Process for preparing ceramic powders in the presence of a source of carbon, powders thus obtained and their use

Patent metadata

Field	Value
Publication number	US-9394205-B2
Application number	US-201414317403-A
Country	US
Kind code	B2
Filing date	Jun 27, 2014
Priority date	May 30, 2002
Publication date	Jul 19, 2016
Grant date	Jul 19, 2016

Abstract

A method for preparing ceramic powders in the presence of a carbon powder including a step which consists in homogenizing a mixture of particles capable of resulting in a ceramic by heat treatment. Said method can be carried out in the presence of an accelerated solvent and provides, at reduced energy consumption, carbon-coated ceramic powders and then ceramics.

First claim

The invention claimed is:

1. A process for the preparation of a ceramic product, said process comprising:
preparing a ceramic powder; and
subjecting the ceramic powder to at least one heat treatment at a temperature higher than 800° C.,
wherein the ceramic powder is prepared from a mixture of precursors of said powder and in the presence of at least one source of carbon by a method comprising the following steps:
a) homogenization, in the presence of the source of carbon and optionally in the presence of a solvent, to obtain an intimate mixture of precursor particles that can result in a ceramic product by heat treatment; and
b) removal of the solvent eventually if present in the intimate mixture obtained in step a);

wherein the source of carbon is selected from the group consisting of liquid forms, gaseous forms and mixtures thereof; and wherein the homogenization step a) is carried out by high-energy grinding.

2. A process for the preparation of a ceramic product, said process comprising:
preparing a ceramic powder; and
subjecting the ceramic powder to at least one heat treatment at a temperature higher than 800° C.,
wherein the ceramic powder is prepared from a mixture of precursors of said powder and in the presence of at least one source of carbon by a method comprising the following steps:
a) homogenization, in the presence of the source of carbon and optionally in the presence of a solvent, to obtain an intimate mixture of precursor particles that can result in a ceramic product by heat treatment; and
b) removal of the solvent eventually if present in the intimate mixture obtained in step a);

wherein the source of carbon is selected from the group consisting of liquid forms, gaseous forms and mixtures thereof; and wherein the homogenization step a) is carried out by mechanofusion.

3. A process for the preparation of a ceramic product, said process comprising:
preparing a ceramic powder; and
subjecting the ceramic powder to at least one heat treatment at a temperature higher than 800° C.,
wherein the ceramic powder is prepared from a mixture of precursors of said powder and in the presence of at least one source of carbon by a method comprising the following steps:
a) homogenization, in the presence of the source of carbon and optionally in the presence of a solvent, to obtain an intimate mixture of precursor particles that can result in a ceramic product by heat treatment; and
b) removal of the solvent eventually if present in the intimate mixture obtained in step a);

wherein the source of carbon is selected from the group consisting of liquid forms, gaseous forms and mixtures thereof; wherein the homogenization step a) is carried out by high-energy grinding; and wherein the intimate mixture of particles that can result in the ceramic product by heat treatment is a mixture of: 1) particles of ZrO 2 and particles of Y 2 O; or 2) particles of Li 2 TiO 3 and of particles of TiO 2 .

4. The process of preparation according to claim 1 , wherein the source of carbon is selected from the group consisting of Ketjen black, Shawinigan black, CH 4 , C 2 H 6 , C 2 H 2 and mixtures thereof.

5. The process of preparation according to claim 1 , wherein a temperature during the removal step b) is between 40 and 150° C.

6. The process of preparation according to claim 1 , wherein the source of carbon and the solvent are introduced during step a).

7. The process of preparation according to claim 1 , carried out at least partially under a reducing atmosphere, said reducing atmosphere preventing transformation of the carbon, that is present in the reaction mixture, into carbon dioxide, and allowing to obtain particles of ceramic powder that are coated with carbon.

8. The process of preparation according to claim 1 , wherein step a) lasts between 1 and 3 hours.

9. The process of preparation according to claim 1 , wherein at least one of the steps is carried out under inert atmosphere.

10. The process of preparation according to claim 1 , wherein at least one step of the process is carried out in the presence of a source of oxygen, in order to remove any trace of residual carbon from the ceramic powder obtained at the end of the process.

11. The process of preparation according to claim 2 , wherein the source of carbon is selected from the group consisting of Ketjen black, Shawinigan black, CH 4 , C 2 H 6 , C 2 H 2 and mixtures thereof.

12. The process of preparation according to claim 2 , wherein a temperature during the removal step b) is between 40 and 150° C.

13. The process of preparation according to claim 2 , wherein the source of carbon and the solvent are introduced during step a).

14. The process of preparation according to claim 2 , carried out at least partially under a reducing atmosphere, said reducing atmosphere preventing transformation of the carbon, that is present in the reaction mixture, into carbon dioxide, and allowing to obtain particles of ceramic powder that are coated with carbon.

15. The process of preparation according to claim 2 , wherein step a) lasts between 1 and 3 hours.

16. The process of preparation according to claim 2 , wherein at least one of the steps is carried out under inert atmosphere.

17. The process of preparation according to claim 2 , wherein at least one step of the process is carried out in the presence of a source of oxygen, in order to remove any trace of residual carbon from the ceramic powder obtained at the end of the process.

18. The process of preparation according to claim 3 , wherein the source of carbon is selected from the group consisting of Ketjen black, Shawinigan black, CH 4 , C 2 H 6 , C 2 H 2 and mixtures thereof.

19. The process of preparation according to claim 3 , wherein a temperature during the removal step b) is between 40 and 150° C.

20. The process of preparation according to claim 3 , wherein the source of carbon and the solvent are introduced during step a).

21. The process of preparation according to claim 3 , carried out at least partially under a reducing atmosphere, said reducing atmosphere preventing transformation of the carbon, that is present in the reaction mixture, into carbon dioxide, and allowing to obtain particles of ceramic powder that are coated with carbon.

22. The process of preparation according to claim 3 , wherein step a) lasts between 1 and 3 hours.

23. The process of preparation according to claim 3 , wherein at least one of the steps is carried out under inert atmosphere.

24. The process of preparation according to claim 3 , wherein at least one step of the process is carried out in the presence of a source of oxygen, in order to remove any trace of residual carbon from the ceramic powder obtained at the end of the process.

25. The process of preparation according to claim 3 , wherein the particles of ZrO 2 and Y 2 O or the particles of Li 2 TiO 3 and TiO 2 have a size that varies between 1 and 10 microns.

26. The process of preparation according to claim 3 , wherein a quantity of Y 2 O 3 in the mixture of particles subject to grinding varies between 5 and 15 weight percent and a quantity of ZrO 2 varies between 5 and 15 weight percent.

27. The process of preparation according to claim 3 , wherein the mixture of particles of ZrO 2 and Y 2 O 3 is a mixture consisting of x weight percent of particles of ZrO 2 and (100-x) weight percent of particles of Y 2 O 3 , where

Assignees

• Hydro Quebec

Inventors

• Zaghib Karim
• Guerfi Abdelbast
• Armand Michel
• Charest Patrick

Classifications

• H01M4/485

  of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy (H01M4/505, H01M4/525 take precedence) · CPC title

• C04B2235/5454

  nanometer sized, i.e. below 100 nm · CPC title

• C01G23/005

  Alkali titanates · CPC title

• H01M4/9025

  Oxides specially used in fuel cell operating at high temperature, e.g. SOFC · CPC title

• C04B2235/5445

  submicron sized, i.e. from 0,1 to 1 micron · CPC title