Methods of increasing the solubility of materials in supercritical carbon dioxide

Patent metadata

Field	Value
Publication number	US-9676944-B2
Application number	US-201414571525-A
Country	US
Kind code	B2
Filing date	Dec 16, 2014
Priority date	Mar 9, 2005
Publication date	Jun 13, 2017
Grant date	Jun 13, 2017

Abstract

Methods of increasing the solubility of a base in supercritical carbon dioxide include forming a complex of a Lewis acid and the base, and dissolving the complex in supercritical carbon dioxide. The Lewis acid is soluble in supercritical carbon dioxide, and the base is substantially insoluble in supercritical carbon dioxide. Methods for increasing the solubility of water in supercritical carbon dioxide include dissolving an acid or a base in supercritical carbon dioxide to form a solution and dissolving water in the solution. The acid or the base is formulated to interact with water to solubilize the water in the supercritical carbon dioxide. Some compositions include supercritical carbon dioxide, a hydrolysable metallic compound, and at least one of an acid and a base. Some compositions include an alkoxide and at least one of an acid and a base.

First claim

What is claimed is:

1. A method of increasing the solubility of a base in supercritical carbon dioxide, comprising:
forming a complex of a Lewis acid and a base, wherein the Lewis acid is soluble in supercritical carbon dioxide, and the base is substantially insoluble in supercritical carbon dioxide; and
dissolving the complex in superciitical carbon dioxide.

2. The method of claim 1 , wherein forming a complex of a Lewis acid and a base comprises reacting the Lewis acid with a base selected from the group consisting of an organic amine, a substituted pyridine, a fluoroamine, potassium hydroxide, and sodium hydroxide.

3. A method for increasing the solubility of water in supercritical carbon dioxide, comprising:
dissolving an acid or a base in supercritical carbon dioxide to form a solution, wherein the acid or the base is formulated to interact with water to solubilize the water in the supercritical carbon dioxide: and
dissolving water in the solution.

4. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide comprises dissolving an acid complexed with tributyl phosphate in the supercritical carbon dioxide.

5. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide comprises dissolving an acid selected from the group consisting of acetic acid, formic acid, citric acid, hydrofluoric acid, hydrochloric acid, nitric acid, sulfuric acid, and phosphoric acid.

6. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide comprises dissolving acetic acid in the supercritical carbon dioxide.

7. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide comprises dissolving a base selected from the group consisting of ammonia, an organic amine, pyridine, a substituted pyridine, a fluoroamine, and a hydroxide.

8. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide comprises dissolving ammonia in the supercritical carbon dioxide.

9. The method of claim 3 , further comprising combining the solution with a hydrolyzable alkoxide.

10. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide to form a solution comprises forming a complex comprising at least one of a Lewis acid and a Lewis base.

11. The method of claim 3 , wherein dissolving an acid or a base in supercritical carbon dioxide to form a solution comprises dissolving at least one material in the supercritical carbon dioxide, wherein the at least one material alone is insoluble in supercritical carbon dioxide.

12. The method of claim 1 , wherein forming a complex of a Lewis acid and a base comprises forming a complex of the base and the Lewis acid selected from the group consisting of acetic acid, formic acid, citric acid, and combinations thereof.

13. The method of claim 1 , further comprising maintaining a temperature of the supercritical carbon dioxide at less than about 150° C.

14. A method comprising:
combining supercritical carbon dioxide, a base that is soluble in the supercritical carbon dioxide, and an acid that is substantially insoluble in the supercritical carbon dioxide to form a supercritical carbon dioxide solution comprising a complex of the base and the acid, the complex soluble in the supercritical carbon dioxide;
combining the supercritical carbon dioxide solution with a hydrolyzable alkoxide; and
reacting the hydrolyzable alkoxide with water to form a solid material.

15. The method of claim 14 , wherein reacting the hydrolyzable alkoxide with water to form a solid material comprises forming a solid material that is insoluble in the supercritical carbon dioxide solution.

16. The method of claim 14 , wherein forming the solid material comprises forming a material having a dielectric constant of less than about 3.

17. The method of claim 14 , wherein combining supercritical carbon dioxide, a base, and an acid comprises combining supercritical carbon dioxide, a Lewis base, and an acid.

18. The method of claim 14 , further comprising dissolving water in the supercritical carbon dioxide solution.

19. The method of claim 18 , wherein dissolving water in the supercritical carbon dioxide solution comprises dissolving water in the supercritical carbon dioxide solution at a higher concentration than a solubility limit of water in supercritical carbon dioxide alone.

20. The method of claim 14 , further comprising maintaining a temperature of the supercritical carbon dioxide solution at less than about 150° C.

Assignees

• Micron Technology Inc
• Univ Of Idaho
• Idaho Res Found

Inventors

• Wai Chien M
• Ohde Hiroyuki
• Kramer Stephen J

Classifications

• H10P70/80

  Cleaning only by supercritical fluids · CPC title

• H10P14/69215

  the material being a silicon oxide, e.g. SiO2 · CPC title

• H10P14/6939

  characterised by the metal · CPC title

• H10P14/6922

  the material containing Si, O and at least one of H, N, C, F or other non-metal elements, e.g. SiOC, SiOC:H or SiONC · CPC title

• H10P14/6903

  containing silicon · CPC title