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Solid electrolyte

A technology of solid electrolyte and electrolyte layer, applied in electrolytes, non-aqueous electrolyte batteries, circuits, etc., can solve problems such as reduced ionic conductivity

Inactive Publication Date: 2014-07-30
IDEMITSU KOSAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the technology of Patent Document 2, although the hydrolyzability is lowered, the ionic conductivity is greatly lowered

Method used

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Examples

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Effect test

manufacture example 1

[0230] Production example 1 [lithium sulfide (Li 2 S) Manufacture, purification]

[0231] Lithium sulfide was produced and purified in the same manner as the method described in the Examples of International Publication No. 2005 / 040039 pamphlet.

[0232] Specifically, it performed as follows.

[0233] (1) Lithium sulfide (Li 2 S) Manufacture

[0234] Lithium sulfide is produced according to the method of the first embodiment (two-step method) of JP-A-7-330312. Specifically, 3326.4 g (33.6 moles) of N-methyl-2-pyrrolidone (NMP) and 287.4 g (12 moles) of lithium hydroxide were added to a 10-liter autoclave with a stirring paddle, and the temperature was raised to 130 ° C at 300 rpm . After the temperature was raised, hydrogen sulfide was blown into the liquid at a supply rate of 3 liters / minute for 2 hours.

[0235] Next, the temperature of the reaction solution was raised under nitrogen flow (200 cc / min), and a part of the reacted hydrogen sulfide was dehydrogenated. As ...

manufacture example 2

[0239] Production Example 2 [Sulfide-based solid electrolyte glass (Li 2 S / P 2 S 5 (Molar ratio) = 75 / 25) Manufacture - Mechanical ball milling method -]

[0240] Using the lithium sulfide produced in Production Example 1, a sulfide-based glass was produced by the method in accordance with Example 1 of WO 07 / 066539 pamphlet.

[0241] Specifically, it was performed as follows.

[0242] 0.383 g (0.00833 mol) of lithium sulfide produced in Production Example 1 and 0.618 g (0.00278 mol) of phosphorus pentasulfide (manufactured by Aldrich) were thoroughly mixed. Then, put this mixed powder together with 10 zirconia balls with a diameter of 10 mm into a planetary ball mill (manufactured by Fritsch Japan Co., Ltd.: model P-7) into an alumina tank and completely seal it. The alumina tank was filled with nitrogen to form a nitrogen atmosphere.

[0243] Then, the planetary ball mill was rotated at a low speed (85 rpm) for the first few minutes to thoroughly mix lithium sulfide and ...

manufacture example 3

[0248] Production Example 3 [Sulfide-based solid electrolyte glass (Li 2 S / P 2 S 5 (Molar ratio) = 75 / 25) production - slurry method -]

[0249] Using the lithium sulfide produced in Production Example 1, a sulfide-based glass was produced by the same method as in Example 1 of JP-A-2010-140893.

[0250] Specifically, it performed as follows.

[0251] use figure 1 The shown apparatus 1 produces sulfide-based glass ceramics. As the mixer 10, Star mill mini Tse A (0.15 L) (bead mill) manufactured by Ashizawa Finetech Ltd. was used, and 450 g of 0.5 mmφ zirconia balls were charged. As the reaction tank 20, a 1.5 L glass reactor equipped with a stirrer was used.

[0252] A mixture obtained by adding 1080 g of dehydrated toluene (moisture content 8 ppm) produced by Hiroshima Wako Pure Chemical Industries, Ltd. to 45.90 g (75 mol%) of lithium sulfide produced in Production Example 1 and 74.10 g (25 mol %) of phosphorus pentasulfide produced by Aldrich Co., Ltd. In the reaction t...

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Abstract

This solid electrolyte contains lithium, phosphorus, and sulfur as constituent components, has a peak (first peak) in the region of 81.0-88.0 ppm inclusive in a 31P-NMR spectrum, either does not have a peak in the regions other than the 81.0-88.0 ppm inclusive region or even if there is a peak the peak strength ratio with respect to the first peak is no greater than 0.5, and has an ion conductivity of at least 510-4 S / cm.

Description

technical field [0001] The present invention relates to solid electrolytes, and electrolyte layers, electrodes and batteries produced using them. Background technique [0002] In the field of all-solid-state batteries, sulfide-based solid electrolyte materials are conventionally known. For example, it is reported in Patent Document 1 that Li 2 S and P 2 S 5 Mixing at a specific molar ratio (68:32~73:27), and performing mechanical ball milling and heat treatment, so as to obtain high ionic conductivity (~2×10 -3 S / cm) glass ceramic electrolyte particles. [0003] However, the material of Patent Document 1 easily generates hydrogen sulfide (hydrolysis) when in contact with water, and its use in a high dew point environment is limited. [0004] Known to be Li 2 S and P 2 S 5 Glass electrolyte particles mixed at a molar ratio of 75:25 and subjected to mechanical ball milling are difficult to be hydrolyzed (for example, Patent Document 2). However, in the technique of Pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01B1/06H01M4/62
CPCH01B1/06H01M10/052H01M10/0525H01M10/0562H01M2300/002Y02E60/10
Inventor 樋口弘幸
Owner IDEMITSU KOSAN CO LTD
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