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Highly purified carbon nanotubes and method of their preparation

a carbon nanotube, high-purification technology, applied in the direction of carbon nanotubes, nano-carbon, etc., can solve the problems of reducing the raman g/d ratio, affecting the electrical, thermal and mechanical properties of the material, and generating amorphous carbon and inorganic impurities in the cnt material, etc., to achieve high purity and high raman g/d ratio

Inactive Publication Date: 2018-07-05
YAZAKI CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The method achieves extremely high purity CNTs with improved Raman G / D ratios, indicating reduced structural defects and enhanced mechanical and electrical properties, suitable for various electronics applications.

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.

Method used

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  • Highly purified carbon nanotubes and method of their preparation
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  • Highly purified carbon nanotubes and method of their preparation

Examples

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example 1

Preparation of a Treatment Solution “AAA-1”

[0091]First, 240 grams de-ionized water e combined in a flask with 160 grams reagent alcohol (Catalog number A995-4, Thermo Fisher Scientific, Waltham Mass.). Then, 100 grams of hydrochloric acid (HCl, 35-38%) (Catalog number A508-500, Thermo Fisher Scientific) are slowly added to the flask. The contents of the flask are mixed thoroughly to form a uniform solution. The concentration of HCl in this solution is about 1.9N. This solution is identified as “AAA-1”.

example 2

Preparation of a Treatment Solution “AAA-2”

[0092]First, 270 grams de-ionized water are combined in a flask with 180 grams reagent alcohol.

[0093]Then, 300 grams of hydrochloric acid (HCl, 35-38%) are slowly added to the flask. Lastly, 7.5 grams of hydrofluoric acid (HF, 47-51%) (Catalog number A513-500, Thermo Fisher Scientific) are slowly added to the flask. The contents of the flask are mixed thoroughly to form a uniform solution. The concentrations of HCl and HF in this solution are about 4.0N and 0.25N, respectively. This solution is identified as “AAA-2”.

example 3

Preparation of Single Wall Carbon Nanotube (SWCNT) Wafers

[0094]Cohesive carbon nanotube assemblies (“wafers”) are prepared according to a method described in detail in WIPO publication WO 2012 / 177555A2. Single wall carbon nanotube (SWCNT) powder is obtained from Thomas Swan and Co., Ltd (Consett, County Durham, United Kingdom), under the product name “Elicarb® SW”. The as-received SWCNT powder is examined using a scanning electron microscope (SEM) (model JSM-7500F, JEOL Ltd, Tokyo) at up to 300,000× magnification. The material appears as randomly oriented tubes and bundles with considerable portion of non-tubular amorphous carbon, as seen in FIG. 2(a).

[0095]In a flask, 2.5 grams of this SWCNT powder are combined with 1250 ml toluene (Catalog number T324-4, Thermo Fisher Scientific). A uniform dispersion of the SWCNT in the toluene is prepared through a combination of mechanical agitation and sonication. The uniform dispersion of SWCNT in toluene is then cast equally into 24 individu...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C01B32/17
CPCC01B32/17
Inventor YAN, YONGANRAYCHAUDHURI, SATYABRATA
Owner YAZAKI CORP
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