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US6936233: Method for purification of as-produced single-wall carbon nanotubes

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Filing Information

Inventor(s) Richard E. Smalley · Daniel T. Colbert · Hongjie Dai · Jie Liu · Andrew G. Rinzler · Jason H. Hafner · Kenneth A. Smith · Ting Guo · Pavel Nikolaev · Andreas Thess ·
Assignee(s) William Marsh Rice University ·
Attorney/Agent(s) Ross Spencer Garsson · Robert C. Shaddox · Winstead Sechrest & Minick, P.C. ·
Primary Examiner Stuart Hendrickson ·
Application Number US10032933
Filing date 12/28/2001
Issue date 08/30/2005
Prior Publication Data
Predicted expiration date 05/30/2019
Patent term adjustment 450
U.S. Classifications 423/447.1  · 423/461  ·
International Classifications --
Kind CodeB2
International Classifications 423461 · 4234471 ·
Related U.S. Application DataRELATED APPLICATIONS
This application is a division of prior U.S. patent application Ser. No. 09/380,545, filed on Dec. 22, 1999, now U.S. Pat. No. 6,683,783, entitled “CARBON FIBERS FORMED FROM SINGLE-WALL CARBON NANOTUBES,” which is the 35 U.S.C. § 371 national application of International Application Number PCT/US98/04513 filed on Mar. 6, 1998, which designated the United States, claiming priority to: provisional U.S. patent application Ser. No. 60/067,325, filed on Dec. 5, 1997; provisional U.S. patent application Ser. No. 60/064,531, filed on Nov. 5, 1997; provisional U.S. patent application Ser. No. 60/063,675, filed on Oct. 29, 1997; provisional U.S. patent application Ser. No. 60/055,037, filed on Aug. 8, 1997; provisional U.S. patent application Ser. No. 60/047,854, filed on May 29, 1997; and provisional U.S. patent application Ser. No. 60/040,152, filed on Mar. 7, 1997. Each of the foregoing applications is commonly assigned to the assignee of the present invention and is hereby incorporated herein by reference in its entirety.
21 Claims, 21 Drawings


Abstract

This invention relates generally to a single-wall carbon nanotube (SWNT) purification process and more particularly to a purification process that comprises heating the SWNT-containing felt under oxidizing conditions to remove the amorphous carbon deposits and other contaminating materials. In a preferred mode of this purification procedure, the felt is heated in an aqueous solution of an inorganic oxidant, such as nitric acid, a mixture of hydrogen peroxide and sulfuric acid, or a potassium permanganate. Preferably, SWNT-containing felts are refluxed in an aqueous solution of an oxidizing acid at a concentration high enough to etch away amorphous carbon deposits within a practical time frame, but not so high that the single-wall carbon nanotube material will be etched to a significant degree. When material having a high proportion of SWNT is purified, the preparation produced will be enriched in single-wall nanotubes, so that the SWNT are substantially free of other material.

Independent Claims | See all claims (21)

  1. 1. A method for purifying a mixture comprising single-wall carbon nanotubes and amorphous carbon contaminate, said method comprising the steps of: (a) heating said mixture under oxidizing conditions sufficient to remove the said amorphous carbon; and (b) recovering a product comprising at least about 80% by weight of single-wall carbon nanotubes, wherein the product is washed with a solution comprising a surfactant.
  2. 4. A method for purifying a mixture comprising single-wall carbon nanotubes and amorphous carbon contaminate, said method comprising the steps of: (a) heating said mixture under oxidizing conditions sufficient to remove the said amorphous carbon; and (b) recovering a product comprising at least about 80% by weight of single-wall carbon nanotubes.
  3. 21. A method for purifying a mixture comprising single-wall carbon nanotubes and amorphous carbon contaminate, said method comprising the steps of: (a) heating said mixture under oxidizing conditions; and (b) recovering a product comprising at least about 80% by weight of single-wall carbon nanotubes, wherein the product comprises fullerene torroids.

References Cited

U.S. Patent Documents

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Foreign Patent Documents

Document NumberAssigneesInventorsIssue/Pub Date
EP1176234HYPERION CATALYSIS INTERNATIONAL, INC.Dec 1993

Other Publications

Bandau et al. ‘Purification of Single-Wall Carbon Nanotubes by Microfiltration’ in J. Phys. Chem. B vol. 101 pp. 8839-8842 1997, no month.*
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Ajayan et al., “Opening carbon nanotubes with oxygen and implications for filing” Nature, vol. 362, pp. 522-525 (Apr. 8, 1993).
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Liu, et al., “Fullerene Pipes,” Science, vol. 280, May 22, 1998, pp. 1253-1256.
Thess, et al., “Crystalline Ropes of Metallic Carbon Nanotubes,” Science, vol. 273, Jul. 26, 1996, pp. 483-487.
Tohji, et al., “Purifying single-walled nanotubes,” Nature, vol. 383, Oct. 24, 1996, pp. 679.
Tohji, et al., “Purification Procedure for Single-Walled Nanotubes,” J. Phys. Chem. B., vol. 101, No. 11, 1997, pp. 1974-1978.
Ajayan, et al., “Nanometre-size tubes of carbon,” Rep. Prog. Phys., vol. 60, 1997, pp. 1025-1062.
Fishbine, “Carbon Nanotube Alignment and Manipulation Using Electrostatic Fields,” Fullerene Science & Technology, vol 4(1), 1996, pp. 87-100.
Ajayan, et al., “Aligned Carbon Nanotubes Arrays Formed by Cutting a Polymer Resin-Nanotube Composite,” Science, vol. 265, Aug. 26, 1994, pp. 1212-1214.
Wang, et al., “Properties of Buckytubes and Derivatives,” Carbon, vol. 33, No. 7, 1995, pp. 949-958.
Sen, et al., “Structures and Images of Novel Derivatives of Carbon Nanotubes, Fullerenes and Related New Carbon Forms,” Fullerene Science and Technology, vol. 5(3), 1997, pp. 489-502.
Dravid, et al., “Buckytubes and Derivatives: Their Growth and Implications for Buckyball Formation,” Science, vol. 259, Mar. 12, 1993, pp. 1601-1604.
Smalley, “From dopyballs to nanowires,” Materials Science and Engineering, vol. B19, 1993, pp. 1-7.
Chen, “Growth and Properties of Carbon Nanotubes,” Thesis for the degree Master of Science, Rice University, Houston, Texas, May 1995.
Rinzler, et al., “Field Emission and Growth of Fullerene Nanotubes,” Presented at the Fall, 1994 MRS Meeting, Nov. 28, 1994, Boston, submitted for MRS proceedings, vol. 359.
Gamaly, et al., “Mechanism of carbon nanotube formation in the arc discharge,” Physical Review B, vol. 52, No. 3, Jul. 15, 1995-I, pp. 2083-2089.
Ge, et al., “Scanning tunneling microscopy of single-shell nanotubes of carbon” Appl. Phys. Lett., vol. 65(18), Oct. 31, 1994, pp. 2284-2286.
* cited by examiner

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