Method of producing lithium ion conductive sulfides comprising simple substances

Patent metadata

Field	Value
Publication number	US-10074871-B2
Application number	US-201615288494-A
Country	US
Kind code	B2
Filing date	Oct 7, 2016
Priority date	Apr 27, 2016
Publication date	Sep 11, 2018
Grant date	Sep 11, 2018

Abstract

A method for preparing a lithium ion conductive sulfide, which is capable of independently controlling the elemental ratio of lithium (Li), phosphorus (P), sulfur (S), etc, is provided. The method for preparing a lithium ion conductive sulfide can provide a lithium ion conductive sulfide having a crystal structure and an anion cluster distribution distinguished from those of existing ones.

First claim

What is claimed is:

1. A method for preparing a lithium ion conductive sulfide comprising lithium (Li), phosphorus (P) and sulfur (S), which comprises:
(1) preparing a mixture comprising lithium sulfide (Li 2 S) and phosphorus pentasulfide (P 2 S 5 );
(2) vitrifying the mixture by pulverizing the mixture; and
(3) crystallizing the vitrified mixture by heat-treating the vitrified mixture,
wherein the composition ratio of lithium, phosphorus and sulfur in the lithium ion conductive sulfide is controlled independently by performing the vitrification and the crystallization after mixing one or more of elemental phosphorus and elemental sulfur to the mixture in (1),
wherein, in (1), the molar ratio of the lithium sulfide, the phosphorus pentasulfide, the elemental phosphorus and the elemental sulfur is 9:2:2:3.

2. The method for preparing a lithium ion conductive sulfide according to claim 1 , wherein (3) is performed at 200° C.-1200° C. for 0.1 hours-100 hours.

3. The method for preparing a lithium ion conductive sulfide according to claim 1 , wherein the lithium ion conductive sulfide exhibits a first peak at 390±5 cm −1 and a second peak at 425±5 cm −1 in a Raman spectrum and the intensity of the second peak is larger than the intensity of the first peak.

4. The method for preparing a lithium ion conductive sulfide according to claim 1 , wherein the lithium ion conductive sulfide has an anion cluster distribution of P 2 S 6 2− and PS 4 3− .

5. The method for preparing a lithium ion conductive sulfide comprising lithium (Li), phosphorus (P) and sulfur (S), which comprises:
(1) preparing a mixture comprising lithium sulfide (Li 2 S) and phosphorus pentasulfide (P 2 S 5 );
(2) vitrifying the mixture by pulverizing the mixture; and
(3) crystallizing the vitrified mixture by heat-treating the vitrified mixture,
wherein the composition ratio of lithium, phosphorus and sulfur in the lithium ion conductive sulfide is controlled independently by performing the vitrification and the crystallization after mixing one or more of elemental phosphorus and elemental sulfur to the mixture in (1), wherein, in (1), the molar ratio of the lithium sulfide, the phosphorus pentasulfide, the elemental phosphorus and the elemental sulfur is 15:5:2:4.

6. The method for preparing a lithium ion conductive sulfide according to claim 5 , wherein the lithium ion conductive sulfide exhibits peaks at 390±5 cm −1 , 410±5 cm −1 and 425±5 cm −1 in a Raman spectrum.

7. The method for preparing a lithium ion conductive sulfide according to claim 5 , wherein the lithium ion conductive sulfide has an anion duster distribution of P 2 S 6 2− , P 2 S 7 4− and PS 4 3− .

Assignees

• Korea Inst Sci & Tech

Inventors

• Kim Hyoung Chul
• Jung Hun Gi
• Lee Jong Ho
• Lee Hae Weon
• Kim Byung Kook
• Son Ji Won
• Jung Wo Dum

Classifications

• H01M10/0562 Primary

  Solid materials · CPC title

• C01B17/22

  Alkali metal sulfides or polysulfides · CPC title

• H01M2300/0068

  inorganic · CPC title

• H01B1/10

  sulfides · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title