Increasing ionic conductivity of lithium titanium thiophosphate by sintering

Patent metadata

Field	Value
Publication number	US-11063289-B2
Application number	US-201616326480-A
Country	US
Kind code	B2
Filing date	Sep 5, 2016
Priority date	Sep 5, 2016
Publication date	Jul 13, 2021
Grant date	Jul 13, 2021

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

The invention claimed is:

1. A 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.,
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.

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

3. A 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., thereby forming a material;
wherein the material obtained through step (γ) is subsequently subjected to the method of claim 1 .

4. The method of preparation of claim 3 , 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.

5. The method of preparation of claim 3 , wherein in the heat treatment step (γ), the maximum plateau temperature is not more than 475° C.

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

Assignees

• Toyota Motor Europe

Inventors

• Katoh Yuki

Classifications

• C01G23/002

  Compounds containing titanium, with or without oxygen or hydrogen, and containing two or more other elements (C01G23/001, C01G23/003 take precedence) · CPC title

• C01B25/14 Primary

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

• H01M10/052 Primary

  Li-accumulators · CPC title

• H01M10/0562

  Solid materials · CPC title

• C01P2002/72

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