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Sulfide-Based Solid Electrolyte for Lithium Ion Batteries

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Sulfide-Based Solid Electrolyte for Lithium Ion Batteries (19) TZZ¥___T (11) EP 3 171 444 A1 (12) EUROPEAN PATENT APPLICATION published in accordance with Art. 153(4) EPC (43) Date of publication: (51) Int Cl.: 24.05.2017 Bulletin 2017/21 H01M 10/0562 (2010.01) H01B 1/06 (2006.01) H01B 1/10 (2006.01) H01M 10/0525 (2010.01) (21) Application number: 15822447.7 (86) International application number: (22) Date of filing: 15.06.2015 PCT/JP2015/067151 (87) International publication number: WO 2016/009768 (21.01.2016 Gazette 2016/03) (84) Designated Contracting States: (72) Inventors: AL AT BE BG CH CY CZ DE DK EE ES FI FR GB • MIYASHITA, Norihiko GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO Ageo-shi PL PT RO RS SE SI SK SM TR Saitama 362-0021 (JP) Designated Extension States: • CHIKUMOTO, Takashi BA ME Ageo-shi Designated Validation States: Saitama 362-0021 (JP) MA • MATSUSHIMA, Hideaki Ageo-shi (30) Priority: 16.07.2014 JP 2014146174 Saitama 362-0021 (JP) • MATSUZAKI, Kenji (71) Applicant: Mitsui Mining and Smelting Co., Ltd. Ageo-shi Shinagawa-ku Saitama 362-0021 (JP) Tokyo 141-8584 (JP) (74) Representative: Gille Hrabal Brucknerstrasse 20 40593 Düsseldorf (DE) (54) SULFIDE-BASED SOLID ELECTROLYTE FOR LITHIUM ION BATTERIES (57) Proposed is a new sulfide-based solid electro- solidelectrolyte for lithiumion batteries,the sulfide-based lyte for lithium ion batteries, the sulfide-based solid elec- solid electrolyte containing a compound that has a cubic trolyte relating to a compound that has a cubic argyrodite argyrodite type crystal structure and is represented by type crystal structure and is represented compositionalby formula (1): Li7-x-2yPS6-x-yClx, in which Li7-x-2yPS6-x-yClx, and having excellent water resistance compositional formula, conditions: 0.8 ≤ x ≤ 1.7 and 0 < and oxidation resistance. Proposed is a sulfide-based y ≤ - 0.25x + 0.5 are satisfied. EP 3 171 444 A1 Printed by Jouve, 75001 PARIS (FR) EP 3 171 444 A1 Description TECHNICAL FIELD 5 [0001] The present invention relates to a sulfide-based solid electrolyte for lithium ion batteries, which can be suitably used as a solid electrolyte for lithium ion batteries. BACKGROUND ART 10 [0002] Lithium ion batteries are secondary batteries having a structure in which, during charging, lithium dissolves out as ions from a positive electrode and migrates to the negative electrode to be stored therein; and on the contrary, during discharging, lithium ions return from the negative electrode to the positive electrode. Since lithium ion batteries have features such as high energy density and a long life cycle, lithium ion batteries are widely used as power supplies for domestic appliances such as video cameras; portable electronic devices such as laptop computers and mobile tele- 15 phones; and electric tools such as power tools. Recently, lithium ion batteries are also applied to large-sized batteries that are mounted in electric vehicles (EV), hybrid electric vehicles, and the like. [0003] A lithium ion battery of this kind is configured to include a positive electrode, a negative electrode, and an ion conducting layer interposed between these two electrodes, and as this ion conducting layer, a separator formed from a porous film of polyethylene, polypropylene or the like, which is filled with a non-aqueous liquid electrolyte, is generally 20 used. However, since such an organic liquid electrolyte which uses a flammable organic solvent as the solvent is used as an electrolyte, improvements in view of structure and material for preventing volatilization or leakage are needed, and installation of a safety device for suppressing temperature increase at the time of a short circuit and improvements in view of structure and material for preventing a short circuit are also needed. [0004] In contrast, an all-solid lithium ion battery formed by solidifying the whole battery using a solid electrolyte that 25 uses lithium sulfide (Li2S) or the like as a starting material, does not use a flammable organic solvent. Therefore, simplification of safety devices can be attempted, and the battery can be made as a battery which is excellent in terms of production cost or productivity. Also, the battery has a feature that the solid electrolyte can be laminated in series in a cell, and thus voltage increase can be promoted. Furthermore, in a solid electrolyte of this kind, since nothing but Li ion moves, side reactions caused by movement of anions do not occur, and it is expected that this leads to enhancement 30 of safety and durability. [0005] A solid electrolyte used in such a battery is required to have high ionic conductivity as far as possible and to be stable chemically and electrochemically. For example, lithium halide, lithium nitride, lithium oxoate, and derivatives of these compounds are known as candidate materials for the solid electrolyte. [0006] In regard to solid electrolytes of this kind, for example, Patent Document 1 discloses a sulfide-based solid 35 electrolyte obtainable by incorporating a high temperature lithium ion conductive compound formed from lithium phos- phate (Li3PO4), into a lithium ion conductive sulfide glass represented by general formula:2 S-XLi (provided that X represents at least one sulfide among SiS 2, GeS2, and B2S3). [0007] Furthermore, Patent Document 2 discloses, as a material that is crystalline and exhibits a very high ionic conductivity such as an ionic conductivity at room temperature of 6.49310-5 Scm-1, a sulfide-based solid electrolyte 40 characterized by including a lithium ion conductive substance as a composite compound represented by general formula: Li2S-GeS2-X (provided that X represents at least one of Ga2S3 and ZnS). [0008] Patent Document 3 discloses a lithium ion conductive sulfide ceramic having high lithium ion conductivity and ahigh decomposition voltage, the sulfideceramic containing Li 2Sand P 2S5as main components andhaving a composition in which Li2S = 82.5 to 92.5 and P 2S5 = 7.5 to 17.5, as expressed in mol%, and preferably a composition (compositional 45 formula: Li7PS6) in which Li2S/P2S5 = 7 as a molar ratio. [0009] Patent Document 4 discloses a lithium ion conductive material having a silver germanium sulfide mineral type + n+ 2- - n+ crystal structure represented by chemical formula: Li (12-n-x)B X (6-x)Y x (wherein B represents at least one selected from P, As, Ge, Ga, Sb, Si, Sn, Al, In, Ti, V, Nb, and Ta; X2- represents at least one selected from S, Se, and Te; and - Y represents at least one selected from F, Cl, Br, I, CN, OCN, SCN, and N 3; while 0 ≤ x ≤ 2). 50 [0010] Patent Document 5 discloses, as a solid compound that can be produced into a single layer in addition to the + n+ 2- high fluidity of lithium ions, a lithium silver germanium sulfide mineral represented by general formula (I): Li (12-n-x)B X - n+ 6-xY x, and in this formula, B is selected from the group consisting of P, As, Ge, Ga, Sb, Si, Sn, Al, In, Ti, V, Nb and Ta; X2- is selected from the group consisting of S, Se and Te; and Y- is selected from the group consisting of Cl, Br, I, F, CN, OCN, SCN, and N3, while 0 ≤ x ≤ 2. 55 2 EP 3 171 444 A1 CITATION LIST PATENT DOCUMENT 5 [0011] Patent Document 1: JP 3184517 B2 Patent Document 2: JP 3744665 B2 Patent Document 3: JP 2001-250580 A 10 Patent Document 4: JP 2011-96630 A Patent Document 5: JP 2010-540396 A SUMMARY OF THE INVENTION 15 PROBLEM TO BE SOLVED BY THE INVENTION [0012] The inventors of the present invention paid attention to a compound represented by Li7-xPS6-xClx and having a cubic argyrodite type crystal structure, as a solid electrolyte material used for lithium ion batteries. [0013] However, since such a compound has very high reactivity with moisture or oxygen, when an all-solid lithium 20 ion battery is assembled using the compound as a solid electrolyte for lithium ion batteries, the operation of assembling the all-solid lithium ion battery needs to be carried out in an environment such as a glove box where an inert gas having an ultralow dew point is supplied. Thus, the compound has a problem to be industrially utilized. [0014] Thus,the presentinvention relates to a sulfide-based solidelectrolyte for lithium ion batteries,the solidelectrolyte containing a compound which has a cubic argyrodite type crystal structure and is represented by formula: Li 7-xPS6-xClx, 25 and the invention is to propose a new sulfide-based solid electrolyte for lithium ion batteries, the sulfide-based solid electrolyte having improved water resistance and oxidation resistance so that, for example, the operation of assembling an all-solid lithium ion battery can be carried out even in an environment where an inert gas having an ultralow dew point is not supplied, such as a dry room. 30 MEANS FOR SOLVING PROBLEM [0015] The present invention proposes a sulfide-based solid electrolyte for lithium ion batteries, the sulfide-based solid electrolyte containing a compound that has a cubic argyrodite type crystal structure and is represented by compositional formula (1): Li7-x-2yPS6-x-yClx, in which compositional formula, the conditions: 0.8 ≤ x ≤ 1.7 and 0 < y ≤ -0.25x + 0.5 are 35 satisfied. EFFECT OF THE INVENTION [0016] The sulfide-based solid electrolyte proposed by the present invention has markedly excellent water resistance 40 and oxidation resistance compared to a sulfide-based solid electrolyte containing a compound represented by formula: Li7-xPS6-xClx, and since deterioration of characteristics occurs at a reduced level even if the sulfide-based solid electrolyte is handled in dry air, for example, the operation of assembling an all-solid lithium ion battery can be carried out even in an environment where an inert gas having an ultralow dew point is not supplied, such as a dry room.
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