7 125 453

7,125,453 Title:

High temperature high pressure capsule for processing materials in supercritical fluids

A capsule for containing at least one reactant and a supercritical fluid in a substantially air-free environment under high pressure, high temperature processing conditions. The capsule includes a closed end, at least one wall adjoining the closed end and extending from the closed end; and a sealed end adjoining the at least one wall opposite the closed end. The at least one wall, closed end, and sealed end define a chamber therein for containing the reactant and a solvent that becomes a supercritical fluid at high temperatures and high pressures. The capsule is formed from a deformable material and is fluid impermeable and chemically inert with respect to the reactant and the supercritical fluid under processing conditions, which are generally above 5 kbar and 550.degree. C. and, preferably, at pressures between 5 kbar and 80 kbar and temperatures between 550.degree. C. and about 1500.degree. C. The invention also includes methods of filling the capsule with the solvent and sealing the capsule, as well as an apparatus for sealing the capsule.

What is claimed is:

1. An apparatus, comprising: a deformable capsule that comprises a closed end structure, a wall, and a sealable end structure, and which defines a chamber configured toreceive a material and a solvent, wherein the wall adjoins the closed end and extends therefrom, and the sealable end structure adjoins the wall opposite the closed end structure, and the solvent is capable of becoming supercritical at a predeterminedtemperature to provide a predetermined pressure in the chamber, and the predetermined pressure is greater than about 5 kbar and is sufficient to deform the capsule, wherein the sealable end structure is operable to seal the chamber such that the capsuleis impermeable to supercritical solvent at the predetermined temperature and predetermined pressure; and a zero-stroke pressure device configured to receive the capsule and operable to counterbalance the predetermined pressure generated within thechamber by the supercritical solvent at the predetermined temperature.

2. The apparatus as defined in claim 1, wherein the zero-stroke pressure device is operable to only counterbalance the predetermined pressure.

3. The apparatus as defined in claim 1, wherein the predetermined temperature is at least about 550 degrees Celsius.

4. The apparatus as defined in claim 1, wherein the capsule comprises one or more of copper, gold, silver, palladium, platinum, iridium, ruthenium, rhodium, osmium, iron, nickel, titanium, vanadium, chromium, zirconium, niobium, molybdenum,tantalum, tungsten, or rhenium.

5. The apparatus as defined in claim 1, wherein the capsule comprises one or more of copper-based alloy, iron-based alloy, or nickel-based alloy.

6. The apparatus as defined in claim 1, wherein the capsule comprises a lid, and the lid is operable to sealingly engage the sealable end structure.

7. The apparatus as defined in claim 6, wherein the lid has a first pipe thread, and the sealable end structure has a second pipe thread configured to engage the first pipe thread, and the lid is sealable to the wall at the sealable endstructure by a pipe thread seal.

8. The apparatus as defined in claim 6, further comprising a compression fitting, and wherein the lid is sealable to the wall at the sealable end structure by a metal-to-metal compression seal formed by the compression fitting.

9. The apparatus as defined in claim 6, further comprising a gasket, and wherein the lid is sealable to the wall at the sealable end structure by a gasket seal formed by the gasket.

10. The apparatus as defined in claim 6, wherein the lid is sealable to the wall by a weld seal.

11. The apparatus as defined in claim 6, wherein the lid is cold-weldable.

12. The apparatus as defined in claim 6, wherein lid is hot-weldable.

13. The apparatus as defined in claim 12, wherein the lid is operable to be welded by one or more of torch welding, arc welding, ultrasound welding, or vibratory welding.

14. The apparatus as defined in claim 6, wherein the lid comprises one or more of copper, gold, silver, palladium, platinum, iridium, ruthenium, rhodium, osmium, titanium, vanadium, chromium, iron, nickel, zirconium, niobium, molybdenum,tantalum, tungsten, rhenium, silicon, or aluminum.

15. The apparatus as defined in claim 14, wherein the lid comprises a fill tube, and the fill tube comprise at least one of copper, copper-based alloy, gold, silver, palladium, platinum, iridium, ruthenium, rhodium, osmium, titanium, vanadium,chromium, iron, iron-based alloy, nickel-based alloy, zirconium, niobium, molybdenum, tantalum, tungsten, rhenium, silica, alumina, or combinations thereof.

16. The apparatus as defined in claim 15, wherein the till tube is cold-weldable.

17. The apparatus as defined in claim 1, further comprising a coating disposed on an inner surface of the capsule, and the coating comprises one or more of nickel, rhodium, gold, silver, palladium, platinum, ruthenium, iridium, tantalum,tungsten, or rhenium, and the coating and the first capsule are formed from different compositions.

18. The apparatus as defined in claim 17, wherein the coating has a thickness in a range of from about 0.5 micron to about 250 microns.

19. The apparatus as defined in claim 1, further comprising a liner disposed on an inner surface of the capsule.

20. The apparatus as defined in claim 19, wherein the liner has a thickness in a range of from about 10 microns to about 5 millimeters.

21. The apparatus as defined in claim 19, further comprising a diffusion barrier disposed within the capsule between the liner and the capsule inner surface.

22. The apparatus as defined in claim 1, wherein each of the wall, the closed end structure, and the sealable end structure has a thickness in a range of from about 0.2 millimeters to about 10 millimeters.

23. The apparatus as defined in claim 1, further comprising a baffle, wherein the chamber is divided into two regions by the baffle.

24. The apparatus as defined in claim 23, wherein the baffle has a fractional open area in a range of from about 0.5% to about 30%.

25. An apparatus, comprising: a first capsule that comprises a closed end structure, a wall, and a sealable end structure, and which defines a chamber, wherein the wall adjoins the closed end and extends therefrom; and the sealable endstructure adjoins the wall opposite the closed end structure, and the chamber is configured to receive a material and a solvent, and the solvent is capable of becoming supercritical at a predetermined temperature to provide a predetermined pressure inthe chamber; and a second capsule comprising a malleable metal and being operable to deform in response to the predetermined pressure, and the first capsule being disposed within the second capsule; and a zero-stroke pressure device configured toreceive the second capsule and operable only to counterbalance the predetermined pressure generated within the chamber by the supercritical solvent at the predetermined temperature.

26. The apparatus as defined in claim 25, wherein the first capsule or the second capsule comprises one or more of copper, gold, silver, palladium, platinum, iridium, ruthenium, rhodium, osmium, iron, nickel, titanium, vanadium, chromium,zirconium, niobium, molybdenum, tantalum, tungsten, or rhenium.

27. The apparatus as defined in claim 25, wherein the first capsule comprises fused silica.

28. The apparatus as defined in claim 25, wherein the first capsule comprises quartz glass.

29. The apparatus as defined in claim 25, wherein the first capsule comprises one or more of borosilicate glass, aluminosilicate glass, soda lime glass, soda barium glass, soda zinc glass, lead glass, potash soda lead glass, potash lead glass,or potash soda barium glass.

30. The apparatus as defined in claim 25, further comprising a pressure medium disposed within the second capsule and outside of the first capsule.

31. The apparatus as defined in claim 30, wherein the pressure medium comprises one or more of water, carbon dioxide, or ammonia.

32. The apparatus as defined in claim 25, wherein the first capsule comprises a lid, and the lid is operable to sealingly engage the sealable end structure.

33. The apparatus as defined in claim 32, wherein the lid has a first pipe thread, and the sealable end structure has a second pipe thread configured to engage the first pipe thread, and the lid is sealable to the wall at the sealable endstructure by a pipe thread seal.

34. The apparatus as defined in claim 32, further comprising a compression fitting, and wherein the lid is sealable to the wall at the sealable end structure by a metal-to-metal compression seal formed by the compression fitting.

35. The apparatus as defined in claim 32, further comprising a gasket, and wherein the lid is sealable to the wall at the sealable end structure by a gasket seal formed by the gasket.

36. The apparatus as defined in claim 32, wherein the lid is sealable to the wall by a weld seal.

37. The apparatus as defined in claim 36, wherein the lid is cold-weldable.

38. The apparatus as defined in claim 36, wherein lid is hot-weldable.

39. The apparatus as defined in claim 38, wherein the lid is operable to be welded by one or more of torch welding, arc welding, ultrasound welding, or vibratory welding.

40. The apparatus as defined in claim 32, wherein the lid comprises one or more of copper, gold, silver, palladium, platinum, iridium, ruthenium, rhodium, osmium, titanium, vanadium, chromium, iron, nickel, zirconium, niobium, molybdenum,tantalum, tungsten, rhenium, silicon, or aluminum.

41. The apparatus as defined in claim 40, wherein the lid comprises a fill tube, and the fill tube comprise at least one of copper, copper-based alloy, gold, silver, palladium, platinum, iridium, ruthenium, rhodium, osmium, titanium, vanadium,chromium, iron, iron-based alloy, nickel-based alloy, zirconium, niobium, molybdenum, tantalum, tungsten, rhenium, silica, alumina, or combinations thereof.

42. The apparatus as defined in claim 25, further comprising a coating disposed on an inner surface of the first capsule, and the coating comprises one or more of nickel, rhodium, gold, silver, palladium, platinum, ruthenium, iridium, tantalum,tungsten, or rhenium, and the coating and the first capsule are formed from different compositions.

43. The apparatus as defined in claim 42, wherein the coating has a thickness in a range of from about 0.5 micron to about 250 microns.

44. The apparatus as defined in claim 25, further comprising a liner disposed on an inner surface of the first capsule.

45. The apparatus as defined in claim 44, wherein the liner has a thickness in a range of from about 10 microns to about 5 millimeters.

46. The apparatus as defined in claim 44, further comprising a diffusion barrier disposed within the first capsule between the liner and the first capsule inner surface.

47. The apparatus as defined in claim 25, wherein each of the wall, the closed end structure, and said sealable end structure has a thickness in a range of from about 0.2 millimeters to about 10 millimeters.

48. The apparatus as defined in claim 25, further comprising a baffle, wherein the chamber is divided into two regions by the baffle.

49. The apparatus as defined in claim 48, wherein the baffle has a fractional open area in a range of from about 0.5% to about 30%.

50. An article comprising the apparatus as defined in claim 25, wherein the sealable end structure is sealed such that the first capsule is impermeable to at least one supercritical fluid.