Highly purified carbon nanotubes and method of their preparation

Abstract

Highly purified carbon nanotubes (CNT) having virtually no carbonaceous impurities (amorphous carbon) nor inorganic impurities (metal and metal oxides), and methods of their preparation are described. The purified CNT feature excellent electrical, mechanical, and thermal properties due to the near total absence of detrimental impurities. The CNT starting material is preferably in the form of wafer, film, or buckypaper for efficient diffusion of purifying media. The highly pure CNT are prepared by heat treating a CNT starting material in a specified amount of oxygen, then treating the CNT in a solution comprising water and acid, or further heat treating the CNT in an atmosphere comprising chlorine (Cl2). Extremely low levels of inorganic impurities may be achieved by treating sequentially with a treatment solution followed by chlorine. Removal of chloride from purified CNT may be achieved by further treating the chlorine-treated material in an atmosphere comprising hydrogen (H2).

Description

[0001]This application is a continuation of U.S. application Ser. No. 14 / 663,339, filed Mar. 19, 2015; which claims the benefit of U.S. Provisional Application No. 61 / 970,821, filed Mar. 26, 2014; the above applications are incorporated herein by reference in their entireties.TECHNICAL FIELD[0002]This invention relates generally to carbon nanotube materials having extremely high purity with regard to amorphous carbon and inorganic impurities, i.e. metals and metal oxides. This invention also relates to methods of preparing extremely pure carbon nanotubes without excessive loss of nanotube material, and without measurable damage to the material. The highly purified carbon nanotubes are useful in various electronics applications requiring high conductivity and durability,BACKGROUND[0003]Carbon nanotubes (CNT) are of substantial interest for numerous potential applications due to their unique electrical, thermal, and mechanical properties. For example, certain nanotubes are believed to...

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Problems solved by technology

However, this process also results in the generation of amorphous carbon, which can be located randomly on the outer surfaces of CNT.

Amorphous carbon is the most common impurity and the hardest to remove, due to bonding on certain carbon atoms.

Amorphous carbon and inorganic impurities in CNT materials are detrimental to the electrical, thermal, and mechanical properties of the material.

The presence of impurities can affect the properties to an extent that renders the CNT material unsuitable for many applications.

For removal of inorganic impurities, prior art methods, such as reacting in highly concentrated acids at elevated temperatures, typically result in significant decrease in G / D ratio, indicating that the purification process imparted damage to the CNT structure.

However, existing methods tend to damage CNT (as mentioned above), cause significant loss of CNT, or result in only partial purification.

Although this protocol has been proven to reduce both amorphous carbon and inorganic content, it is unsafe, and a substantial amount of contamination can still remain on the surface.

Furthermore, treatment with concentrated acids is somewhat counterproductive, as it also introduces structural defects while removing superficial ones.

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