METHOD OF SYNTHESIS OF LiTi2(PS4)3

Patent metadata

Field	Value
Publication number	US-2019177163-A1
Application number	US-201616325234-A
Country	US
Kind code	A1
Filing date	Sep 5, 2016
Priority date	Sep 5, 2016
Publication date	Jun 13, 2019
Grant date	—

Abstract

A method of synthesis of lithium titanium thiophosphate LiTi2(PS4)3 including the steps of: (a) providing a mixture of lithium sulfide Li2S, phosphorus sulfide P2S5 and titanium sulfide TiS2; (b) subjecting the mixture prepared in step (a) to a preliminary reaction step through mechanical milling or melt-quenching to produce an intermediate amorphous sulfide mixture; (c) subjecting the mixture prepared in step (b) to a heat treatment step at a maximum plateau temperature of at least 350° C. and less than 500° C.

First claim

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

2 . Method of synthesis according to claim 1 , wherein the mechanical milling procedure used in step (b) to produce an intermediate amorphous sulfide mixture is planetary ball milling, vibration milling or jet milling.

3 . Method of synthesis according to claim 2 , wherein planetary ball milling is used, and the ball size range is chosen within the range 1 mm≤ϕ≤10 mm), the temperature range is chosen within the range 0° C.≤T≤60° C., the rotation speed is chosen within the range 200 rpm≤R≤500 rpm, and the duration is chosen within the range 5 h≤t≤200 h.

4 . Method according to claim 1 , wherein in heat treatment step (c), the maximum plateau temperature is not more than 475° C.

5 . Method according to claim 1 , wherein in heat treatment step (c), the maximum plateau temperature during heat treatment is maintained for at least 1 hour and at most 300 hours.

6 . Method according to claim 1 , wherein the lithium sulfide Li 2 S, phosphorus sulfide P 2 S 5 and titanium sulfide TiS 2 starting materials are used in an Li 2 S:P 2 S 5 :TiS 2 mole ratio of 1:3:4.

Assignees

• Toyota Motor Europe

Inventors

• Katoh Yuki

Classifications

• C01B25/14 Primary

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

• H01M10/0562

  Solid materials · CPC title

• H01M10/052

  Li-accumulators · CPC title

• H01M2300/0068

  inorganic · CPC title

• Y02E60/10

  Energy storage using batteries · CPC title