Rapid Thermal Processing Methods and Apparatus

Patent metadata

Field	Value
Publication number	US-2024361076-A1
Application number	US-202318473177-A
Country	US
Kind code	A1
Filing date	Sep 22, 2023
Priority date	Feb 14, 2022
Publication date	Oct 31, 2024
Grant date	—

Abstract

Methods and apparatus for fabricating separators for solid-state lithium metal batteries employ rapid thermal processing. Aspects include high temperature sintering. Temperatures, durations of heat application, and proximity of heating elements to materials undergoing sintering combine to provide separators with desirable physical characteristics, including porosity, in a batch process.

First claim

1 - 36 . (canceled)

37 . A process for sintering, the process comprising:
heating a bilayer comprising a green body layer disposed on a metal layer in a furnace at about 1050° C. to about 1250° C. for about 2 minutes to about 10 minutes; thereby providing a sintered bilayer comprising a lithium-stuffed garnet layer on the metal layer; wherein the bilayer has a thickness, after sintering, of between about 10 μm and about 50 μm.

38 . The process of claim 37 , comprising heating the bilayer comprising a green body layer disposed on a metal layer in the furnace at about 1100° C. to about 1200° C.

39 . The process of claim 37 , comprising ramping the temperature in the furnace at a rate of up to about 50° C. per minute; or at a rate of about 5° C. per minute to about 35° C. per minute.

40 . The process of claim 37 , wherein the bilayer moves through the furnace at a rate of between about 20 mm/min to about 80 mm/min.

41 . The process of claim 37 , wherein the bilayer dwells in the furnace for about 1 minute to about 10 minutes.

42 . The process of claim 37 , further comprising a binder burn-out step prior to heating the bilayer at about 1050° C. to about 1250° C. for about 2 minutes to about 10 minutes.

43 . The process of claim 42 , wherein the binder burn-out step occurs for about 1 second to about 5 minutes.

44 . The process of claim 42 , wherein the bilayer, prior to the binder burn-out step, comprises at least one member selected from a solvent, a binder, a dispersant, a plasticizer, a surfactant, or a combination thereof.

45 . The process of claim 37 , wherein the lithium-stuffed garnet layer comprises compounds having the formula Li A La B Zr C O F , Li A La B M′ C M″ D Ta E O F , or Li A La B M′ C M″ D Nb E O F , wherein 4<A<8.5, 1.5<B<4, 0<C≤2, 0<D<2; 0<E<2.5, 10<F<13, and M′ and M″ are each, independently in each instance selected from Al, Mo, W, Nb, Ga, Sb, Ca, Ba, Sr, Ce, Hf, Rb, and Ta; or Li a La b Zr c Al d Me″ e O f , wherein 5<a<7.7; 2<b<4; 0<c≤2.5; 0<d<2; 0<e<2, 10<f<13 and Me″ is a metal selected from Nb, V, W, Mo, Ta, Ga, and Sb.

46 . The process of claim 37 , wherein the metal layer comprises a metal selected from the group consisting of nickel, tungsten, copper, iron, titanium, molybdenum, alloys thereof, and combinations thereof.

47 . The process of claim 37 , wherein the bilayer has a thickness, after sintering, of about m to about 40 μm; or wherein the bilayer has a thickness, after sintering, of about 1 μm to about 20 μm.

48 . The process of claim 37 , wherein the bilayer has a width, after sintering, of between about 10 mm to about 100 mm.

49 . The process of claim 37 , wherein the furnace comprises an atmospheric controller that maintains an atmosphere in the furnace that comprises argon (Ar) gas; nitrogen (N 2 ) gas; hydrogen gas; forming gas, or a mixture thereof, and wherein the atmospheric controller maintains an atmosphere in the furnace comprising less than 500 ppm O 2 ; or wherein the atmospheric controller maintains an atmosphere in the furnace comprising less than 250 ppm O 2 .

50 . The process of claim 37 , wherein the bilayer comprising a green body layer disposed on a metal layer contacts, or is inside, furniture.

51 . The process of claim 50 , wherein the furniture contacts the metal layer of the bilayer and comprises a first plate made of material selected from the group consisting of alumina (Al 2 O 3 ), zirconium toughened alumina (ZTA), mullite (3Al 2 O 3 2SiO 2 or 2Al 2 O 3 SiO 2 ), aluminum nitride (AlN), or silicon carbide (SiC).

52 . The process of claim 51 , wherein the furniture further comprises a second plate disposed above the green body layer of the bilayer and made of material selected from the group consisting of alumina (Al 2 O 3 ), zirconium toughened alumina (ZTA), mullite (3Al 2 O 3 2SiO 2 or 2Al 2 O 3 SiO 2 ), aluminum nitride (AlN), or silicon carbide (SiC).

53 . The process of claim 52 , further comprising a frame interposed between the bilayer structure and the second plate, the frame being made of material selected from the group comprising porous alumina, zirconia, lithium aluminate, lithium tantalate, alumina, silica, cordierite, Ni, kovar, or invar.

54 . The process of claim 37 , wherein the bilayer is in contact with a bottom surface.

55 . The process of claim 37 , wherein the bilayer is between a center-less cover and a bottom setter.

56 . A sintered bilayer prepared by the process of claim 37 .

Assignees

• Quantumscape Battery Inc

Inventors

• Holme Timothy
• Winterkorn Martin
• Tozier Dylan
• Ramaswamy Murugan

Classifications

• C04B35/486

  Fine ceramics · CPC title

• F27D21/00

  Arrangement of monitoring devices; Arrangement of safety devices · CPC title

• F27D19/00

  Arrangements of controlling devices · CPC title

• C04B2235/9623

  Ceramic setters properties · CPC title

• C04B2235/666

  Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS] · CPC title