Method for manufacturing catalyst for carbon nanotube synthesis

Patent metadata

Field	Value
Publication number	US-10077495-B2
Application number	US-201314424229-A
Country	US
Kind code	B2
Filing date	Aug 21, 2013
Priority date	Aug 29, 2012
Publication date	Sep 18, 2018
Grant date	Sep 18, 2018

Abstract

Single walled carbon nanotubes can be synthesized and production efficiency of carbon nanotubes can be enhanced by a method including a supplying step (S 11 ) in which particulate carriers are supplied into a drum, a sputtering step (S 12 ) for supporting a catalyst, in which sputtering is performed while this drum 10 is rotated around the axis and is swung so that one end portion and the other end portion in the axial direction of the drum 10 are relatively vertically switched, and a recovering step (S 13 ) in which the particulate carriers are recovered by inclining the drum to discharge the particulate carriers from the drum.

First claim

The invention claimed is:

1. A method for manufacturing a catalyst for carbon nanotube synthesis, the method comprising the following steps in the following order:
a supplying step comprising supplying particulate carriers into a tubular drum, wherein the particulate carriers comprise support particles comprising at least one material selected from the group consisting of SiO 2 , Al 2 O 3 , MgO, SiN 4 , AIN and SiC, and wherein each support particle comprises a catalyst supporting layer comprising at least one material selected from the group consisting of SiO 2 , Al 2 O 3 , MgO, Si 3 N 4 , AlN and SiC;
a catalyst depositing sputtering step comprising performing sputtering while the tubular drum containing the particulate carriers is rotated around an axis to deposit the catalyst for carbon nanotube synthesis on the particulate carriers, wherein the catalyst for carbon nanotube synthesis comprises at least one element selected from the group consisting of Ti, Ta, V, Cr, Fe, Co, Ni, W and Au, and wherein, in the catalyst depositing sputtering step, the tubular drum is swung so that one end portion and another end portion in an axial direction of the tubular drum are relatively vertically switched with a maximum inclination angle of the axial direction of the tubular drum with respect to a horizontal axis is between 3.0° or larger and 15.0° or smaller, and oxygen is supplied to a vacuum container that houses the tubular drum;
a recovering step comprising recovering the particulate carriers from the tubular drum by inclining the tubular drum; and
a reducing step comprising reducing the catalyst for carbon nanotube synthesis on the particulate carriers by heating while a reducing gas is flown over the catalyst for carbon nanotube synthesis on the particulate carriers.

2. The method for manufacturing a catalyst for carbon nanotube synthesis according to claim 1 , wherein
a particulate carrier supplying chamber is connected to the vacuum container that houses the tubular drum, a first opening and closing device that opens and closes a space between the vacuum container and the particulate carrier supplying chamber is provided, and
the supplying step is conducted in a state where the first opening and closing device is closed, the particulate carrier supplying chamber is brought into a vacuum state, the first opening and closing device is opened, the particulate carriers supplied to the particulate carrier supplying chamber are supplied into the tubular drum, the first opening and closing device is closed, and the particulate carrier supplying chamber is opened to atmosphere.

3. The method for manufacturing a catalyst for carbon nanotube synthesis according to claim 2 , wherein
a particulate carrier recovering chamber is connected below a vacuum container that houses the tubular drum, a second opening and closing device that opens and closes a space between the vacuum container and the particulate carrier recovering chamber is provided, and
the recovering step recovers the particulate carriers from the particulate carrier recovering chamber in which the particulate carrier recovering chamber is brought into a vacuum state, the second opening and closing device is opened, the tubular drum is inclined to drop the particulate carriers in the tubular drum into the particulate carrier recovering chamber, the second opening and closing device is closed, and the particulate carrier recovering chamber is opened to atmosphere.

4. The method for manufacturing a catalyst for carbon nanotube synthesis according to claim 1 , wherein the supplying step comprises, before the catalyst depositing sputtering step, supplying the support particles into the tubular drum, and then conducting a catalyst supporting layer depositing sputtering step comprising performing sputtering while the tubular drum containing support particles of the particulate carriers is rotated around the axis to form the catalyst supporting layer for supporting the catalyst for carbon nanotube synthesis on the support particles.

Assignees

• Hitachi Chemical Co Ltd

Inventors

• Ueda Shunsuke
• Haba Eisuke

Classifications

• B01J37/347

  Ionic or cathodic spraying; Electric discharge · CPC title

• C23C14/14

  Metallic material, boron or silicon · CPC title

• B01J23/745

  Iron · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title