IP Library Granted Patent US 9,499,407
Granted Patent B2
US 9,499,407 · App. 13/824,125 · Granted Nov 22, 2016

Carbon and carbon/silicon composite nanostructured materials and casting formation method

Inventors: Michael J. Sailor (La Jolla, CA); Timothy Kelly (San Diego, CA)
Assignee: The Regents of the University of California
C01B31/022B82Y30/00B82Y40/00C01B31/0226C01B31/0246D01D5/00D01F9/14G02B1/005B82B1/00Y10T428/249994Y10T428/2918
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Quick Facts
Patent No.
US 9,499,407
App. No.
13/824,125
Granted
Nov 22, 2016
Kind
B2
Abstract

The invention provides nanostructure composite porous silicon and carbon materials, and also provides carbon nanofiber arrays having a photonic response in the form of films or particles. Composite materials or carbon nanofiber arrays of the invention are produced by a templating method of the invention, and the resultant nanomaterials have a predetermined photonic response determined by the pattern in the porous silicon template, which is determined by etching conditions for forming the porous silicon. Example nanostructures include rugate filters, single layer structures and double layer structures. In a preferred method of the invention, a carbon precursor is introduced into the pores of a porous silicon film. Carbon is then formed from the carbon precursor. In a preferred method of the invention, liquid carbon-containing polymer precursor is introduced into the pores of an porous silicon film The precursor is thermally polymerized to form a carbon-containing polymer in the pores of the porous silicon film, which is then thermally carbonized to produce the nano structured composite material. A carbon nanofiber array is obtained by dissolving the porous silicon. A carbon nanofiber array can be maintained as a film in liquid, and particles can be formed by drying the material.

Claims (34)

1. A method for forming a nanostructured material, comprising:

introducing a carbon precursor into the pores of a porous silicon film; and

forming carbon from the carbon precursor in the pores of the porous silicon film to form a carbon-silicon nanostructured material, wherein said carbon precursor comprises liquid, carbon-containing, polymer precursor, and said forming comprises:

thermally polymerizing the liquid, carbon-containing polymer precursor to form a carbon-containing polymer in the pores of the porous silicon film; and

thermally carbonizing the carbon-containing polymer to produce the carbon-silicon nanostructured material.

2. The method of claim 1 , wherein the liquid, carbon-containing, polymer precursor comprises oxalic acid in furfuryl alcohol.

3. The method of claim 2 , wherein said introducing comprises immersing the porous silicon film in the liquid, carbon-containing, polymer precursor.

4. The method of claim 1 , wherein said thermally carbonizing is conducted under flowing nitrogen.

5. The method of claim 1 , further comprising a preliminary step of electrochemically etching a highly doped, p-type, silicon wafer, to create a porous silicon film and then oxidizing the porous silicon film.

6. The method of claim 5 , wherein said oxidizing comprises oxidizing the porous silicon wafer in ozone.

7. A method of forming a free-standing carbon nanofiber array, comprising:

performing the method of claim 1 , and

releasing the carbon from the nanostructured material by dissolving the porous silicon film to form the free-standing carbon nanofiber array.

8. A method of forming a free-standing carbon nanofiber array, comprising:

introducing a carbon precursor into the pores of a porous silicon film;

forming carbon from the carbon precursor in the pores of the porous silicon film to form a carbon-silicon nanostructured material, and

releasing the carbon from the nanostructured material by dissolving the porous silicon film to form the free-standing carbon nanofiber array.

9. The method of claim 8 , further comprising rinsing the carbon nanofiber array.

10. The method of claim 9 , further comprising maintaining the carbon nanofiber array as a film in liquid.

11. The method of claim 8 , further comprising drying the carbon nanofiber array to form carbon nanofiber particles.

12. The method of claim 8 , wherein said releasing comprises soaking in a solution of dimethylsulfoxide, aqueous hydrofluoric acid, and ethanol.

13. A method for forming a nanostructured material, comprising:

introducing a carbon precursor into the pores of a porous silicon film; and

forming carbon from the carbon precursor in the pores of the porous silicon film to form a carbon-silicon nanostructured material, wherein said introducing comprises filling the pores of the porous silicon with a solution of oxalic acid in furfuryl alcohol, followed by thermal polymerization of the furfuyl alcohol and carbonization of a resultant poly(furfuryl alcohol) resin to form the carbon-silicon nanostructured material with carbon in the pores of the porous silicon.

14. A method for forming a free-standing carbon nanofiber array, comprising:

introducing a carbon precursor into the pores of a porous silicon film;

forming carbon from the carbon precursor in the pores of the porous silicon film to form a carbon-silicon nanostructured material, wherein said introducing comprises filling the pores of the porous silicon with a solution of oxalic acid in furfuryl alcohol, followed by thermal polymerization of the furfuyl alcohol and carbonization of a resultant poly(furfuryl alcohol) resin to form the carbon-silicon nanostructured material with carbon in the pores of the porous silicon; and

further comprising releasing a free standing carbon nanofiber array by dissolving the porous silicon in solution.

15. The method of claim 14 , further comprising rinsing the carbon nanofiber array.

16. The method of claim 15 , further comprising maintaining the carbon nanofiber array as a film in liquid.

17. The method of claim 14 , further comprising drying the carbon nanofiber array to form carbon nanofiber particles.

18. The method of claim 14 , wherein said releasing comprises soaking in a solution of dimethylsulfoxide, aqueous hydrofluoric acid, and ethanol.

19. The method of claim 14 , wherein the porous silicon film comprises an oxidized porous silicon film.

20. The method of claim 19 , comprising a preliminary step of ozone oxidizing a freshly etched porous silicon film to form the oxidized porous silicon film.

Assignments (2)
CONFIRMATORY LICENSE Recorded May 22, 2020
From: UNIVERSITY OF CALIFORNIA, SAN DIEGO
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 052743/0681 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 30, 2013
From: SAILOR, MICHAEL J.; KELLY, TIMOTHY L.
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 030512/0032 →
Continuity (2)
Provisional Application 61387566 · Sep 29, 2010
Related Publication 20130309484A1 · Nov 21, 2013