Method for preparing single-wall carbon nanotube fiber assembly

Patent metadata

Field	Value
Publication number	US-11274041-B2
Application number	US-201716321951-A
Country	US
Kind code	B2
Filing date	Aug 11, 2017
Priority date	Oct 12, 2016
Publication date	Mar 15, 2022
Grant date	Mar 15, 2022

Abstract

The present invention relates to a method for preparing a carbon nanotube fiber aggregate formed of single-wall carbon nanotubes, and the manufacturing efficiency of a carbon nanotube fiber comprising single-wall carbon nanotubes can be improved by controlling the molar ratio of a carbon source and of a reducing gas in a carrier gas.

First claim

The invention claimed is:

1. A method for producing an aggregate of carbon nanotube fibers composed of single-wall carbon nanotubes by spinning a raw material containing a carbon source in the presence of an inert carrier gas containing a reducing gas, the method comprising:
controlling a molar ratio of the carbon source to the reducing gas in the carrier gas and (carbon source/reducing gas) to less than 0.065, thereby producing the aggregate composed of single-wall carbon nanotubes;
wherein the molar ratio (A) of the carbon source to the reducing gas, and the value of IG/ID greater than 6, satisfy the following Equation 1:
(−4.06×10 2 ) A+ 29.4≤ IG/ID ≤(−4.06×10 2 ) A+ 37.5  (Equation 1)

wherein, the IG/ID means the maximum peak intensity IG in the range of 1560 cm −1 to 1600 cm −1 and the maximum peak intensity ID in the range of 1310 cm −1 to 1350 cm −1 , by the resonance Raman scattering measurement scheme;
wherein a supply flow rate of the raw material for spinning is 10 to 500 ml/min, and a supply flow rate of the carrier gas is 1 to 5 L/min.

2. The method for producing the aggregate of carbon nanotube fibers according to claim 1 , wherein the reducing gas comprises hydrogen gas, ammonia gas or a mixed gas thereof.

3. The method for producing the aggregate of carbon nanotube fibers according to claim 1 , wherein the raw material is a catalyst precursor dispersed in a liquid or gaseous carbon compound.

4. The method for producing the aggregate of carbon nanotube fibers according to claim 3 , wherein the liquid or gaseous carbon compound may include at least one selected from the group consisting of methane, ethylene, acetylene, methyl acetylene, vinyl acetylene, ethanol, methanol, propanol, acetone, xylene, chloroform, ethyl acetic acid, diethyl ether, polyethylene glycol, ethyl formate, mesitylene, tetrahydrofuran (THF), dimethylformamide (DMF), dichloromethane, hexane, benzene, carbon tetrachloride, and pentane.

5. The method for producing the aggregate of carbon nanotube fibers according to claim 3 , wherein the catalyst precursor may include at least one selected from the group consisting of iron, nickel, cobalt, platinum, ruthenium, molybdenum, vanadium, and oxides thereof.

6. The method for producing the aggregate of carbon nanotube fibers according to claim 5 , wherein the catalyst precursor is in a metallocene form.

7. The method for producing the aggregate of carbon nanotube fibers according to claim 1 , wherein carbon nanotubes are formed from a raw material for spinning and fused continuously to spin carbon nanotube fibers directly.

Assignees

• Lg Chemical Ltd

Inventors

• Oh Eugene
• Kim Juhan
• Kim Ji Eun
• Lee Won Jae

Classifications

• C01B32/159

  single-walled · CPC title

• C01B2202/02

  Single-walled nanotubes · CPC title

• D01F9/133

  Apparatus therefor · CPC title

• C01B32/162

  characterised by catalysts · CPC title

• D01D7/00

  Collecting the newly-spun products ({D01D5/0076 takes precedence;} collecting newly-spun products with the imparting of twist D01H) · CPC title