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Solid Electrolyte Production Method (19) TZZ¥¥_ _T (11) EP 3 312 846 A1 (12) EUROPEAN PATENT APPLICATION published in accordance with Art. 153(4) EPC (43) Date of publication: (51) Int Cl.: 25.04.2018 Bulletin 2018/17 H01B 13/00 (2006.01) C01B 25/14 (2006.01) H01M 6/18 (2006.01) H01M 10/0562 (2010.01) (21) Application number: 16811727.3 (86) International application number: (22) Date of filing: 16.06.2016 PCT/JP2016/068009 (87) International publication number: WO 2016/204253 (22.12.2016 Gazette 2016/51) (84) Designated Contracting States: (72) Inventors: AL AT BE BG CH CY CZ DE DK EE ES FI FR GB • SATO, Atsushi GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO Sodegaura-shi PL PT RO RS SE SI SK SM TR Chiba 2990-293 (JP) Designated Extension States: • SENGA, Minoru BA ME Sodegaura-shi Designated Validation States: Chiba 299-0293 (JP) MA MD • AIDA, Masao Sodegaura-shi (30) Priority: 17.06.2015 JP 2015122371 Chiba 299-0293 (JP) (71) Applicant: Idemitsu Kosan Co., Ltd (74) Representative: Hoffmann Eitle Tokyo 100-8321 (JP) Patent- und Rechtsanwälte PartmbB Arabellastraße 30 81925 München (DE) (54) SOLID ELECTROLYTE PRODUCTION METHOD (57) The invention provides a method for producing trolytes with excellent productivity and mass-productivity, a solid electrolyte, which includes reacting two or more as well as a method for producing a crystalline solid elec- kinds of solid raw materials using a multi-axial kneading trolyte including producing the amorphous solid electro- machine to give an amorphous solid electrolyte, and lyte followed by heating the solid electrolyte. which can provide amorphous and crystalline solid elec- EP 3 312 846 A1 Printed by Jouve, 75001 PARIS (FR) 1 EP 3 312 846 A1 2 Description Fig. 2 is a plan view cut vertically to the rotary shaft in a part provided with paddles of the rotary shaft of Technical Field the multi-axial kneading machine for use in the present invention. [0001] The present invention relates to a solid electro- 5 Fig. 3 is an X-ray analysis spectrum of an amorphous lyte production method. solid electrolyte obtained in Example 1. Fig. 4 is an X-ray analysis spectrum of an amorphous Background Art solid electrolyte obtained in Example 2. Fig. 5 is an X-ray analysis spectrum of an amorphous [0002] With rapid spread of information-related instru- 10 solid electrolyte obtained in Example 3. ments, communication instruments and others such as Fig. 6 is an X-ray analysis spectrum of an amorphous personal computers, video cameras, cell phones and the solid electrolyte obtained in Example 4. like in recent years, development of batteries that are utilized as power sources for them is considered to be Summary of Invention important. Heretofore, in batteries for such uses, an elec- 15 trolytic solution containing a flammable organic solvent Technical Problem has been used, but development of batteries having a solid electrolyte layer in place of an electrolytic solution [0006] However, the mechanical milling method or the is being made, which are solid as a whole not using a method of melting raw materials at a high temperature flammable organic solvent inside the batteries, in which, 20 described in PTL 1 requires a special equipment, and therefore, a safety unit can be simplified and which can therefore cannot be said to be suitable for productivity drive down manufacturing costs and are excellent in pro- and mass-productivity. The method using a hydrocar- ductivity. bon-based organic solvent described in PTLs 2 and 3 [0003] As a method for producing a solid electrolyte uses an organic solvent and therefore requires a step of for use in the solid electrolyte layer, there are known a 25 drying and recovering the solvent, and as the case may method of mechanically milling raw materials using a be, the process is often complicated. planetary ball mill or the like, a method of melting raw [0007] The production apparatus described in PTL 4 materials at a high temperature and the like (for example, requires a high temperature of 600°C or higher for making PTL 1). In addition, as a method excellent in industrial the compressed raw materials a molten body, for exam- 30 productivity and mass-productivity, a method of making ple, 800°C or so in the case of producing Li 3PS4 (PTL 4, raw materials kept in contact with each other in a state paragraph [0031]). Consequently, a driving part of where a hydrocarbon-based organic solvent has been screws in the production apparatus is, though made of added thereto, or mechanically milling them has been high-chromium steel, exposed to the high pressure in the proposed (for example, PTLs 2, 3). Further, PTL 4 dis- compression part and to the high temperature in the melt- closes a solid electrolyte glass production apparatus35 ing part, therefore resulting in reduction in the material equipped with a screw and having a compression part strength. In addition, the apparatus needs a special heat- forcompressing raw materialsand a melting part forheat- ing equipment and needs a large energy consumption ing the compressed raw materials to be a molten body amount, that is, the apparatus could not be said to have (for example, PTL 4). excellent productivity and mass-productivity. 40 [0008] The present invention has been made in con- Citation List sideration of the situation as above, and its object is to provide a method for producing amorphous and crystal- Patent Literature line solid electrolytes excellent in productivity and mass- productivity, as well as a multi-axial kneading machine. [0004] 45 Solution to Problem PTL 1: JP 11-134937 A PTL 2: JP 2009-110920 A [0009] Thepresent inventors haveassiduously studied PTL 3: WO 2009/047977 A1 for the purpose of solving the above-mentioned problems PTL 4: JP 2012-96973 A 50 and, as a result, have found that the problems can be solved by the following invention. Brief Description of Drawings [0010] [0005] [1] A method for producing a solid electrolyte, includ- 55 ing reacting two or more kinds of solid raw materials Fig. 1 is a plane view cut at the center of a rotary using a multi-axial kneading machine to give an shaft of a multi-axial kneading machine for use in the amorphous solid electrolyte. present invention. [2] The method for producing a solid electrolyte ac- 2 3 EP 3 312 846 A1 4 cording to the above [1], wherein the temperature at amorphous solid electrolyte containing a lithium el- the reaction is not higher than the crystallization tem- ement, a phosphorus element, a sulfur element, and perature of the amorphous solid electrolyte. at least one of a bromine element and an iodine el- [3] The method for producing a solid electrolyte ac- ement. cording to the above [1] or [2], wherein the reaction 5 [16] A method for producing a solid electrolyte in- is carried out while cooling. cluding reacting two or more kinds of solid raw ma- [4] The method for producing a solid electrolyte ac- terials containing lithium sulfide and phosphorus cording to any one of the above [1] to [3], wherein sulfide, using a multi-axial kneading machine, to give the reaction is carried out in a solid state. an amorphous solid electrolyte containing a lithium [5] The method for producing a solid electrolyte ac- 10 element, a phosphorus element and a sulfur ele- cording to any one of the above [1] to [4], wherein ment, wherein the temperature at the reaction is not the solid raw materials contain a lithium element, a higher than the crystallization temperature of the phosphorus element and a sulfur element. amorphous solid electrolyte. [6] The method for producing a solid electrolyte ac- [17] A method for producing a solid electrolyte in- cording to the above [5], wherein the solid raw ma- 15 cluding reacting two or more kinds of solid raw ma- terials contain at least one of a lithium compound terials containing lithium sulfide, phosphorus sulfide, and a lithium metal elementary substance, and at and at least one of lithium bromide and lithium iodide, least one of a phosphorus compound and a phos- using a multi-axial kneading machine, to give an phorus elementary substance. amorphous solid electrolyte containing a lithium el- [7] The method for producing a solid electrolyte ac- 20 ement, a phosphorus element, a sulfur element, and cording to the above [5] or [6], wherein the solid raw at least one of a bromine element and an iodine el- materials contain lithium sulfide and phosphorus ement, wherein the temperature at the reaction is sulfide. not higher than the crystallization temperature of the [8] The method for producing a solid electrolyte ac- amorphous solid electrolyte. cording to any one of the above [5] to [7], wherein 25 [18] A method for producing a crystalline solid elec- the solid raw materials further contain a halogen el- trolyte, including reacting two or more kinds of solid ement. raw materials containing lithium sulfide and phos- [9] The method for producing a solid electrolyte ac- phorus sulfide using a multi-axial kneading machine cording to the above [8], wherein the halogen ele- to give an amorphous solid electrolyte containing a ment is at least one of bromine and iodine. 30 lithium element, a phosphorus element and a sulfur [10] The method for producing a solid electrolyte ac- element, followed by heating the amorphous solid cording to the above [8] or [9], wherein the solid raw electrolyte. materials contain at least one of lithium bromide and [19] A method for producing a crystalline solid elec- lithium iodide.
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