WO2003011755B1 - Production of carbon nanotubes - Google Patents

Production of carbon nanotubes

Info

Publication number
WO2003011755B1
WO2003011755B1 PCT/GB2002/003438 GB0203438W WO03011755B1 WO 2003011755 B1 WO2003011755 B1 WO 2003011755B1 GB 0203438 W GB0203438 W GB 0203438W WO 03011755 B1 WO03011755 B1 WO 03011755B1
Authority
WO
WIPO (PCT)
Prior art keywords
substrate
plasma
catalyst
carbon
carbon nanotubes
Prior art date
Application number
PCT/GB2002/003438
Other languages
French (fr)
Other versions
WO2003011755A1 (en
Inventor
Professor Sembukutiarach Silva
Sajad Haq
Bojan O Boskovic
Original Assignee
Univ Surrey
Professor Sembukutiarach Silva
Sajad Haq
Bojan O Boskovic
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GBGB0118279.9A external-priority patent/GB0118279D0/en
Priority claimed from GBGB0118341.7A external-priority patent/GB0118341D0/en
Priority claimed from GBGB0118276.5A external-priority patent/GB0118276D0/en
Application filed by Univ Surrey, Professor Sembukutiarach Silva, Sajad Haq, Bojan O Boskovic filed Critical Univ Surrey
Priority to US10/484,894 priority Critical patent/US8715790B2/en
Priority to KR1020047001223A priority patent/KR100951013B1/en
Priority to EP02749069A priority patent/EP1414744A1/en
Publication of WO2003011755A1 publication Critical patent/WO2003011755A1/en
Publication of WO2003011755B1 publication Critical patent/WO2003011755B1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C01B32/162—Preparation characterised by catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

A method of forming carbon nanotubes by plasma enhanced chemical vapour deposition using a carbon containing gas plasma, wherein the carbon nanotubes are not formed on a substrate at a temperature 300 °C or above.

Claims

35
AMENDED CLAIMS
[received by the International Bureau on 21 February 2003 (21.02.03); original claim 9 amended; claims 14, 15, 28, 61-63 added; remaining claims unchanged (9 pages)]
7. A method according to claim 6 wherein the substrate is kept at
a temperature of 50°C or below.
8. A method according to claim 7 wherein the substrate is kept at substantially room temperature.
9. A method according to claim 1 further comprising the step of cooling the substrate during the formation of the carbon nanotubes.
10. A method according to claim 9 wherein the substrate is kept at
a temperature below 0°C.
11. A method according to claim 9 further comprising the step of cooling the substrate with liquid nitrogen.
12. A method according to any preceding claim further comprising the step of growing carbon nanotubes within a chamber on a substrate that is placed within the chamber.
13. A method according to claim 12 further comprising the step of placing a catalyst on a surface of the substrate. 36
14. A method according to claim 13 wherein the catalyst is placed directly on the substrate surface.
15. A method according to claim 13 wherein the carbon nanotubes are grown from the catalyst as deposited on the substrate.
16. A method according to any preceding claim wherein the substrate is placed on an earthed electrode of a plasma generator, within the sheathed region of the plasma.
17. A method according to claim 16 wherein the potential difference between the substrate/catalyst and the plasma is less than 100 volts.
18. A method according to claim 17 wherein the potential difference between the material/catalyst and the plasma is less than 70 volts.
19. A method according to claim 18 wherein the potential difference between the material/catalyst and the plasma is less than 40 volts.
20. A method according to any preceding claim effected within a plasma chamber further comprising the step of cooling the electrodes.
21. A method according to claim 20 wherein the electrodes are cooled by water.
22. A method according to claim 1 further comprising the step of growing the carbon nanotubes within a chamber and then depositing the carbon nanotubes on a substrate that is external to the chamber.
23. A method according to claim 22 further comprising the step of injecting a catalyst into the chamber.
24. A method according to claims 13 or 23 wherein the catalyst is a metal.
25. A method according to claim 24 wherein the metal is a transition metal.
26. A method according to claim 25 wherein the transition metal includes a metal, or mixture of metals, from the group comprising nickel (Ni), cobalt (Co) and iron (Fe).
27. A method according to claim 23 wherein the catalyst is in the form of a powder. 38
28. A method according to claim 23 wherein the catalyst is in the form of a gas.
29. A method according to claim 13 wherein the catalyst is in the form of a powder, film or island arrays.
30. A method according to claim 29 wherein the island arrays are etched island arrays of which the particle size is between 2nm and lOOnm.
31. A method according to claim 27 or 29 wherein the powder has
a particle size from lμm to lOμm.
32. A method according to any preceding claim wherein the substrate is of organic material.
33. A method according to any of claims 1 to 32 wherein the substrate is a fabric.
34. A method according to any of claims 1 to 33 wherein the substrate is a plastics material.
35. A method according to any of claims 1 to 33 wherein the substrate is a polymer. 39
36. A method according to any of claims 1 to 32 wherein the substrate is paper.
37. A method according to any preceding claim wherein the plasma is of an ionised gas or gas mixture.
38. A method according to any preceding claim wherein the plasma is in the form of a beam.
39. A method according to any preceding claim wherein the plasma is generated by radio-frequency energy.
40. A method according to any preceding claim wherein the plasma is generated by radio-frequency energy combined with microwave energy.
41. A method according to any of claims 1 to 38 wherein the plasma is generated by microwave energy.
42. A method according to any of claims 1 to 38 wherein the plasma is generated using a pulsed power supply. 40
43. A method according to any preceding claim wherein the plasma is generated by a primary power source and combined with at least one secondary power source.
44. A method according to any preceding claim wherein the carbon containing gas is a hydrocarbon gas.
45. A method according to claim 44 wherein the hydrocarbon gas is methane, acetylene, ethylene or any mixture of the said gases.
46. A method according to any of claims 1 to 43 wherein the carbon containing gas is carbon monoxide or carbon dioxide.
47. A method according to any of claims 1 to 43 wherein the carbon containing gas is non-destructive and non-etching of the substrate or chamber when in a plasma state.
48. A method according to any preceding claim wherein the carbon containing gas is combined with a carrier gas.
49. A method according to claim 48 wherein the carrier gas is from the group comprising nitrogen, hydrogen, argon and ammonia. 41
50. A method according to any preceding claim further comprising the step of performing the method in a vacuum chamber constructed to generate, maintain and withstand a gaseous plasma.
51. A method according to any preceding claim further comprising the step of inserting the carbon nanotubes into a liquid which will cause them to self-organise into ropes.
52. A method according to claim 51 wherein the liquid is water.
53. A method according to any of claims 1 to 50 subsequently followed by an acid treatment step for removal of excess catalyst particles.
54. A method according to claim 53 subsequently followed by a wash step to remove the acid.
55. A method according to any preceding claim, wherein a proportion of formed nanotubes are in at least one of the following forms: bidirectional, branched, multiple-coaxial, coiled or densely packed ropes of nanotubes.
56. A carbon nanotube formed by a method according to claim 55 wherein the carbon nanotube comprises a substantially Y-shaped junction. 42
57. A carbon nanotube formed by a method according to claim 55 wherein the carbon nanotube comprises a substantially H-shaped junction.
58. A rope of carbon nanotubes obtained by a method according to claim 55.
59. A method of providing a pattern of carbon nanotubes on a fabric or organic material.
60. A method of forming ropes of partially aligned carbon nanotubes, comprising placing said nanotubes in a liquid selected so that the nanotubes self-organise into bundles.
61. A method according to claim 60 wherein the liquid is a nitric acid solution.
62. A method according to claim 61 including the step of diluting the solution with water.
63. A method according to claim 62 wherein the ropes are formed in the diluted solution. 43
64. A method according to claim 60, in which said liquid comprises water.
PCT/GB2002/003438 2001-07-27 2002-07-26 Production of carbon nanotubes WO2003011755A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US10/484,894 US8715790B2 (en) 2001-07-27 2002-07-26 Production of carbon nanotubes
KR1020047001223A KR100951013B1 (en) 2001-07-27 2002-07-26 Production of carbon nanotubes
EP02749069A EP1414744A1 (en) 2001-07-27 2002-07-26 Production of carbon nanotubes

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
GB0118279.9 2001-07-27
GBGB0118279.9A GB0118279D0 (en) 2001-07-27 2001-07-27 Low temperature growth of catalyic carbon nanotubes
GBGB0118341.7A GB0118341D0 (en) 2001-07-27 2001-07-27 Production of carbon nanotubes
GBGB0118276.5A GB0118276D0 (en) 2001-07-27 2001-07-27 Ropes of CVD grown carbon nanotubes
GB0118341.7 2001-07-27
GB0118276.5 2001-07-27

Publications (2)

Publication Number Publication Date
WO2003011755A1 WO2003011755A1 (en) 2003-02-13
WO2003011755B1 true WO2003011755B1 (en) 2003-04-03

Family

ID=27256233

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2002/003438 WO2003011755A1 (en) 2001-07-27 2002-07-26 Production of carbon nanotubes

Country Status (6)

Country Link
US (1) US8715790B2 (en)
EP (1) EP1414744A1 (en)
KR (1) KR100951013B1 (en)
CN (1) CN1325372C (en)
TW (1) TWI299320B (en)
WO (1) WO2003011755A1 (en)

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