Substrate structures and methods of manufacture
US-2016323997-A1 · Nov 3, 2016 · US
US2024116826A1 · US · A1
| Field | Value |
|---|---|
| Publication number | US-2024116826-A1 |
| Application number | US-202318460360-A |
| Country | US |
| Kind code | A1 |
| Filing date | Sep 1, 2023 |
| Priority date | Mar 9, 2021 |
| Publication date | Apr 11, 2024 |
| Grant date | — |
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Provided herein are rapid, high quality film sintering processes that include high-throughput continuous sintering of lithium-lanthanum zirconium oxide (lithium-stuffed garnet). The instant disclosure sets forth equipment and processes for making high quality, rapidly-processed ceramic electrolyte films. These processes include high-throughput continuous sintering of lithium-lanthanum zirconium oxide for use as electrolyte films. In certain processes, the film is not in contact with any surface as it sinters (i.e., during the sintering phase).
Opening claim text (preview).
1 .- 32 . (canceled) 33 . 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 1100° C. to about 1300° C. for about 5 seconds to about 3 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. 34 . The process of claim 33 , wherein the bilayer moves through the furnace at a rate of between about 2 inches/min to 25 inches/min. 35 . The process of claim 33 , further comprising a binder burn-out step prior to heating a bilayer at about 1100° C. to about 1300° C. for about 5 seconds to about 3 minutes. 36 . The process of claim 35 , wherein the binder burn-out step occurs in a binder burn-out furnace. 37 . The process of claim 35 , wherein the binder burn-out step occurs from about 1 second to about 5 minutes. 38 . The process of claim 33 , 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. 39 . The process of claim 37 , 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. 40 . The process of claim 33 , wherein the metal layer comprises a metal selected from the group consisting of nickel, copper, iron, alloys thereof, and combinations thereof. 41 . The process of claim 33 , wherein the bilayer has a thickness, after sintering, of between about 20 μm and about 40 μm. 42 . The process of claim 33 , wherein the metal layer has a thickness of about 1 μm to about 20 μm. 43 . The process of claim 33 , wherein the bilayer has a width, after sintering, of between about 0.8 mm to about 5 m. 44 . The process of claim 33 , 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; or a mixture thereof. 45 . The process of claim 44 , wherein the atmospheric controller maintains an atmosphere in the furnace comprising less than 500 ppm O 2 . 46 . The process of claim 33 , further comprising rolling up the sintered bilayer. 47 . A sintered bilayer prepared by the process of claim 33 .
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