Methods of extracting volatiles from ceramic green bodies

Patent metadata

Field	Value
Publication number	US-12024472-B2
Application number	US-202318135348-A
Country	US
Kind code	B2
Filing date	Apr 17, 2023
Priority date	Jul 21, 2017
Publication date	Jul 2, 2024
Grant date	Jul 2, 2024

Abstract

Methods of producing a ceramic article include heating the ceramic green body containing a quantity of one or more organic materials to extract only a fraction of the organic materials from the ceramic green body by exposing the ceramic green body to a process atmosphere which is heated to a hold temperature of from 225° C. to about 400° C. and has from 2% to 7% O 2 by volume of the process atmosphere. The method further includes cooling the ceramic green body to a temperature of below 200° C., exposing the ceramic green body to a higher concentration of O 2 than in the process atmosphere of the heating step, and firing the ceramic green body to form the ceramic article. Volatile extraction units for implementing the methods are also described.

First claim

What is claimed is:

1. A method of producing a ceramic article, the method comprising:
heating a ceramic green body containing a quantity of one or more organic materials to extract at least a portion of the organic materials from the ceramic green body by exposing the ceramic green body to a process atmosphere which is heated to a hold temperature of from 100° C. to 225° C. and has from 2% to 7% O 2 by volume of the process atmosphere; then
cooling the ceramic green body to a temperature below the hold temperature;
after the ceramic green body is cooled to a temperature below the hold temperature, exposing the ceramic green body to a higher concentration of O 2 than in the process atmosphere of the heating step; and
firing the ceramic green body to form the ceramic article.

2. The method of claim 1 , wherein the heating step is performed inside a kiln.

3. The method of claim 1 , wherein the heating step and the cooling step are performed inside a kiln.

4. The method of claim 1 , wherein the step of exposing the ceramic green body to the higher concentration of O 2 is performed inside a kiln.

5. The method of claim 1 , wherein the heating step is performed inside a first kiln and the firing step is performed in a second kiln different from the first kiln.

6. The method of claim 5 , wherein a process atmosphere within the kiln in which the firing step is performed is permitted to freely fluctuate.

7. The method of claim 1 , wherein the cooling step comprises maintaining the ceramic green body in the process atmosphere containing 2% to 7% O 2 by volume.

8. The method of claim 1 , wherein at least 50% of the volatiles are extracted from the ceramic green body during the heating step.

9. The method of claim 1 , wherein a remainder of the organic materials remains in the ceramic green body after the heating step, and the remainder is removed from the ceramic green body during the firing step.

10. The method of claim 1 , wherein the firing step comprises increasing a temperature of a firing process atmosphere at a rate greater than 50° C./hr.

11. The method of claim 1 , wherein a rate of temperature increase of the process atmosphere during the heating step is limited to 200° C./hr or less.

12. The method of claim 1 , wherein the temperature of the process atmosphere in the heating step is decreased from the hold temperature after a peak lower flammability limit (LFL) has been reached in the process atmosphere.

13. The method of claim 1 , wherein the temperature of the process atmosphere in the heating step is decreased from the hold temperature after a peak lower flammability limit (LFL) has been reached in the process atmosphere and the LFL has decreased to 50% or less of the peak LFL.

14. The method of claim 1 , wherein the temperature of the process atmosphere in the heating step is decreased from the hold temperature after a target weight loss of the ceramic green body is reached.

15. The method of claim 1 , further comprising measuring lower flammability limit (LFL) in the process atmosphere and controlling the duration of exposure of the ceramic green body to the hold temperature based on LFL measurement.

16. The method of claim 1 , wherein the ceramic green body is heated for a time sufficient to volatilize at least 75% of volatiles in the organic materials.

17. The method of claim 1 , further comprising holding the ceramic green body at the hold temperature for a hold time of ≥0 hours to 4 hours.

18. The method of claim 1 , further comprising measuring a lower flammability limit in the process atmosphere, wherein heating the ceramic green body comprises heating the ceramic green body for a time sufficient for the lower flammability limit to reach a peak level.

19. The method of claim 18 , wherein heating the ceramic green body comprises heating the ceramic green body for a time sufficient for the lower flammability limit to decrease to an amount of at least 50% of the peak level.

20. The method of claim 1 , wherein from 30 wt % to 50 wt % of the organic materials are extracted from the ceramic green body upon completion of the heating.

Assignees

• Corning Inc

Inventors

• Wing Douglas Richard

Classifications

• C04B2235/6584

  at an oxygen percentage below that of air · CPC title

• C04B2235/6567

  Treatment time · CPC title

• C04B2235/6562

  Heating rate · CPC title

• C04B35/6365

  Cellulose or derivatives thereof · CPC title

• C04B2235/6583

  Oxygen containing atmosphere, e.g. with changing oxygen pressures · CPC title