Thin film lithium conducting powder material deposition from flux

Patent metadata

Field	Value
Publication number	US-11876208-B2
Application number	US-202117472558-A
Country	US
Kind code	B2
Filing date	Sep 10, 2021
Priority date	Jan 7, 2013
Publication date	Jan 16, 2024
Grant date	Jan 16, 2024

Abstract

The present invention is directed to battery technologies and processing techniques thereof. In various embodiments, ceramic electrolyte powder material (or component thereof) is mixed with two or more flux to form a fluxed powder material. The fluxed powder material is shaped and heated again at a temperature less than 1100° C. to form a dense lithium conducting material. There are other variations and embodiments as well.

First claim

What is claimed is:

1. A method for forming a dense lithium conducting material, the method comprising:
providing a lithium conducting ceramic powder material at a first quantity, the ceramic powder material being characterized by a first density, the lithium conducting ceramic powder material being characterized by a median particle size of about 100 nm to 10 μm;
providing a first flux material at a second quantity, the second quantity being less than 51% of the first quantity, the first flux material comprising lithium material, the first flux material being characterized by a melting temperature of about 500-1000° C.;
providing a second flux material at a third quantity, the second flux material being characterized by a melting temperature of about 500-1000° C.;
mixing at least the first flux material and the second flux material to form a eutectic mixture;
mixing the eutectic mixture with the lithium conducting ceramic powder material to form a fluxed ceramic powder material;
flux sintering the shaped fluxed ceramic powder material to a temperature of less than 1100° C.; and
forming a dense lithium conducting material, the dense lithium conducting material being characterized by a second density, the second density is at least 20% higher than the first density.

2. The method of claim 1 wherein the lithium conducting ceramic powder material comprises electrolyte component powders selected from one or more of metal oxides, nitrates, carbonates, sulfates, borates, and hydroxides.

3. The method claim 2 wherein electrolyte component powders is characterized a quantity less than the second quantity.

4. The method of claim 1 wherein the first flux material comprises inorganic salts of lithium material.

5. The method of claim 1 further comprising providing a substrate material, the substrate having a metallic surface.

6. The method of claim 1 wherein the second density is at least 40% higher than the first density.

7. The method of claim 1 further comprising melting the lithium conducting ceramic powder material by the eutectic mixture at a temperature of less than 800° C.

8. The method of claim 1 further comprising dissolving the lithium conducting ceramic powder material by the eutectic mixture at a temperature of less than 800° C.

9. The method of claim 1 wherein the eutectic mixture comprises less than 80% of a total mass of the fluxed ceramic powder material.

10. The method of claim 1 wherein the predetermined shape is disc, sheet, cylinder, or pellet.

11. The method of claim 1 wherein the second quantity being about 15-30% of the first quantity.

12. The method of claim 1 wherein the first flux material comprises one or more materials selected from LiOH, LiCl, LiBr, LiNO 3 , Li 3 BO 3 and LiSO 4 .

13. The method of claim 1 wherein the second flux material comprises one or more materials selected from NaOH, NaCl, NaNO 3 , NaSO 4 , NaBr, and Na 2 CO 3 .

14. The method of claim 1 wherein the eutectic mixture is characterized by a melting point of about 200 to 800° C.

15. The method of claim 1 further comprising subjecting the flux material to a temperature of about 200 to 1000° C.

16. The method of claim 1 wherein the lithium conducting ceramic powder material being characterized by a median particle size of about 100 nm to 2 um.

17. The method of claim 1 wherein the lithium conducting ceramic powder material comprises a garnet material.

18. The method of claim 1 wherein the lithium conducting ceramic powder material comprises a perovskite material.

19. The method of claim 1 wherein the lithium conducting ceramic powder material comprises Nasicon material, Lisicon material, and/or a Tungsten Bronze material.

20. The method of claim 1 wherein the substrate comprises a polymer material and a metal surface overlaying the polymer material.

21. The method of claim 1 further comprising providing a third flux material at a third quantity, the third flux material comprising KOH, KCl, KNO 3 , KSO 4 , KBr, and/or K 2 CO.

22. The method of claim 1 further comprising removing the first flux material and the second flux material by subjecting the dense lithium conducting material to one or more solvent washings, the one or more solvent comprising water, ethanol, isopropanol, acetone, acetonitrile, an acid, and/or a base.

23. The method of claim 1 wherein the dense lithium conducting material is deposited on a metal conductive material.

24. The method of claim 1 further comprising:
providing a substrate material, the substrate material comprises a layer of metal conductive material, wherein the lithium conducting ceramic powder material is provided on the layer of metal conductive material.

25. A method for depositing material, the method comprising:
providing components of lithium conducting ceramic powder material at a first quantity, the components being characterized by a first density, the components being characterized by a median particle size of about 100 nm to 10 μm;
providing a first flux material at a second quantity, the first flux material comprising inorganic salts of lithium material, the first flux material being characterized by melting temperature of about 500-1000° C.;
providing a second flux material at a third quantity, the second flux material being characterized by melting temperature of about 500-1000° C.;
mixing the first flux material and the second flux material with the components to form a eutectic mixture;
mixing the eutectic mixture with the lithium conducting ceramic powder material to form a fluxed ceramic powder material;
shaping the fluxed ceramic powder material in to a predetermined shape;
flux sintering the shaped fluxed ceramic powder; and
forming a dense lithium conducting material, the dense lithium conducting material being characterized by a second density, the second density is at least 20% higher than the first density.

26. The method of claim 25 comprising:
wherein the eutectic mixture being characterized by a melting point of less than 800° C.;
subjecting the eutectic mixture to a temperature of about 100 to 1000° C.

27. A method for depositing lithium garnet material, the method comprising:
providing components of lithium conducting ceramic powder material at a first quantity, the components being characterized by a first density, the components being characterized by a median particle size of about 100 nm to 10 μm;
providing a first flux material at a second quantity, the first quantity being more than 100% of the second quantity, the first flux material comprising inorganic salts of lithium material, the first flux material being characterized by a melting temperature of about 500-1000° C.;
providing a second flux material at a third quantity, the second flux material being characterized by a melting temperature of about 500-1000° C.;
mixing the first flux material and the second flux material with the components to form a eutectic mixture;
mixing the eutectic mixture with the lithium conducting ceramic powder material to form a fluxed ceramic powder material;
shaping the fluxed ceramic powder material into a predetermined shape;
flux sintering the shaped fluxed ceramic powder material; and
forming a dense lithium conducting material, the dense lithium conducting material being characterized by a second density, the second density is at least 20% higher than the first density.

Assignees

• Quantumscape Battery Inc

Inventors

• Donnelly Niall
• Holme Timothy

Classifications

• Y02E60/10

  Energy storage using batteries · CPC title

• H01M4/0409 Primary

  by a doctor blade method, slip-casting or roller coating · CPC title

• C01G25/006 Primary

  Compounds containing zirconium, with or without oxygen or hydrogen, and containing two or more other elements · CPC title

• C04B35/00

  Shaped ceramic products characterised by their composition {(porous ceramic products C04B38/00; ceramic articles characterised by particular shape, see the relevant classes, e.g. linings for casting ladles, tundishes, cups or the like B22D41/02; ceramic substrates for microelectronic semi-conductors H10W70/692)}; Ceramics compositions ({shaping of ceramics B28B;} containing free metal bonded to carbides, diamond, oxides, borides, nitrides, silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides or sulfides other than as macroscopic reinforcing agents C22C); Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products {(infiltration of sintered ceramic preforms with molten metal C04B41/51; chemical preparation of powders of inorganic compounds C01)} · CPC title

• C04B35/486

  Fine ceramics · CPC title