IP Library Granted Patent US 8,916,505
Granted Patent B2
US 8,916,505 · App. 12/951,347 · Granted Dec 23, 2014

Cordierite having an increased alpha-cordierite phase and a proppant containing the same

Inventor: Robert D. Skala (Katy, TX)
Assignee: Oxane Materials, Inc.
C09K8/80C04B2235/96C04B2111/00612C04B35/62675C04B2235/80C04B2235/3481C04B2235/77C04B38/0074C04B35/195
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Quick Facts
Patent No.
US 8,916,505
App. No.
12/951,347
Granted
Dec 23, 2014
Kind
B2
Abstract

A cordierite material having an increased α-cordierite phase and a reduced β-cordierite phase is described. Methods of making the cordierite material are further described, and a proppant containing the cordierite is further described, as well as use of the proppant.

Claims (43)

1. A cordierite powder or sintered cordierite ceramic article comprising an α-cordierite phase and a β-cordierite phase and wherein said α-cordierite phase is present in an average amount of at least 10 wt % based on the weight percent of all cordierite phases present in said powder, and said cordierite powder has a mechanical strength of at least 70 MPa and optionally, a total pore volume of 40 vol % or less, wherein said cordierite powder has a mean particle size of from 0.3 micron to 35 microns, and

wherein said sintered cordierite ceramic article is formed from said cordierite powder, and

wherein said mechanical strength is flexural strength.

2. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said α-cordierite phase is present in an average amount of from 10 wt % to 99.9 wt %.

3. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said α-cordierite phase is present in an average amount of from 45 wt % to 85 wt %.

4. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said β-cordierite phase is present in an amount of less than 50 wt %.

5. The cordierite powder or sintered cordierite ceramic article comprising an α-cordierite phase and a β-cordierite phase and wherein said α-cordierite phase is present in an average amount of at least 10 wt % based on the weight percent of all cordierite phases present in said powder, and said cordierite powder has a mechanical strength of at least 70 MPa and optionally, a total pore volume of 40 vol % or less, wherein said β-cordierite phase is present in an amount of less than 10 wt %, and wherein said mechanical strength is flexural strength.

6. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein a μ-cordierite phase is present in an amount of 10 wt % or less.

7. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein a μ-cordierite phase is present in an amount of 1 wt % or less.

8. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein all other crystalline forms of cordierite are present in an amount of less than 40 wt %.

9. The cordierite powder or sintered cordierite ceramic article of claim 1 , having a cordierite purity of at least 90 wt %, based on the total weight percent of the cordierite powder.

10. The cordierite powder or sintered cordierite ceramic article of claim 1 , having a cordierite purity of from 90 wt % to 99.99 wt %, based on the total weight percent of the cordierite powder.

11. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein the α-cordierite phase is the largest weight percent cordierite phase present in said cordierite powder.

12. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said mechanical strength is from 70 MPa to 220 MPa.

13. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said mechanical strength is from 80 MPa to 110 MPa.

14. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said total pore volume is 1% by volume to 40% by volume.

15. The cordierite powder or sintered cordierite ceramic article of claim 1 , wherein said total pore volume is from 3% by volume to 15% by volume.

16. The cordierite powder or sintered cordierite ceramic article comprising an α-cordierite phase and a β-cordierite phase and wherein said α-cordierite phase is present in an average amount of at least 10 wt % based on the weight percent of all cordierite phases present in said powder, and said cordierite powder has a mechanical strength of at least 70 MPa and optionally, a total pore volume of 40 vol % or less, wherein said powder is agglomerated, and wherein said mechanical strength is flexural strength.

17. A sintered layer comprising said cordierite powder of claim 1 in a sintered state.

18. A proppant comprising the sintered layer of claim 17 .

19. The proppant of claim 18 , wherein said sintered layer is on a core.

20. The proppant of claim 19 , wherein said core is a hollow core.

21. The proppant of claim 19 , wherein said core is a porous core or a core having one or more voids.

22. The proppant of claim 19 , wherein said core is a solid core.

23. The proppant of claim 19 , wherein said core is a cenosphere.

24. The proppant of claim 19 , wherein said sintered layer is in direct contact with said core.

25. The proppant of claim 19 , wherein one or more intermediate layers are present between said sintered layer and said core.

26. The cordierite powder of claim 1 , further comprising at least one dopant.

27. The cordierite powder of claim 1 , further comprising a metal, metal oxide, mineral, oxide or any combination thereof.

28. A method to make the cordierite powder of claim 1 , comprising heating a starting cordierite powder having a β-cordierite phase and having an α-cordierite phase in an amount of less than said cordierite powder, to a conversion temperature sufficient to convert at least a portion of said β-cordierite phase to α-cordierite phase and form a heated powder, and then subjecting said heated powder to cooling below said conversion temperature.

29. The method of claim 28 , wherein said heating occurs in a mill, and wherein the average particle size of the cordierite powder is reduced.

30. The method of claim 29 , wherein said mill is a high-energy mill.

31. The method of claim 28 , further comprising repeating one or more times said heating step and then said cooling step.

32. The method of claim 28 , wherein at least one dopant is present in said starting cordierite powder prior to said heating.

33. The method of claim 28 , wherein said conversion temperature is from about 1,200° C. to about 1,400° C.

34. The method of claim 28 , wherein said cooling is a quenching such that the conversion temperature is reduced in an amount of from 20° C. to 1000° C. per minute until the temperature of the powder is less than at least 900 ° C.

35. The method of claim 28 , wherein said average particle size is about 0.1 to 10 microns.

36. A dense body comprising the cordierite powder of claim 1 in a sintered state, wherein the dense body has a total porosity of less than 5 vol %, based on the volume of the dense body.

37. A porous body comprising the cordierite powder of claim 1 in a sintered state, wherein the porous body has a total porosity of from about 10 vol % to about 40 vol %, based on the volume of the porous body.

38. The dense body of claim 36 , wherein the dense body has a spherical shape.

39. The porous body of claim 37 , wherein the porous body has a spherical shape.

40. The cordierite powder of claim 1 , wherein said cordierite powder has a mean particle size of from 0.3 micron to 10 microns.

41. The cordierite powder of claim 1 , wherein said cordierite powder has a mean particle size of from 0.3 micron to 5 microns.

Assignments (6)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 23, 2015
From: OXANE MATERIALS, INC.
To: HALLIBURTON ENERGY SERVICES, INC.
Reel/Frame 036174/0785 →
RELEASE OF SECURITY INTEREST Recorded Jul 9, 2015
From: COMERICA BANK
To: OXANE MATERIALS, INC.
Reel/Frame 036043/0417 →
RELEASE OF SECURITY INTEREST Recorded Jul 9, 2015
From: DELTA CENTAURI LLC
To: OXANE MATERIALS, INC.
Reel/Frame 036043/0665 →
SECURITY AGREEMENT Recorded Feb 28, 2014
From: OXANE MATERIALS, INC.
To: DELTA CENTAURI LLC
Reel/Frame 032367/0422 →
SECURITY AGREEMENT Recorded Jul 21, 2011
From: OXANE MATERIALS, INC., A DELAWARE CORPORATION
To: COMERICA BANK, A TEXAS BANKING ASSOCIATION
Reel/Frame 026627/0887 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 22, 2010
From: SKALA, ROBERT D.
To: OXANE MATERIALS, INC.
Reel/Frame 025390/0757 →
Continuity (2)
Provisional Application 61286833 · Dec 16, 2009
Related Publication 20110143969A1 · Jun 16, 2011