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

Patent metadata

Field	Value
Publication number	US-9499407-B2
Application number	US-201113824125-A
Country	US
Kind code	B2
Filing date	Sep 29, 2011
Priority date	Sep 29, 2010
Publication date	Nov 22, 2016
Grant date	Nov 22, 2016

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.

First claim

The invention claimed is:

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.

Assignees

• Sailor Michael J
• Kelly Timothy
• Univ California

Inventors

• Sailor Michael J
• Kelly Timothy

Classifications

• C01B32/16 Primary

  Preparation · CPC title

• B82B1/00

  Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units · CPC title

• Y10T428/249994

  Composite having a component wherein a constituent is liquid or is contained within preformed walls [e.g., impregnant-filled, previously void containing component, etc.] · CPC title

• D01D5/00

  Formation of filaments, threads, or the like · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title