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High tensile strength carbon nanotube film and process for making the same

Inactive Publication Date: 2006-02-09
GEORGIA TECH RES CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0007] In another embodiment, a method for making a conductive carbon nanotube film comprising refluxing an aqueous mixture comprising carbon nanotubes and an oxidizing agent to form a refluxed nanotube dispersion; forming a carbon nanotube film from the refluxed nanotube dispersion; drying the carbon nanotube film; and heat-treating the carbon nanotube film to form a heat-treated carbon nanotube film. In one embodiment, the method can further comprise removing the oxidizing agent from the carbon nanotube film. In another embodiment, the method can further comprise sonicating the nanotubes prior to or after refluxing. In yet another embodiment, the method can further comprise sonicating the nanotubes prior to adding the oxidizing agent. In another embodiment, the carbon nanotubes comprise single-wall small-diameter carbon nanotubes. In another embodiment, the carbon nanotubes comprise small-diameter carbon nanotubes wherein the small-diameter carbon nanotubes have a diameter of at most about 3 nm and can have one or more walls. In another embodiment, the forming of the carbon nanotube film is done by filtering.
[0008] In another embodiment, a film consists essentially of small-diameter carbon nanotubes, wherein the small-diameter carbon nanotubes are crosslinked.
[0009] In another embodiment, a heat-treated carbon nano

Problems solved by technology

Because large-diameter multi-wall carbon nanotubes have substantially greater density of defects in their side-walls, they are, consequently, mechanically less strong and electrically less conductive than small-diameter carbon nanotubes.
The fabrication of high strength films comprising small-diameter nanotubes for these and other applications remains a major challenge.

Method used

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  • High tensile strength carbon nanotube film and process for making the same
  • High tensile strength carbon nanotube film and process for making the same
  • High tensile strength carbon nanotube film and process for making the same

Examples

Experimental program
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example 1

[0056] This example demonstrates a method for preparing a high strength film comprising predominantly single-wall carbon nanotubes (SWNT). Purified, HIPCO® small-diameter carbon nanotubes, comprising almost entirely single-wall carbon nanotubes, obtained from Rice University and Carbon Nanotechnologies, Inc., were made in a high temperature, high pressure, gas phase process through the disproportionation of carbon monoxide to primarily single-wall carbon nanotubes and CO2 using iron as the transition metal catalyst. (HIPCO is a registered trademark of Carbon Nanotechnologies, Incorporated, Houston, Tex.) 100 mg purified small-diameter carbon nanotubes were dispersed in 100 mls distilled water and sonicated for 2 hours using a Fisher Scientific bath sonicator (frequency 43 KHz, power 150 Watts). Nitric acid was then added to the dispersion to obtain a nitric acid concentration of 3M, 6M, or 10M. Each dispersion was then sonicated for 2 more hours, then refluxed for two hours, and sub...

example 2

[0059] Tensile mechanical properties and dc conductivity were measured on the small-diameter carbon nanotube films prepared in Example 1. The film samples tested in the tensile tests were 1 mm wide and 0.06 mm thick. The gauge length was 10 mm between the clamps. The tensile tests were conducted on a Rheometrics Solids Analyzer, RSA III, at a strain rate of 0.5% per second. The tensile test data are summarized in Table 1.

[0060] The mechanical studies showed a tensile strength of 74 MPa for the “as prepared” (heat-treated at 200° C.) small-diameter carbon nanotube film prepared with 10M nitric acid, a greater than seven-fold increase in tensile strength over the control film, which had a tensile strength of 10 MPa. The results also showed an initial tensile modulus of 5.0 GPa for the heat-treated small-diameter carbon nanotube film prepared with 10M nitric acid, a greater than six-fold increase in initial tensile modulus over the control film, which had an initial tensile modulus of...

example 3

[0063] Dynamic mechanical analysis (DMA) as a function of temperature was done on the “as prepared” (200° C. heat-treated) small-diameter carbon nanotube films, prepared in Example 1, at a frequency of 10 Hz and at 0.1% dynamic strain using a RSA III Rheometrics Solids Analyzer. During the dynamic test, the static force adjusted automatically to 40% larger than dynamic force.

[0064] The results show a fairly constant E′ storage modulus for the “as prepared” small-diameter carbon nanotube films throughout the temperature range of about 30° C. to about 210° C., with a slight increase in storage modulus above 150° C. The Tan δ values were very low (i.e., about 0.02), indicating that the films are fairly elastic throughout the 30° C. to about 210° C. temperature range. A plot of the dynamic mechanical behavior for the “as prepared” film made with small-diameter carbon nanotubes processed in 6 M nitric acid is shown in FIG. 1.

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Abstract

A conductive carbon nanotube film having high tensile strength and initial tensile modulus comprises primarily oxidized small-diameter carbon nanotubes wherein the diameter of the small-diameter carbon nanotubes are at most about 3 nm. A method for making the film comprises refluxing an aqueous mixture comprising carbon nanotubes and an oxidizing agent to form a refluxed nanotube dispersion; forming a carbon nanotube film from the refluxed carbon nanotube dispersion; optionally removing nitric acid or other oxidizing agent from the carbon nanotube film; drying the carbon nanotube film; and heat-treating the carbon nanotube film to form a heat-treated carbon nanotube film. The method can also comprise sonicating the nanotubes prior to or after refluxing. A heat-treated small-diameter carbon nanotube film can have a tensile strength of over 70 MPa and an initial tensile modulus of about 5 GPa.

Description

CROSS-REFERENCE TO RELATED APPLICATION [0001] This application claims priority from provisional United Patent application Ser. No. 60 / 523,806, filed Nov. 19, 2003, which application is incorporated herein by reference.[0002] This invention was made in part with United States Government support under Grant No. F49620-03-1-0124 awarded by the Air Force Office of Scientific Research and under Grant No. N00014-01-1-0657 awarded by the Office of Naval Research. Government may have certain rights in the invention.FIELD OF THE INVENTION [0003] This invention relates generally to carbon nanotubes, and more particularly to a high tensile strength film comprising carbon nanotubes. BACKGROUND OF THE INVENTION [0004] Small-diameter carbon nanotubes having diameters between about 0.5 and about 3 nanometers, commonly known as “buckytubes,” have been the subject of intense research since their discovery due to their unique properties, including high strength, stiffness, thermal and electrical cond...

Claims

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Application Information

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IPC IPC(8): D01F9/12
CPCB82Y30/00D01F11/12D01F11/123D01F11/122D01F11/121
Inventor ZHANG, XIEFEIVEEDU, SREEKUMAR T.LIU, TAOKUMAR, SATISH
Owner GEORGIA TECH RES CORP
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