Method of preparing an electrochemical half-cell

Patent metadata

Field	Value
Publication number	US-9799908-B2
Application number	US-201214112341-A
Country	US
Kind code	B2
Filing date	Apr 19, 2012
Priority date	Apr 22, 2011
Publication date	Oct 24, 2017
Grant date	Oct 24, 2017

Abstract

The present invention relates to a method for preparing an electrode-supported electrochemical half-cell including a step consisting in subjecting a green electrode layer on which a precursor gel of the electrolyte or a precursor thereof is deposited to sintering at a temperature of less than or equal to 1350° C.

First claim

The invention claimed is:

1. A method for preparing an electrode-supported electrochemical half-cell including a single step of sintering, said step consisting of subjecting a green electrode layer on which a precursor gel of an electrolyte or a sol precursor of said gel is deposited to sintering at a temperature of less than or equal to 1350° C., said gel comprising a solid network wherein metallic cations are uniformly distributed in an organic matrix, and said sol precursor of said gel comprising a colloidal or polymer suspension wherein the metallic cations contribute to forming a colloidal or polymer network, and wherein said green electrode layer is obtained from a ceramic ink corresponding to a dispersion (or suspension) of powders of the electrode material in an aqueous or organic solvent.

2. A method according to claim 1 , wherein said powder is a powder of a material chosen from among perovskite materials of structure ABO 3 , where A represents a rare earth and B a transition metal; stabilised zirconias, optionally blended with NiO; substituted cerias, optionally blended with NiO, and blends thereof.

3. A method according to claim 1 , wherein said ceramic ink includes at least one element chosen from among a solvent, a dispersing agent, a binder, a plasticiser and a pore-forming agent.

4. A method according to claim 1 , wherein the gel or its sol precursor is prepared by a sol-gel process, by a polymer process derived from the Péchini method, or by an NPG (nitrate polyacrylamide gel) synthesis process.

5. A method according to claim 4 , wherein the gel or its sol precursor is prepared by a sol-gel process and said sol-gel process uses at least one organometallic precursor.

6. A method according to claim 5 , wherein R has 1 to 10 carbon atoms.

7. A method according claim 1 , wherein the sintering temperature is between 1000 and 1350° C., and wherein the green electrode layer on which a precursor gel of the electrolyte or a sol precursor of said gel is deposited is maintained at the sintering temperature for a period of between 1 and 5 h.

8. A method according to claim 7 , wherein the sintering temperature is between 1000 and 1300° C.

9. A method according to claim 1 , wherein before being brought to the sintering temperature, the green electrode layer on which a precursor gel of the electrolyte or a sol precursor of said gel is brought to an intermediate temperature of between 400 and 800° C. and wherein it is maintained at this intermediate temperature for a period of between 15 and 120 min.

10. A method according to claim 9 , wherein said green electrode layer on which a precursor gel of the electrode or a sol precursor of said gel is deposited is brought to an intermediate temperature by means of a slow rising temperature gradient of between 10 and 50° C./h[L].

11. A method according to claim 10 , wherein the temperature gradient is between 15 and 40° C./h.

12. A method according to claim 9 , wherein said green electrode layer on which a precursor gel of the electrode or a sol precursor of said gel is deposited is brought from the intermediate temperature to the sintering temperature by means of a rising temperature gradient of between 25 and 100° C./h.

13. A method according to claim 9 , wherein the intermediate temperature is between 500 and 700° C.

14. A method according to claim 1 , including the steps consisting of:
a) preparing the green electrode layer;
b) depositing, on said green electrode layer, the precursor gel of the electrolyte or the sol precursor of said gel and
c) subjecting said green electrode layer on which said precursor gel of the electrolyte or the sol precursor of said gel is deposited to a sintering temperature of less than or equal to 1350° C.

15. A method according to claim 14 , wherein, in step (a), the green electrode layer is obtained by deposition of a ceramic ink corresponding to a dispersion (or suspension) of powders of the electrode material in an aqueous or organic solvent by tape casting.

16. A method according to claim 14 , wherein, in step (b), the deposition is accomplished by screen printing.

17. A method according to claim 14 , wherein, following step (c), the sintered material is subjected to a reduction.

18. A method according to claim 17 , wherein the electrode-supported electrochemical half-cell obtained following the step of reduction has a porous support electrode and a thin, dense electrolyte.

19. A method according to claim 1 , wherein the electrode-supported electrochemical half-cell obtained following the step of sintering has a porous support electrode and a thin, dense electrolyte.

20. A method according to claim 5 , wherein the at least one organometallic precursor comprises at least one metallic alkoxide selected from the group consisting of zirconium methoxide, zirconium ethoxide, zirconium n-propoxide, zirconium butoxide, zirconium pentoxide, cerium methoxide, cerium ethoxide, cerium n-propoxide, cerium butoxide and cerium penoxide.

Assignees

• Delahaye Thibaud
• Rieu Mathilde
• Commissariat Energie Atomique

Inventors

• Delahaye Thibaud
• Rieu Mathilde

Classifications

• C25B11/04

  characterised by the material · CPC title

• H01M4/8889

  Cosintering or cofiring of a catalytic active layer with another type of layer · CPC title

• C04B35/6263

  characterised by their solids loadings, i.e. the percentage of solids · CPC title

• C04B35/01 Primary

  based on oxide ceramics · CPC title

• C04B2235/6567

  Treatment time · CPC title