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Patent metadata

Field	Value
Publication number	US-2023287570-A1
Application number	US-202118002849-A
Country	US
Kind code	A1
Filing date	Jun 24, 2021
Priority date	Jun 25, 2020
Publication date	Sep 14, 2023
Grant date	—

Abstract

A method of manufacturing a layer of crystalline ytterbium doped zirconia on a substrate is disclosed. The method includes depositing a solution including precursor metal salts of the ytterbium doped zirconia onto a surface of the substrate, wherein the surface is a metallic or a ceramic surface. The solution is dried to form a film of the precursor metal salts on the surface. The film of the precursor metal salts is heated to decompose it to form an ytterbium doped zirconia. The previous steps may optionally be repeated. The film(s) are fired in order to form the layer of crystalline ytterbium doped zirconia. The ytterbium doped zirconia has a formula:
([Yb x M 1−x ] 2 O 3 ) z (ZrO 2 ) 1−z
wherein M is a metallic dopant ion; z is in the range of 0.03 to 0.13; and x is in the range of 0.05 to 1.

First claim

1 . A method of manufacturing a layer of crystalline ytterbium doped zirconia on a substrate, wherein the method comprises the steps of:
(i) depositing a solution comprising precursor metal salts of the ytterbium doped zirconia onto a surface of the substrate, wherein the surface is a metallic or a ceramic surface; (ii) drying the solution to form a film of the precursor metal salts on the surface; (iii) heating the film of the precursor metal salts to decompose it to form an ytterbium doped zirconia; (iv) firing said film(s) to form the layer of crystalline ytterbium doped zirconia.

2 . The method according to claim 1 , wherein the substrate comprises a dense solid oxide electrolyte for a solid oxide cell, and the layer of crystalline ytterbium doped zirconia is formed on the substrate.

3 . The method according to claim 1 , wherein
the layer comprises a crystalline ytterbium doped zirconia with a cubic crystal structure.

4 . The method according to claim 1 , wherein the substrate in step (i) has a temperature of 10° C. to 100° C.

5 . The method according to claim 1 , wherein a temperature of step (iii) is 200° C. to 600° C.

6 . The method according to claim 1 , wherein the precursor metal salts comprise a zirconium salt and a ytterbium salt, wherein the zirconium salt is zirconium acetylacetonate.

7 . The method according to claim 1 , wherein the precursor metal salts comprise a zirconium salt and a ytterbium salt, wherein the ytterbium salt comprises one or more of: ytterbium nitrate, ytterbium acetate tetrahydrate, and ytterbium acetylacetonate, or combinations thereof.

8 . The method according to claim 1 , wherein a concentration of metal ions in the solution is 0.05M to 0.2M.

9 . The method according to claim 1 , wherein the solution comprises a solvent comprising one or more of: methanol, ethanol, propanol, methoxypropanol, ethylacetate, acetone, and butyl carbitol.

10 . The method according to claim 1 , wherein a pH of the solution is 2 to 6.

11 . The method according to claim 1 , wherein the solution further comprises an acid comprising one or more of: acetic acid, citric acid, and nitric acid.

12 . The method according to claim 1 , wherein step (i) involves depositing the solution via spraying, jetting, dipping, or spin coating the solution onto the substrate.

13 . (canceled)

14 . The method according to claim 1 , wherein a temperature in step (iv) is 500° C. to 1100° C.

15 . The method according to claim 1 , wherein step (iii) further comprises cooling the layer to a temperature of less than 150° C.

16 . (canceled)

17 . The method according to claim 1 , wherein the ytterbium doped zirconia has a formula:
([Yb x M 1−x ] 2 O 3 ) z (ZrO 2 ) 1−z wherein M is a metallic dopant ion; z is 0.03 to 0.13; and x is 0.05 to 1.

18 . The method according to claim 17 , wherein x is 1.

19 . The method according to claim 17 , wherein z is 0.06 to 0.12.

20 . A method according to claim 1 , comprising an additional step in which steps (i) to (iv) are repeated at least once, whereby in the additional step the substrate comprises the layer of crystalline ytterbium doped zirconia produced in step (iv).

21 . (canceled)

22 . The method according to claim 1 , wherein any or all of steps (ii), (iii), and (iv) is or are conducted in air.

23 - 32 . (canceled)

33 . The method of claim 1 , further comprising repeating steps (i) to (iii) prior to firing the film(s).

Assignees

• Ceres Ip Co Ltd

Inventors

• Leah Robert
• Lankin Mike

Classifications

• C23C18/1208 Primary

  Oxides, e.g. ceramics · CPC title

• C23C18/1216 Primary

  Metal oxides (C23C18/1212 takes precedence) · CPC title

• C23C18/1291

  by heating of the substrate · CPC title

• C23C18/1295

  with after-treatment of the deposited inorganic material · CPC title

• C23C18/1283

  Control of temperature, e.g. gradual temperature increase, modulation of temperature · CPC title