Increasing ionic conductivity of liti2(ps4)3 by sintering

Patent metadata

Field	Value
Publication number	US-2019341646-A1
Application number	US-201616326480-A
Country	US
Kind code	A1
Filing date	Sep 5, 2016
Priority date	Sep 5, 2016
Publication date	Nov 7, 2019
Grant date	—

Abstract

A method of treatment of a sample of lithium titanium thiophosphate LiTi2(PS4)3 including: (a) providing a solid sample of lithium titanium thiophosphate LiTi2(PS4)3, (b) compressing the lithium titanium thiophosphate sample provided in step (a) to form a compressed powder layer; and (c) sintering the lithium titanium thiophosphate obtained as a compressed powder layer in step (b) at a temperature of at least 200° C. and at most 400° C.

First claim

1 . Method of treatment of a sample of lithium titanium thiophosphate LiTi 2 (PS 4 ) 3 comprising the steps of:
(a) providing a solid sample of lithium titanium thiophosphate LiTi 2 (PS 4 ) 3 , (b) compressing the lithium titanium thiophosphate sample provided in step (a) to form a compressed powder layer; and (c) sintering the lithium titanium thiophosphate obtained as a compressed powder layer in step (b) at a temperature of at least 200° C. and at most 400° C.

2 . Method of treatment of a sample of lithium titanium thiophosphate according to claim 1 , wherein in step (b), the sample of lithium titanium thiophosphate is compressed at a pressure range of at least 100 MPa and at most 1500 MPa.

3 . Method of treatment of a sample of lithium titanium thiophosphate according to claim 1 , wherein in step (c), the sintering time is at least 1 hour and at most 300 hours.

4 . Method of preparation of lithium titanium thiophosphate LiTi 2 (PS 4 ) 3 comprising the steps of:
(α) providing a mixture of lithium sulfide Li 2 S, phosphorus sulfide P 2 S 5 and titanium sulfide TiS 2 ; (β) subjecting the mixture prepared in step (α) to a preliminary reaction step through mechanical milling or melt-quenching to produce an intermediate amorphous sulfide mixture; (γ) subjecting the mixture prepared in step (β) to a heat treatment step at a maximum plateau temperature of at least 350° C. and less than 500° C.; wherein the material obtained through step (γ) is subsequently subjected to the method of claim 1 .

5 . Method of preparation of claim 4 , wherein the mechanical milling procedure used in step (β) to produce an intermediate amorphous sulfide mixture is planetary ball milling, vibration milling or jet milling.

6 . Method of preparation of claim 4 , wherein in heat treatment step (γ), the maximum plateau temperature is not more than 475° C.

7 . Method of treatment of a sample of lithium titanium thiophosphate according to claim 2 , wherein in step (c), the sintering time is at least 1 hour and at most 300 hours.

8 . Method of preparation of claim 5 , wherein in heat treatment step (γ), the maximum plateau temperature is not more than 475° C.

Assignees

• Toyota Motor Europe

Inventors

• Katoh Yuki

Classifications

• H01M10/0562

  Solid materials · CPC title

• H01M10/052 Primary

  Li-accumulators · CPC title

• C01B25/14 Primary

  Sulfur, selenium, or tellurium compounds of phosphorus · CPC title

• H01M2300/0068

  inorganic · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title