyllithium, sec-butynolelithium, tert-putinolelithium, hexyllithium, and lithium alkoxide. Each of these compounds can be used alone or in combination of two or more.
  • one or more selected from the group consisting of lithium phosphate, lithium borate, lithium silicate and lithium sulfate are further used. Can be present. By the presence of these compounds, the crystallization can be further facilitated.
  • a polymer component can be further present at the time of the reaction in the methods of the first and second inventions.
  • the processability of the obtained lithium ion conductive solid electrolyte can be improved. If the processability can be improved, it becomes easier to form the solid electrolyte into a thin sheet. As a result, the electrode spacing of the applied battery can be reduced, so that a lithium-ion secondary battery with further increased energy density can be configured.
  • thermoplastic resin Either a thermoplastic resin or a thermosetting resin can be used as the polymer component.
  • Preferred polymer components are, for example, polyethylene, polypropylene Len, polytetrafluoroethylene (PTFE), polyvinylidene polyfluoride (PVDF).
  • Tetrafluoroethylene-hexafluoroethylene copolymer Tetrafluoroethylene-hexafluoroethylene copolymer, tetrafluoroethylene-hexafluoropropylene copolymer (FEP) , Tetrafluoroethylene-perfluoroalkylbutylether copolymer (PFA), vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride monochloro trifluoroethylene copolymer, ethylene-tetra Fluoroethylene copolymer (ETFE resin), Polyethylene trifluoroethylene (PCTFE), Vinylidene fluoride-pentafluoropropylene copolymer, Pyrene-tetrafluoronoreloethylene copolymer, Ethylene-chloro trif Fluoroethylene copolymer (ECTFE), vinylidene fluoride-hexafluoropropyl N-tetrafluoro
  • reaction raw materials can be appropriately adjusted and supplied according to the composition of the desired type of solid electrolyte.
  • the general formula L i 2 S- P 2 S 5 , L i 2 S- S i S 2, L i 2 S- B 2 S 3, L i 2 S - Ge S 2 ho represented ones are in Kaka L i 2 S- P 2 S 5 - S i S 2, L i 2 S- P 2 S 5 - , and the like as represented by G e S 2 and the like.
  • lithium sulfide / 5 phosphorus pentasulfide (molar ratio) is preferably 0.2 to 10 and more preferably 0.2 to 10.
  • the reaction is carried out in an organic solvent, but the reaction can be advanced by applying a conventional method.
  • a lithium component, a sulfur component, and one or more components selected from the group consisting of phosphorus, silicon, boron, and germanium are described.
  • the reaction can be carried out at a temperature of 50 ° C. to 300 ° C., preferably 80 ° C. to 250 ° C., more preferably 100 ° C. to 200 ° C., with stirring. it can. If the temperature is lower than 80 ° C, the reaction rate becomes extremely slow, so that the time required for the synthesis becomes longer and the process becomes uneconomical. On the other hand, when the temperature exceeds 300 ° C., the boiling point of the solvent may be exceeded.
  • the reaction pressure may be normal pressure or pressurization.
  • the reaction time may be generally 0.1 to 10 hours, preferably 1 to 5 hours.
  • a precipitant is added to the reaction product, and the reaction solvent is distilled off to precipitate a solid.After washing and drying, a solid electrolyte having a uniform particle size can be obtained. A powder can be obtained.
  • the solid electrolyte of the present invention thus obtained has a high ionic conductivity of 1 to 1 O-ss Z cm at room temperature, a low ionic conductivity, and an oxidative decomposition voltage of 3 V or more. It exhibits excellent electrochemical properties of preferably 5 V or more '. Further, by changing the composition of the raw materials, lithium ion conductive solid electrolytes having various compositions as described above can be obtained. When the solid electrolyte obtained by the method of the present invention is incorporated in an all-solid-state lithium secondary battery, there is no particular limitation, and the solid electrolyte can be applied to known embodiments.
  • sealing plate for example, sealing plate, insulating packing, electrode plate, positive electrode plate,
  • the solid electrolyte can be formed into a sheet and used in a battery case.
  • any of coin type, button type, sheet type, stacked type, cylindrical type, flat type, square type, large type used for electric vehicles, and the like can be applied.
  • the solid electrolyte obtained according to the method of the present invention can be used for all types of portable information terminals, portable electronic devices, small household electric power storage devices, motorcycles using a motor as a power source, electric vehicles, hybrid electric vehicles, and the like. It can be suitably used for a solid-type lithium ion secondary battery, but is not particularly limited to these uses.
  • the obtained solid was subjected to thermal analysis, X-ray diffraction, and ionic conductivity measurement.
  • thermal analysis a crystallization peak was observed at 210 ° C.
  • X-ray diffraction showed no peak of lithium sulfide, and it was confirmed that lithium sulfide had completely disappeared by the reaction.
  • the ionic conductivity at room temperature was measured. As a result, it was 4 ⁇ 10 4 S / cm after heat treatment at 8 ⁇ 10—s sZcrn 230 ° C. before heat treatment. From this, it was found that the obtained solid can be effectively used as a lithium ion conductive solid electrolyte.
  • N-methyl-2-pyrrolidone solution in which 3.942 g of lithium hydrosulfide was dissolved 2.10 g, diline pentasulfide 5.47 g was added and mixed well with stirring.
  • the reaction was heated to a liquid temperature of 150 ° C. and reacted at 150 ° C. for 3 hours. The reaction became a green homogeneous solution.
  • 1.6 mol / 1 of n-butyllithium hexane solution (63 ml) was added, and the temperature was raised to 150 ° C again.
  • An all-solid-state lithium secondary battery was manufactured using the pellet-shaped solid electrolyte obtained in Example 1. Lithium cobaltate was used for the positive electrode, and indium metal was used for the negative electrode. When a constant current charge / discharge measurement was performed at a current density of 50 AZ cm 2 , charge / discharge was possible. In addition, the charge / discharge efficiency was 100%, indicating that excellent cycle characteristics were exhibited. Industrial potential
  • lithium ion conductivity can be efficiently achieved at a relatively low temperature of 300 ° C or lower using equipment such as a reaction tank commonly used in ordinary chemical plants without using special equipment.
  • the solid electrolyte can be mass-produced.
  • the resulting solid electrolyte the particle size of the composition is homogeneous powder becomes a uniform excellent solid electrolyte material, the ionic conductivity at room temperature 1 0 5 to 1 0 over 3 S / cm, oxidative decomposition voltage Is 3 V or more, preferably 5 V or more. Therefore, the solid electrolyte obtained by the method of the present invention can be suitably used as a high-performance solid electrolyte for various products such as an all-solid lithium secondary battery.

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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Conductive Materials (AREA)

Abstract

Selon la présente invention, un procédé de production d'un électrolyte solide conducteur d'ion lithium est caractérisé en ce qu'il consiste à faire réagir un composé de lithium, un composé de soufre et au moins un composé sélectionné parmi le groupe comprenant le phosphore, le silicium, le bore et le germanium dans un solvant organique, de préférence, un solvant organique aprotique, idéalement, N-méthyl-2-pyrroridone. Ladite invention concerne également une pile secondaire de type entièrement solide à l'aide d'un électrolyte solide susmentionné. Ledit procédé permet de produire, facilement et en masse, un électrolyte solide conducteur d'ion lithium sans l'utilisation d'un appareil spécial, à une température relativement basse. Ce procédé est donc avantageux commercialement.
PCT/JP2004/005248 2003-04-15 2004-04-13 Procede de production d'un electrolyte solide conducteur de ion lithium et pile secondaire de type entierement solide au moyen dudit electrolyte Ceased WO2004093099A1 (fr)

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Cited By (21)

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JP2008103285A (ja) * 2006-10-20 2008-05-01 Idemitsu Kosan Co Ltd 全固体バイポーラ電池
WO2009047977A1 (fr) 2007-10-11 2009-04-16 Idemitsu Kosan Co., Ltd. Procédé de production d'un électrolyte solide conducteur lithium-ion
WO2010116732A1 (fr) * 2009-04-10 2010-10-14 出光興産株式会社 Verre comprenant des particules d'électrolyte solide et batterie au lithium
JP2010241643A (ja) * 2009-04-07 2010-10-28 Toyota Motor Corp リチウムイオン伝導性硫化物系結晶化ガラスの製造方法、及びリチウムイオン伝導性硫化物系結晶化ガラス成形体の製造方法
JP2012041207A (ja) * 2010-08-13 2012-03-01 Idemitsu Kosan Co Ltd 固体電解質ガラス及びその製造方法
JP2012212652A (ja) * 2011-03-18 2012-11-01 Toyota Motor Corp スラリー、固体電解質層の製造方法、電極活物質層の製造方法、および全固体電池の製造方法
WO2012176266A1 (fr) * 2011-06-20 2012-12-27 トヨタ自動車株式会社 Procédé de production de microparticules pour électrolyte solide
WO2013069243A1 (fr) 2011-11-07 2013-05-16 出光興産株式会社 Electrolyte solide
WO2014002483A1 (fr) 2012-06-29 2014-01-03 出光興産株式会社 Mélange pour électrode positive
US20140084224A1 (en) * 2011-05-27 2014-03-27 Chemetall Gmbh Process for preparing lithium sulfide
WO2014073197A1 (fr) 2012-11-06 2014-05-15 出光興産株式会社 Electrolyte solide
JP2014179265A (ja) * 2013-03-15 2014-09-25 Toyota Motor Corp 硫化物固体電解質材料の製造方法
JP2014220051A (ja) * 2013-05-02 2014-11-20 出光興産株式会社 硫化物固体電解質の製造方法
WO2014192309A1 (fr) 2013-05-31 2014-12-04 出光興産株式会社 Procédé de production d'électrolyte solide
KR20150039573A (ko) 2013-10-02 2015-04-10 삼성전자주식회사 황화물 고체 전해질과 이의 제조 방법, 및 이를 포함하는 고체 전지
JP2015232965A (ja) * 2014-06-10 2015-12-24 三星電子株式会社Ｓａｍｓｕｎｇ Ｅｌｅｃｔｒｏｎｉｃｓ Ｃｏ．，Ｌｔｄ． 硫化物固体電解質、および硫化物固体電解質の製造方法
JP2016006798A (ja) * 2015-10-07 2016-01-14 出光興産株式会社 リチウムイオン二次電池用硫化物系固体電解質
US9793574B2 (en) 2013-04-24 2017-10-17 Idemitsu Kosan Co., Ltd. Method for producing solid electrolyte
US10020535B2 (en) 2015-12-01 2018-07-10 Idemitsu Kosan Co., Ltd. Method for producing sulfide solid electrolyte
US20220123359A1 (en) * 2019-01-25 2022-04-21 Solid Power, Inc. Solid electrolyte material synthesis method
KR20220089899A (ko) 2020-12-22 2022-06-29 울산대학교 산학협력단 고체 전해질의 제조방법 및 이로부터 제조된 고체 전해질

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Cited By (37)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008103285A (ja) * 2006-10-20 2008-05-01 Idemitsu Kosan Co Ltd 全固体バイポーラ電池
JP2013232418A (ja) * 2007-10-11 2013-11-14 Idemitsu Kosan Co Ltd リチウムイオン伝導性固体電解質の製造方法
WO2009047977A1 (fr) 2007-10-11 2009-04-16 Idemitsu Kosan Co., Ltd. Procédé de production d'un électrolyte solide conducteur lithium-ion
US8518585B2 (en) 2007-10-11 2013-08-27 Idemitsu Kosan Co., Ltd. Method for producing lithium ion conductive solid electrolyte
JP5270563B2 (ja) * 2007-10-11 2013-08-21 出光興産株式会社 リチウムイオン伝導性固体電解質の製造方法
JP2010241643A (ja) * 2009-04-07 2010-10-28 Toyota Motor Corp リチウムイオン伝導性硫化物系結晶化ガラスの製造方法、及びリチウムイオン伝導性硫化物系結晶化ガラス成形体の製造方法
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