Lithium stuffed garnet setter plates for solid electrolyte fabrication

Patent metadata

Field	Value
Publication number	US-2017062873-A1
Application number	US-201615286509-A
Country	US
Kind code	A1
Filing date	Oct 5, 2016
Priority date	Apr 16, 2015
Publication date	Mar 2, 2017
Grant date	—

Abstract

Setter plates are fabricated from Li-stuffed garnet materials having the same, or substantially similar, compositions as a garnet Li-stuffed solid electrolyte. The Li-stuffed garnet setter plates, set forth herein, reduce the evaporation of Li during a sintering treatment step and/or reduce the loss of Li caused by diffusion out of the sintering electrolyte. Li-stuffed garnet setter plates, set forth herein, maintain compositional control over the solid electrolyte during sintering when, upon heating, lithium is prone, to diffuse out of the solid electrolyte.

First claim

1 . A setter plate for fabricating solid electrolytes of a rechargeable battery, the setter plate comprising:
a Li-stuffed garnet compound characterized by the formula Li x La y Zr z O t .qAl 2 O 3 , wherein 4<x<10, 1<y<4, 1<z<3, 6<t<14, 0≦q≦1; a surface defined by a first lateral dimension from 2 cm to 30 cm and a second lateral dimension from 2 cm to 30 cm; and a thickness from 0.1 mm to 100 mm.

2 - 3 . (canceled)

4 . The setter plate of claim 1 , wherein the thickness is from 0.1 mm to 10 mm.

5 - 9 . (canceled)

10 . The setter plate of claim 1 , wherein the surface has a surface roughness from 1.0 μm Ra to 4 μm Ra, wherein Ra is an arithmetic average of absolute values of sampled surface roughness amplitudes.

11 - 20 . (canceled)

21 . A method of using a setter plate to fabricate a Li-stuffed garnet solid electrolyte for a rechargeable battery, the method comprising:
placing a green film of unsintered Li-stuffed garnet precursor materials between two setter plates; and sintering the green film between the two Li-stuffed garnet setter plates,
wherein the setter plates comprise a Li-stuffed garnet.

22 . (canceled)

23 . The method of claim 21 , further comprising placing a metal foil or metal powder between at least one setter plate and the green film prior to the sintering the green film.

24 - 25 . (canceled)

26 . The method of claim 21 , wherein the green film has a surface defined by a first lateral dimension from 1 cm to 50 cm and a second lateral dimension from 1 cm to 50 cm.

27 - 31 . (canceled)

32 . The method of claim 21 , wherein the sintering comprises exposing, during the heating, the green film and the two Li-stuffed garnet setter plates to an Argon:H 2 mixed atmosphere.

33 - 38 . (canceled)

39 . The method of claim 21 , wherein the sintering produces a sintered Li-stuffed garnet solid electrolyte less than 100 microns thick and more than 1 nm thick.

40 - 46 . (canceled)

47 . The method of claim 21 , wherein the sintered Li-stuffed garnet solid electrolyte has an ASR from between 0.1 Ω.cm 2 to 10 Ω.cm 2 at 50° C.

48 .- 73 . (canceled)

74 . A method of using a setter plate to fabricate a Li-stuffed garnet solid electrolyte for a rechargeable battery, the method comprising:
placing a green film of unsintered Li-stuffed garnet precursor materials between two setter plates, wherein the setter plate comprises a member selected from Li 2 ZrO 3 , xLi 2 O-(1−x)SiO 2 (where x=0.01-0.99), aLi 2 O-bB 2 O 3 -cSiO 2 (where a+b+c=1), LiLaO 2 , LiAlO 2 , Li 2 O, Li 3 PO 4, a Li-stuffed garnet, and combinations thereof; and sintering the green film between the two setter plates.

75 - 84 . (canceled)

85 . The method of claim 74 , wherein the green film is a tape-cast film.

86 . The method of claim 74 , wherein the sintering atmosphere comprises, Air, Argon, Nitrogen, an Argon:H 2 mixture, or an Argon:H 2: H 2 O mixture.

87 - 92 . (canceled)

93 . The method of claim 74 , further comprising placing a metal foil or metal powder between the setter plate and the green film prior to the sintering the green film.

94 . The method of claim 93 , wherein the metal is Ni, Cu, Fe, Al, Ag, combinations thereof, or alloys thereof.

95 . The method of claim 74 , wherein the green film has a surface defined by a first lateral dimension from 1 cm to 50 cm and a second lateral dimension from 1 cm to 50 cm.

96 . The method of claim 74 , wherein the green film has a thickness between 1 μm to about 100 μm.

97 . (canceled)

98 . The method of claim 74 , wherein the sintering comprises heating the green electrolyte film and the setter plate to between 450° C. and 1300° C.

99 . The method claim 74 , wherein the sintering comprises exposing, during the heating, the green film and the two Li stuffed garnet setter plate to an Argon:H 2 mixed atmosphere.

100 - 106 . (canceled)

107 . The method of claim 74 , wherein the sintering produces a sintered Li-stuffed garnet solid electrolyte less than 50 microns thick.

108 - 116 . (canceled)

117 . The setter plate of claim 1 having a flatness of between 0.1 μm and 100 μm.

118 . The setter plate of claim 1 having a flatness of between 0.5 μm and 20 μm.

119 . The method of claim 74 , further comprising providing a rechargeable battery comprising the Li-stuffed garnet solid electrolyte.

Assignees

• Quantumscape Corp

Inventors

• Iyer Sriram
• Holme Tim
• Donnelly Niall

Classifications

• C08K5/09

  Carboxylic acids; Metal salts thereof; Anhydrides thereof · CPC title

• C08K3/105

  Compounds containing metals of Groups 1 to 3 or of Groups 11 to 13 of the Periodic Table · CPC title

• C08K2003/2203

  of lithium · CPC title

• C08K5/12

  of cyclic polycarboxylic acids · CPC title

• C04B35/486

  Fine ceramics · CPC title