Method of producing metal oxide nanorods

• US 6,036,774 A
• Filed: 01/22/1997
• Issued: 03/14/2000
• Est. Priority Date: 02/26/1996
• Status: Expired due to Term

• Current Assignee: President and Fellows of Harvard College (Harvard Corporation)
• Original Assignee: President and Fellows of Harvard College (Harvard Corporation)
• Inventors: Yang, Peidong, Lieber, Charles M.
• Primary Examiner(s): KUNEMUND, ROBERT M
• Application Number:
  US08/790,824
• Time in Patent Office: 1,147 Days
• Field of Search: 117/84, 117/105, 117/106, 117/109, 117/921
• US Class Current: 117/105
• CPC Class Codes: C30B 23/00 Single-crystal growth by condensing evaporated or sublimed materials
• CPC Class Codes: C30B 29/16 Oxides
• CPC Class Codes: C30B 29/605 Products containing multiple oriented crystallites, e.g. columnar crystallites
• CPC Class Codes: H10N 60/85 Superconducting active materials
• CPC Class Codes: H10N 60/857 comprising copper oxide

Abstract

Methods of preparing metal oxide nanorods are described. The metal oxide nanorods have diameters between 1 and 200 nm and aspect ratios between 5 and 2000. The methods include the steps of generating a metal vapor in a furnace, exposing the nanorod growth substrate to the metal vapor within a growth zone in the furnace for a sufficient time to grow metal oxide nanorods on a surface of the nanorod growth substrate, removing the nanorod growth substrate from the growth zone after the sufficient time to grow metal oxide nanorods on a surface of the nanorod growth substrate, and removing the metal oxide nanorods from the furnace. The methods can be used to prepared large quantities of metal oxide nanorods.

Claims

1. A method of producing metal oxide nanorods comprising:

generating a metal vapor in a furnace;

exposing a nanorod growth substrate to the metal vapor within a growth zone in the furnace for a sufficient time to form metal oxide nanorods on a surface of the nanorod growth substrate;

removing the nanorod growth substrate from the growth zone; and

collecting the metal oxide nanorods thus formed, each nanorod having a diameter between 1 and 200 nm.

2. The method of claim 1, wherein the growth zone is a region within a 100°

C. temperature drop between a location of highest metal vapor concentration and a location of the substrate.

3. The method of claim 1, wherein the nanorod growth substrate is a metal oxide nanocluster, a single crystal, graphite, or a metal coated substrate.

4. The method of claim 3, wherein the growth zone is a region within a 100°

C. temperature drop between a location of highest metal vapor concentration and a location of the substrate.

5. The method of claim 4, wherein the metal vapor source comprises magnesium.

6. The method of claim 5, further comprising mechanically separating the metal oxide nanorods from the substrate.

7. The method of claim 5, wherein the nanorod growth substrate is graphite.

8. The method of claim 7, further comprising purifying the metal oxide nanorods by heating the metal oxide nanorods in an oxidizing atmosphere to convert the graphite to carbon dioxide.

9. The method of claim 1, further comprising the step of moving the nanorod growth substrate through the growth zone during the exposing step.

33. The method of claim 1, wherein said metal oxide nanorod is aligned relative to a surface of the substrate.

10. A method of producing metal oxide nanorods comprising:

placing a metal vapor source in a furnace;

providing a nanorod growth substrate in the furnace;

heating the metal vapor source to a temperature between 500°

C. and 1600°

C.;

maintaining the temperature for a sufficient time to form metal oxide nanorods on a surface of the nanorod growth substrate; and

collecting the metal oxide nanorods thus formed, each nanorod having a diameter between 1 and 200 nm.

11. The method of claim 10, further comprising flowing a carrier gas through the furnace.

12. The method of claim 11, wherein providing the nanorod growth substrate comprises placing the nanorod growth substrate downstream of the metal vapor source.

13. The method of claim 10, wherein providing the nanorod growth substrate comprises placing the nanorod growth substrate within a growth zone.

14. The method of claim 13, wherein the growth zone is a region within a 100°

C. temperature gradient drop between the metal vapor source and the substrate when heated to the temperature between 500°

C. and 1600°

C.

15. The method of claim 14, further comprising removing the nanorod growth substrate from the growth zone after the sufficient time to form metal oxide nanorods on a surface of the nanorod growth substrate.

16. The method of claim 15, further comprising mechanically separating the metal oxide nanorods from the substrate.

17. The method of claim 15, wherein the nanorod growth substrate is graphite.

18. The method of claim 17, further comprising purifying the metal oxide nanorods by heating the metal oxide nanorods in an oxidizing atmosphere to convert the graphite to carbon dioxide.

19. The method of claim 18, wherein the metal oxide is magnesium oxide.

20. The method of claim 15, further comprising moving the nanorod growth substrate through the growth zone during the sufficient time to form the metal oxide nanorods.

21. The method of claim 10, further comprising cooling the metal vapor source to stop the formation of the metal oxide nanorods.

22. The method of claim 10, wherein the metal vapor source comprises an elemental metal or a mixture of metal oxide and carbon, wherein the metal is selected from the group consisting of titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, manganese, technetium, rhenium, iron, osmium, cobalt, nickel, copper, zinc, scandium, yttrium, lanthanum, a lanthanide series element, boron, aluminum, gallium, indium, thallium, silicon, germanium, tin, lead, magnesium, calcium, strontium, and barium.

23. The method of claim 10, wherein the nanorod growth substrate comprises a metal oxide nanocluster, a surface of the metal vapor source, a single crystal, graphite, or a metal coated substrate.

24. The method of claim 22, wherein said metal oxide is magnesium oxide.

34. The method of claim 10, wherein said metal oxide nanorod is aligned relative to a surface of the substrate.

25. A method of producing magnesium oxide nanorods comprising:

placing a magnesium vapor source in a furnace;

providing a nanorod growth substrate in the furnace;

generating a magnesium vapor in the furnace by heating the magnesium vapor source to a temperature between 500°

C. and 1600°

C.;

exposing the nanorod growth substrate to the magnesium vapor within a growth zone in the furnace for a sufficient time to form magnesium oxide nanorods on a surface of the nanorod growth substrate, the growth zone being a region in the furnace within a 100°

C. temperature drop of the magnesium vapor source;

removing the nanorod growth substrate from the growth zone after the sufficient time to grow metal oxide nanorods on a surface of the nanorod growth substrate; and

collecting the magnesium oxide nanorods thus formed.

26. The method of claim 25, wherein the nanorod growth substrate is graphite, metal coated substrate, a surface of the magnesium vapor source, or a magnesium oxide nanocluster.

27. The method of claim 26, wherein the nanorod growth substrate is graphite.

28. The method of claim 27, further comprising purifying the metal oxide nanorods by heating the metal oxide nanorods in an oxidizing atmosphere to convert the graphite to carbon dioxide.

29. The method of claim 28, further comprising moving the nanorod growth substrate through the growth zone during the exposing step.

30. The method of claim 29, further comprising mechanically separating the metal oxide nanorods from the substrate.

31. A method of producing metal oxide nanorods comprising:

generating a metal vapor in a furnace;

exposing a nanorod growth substrate to the metal vapor within a growth zone in the furnace for a sufficient time to form metal oxide nanorods on a surface of the nanorod growth substrate;

removing the nanorod growth substrate from the growth zone; and

collecting the metal oxide nanorods thus formed, wherein said metal oxide is magnesium oxide.

32. A method of producing metal oxide nanorods comprising:

placing a metal vapor source in a furnace;

providing a nanorod growth substrate in the furnace;

heating the metal vapor source to a temperature between 500°

C. and 1600°

C.;

maintaining the temperature for a sufficient time to form metal oxide nanorods on a surface of the nanorod growth substrate; and

collecting the metal oxide nanorods thus formed, wherein said metal oxide is magnesium oxide.