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Method for producing ion-conductive substance, ion-conductive substance, crystallized ion-conductive substance, and cell

A technology of ion conductivity and manufacturing method, which is applied in the field of manufacture of ion conductive materials, ion conductive materials, crystalline ion conductive materials and batteries, can solve the problems of reduced operating efficiency and low yield, and achieve high operating efficiency , High yield effect

Inactive Publication Date: 2015-03-11
IDEMITSU KOSAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the sulfide-based solid electrolyte described in Patent Document 1 is produced by a ball mill, and therefore, the balls and the electrolyte in the mill container are attached during production, so there is a disadvantage in that the work efficiency is reduced and the yield is low.

Method used

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  • Method for producing ion-conductive substance, ion-conductive substance, crystallized ion-conductive substance, and cell
  • Method for producing ion-conductive substance, ion-conductive substance, crystallized ion-conductive substance, and cell
  • Method for producing ion-conductive substance, ion-conductive substance, crystallized ion-conductive substance, and cell

Examples

Experimental program
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Effect test

manufacture example 1

[0177] [lithium sulfide (Li 2 S) Manufacture]

[0178] Under nitrogen flow, 270 g of toluene as a non-polar solvent was added to a 600 ml detachable flask, 30 g of lithium hydroxide (Honjo Chemical Co., Ltd.) was added, and it was kept at 95° C. while stirring at 300 rpm using a FULLZONE stirring blade. While blowing hydrogen sulfide into the slurry at a supply rate of 300 ml / min, the temperature was raised to 104°C. The azeotropic gas of water and toluene was continuously discharged from the separable flask. Dehydration is performed by condensing the azeotropic gas with a condenser outside the system. During this period, the same amount of toluene as distilled was continuously supplied to keep the level of the reaction liquid constant.

[0179] The water content in the condensate gradually decreased, and 6 hours after the introduction of hydrogen sulfide, no distillation of water was recognized (the water content was 22 ml in total). During the reaction, solids were dispe...

manufacture example 2

[0183] [micronization processing]

[0184] 26 g of lithium sulfide obtained in Production Example 1 was weighed into a Schlenk bottle in a glove box. 500 ml of dehydrated toluene (Wako Pure Chemical Industries, Ltd.) and 250 ml of dehydrated ethanol (Wako Pure Chemical Industries, Ltd.) were sequentially added thereto under a nitrogen atmosphere, and stirred with a stirrer at room temperature for 24 hours. After the reforming treatment, the bath temperature was raised to 120° C., and hydrogen sulfide gas was circulated at 200 ml / min for 90 minutes for treatment. After hydrogen sulfide gas treatment, the solvent was distilled off under nitrogen flow at room temperature, and then dried under vacuum at room temperature for 2 hours to recover micronized lithium sulfide.

[0185] Micronized lithium sulfide was evaluated in the same manner as in Production Example 1. The purity of lithium sulfide is 97.2%, the amount of lithium hydroxide is 0.3%, the average particle size is 9.1μm...

Embodiment 1

[0188] Lithium sulfide (LiS 2 ), so that the average particle size is 0.3 μm. The lithium sulfide 1.0g (64 mol%), phosphorus pentasulfide (P 2 S 5 ) (Aldrich Corporation) 1.61g (21 mol%) and lithium bromide (LiBr) (Aldrich Corporation) 0.42g (15mol%) were added to a flask with a stirrer replaced with nitrogen, and 50ml of di Toluene (Wako Pure Chemical Industries, Ltd.) was brought into contact at 140° C. for 24 hours.

[0189] The solid content was separated by filtration, and vacuum-dried at 120° C. for 40 minutes to obtain an ion conductive material (solid electrolyte). The recovery rate of the solid electrolyte was 95%. No deposits were found on the used flask or stirrer.

[0190] The ionic conductivity of the solid electrolyte is 4.6×10 -4 S / cm.

[0191] In addition, the particle diameter of lithium sulfide was measured using the laser diffraction and scattering type particle size distribution measuring instrument LMS-30 (Seishin Co., Ltd.).

[0192] In addition, ...

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Abstract

Provided is a method for producing an ion-conductive substance from starting materials of: one or more types of compound selected from phosphorus sulfide, germanium sulfide, silicon sulfide, and boron sulfide; a sulfide of a metal element belonging to Group I or Group II of the periodic table; and a halogen compound represented by MwXx, and including a step for contact thereof within a solvent. (In the formula, M is Li, B, Na, K, Rb, Cs, Ca, Mg, Sr, Ba, Al, Si, P, S, Ge, As, Se, Sn, Sb, Te, Pb or Bi; w is 1 or 2; X is F, Cl, Br, or I; and x is any integer selected from 1 to 10 inclusive);.

Description

technical field [0001] The present invention relates to a method for producing an ion conductive material, an ion conductive material, a crystalline ion conductive material, and a battery. Background technique [0002] In recent years, the demand for high-performance lithium secondary batteries used in personal digital assistants, portable electronic devices, small household power storage devices, motorcycles powered by electric motors, electric vehicles, hybrid electric vehicles, etc. has increased. Here, the secondary battery refers to a battery that can be charged and discharged. As the usage of the secondary battery expands, the safety and performance of the secondary battery are required to be further improved. [0003] Conventionally, electrolytes exhibiting high lithium ion conductivity at room temperature were mostly limited to organic electrolytes. However, conventional organic electrolytes are flammable because they contain organic solvents. Therefore, when an i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01B13/00H01B1/06H01M10/0562
CPCH01M10/0562H01M2300/0074H01M10/054H01B1/06H01M10/3918H01M2300/0068Y02E60/10H01M2300/008
Inventor 菅原孝宜顺毛直宪油谷亮
Owner IDEMITSU KOSAN CO LTD
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