Metallic crucibles and methods of forming the same

Patent metadata

Field	Value
Publication number	US-9457405-B2
Application number	US-201313799796-A
Country	US
Kind code	B2
Filing date	Mar 13, 2013
Priority date	May 29, 2012
Publication date	Oct 4, 2016
Grant date	Oct 4, 2016

Abstract

In various embodiments, a precursor powder is pressed into an intermediate volume and chemically reduced, via sintering, to form a metallic shaped article.

First claim

What is claimed is:

1. A method of fabricating a shaped article having a target set of final dimensions and consisting essentially of at least one metal, the method comprising:
pressing a precursor powder into a volume having intermediate dimensions larger than the final dimensions along at least one direction, the precursor powder comprising a compound comprising (i) the at least one metal and (ii) a non-metallic chemical species; and
thereafter, sintering the pressed precursor powder to (i) chemically reduce the precursor powder, (ii) shrink the volume having intermediate dimensions into the shaped article having the final dimensions, and (iii) release a non-metallic by-product,
wherein sintering the pressed precursor powder comprises:
sintering at a first temperature selected from the range of approximately 450° C. to approximately 650° C. for a first time selected from the range of approximately 4 hours to approximately 6 hours;
thereafter, sintering at a second temperature selected from the range of approximately 500° C. to approximately 700° C. for a second time selected from the range of approximately 5 hours to approximately 7 hours;
thereafter, sintering at a third temperature selected from the range of approximately 800° C. to approximately 1000° C. for a third time selected from the range of approximately 1 hour to approximately 5 hours; and
thereafter, sintering at a fourth temperature selected from the range of approximately 1450° C. to approximately 1800° C. for a fourth time selected from the range of approximately 6 hours to approximately 25 hours.

2. The method of claim 1 , wherein the non-metallic species comprises at least one of oxygen or ammonium.

3. The method of claim 1 , wherein the at least one metal comprises molybdenum.

4. The method of claim 1 , wherein the precursor powder comprises ammonium dimolybdate.

5. The method of claim 1 , wherein the volume shrinkage from the intermediate dimensions to the final dimensions is within the range of approximately 50% to approximately 70%.

6. The method of claim 1 , wherein the precursor powder is pressed by cold isostatic pressing.

7. The method of claim 1 , wherein each of at least two of the sintering stages comprises chemical reduction of the pressed powder to a different intermediate product.

8. The method of claim 1 , wherein the shaped article has a density ranging between approximately 90% and approximately 95% after sintering.

9. The method of claim 1 , wherein the sintering is performed in an atmosphere comprising hydrogen.

10. The method of claim 1 , wherein the shaped article comprises a crucible.

11. The method of claim 1 , wherein the by-product comprises at least one of ammonia, oxygen, or water vapor.

12. The method of claim 1 , further comprising, after sintering the pressed precursor powder:
cooling the shaped article to a fifth temperature less than the fourth temperature and greater than 100° C.; and
holding the shaped article at the fifth temperature (i) for a fifth time selected from the range of approximately 1 hour to approximately 8 hours and (ii) within an ambient comprising hydrogen.

13. The method of claim 12 , further comprising, after holding the shaped article at the fifth temperature for the fifth time, holding the shaped article at a sixth temperature less than the fourth temperature and greater than 100° C. (i) for a sixth time selected from the range of approximately 1 hour to approximately 8 hours and (ii) within an ambient comprising nitrogen.

14. The method of claim 13 , wherein the fifth temperature is approximately equal to the sixth temperature.

15. The method of claim 1 , further comprising disposing an additive on at least one surface of the shaped article.

16. The method of claim 15 , further comprising annealing the shaped article, thereby at least one of alloying or mixing the additive with the at least one metal to form a treated article.

17. The method of claim 16 , wherein the treated article comprises (i) an inner layer comprising an alloy or mixture of the additive and the at least one metal, (ii) an outer layer consisting essentially of the at least one metal, and (iii) therebetween, a zone comprising a graded concentration of the alloy or mixture of the additive and the at least one metal.

18. The method of claim 16 , wherein the at least one surface of the treated article comprises an alloy of the at least one metal and the additive.

19. The method of claim 16 , wherein a concentration of the additive varies as a function of thickness of the treated article.

20. The method of claim 19 , wherein the concentration of the additive is graded.

21. The method of claim 16 , wherein a portion of a thickness of the treated article is substantially free of the additive.

22. The method of claim 16 , wherein a grain size of the treated article is approximately equal to a grain size of the shaped article.

23. The method of claim 15 , wherein the additive comprises at least one of tungsten or copper.

24. The method of claim 15 , wherein the additive is a powder.

25. The method of claim 24 , wherein disposing the additive comprises at least one of sprinkling, applying a slurry, or spray deposition.

26. A method of fabricating a shaped article having a target set of final dimensions and consisting essentially of at least one metal, the method comprising:
pressing a precursor powder into a volume having intermediate dimensions larger than the final dimensions along at least one direction, the precursor powder comprising a compound comprising (i) the at least one metal and (ii) a non-metallic chemical species; and
thereafter, sintering the pressed precursor powder to (i) chemically reduce the precursor powder, (ii) shrink the volume having intermediate dimensions into the shaped article having the final dimensions, and (iii) release a non-metallic by-product,
wherein sintering the pressed precursor powder comprises:
sintering at a first temperature selected from the range of approximately 450° C. to approximately 650° C. for a first time selected from the range of approximately 4 hours to approximately 6 hours;
thereafter, sintering at a second temperature greater than the first temperature and less than approximately 700° C. for a second time selected from the range of approximately 5 hours to approximately 7 hours;
thereafter, sintering at a third temperature greater than the second temperature and less than approximately 1000° C. for a third time selected from the range of approximately 1 hour to approximately 5 hours; and
thereafter, sintering at a fourth temperature greater than the third temperature and less than approximately 1800° C. for a fourth time selected from the range of approximately 6 hours to approximately 25 hours.

27. The method of claim 26 , wherein the non-metallic species comprises at least one of oxygen or ammonium.

28. The method of claim 26 , wherein the at least one metal comprises molybdenum.

29. The method of claim 26 , wherein the precursor powder comprises ammonium dimolybdate.

30. The method of claim 26 , wherein the volume shrinkage from the intermediate dimensions to the final dimensions is within the range of approximately 50% to approximately 70%.

31. The method of claim 26 , wherein the precursor powder is pressed by cold isostatic pressing.

Assignees

• Winnicka Maria Bozena
• Rozak Gary A
• Starck H C Inc

Inventors

• Winnicka Maria Bozena
• Rozak Gary A

Classifications

• B22F3/1017

  Multiple heating or additional steps (B22F3/101 takes precedence) · CPC title

• B22F7/06

  of composite workpieces or articles from parts, e.g. to form tipped tools {(B22F7/002 takes precedence)} · CPC title

• B22F3/001

  Starting from powder comprising reducible metal compounds (making ferrous alloys starting from compounds C22C33/0235) · CPC title

• B22F2998/10

  Processes characterised by the sequence of their steps · CPC title

• C30B15/10

  Crucibles or containers for supporting the melt · CPC title