Method for producing electrodes for all-solid state batteries

Patent metadata

Field	Value
Publication number	US-2020243900-A1
Application number	US-201716635580-A
Country	US
Kind code	A1
Filing date	Aug 4, 2017
Priority date	Aug 4, 2017
Publication date	Jul 30, 2020
Grant date	—

Abstract

A method ( 100 ) for producing a sintered component being a solid electrolyte and/or an electrode including titanium and sulfur for an all-solid state battery, the method including mixing powders ( 102 ) so as to obtain a powder mixture comprising titanium and sulfur, pressing ( 106 ) a component with the powder mixture, sintering ( 108 ) the component under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa so as to obtain an intermediate sintered component comprising titanium and sulfur, and sintering ( 114 ) the intermediate sintered component under a partial pressure of sulfur equal to or smaller than 150 Pa at a temperature plateau comprised between 200° C. and 400° C. so as to obtain a sintered component comprising titanium and sulfur, the solid electrolyte exhibiting the peaks in positions of 2θ=15.08° (±0.50°), 15.28° (±0.50°), 15.92° (±0.50°), 17.5° (±0.50°), 18.24° (±0.50°), 20.30° (±0.50°), 23.44° (±0.50°), 24.48° (±0.50°), and 26.66° (±0.50°) in a X-ray diffraction measurement using CuKα line.

First claim

1 .- 15 . (canceled)

16 . A method for producing a sintered component being a solid electrolyte and/or an electrode comprising titanium and sulfur for an all-solid state battery, the method comprising:
mixing powders so as to obtain a powder mixture comprising titanium and sulfur; pressing a component with the powder mixture; and sintering the component under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa so as to obtain an intermediate sintered component comprising titanium and sulfur; sintering the intermediate sintered component under a partial pressure of sulfur equal to or smaller than 150 Pa at a temperature plateau comprised between 200° C. and 400° C. so as to obtain a sintered component comprising titanium and sulfur; wherein the sintered component exhibits the peaks in positions of 2θ=15.08° (±0.50°), 15.28° (±0.50°), 15.92° (±0.50°), 17.5° (±0.50°), 18.24° (±0.50°), 20.30° (±0.50°), 23.44° (±0.50°), 24.48° (±0.50°), and 26.66° (±0.50°) in a X-ray diffraction measurement using CuKα line.

17 . The method according to claim 16 , wherein partial pressure of sulfur equal to or smaller than 150 Pa is obtained by flushing the intermediate sintered component with a noble gas or nitrogen.

18 . The method according to claim 16 , wherein partial pressure of sulfur equal to or smaller than 150 Pa is obtained by continuous evacuation of the gas present in a closed container comprising the intermediate sintered component.

19 . The method according to claim 16 , wherein the sintered component comprises XTi 2 (PS 4 ) 3 , X being lithium (Li), sodium (Na) or silver (Ag).

20 . The method according to claim 16 , the method comprising a step of amorphasizing the powder mixture so as to obtain an amorphasized powder mixture.

21 . The method according to claim 20 , wherein sintering under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa comprises a sintering plateau temperature equal to or smaller than 500° C.

22 . The method according to claim 20 , wherein sintering under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa comprises a sintering plateau time equal to or smaller than 20 hours.

23 . The method according to claim 16 , wherein the partial pressure of sulfur comprised between 200 Pa and 0.2 MPa is obtained by evaporating solid sulfur, the component being placed in a container and sealed under Argon at a pressure equal to or smaller than 100 Pa or from a sulfur containing gas.

24 . The method according to claim 16 , wherein the component is pressed at a pressure equal to or greater than 25 MPa and equal to or smaller than 500 MPa.

25 . The method according to claim 16 , wherein between the two sintering steps, the intermediate sintered component is grounded and pressed at a pressure equal to or greater than 25 MPa and equal to or smaller than 500 MPa.

26 . A method for producing a sintered component being a solid electrolyte and/or an electrode comprising titanium and sulfur for an all-solid state battery, the method comprising:
mixing powders so as to obtain a powder mixture comprising titanium and sulfur; pressing a component with the powder mixture; and sintering the component under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa so as to obtain an intermediate sintered component comprising titanium and sulfur; sintering the intermediate sintered component under a gradient of temperature, the maximum temperature of the intermediate sintered component being comprised between 200° C. and 400° C. so as to obtain a sintered component; wherein the sintered component exhibits the peaks in positions of 2θ=15.08° (±0.50°), 15.28° (±0.50°), 15.92° (±0.50°), 17.5° (±0.50°), 18.24° (±0.50°), 20.30° (±0.50°), 23.44° (±0.50°), 24.48° (±0.50°), and 26.66° (±0.50°) in a X-ray diffraction measurement using CuKα line.

27 . The method according to claim 26 , wherein the intermediate sintered component is sealed in a closed container during sintering under the gradient of temperature.

28 . The method according to claim 26 , wherein the sintered component comprises XTi 2 (PS 4 ) 3 , X being lithium (Li), sodium (Na) or silver (Ag).

29 . The method according to claim 26 , the method comprising a step of amorphasizing the powder mixture so as to obtain an amorphasized powder mixture.

30 . The method according to claim 29 , wherein sintering under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa comprises a sintering plateau temperature equal to or smaller than 500° C.

31 . The method according to claim 29 , wherein sintering under a partial pressure of sulfur comprised between 200 Pa and 0.2 MPa comprises a sintering plateau time equal to or smaller than 20 hours.

32 . The method according to claim 26 , wherein the partial pressure of sulfur comprised between 200 Pa and 0.2 MPa is obtained by evaporating solid sulfur, the component being placed in a container and sealed under Argon at a pressure equal to or smaller than 100 Pa or from a sulfur containing gas.

33 . The method according to claim 26 , wherein the component is pressed at a pressure equal to or greater than 25 MPa and equal to or smaller than 500 MPa.

34 . The method according to claim 26 , wherein between the two sintering steps, the intermediate sintered component is grounded and pressed at a pressure equal to or greater than 25 MPa and equal to or smaller than 500 MPa.

Assignees

• Toyota Motor Europe

Inventors

• Katoh Yuki

Classifications

• H01M10/0525

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

• Y02E60/10

  Energy storage using batteries · CPC title

• H01M2300/0068

  inorganic · CPC title

• H01M10/0562 Primary

  Solid materials · CPC title

• H01M10/052

  Li-accumulators · CPC title