US 12,012,335 B2
Preparation method and working electrode application of 3D bundle-shaped multi-walled carbon nanotubes
Hao-Lin Hsu, Tainan (TW); and Jean-Hong Chen, Tainan (TW)
Assigned to KUN SHAN UNIVERSITY, Tainan (TW)
Filed by Kun Shan University, Tainan (TW)
Filed on Oct. 18, 2021, as Appl. No. 17/503,488.
Prior Publication US 2023/0122386 A1, Apr. 20, 2023
Int. Cl. H01M 4/133 (2010.01); B01J 19/14 (2006.01); B01J 21/08 (2006.01); B01J 23/887 (2006.01); B01J 37/04 (2006.01); B01J 37/08 (2006.01); B01J 37/18 (2006.01); C01B 32/162 (2017.01); C23C 16/26 (2006.01); H01M 4/04 (2006.01)
CPC C01B 32/162 (2017.08) [B01J 19/14 (2013.01); B01J 21/08 (2013.01); B01J 23/8872 (2013.01); B01J 37/04 (2013.01); B01J 37/08 (2013.01); B01J 37/18 (2013.01); C23C 16/26 (2013.01); H01M 4/0428 (2013.01); H01M 4/133 (2013.01); C01B 2202/06 (2013.01); C01B 2202/22 (2013.01)] 13 Claims
OG exemplary drawing
 
1. A preparation method of 3D bundle-shaped multi-walled carbon nanotubes, comprising:
Step S1: providing a bi-component alloy catalyst and a transition metal element, mixing uniformly in an inert gas environment and performing a heat treatment for 30˜90 minutes in order to obtain an intermetallic catalyst;
Step S2: providing a substrate, and disposing the intermetallic catalyst on the substrate;
Step S3: providing a hydrogen flowing through the substrate, heating the substrate to a first temperature, and using the hydrogen to undergo a reduction of the intermetallic catalyst at the first temperature for 15˜45 minutes;
Step S4: providing a protective gas and a carbon source gas, heating the substrate to a second temperature, allowing the protective gas and the carbon source gas to flow through the substrate, undergoing a reaction at the second temperature for 30˜90 minutes, thereby allowing carbon atoms generated from pyrolysis of the carbon source gas to deposit at a bottom of the intermetallic catalyst, and gradually generating a 3D bundle-shaped multi-walled carbon nanotubes; after completion of the reaction at the second temperature, cooling to room temperature and collecting the 3D bundle-shaped multi-walled carbon nanotubes;
wherein the inert gas comprises a Group 18 element, the second temperature is greater than or equal to the first temperature, and a volume mixing ratio of the protective gas and the carbon source gas is 1:6˜1:12.