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Carbon nano-tube manufacturing method and carbon nano-tube manufacturing apparatus

A technology of carbon nanotubes and a manufacturing method, which is applied in the field of carbon nanotube manufacturing devices and can solve the problems of inability to remove carbon precipitates in fluid layers, mixing of impurities, high carbon nanotubes and the like

Inactive Publication Date: 2013-05-08
HITACHI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the continuous supply of these three gases is the premise, there is no need to mention the switching operation of the gas.
In addition, in the method of Patent Document 1, the catalyst is attached to the carbon nanotubes, so impurities are mixed into the product.
In addition, according to the method of Patent Document 1, the carbon precipitates remaining in the fluidized bed cannot be removed, and the carbon precipitates will accumulate
As a result, until more carbon nanotubes are obtained, the particles of the fluidization medium are covered with carbon and cannot be used.
[0027] Thus, in the conventional fluidized bed production method, it is impossible to produce high-purity carbon nanotubes
Also, low productivity
Catalyst height control is difficult due to simultaneous carbon nanotube synthesis and catalyst loading

Method used

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  • Carbon nano-tube manufacturing method and carbon nano-tube manufacturing apparatus
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  • Carbon nano-tube manufacturing method and carbon nano-tube manufacturing apparatus

Examples

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Embodiment 1

[0164] Example 1 of the present invention will be described. Here, as a support, alumina beads are used, on which Al 2 o 3 . Al 2 o 3 The carrier was sputtered into a film on alumina beads. The alumina beads had a diameter of 0.5 mm. Al 2 o 3 The thickness of the carrier (carrier layer) was 20 nm. Moreover, in Al 2 o 3 Fe is supported on the carrier as a catalyst. This loading is carried out by sputtering. Loaded on Al 2 o 3 The thickness of Fe on the support was 1 nm. Put this support in the reactor, while supplying 60Torr C to the reactor 2 h 4 / 200TorrH 2 / 100ppmvH 2 Carbon nanotubes are synthesized in a fluidized bed state while using atmospheric pressure gas of O / Ar balance.

[0165] The reactor is Figure 5 The shown quartz glass is a vertical CVD reactor that can be used both as a fixed bed and as a fluid bed. The temperature of the reaction part in the reactor was 800°C. The supply of normal-pressure gas was performed for 10 minutes, and the synth...

Embodiment 2

[0174] Next, Embodiment 2 of the present invention will be described. In Example 2, the catalyst was supported by circulating the carrier raw material vapor and the catalyst raw material vapor over the alumina beads in a high temperature state. Thereafter, carbon source steam was circulated over the catalyst-loaded high-temperature alumina beads to synthesize carbon nanotubes. Here, alumina beads were used as the support. As the alumina beads, those having a diameter of 0.5 mm were used. In this example 2, in Figure 4 Alumina beads were installed in the shown horizontal CVD apparatus, and the following processes were performed.

[0175] First, 0.2 to 0.5 mL of tetraethoxyorthosilicate (TEOS) was supplied under normal pressure with the entire apparatus heated to about 700°C. The TEOS supplied into the reactor evaporates and reacts on the surface of the alumina beads to form SiO 2 carrier layer. Next, set the device as a whole to about 400°C, and use SiO 2 Coated alumina...

Embodiment 3

[0178] Next, Embodiment 3 of the present invention will be described. In Example 3, the synthesis of carbon nanotubes was repeated. Here, as the support, alumina beads with a diameter of 0.5 mm were used. In this embodiment 3, in Figure 4 Alumina beads were installed in the horizontal CVD apparatus shown, and the following treatments were performed. First, SiO is formed on the surface of the alumina beads 2 carrier layer. Specifically, after heating the entire reaction apparatus to about 700° C., 0.2 to 0.5 mL of TEOS was supplied onto the alumina beads under normal pressure. The TEOS supplied into the reactor evaporates and reacts on the surface of the alumina beads to form SiO 2 carrier layer.

[0179] made of SiO 2 Coated alumina beads are loaded with Al at the same time 2 o 3 Support and Fe catalyst. This simultaneous loading is performed after heating the entire reaction apparatus to about 400°C. Simultaneously supply 3 mg of aluminum isopropoxide vapor as car...

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Abstract

The method for producing carbon nanotubes of the invention employs a carbon source that contains carbon and is decomposed when heated and a catalyst that serves as a catalyst for production of carbon nanotubes from the carbon source, to synthesize the carbon nanotubes on a heated support placed in a reactor, the method comprising a catalyst loading step in which the catalyst starting material, as the starting material for the catalyst, is distributed over the support to load the catalyst onto the support, a synthesis step in which the carbon source is distributed over the support to synthesize the carbon nanotubes on the support, and a separating step in which a separating gas stream is distributed over the support to separate the carbon nanotubes from the support, wherein the catalyst loading step, the synthesis step and the separating step are carried out while keeping the support in a heated state and switching supply of the catalyst starting material, the carbon source and the separating gas stream.

Description

technical field [0001] The present invention relates to a method for manufacturing carbon nanotubes and a device for manufacturing carbon nanotubes. More specifically, the present invention relates to a production method for mass-producing carbon nanotubes having various structures at low cost and on a large scale, and a carbon nanotube production apparatus used in the production method. Background technique [0002] Carbon nanotubes are materials having a rolled graphene sheet structure and a one-dimensional structure with a very large aspect ratio (see Non-Patent Document 1). It is known that carbon nanotubes have excellent mechanical strength and flexibility; have semiconductor or metal conductivity; and also have very stable chemical properties. As methods for producing carbon nanotubes, arc discharge method, laser evaporation method, and chemical vapor growth method (hereinafter referred to as CVD (Chemical Vapor Deposition) method) have been reported. In particular, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02B01J23/745
CPCB01J8/1836B01J37/0209C01B2202/04B01J37/0221B82Y40/00B01J8/0055B01J37/0238B01J2208/00407B01J8/34C01B31/0226B01J23/745B01J23/28B01J37/347B01J37/0217B01J37/0244B01J23/70B82Y30/00C01B32/16B82B3/0004B82B3/0009C01B32/162
Inventor 野田优杉目恒志山口由岐夫大泽利男笕和宪长谷川馨金东荣
Owner HITACHI CHEM CO LTD
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