KR19990073593A - Chemical vapor deposition system for massive synthesis of carbon nanotubes - Google Patents

Chemical vapor deposition system for massive synthesis of carbon nanotubes Download PDF

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KR19990073593A
KR19990073593A KR1019990030700A KR19990030700A KR19990073593A KR 19990073593 A KR19990073593 A KR 19990073593A KR 1019990030700 A KR1019990030700 A KR 1019990030700A KR 19990030700 A KR19990030700 A KR 19990030700A KR 19990073593 A KR19990073593 A KR 19990073593A
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carbon nanotubes
vapor deposition
transition metal
chemical vapor
metal film
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KR1019990030700A
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Korean (ko)
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이철진
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이철진
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Priority to KR1019990030700A priority Critical patent/KR19990073593A/en
Publication of KR19990073593A publication Critical patent/KR19990073593A/en
Priority to KR1020000036509A priority patent/KR100345079B1/en
Priority to EP00306169A priority patent/EP1072693A1/en
Priority to JP2000225525A priority patent/JP2001081564A/en
Priority to CN00121138A priority patent/CN1282801A/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C01B32/162—Preparation characterised by catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/20—Nanotubes characterized by their properties
    • C01B2202/30—Purity

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

본 발명은 탄소나노튜브의 대량합성을 위한 화학기상증착장치에 관한 것으로써, 특히 열화학기상증착법을 이용하여 여러개의 대면적 기판위에서 탄소나노튜브를 대량으로 합성시키는 장치에 관한 것이다. 본 발명에 따른 탄소나노튜브의 대량합성을 위한 화학기상증착장치는 탄소나노튜브를 합성시키는 반응로를 기존의 튜브형태와 달리 대면적인 직육면체형태로 제작하고 또한 대면적 기판을 수평으로 평행하게 여러장 놓을 수 있는 직육면체형태의 보트로 구성된다. 본 발명에 의한 화학기상증착장치를 이용한 탄소나노튜브의 합성은 대면적 기판위에 전이금속막을 증착시킨 후, 상기 전이금속막이 증착된 기판들을 보트에 장착시킨 후, 상기 보트를 반응로내로 넣은 후, 상압 또는 저압에서 열분해방식을 사용하여 상기 전이금속막의 표면을 암모니아가스로 식각시켜 상기 전이금속막의 표면에 미세한 그레인을 형성시킨 후, 상기 미세한 그레인위에 550 - 1100℃ 범위의 온도에서 아세틸렌가스 또는 탄화가스를 반응시켜, 상기 전이금속막위에 탄소나노튜브를 수직방향으로 정렬시켜 성장시킨다. 본 발명에 의한 화학기상증착장치는 기존의 전기방전장치, 레이저증착장치, 플라즈마 화학기상증착장치, 열화학기상증착장치에 비해서 대면적 기판위에서 탄소나노튜브를 대량으로 합성시키는 것이 가능하기 때문에 탄소나노튜브의 대량생산에 유리한 방법이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a chemical vapor deposition apparatus for mass synthesis of carbon nanotubes, and more particularly, to a device for synthesizing a large amount of carbon nanotubes on several large-area substrates using thermochemical vapor deposition. The chemical vapor deposition apparatus for mass synthesis of carbon nanotubes according to the present invention is manufactured in a large rectangular parallelepiped form, unlike a conventional tube, to synthesize carbon nanotubes. It consists of a cuboid boat that can be placed. In the synthesis of carbon nanotubes using the chemical vapor deposition apparatus according to the present invention, after depositing a transition metal film on a large-area substrate, mounting the substrate on which the transition metal film is deposited in a boat, and then placing the boat into the reactor, The surface of the transition metal film is etched with ammonia gas using a pyrolysis method at atmospheric pressure or low pressure to form fine grains on the surface of the transition metal film, followed by acetylene gas or carbonized gas at a temperature in the range of 550-1100 ° C. Is reacted and grown by aligning carbon nanotubes vertically on the transition metal film. The chemical vapor deposition apparatus according to the present invention is capable of synthesizing a large amount of carbon nanotubes on a large-area substrate, compared to conventional electric discharge apparatuses, laser deposition apparatuses, plasma chemical vapor deposition apparatuses, and thermochemical vapor deposition apparatuses. Is an advantageous method for mass production.

Description

탄소나노튜브의 대량합성을 위한 화학기상증착장치.{Chemical vapor deposition system for massive synthesis of carbon nanotubes}Chemical vapor deposition system for mass synthesis of carbon nanotubes. {Chemical vapor deposition system for massive synthesis of carbon nanotubes}

본 발명은 대면적 기판위에서 탄소나노튜브를 대량으로 합성하기 위한 화학기상증착장치를 제공하는데 있다.The present invention provides a chemical vapor deposition apparatus for synthesizing a large amount of carbon nanotubes on a large area substrate.

본 발명은 탄소나노튜브의 대량합성을 위한 화학기상증착장치에 관한 것으로써, 특히 열화학기상증착법을 이용하여 여러개의 대면적 기판위에서 탄소나노튜브를 대량으로 합성시키는 장치에 관한 것이다. 근래에 탄소나노튜브 합성에 관한 여러 가지 방법이 제안되었고 이러한 방법을 실현시키기 위한 여러 가지 장치가 사용되고 있는데, 현재 사용되고 있는 대부분의 전기방전장치, 레이저증착장치, 플라즈마 화학기상증착장치, 열화학기상증착장치 등은 여러장의 대면적 기판에 탄소나노튜브를 합성시키는 것이 불가능하기 때문에 탄소나노튜브의 대면적 성장에 한계가 있다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a chemical vapor deposition apparatus for mass synthesis of carbon nanotubes, and more particularly, to a device for synthesizing a large amount of carbon nanotubes on several large-area substrates using thermochemical vapor deposition. Recently, various methods for synthesizing carbon nanotubes have been proposed, and various apparatuses have been used to realize these methods. Most of the current electric discharge apparatuses, laser deposition apparatuses, plasma chemical vapor deposition apparatuses and thermochemical vapor deposition apparatuses are used. The back is limited in the large-area growth of carbon nanotubes because it is impossible to synthesize the carbon nanotubes on several large-area substrates.

본 발명은 상기 문제점을 해결하기 위하여 창출한 것으로써, 탄소나노튜브의 대량합성을 위한 화학기상증착장치의 반응로가 기존의 튜브형태와 달리 대면적인 직육면체형태로 구성되고 또한 보트는 대면적 기판을 수평으로 평행하게 여러장 놓을 수 있는 형태로 구성된다. 본 발명에 의한 화학기상증착장치를 사용하면 전이금속막이 증착된 대면적 글라스기판 또는 알루미나 기판 또는 실리콘 기판위에 열화학기상증착법으로 아세틸렌 등의 탄화가스를 분해시켜 기판에 수직방향으로 정렬된 탄소나노튜브를 합성시킬 수 있다.The present invention was created in order to solve the above problems, the chemical vapor deposition apparatus for the mass synthesis of carbon nanotubes, unlike the conventional tube form is composed of a large rectangular parallelepiped shape and the boat is a large area substrate It consists of a form that can be placed in parallel to several horizontally. When the chemical vapor deposition apparatus according to the present invention is used, carbon nanotubes aligned in a direction perpendicular to the substrate are decomposed by decomposing carbonaceous gases such as acetylene on a large-area glass substrate or an alumina substrate or a silicon substrate on which a transition metal film is deposited. Can be synthesized.

도 1은 본 발명에 따른 탄소나노튜브를 대량합성하는 화학기상증착장치의 구조도이다.1 is a structural diagram of a chemical vapor deposition apparatus for mass synthesis of carbon nanotubes according to the present invention.

도 2는 본 발명에 따른 대면적 기판을 여러장 장착할 수 있는 화학기상증착장치에 부속된 보트의 구조도이다.2 is a structural diagram of a boat attached to a chemical vapor deposition apparatus that can be mounted to a large area substrate in accordance with the present invention.

상기 목적을 달성하기 위한 본 발명에 따른 탄소나노튜브의 대량합성을 위한 화학기상증착장치는 [도 1]에 나타낸 바와같이 가스공급부와 반응로와 가스배기부로 구성된다. 가스공급부에는 반응가스유량을 조절하기 위한 밸브가 설치되어 있다. 반응로는 기존의 튜브형태와 달리 대면적인 직육면체형태로 구성되어 대면적의 편평한 기판을 반응로에 집어넣을수 있고, 직육면체인 반응로의 외부에는 열에너지를 공급하기 위한 저항코일이 설치되어 있으며 반응로내에는 [도 2]에 나타낸 바와 같이 대면적 기판을 수평으로 평행하게 여러장 놓을 수 있는 형태인 석영보트가 장착된다. 가스 배기부에는 반응 후 배기가스의 유량을 조절할 수 있는 밸브가 설치되어 있고 저압에서 탄소나노튜브를 합성할 경우에는 로터리펌프를 설치하여 가스를 외부로 배출시킨다. 본 발명에 의한 화학기상증착장치를 사용하면 전이금속막이 증착된 여러장의 대면적 글라스 기판위에 열화학기상증착법으로 아세틸렌 등의 탄화가스를 분해시켜 기판에 수직방향으로 정렬된 탄소나노튜브를 합성시킬 수 있다.Chemical vapor deposition apparatus for mass synthesis of carbon nanotubes according to the present invention for achieving the above object is composed of a gas supply unit, a reactor and a gas exhaust unit as shown in FIG. The gas supply unit is provided with a valve for adjusting the reaction gas flow rate. Unlike the existing tube type, the reactor is composed of a large rectangular parallelepiped that can put a large-area flat substrate into the reactor, and a resistance coil for supplying thermal energy is installed outside the rectangular reactor. As shown in FIG. 2, the quartz boat is mounted in such a way that a large-area substrate can be placed in parallel and in parallel. The gas exhaust part is provided with a valve for controlling the flow rate of the exhaust gas after the reaction, and when synthesizing carbon nanotubes at low pressure, a rotary pump is installed to discharge the gas to the outside. When the chemical vapor deposition apparatus according to the present invention is used, carbon nanotubes aligned in a direction perpendicular to the substrate can be synthesized by decomposing carbonaceous gases such as acetylene on a large-area glass substrate on which a transition metal film is deposited by thermochemical vapor deposition. .

실제로 본 발명에 의한 화학기상증착장치를 사용한 탄소나노튜브의 대량합성은, 글라스또는 알루미나 또는 실리콘 등의 대면적 기판(1)위에 코발트-니켈 합금의 전이금속막(2)을 열증착법이나 스퍼터링법을 사용하여 약 50 - 200 nm 증착시키고 나서, 상기 전이금속막(2)을 석영보트에 올려놓은 후, 반응로안으로 석영보트를 집어넣은 다음, 700 - 1100℃ 온도범위에서 상기 반응로내부로 암모니아가스를 80 - 1000 sccm 범위로 공급하여 반응로의 압력을 0.1 - 수십 Torr 정도의 저압으로 유지하면서 10 - 30 min 동안 상기 전이금속막(2)의 표면을 식각시켜 표면에 미세한 그레인을 형성시킨 후, 이어서 열화학기상증착장치의 반응로 온도가 500 - 1100 ℃ 범위에서 아세틸렌가스, 메탄가스, 프로판가스, 또는 에틸렌가스등의 탄화가스를 20 - 500 sccm 범위로 흘려주어 반응로의 압력을 0.1 - 수십 Torr 정도로 유지시키면서 10 - 60 min 동안 상기 전이금속막(2) 표면의 미세한 그레인위에 수직방향으로 정렬된 탄소나노튜브(3)를 합성시킨다. 이어서 상기 탄소나노튜브(3)의 끝부분에 존재하는 전이금속 덩어리와 탄소나노튜브의 표면에 존재하는 탄소파티클을 제거하기 위하여 500- 1000 ℃ 온도범위에서 상기 반응로내부로 암모니아가스를 80 - 1000 sccm 범위로 10 - 30 min 동안 공급함으로써, 상기 탄소나노튜브(3)의 끝부분에 존재하는 전이금속 덩어리와 탄소나노튜브의 표면에 존재하는 탄소파티클을 깨끗하게 제거시킨다.In practice, the mass synthesis of carbon nanotubes using the chemical vapor deposition apparatus according to the present invention is carried out by thermally depositing or sputtering a transition metal film 2 of cobalt-nickel alloy on a large-area substrate 1 such as glass or alumina or silicon. Using about 50-200 nm, and then put the transition metal film (2) on a quartz boat, put a quartz boat into the reactor, and then ammonia into the reactor in the temperature range of 700-1100 ℃ After supplying the gas in the range of 80-1000 sccm, the surface of the transition metal film 2 was etched for 10-30 min while maintaining the pressure of the reactor at a low pressure of about 0.1-several tens of Torr to form fine grain on the surface. Then, the reaction furnace of the thermochemical vapor deposition apparatus flows carbonized gas such as acetylene gas, methane gas, propane gas, or ethylene gas in the range of 500-1100 ° C. in the range of 20-500 sccm. The pressure 0.1 - 60 min to thereby synthesize the transition metal film (2) of carbon arranged in the vertical direction on the surface of the fine grain nanotubes for 3-tens maintaining about 10 Torr. Subsequently, in order to remove the transition metal lumps present at the end of the carbon nanotubes (3) and the carbon particles present on the surfaces of the carbon nanotubes, ammonia gas was introduced into the reactor in the temperature range of 500-1000 ° C. By supplying the sccm in the range of 10-30 min, the transition metal lumps present at the ends of the carbon nanotubes 3 and the carbon particles present on the surfaces of the carbon nanotubes are cleanly removed.

상술한 바와 같이 본 발명에 따른 탄소나노튜브의 대량합성을 위한 화학기상증착장치는 반응로가 기존의 튜브형태와 달리 대면적인 직육면체형태로 구성되고 또한 보트는 대면적 기판을 수평으로 평행하게 여러장 놓을 수 있는 형태로 구성됨으로써, 전이금속막이 증착된 다수의 대면적 기판위에 열화학기상증착법으로 아세틸렌 등의 탄화가스를 분해시켜 기판에 수직방향으로 정렬된 탄소나노튜브를 대량으로 합성시킬 수 있다.As described above, the chemical vapor deposition apparatus for mass synthesis of carbon nanotubes according to the present invention has a large rectangular parallelepiped shape in which the reactor is different from the conventional tube type, and the boat has several sheets horizontally parallel to the large-area substrate. Since the carbon nanotubes are arranged in a form that can be placed, carbon nanotubes aligned vertically to the substrate can be synthesized in a large amount by decomposing carbonic acid gas such as acetylene on the large-area substrate on which the transition metal film is deposited by thermochemical vapor deposition.

Claims (4)

반응로가 기존의 튜브형태와 달리 대면적인 직육면체형태로 제작되고 또한 반응로내에 대면적 기판을 수평으로 평행하게 여러장 놓을 수 있는 형태인 보트로 구성된 화학기상증착장치의 제작.Unlike conventional tubes, the reactor is manufactured in a large rectangular parallelepiped form and a chemical vapor deposition apparatus is constructed of boats in which multiple large substrates can be placed horizontally and parallel in the reactor. 제1항에 있어서, 상기 화학기상증착장치를 사용하여 상압 또는 저압에서 탄화가스를 사용하여 전이금속막위에서 탄소나노튜브를 대량으로 합성하는 방법.The method according to claim 1, wherein the chemical vapor deposition apparatus is used to synthesize carbon nanotubes in large quantities on a transition metal film using carbonized gas at atmospheric pressure or low pressure. 제2항에 있어서, 전이금속막의 표면에 미세한 그레인을 형성시키는 방법과 상기 전이금속막의 미세한 그레인위에 저압에서 아세틸렌등의 탄화가스를 사용하여 탄소나노튜브를 수직방향으로 정렬시켜 합성하는 방법과 상기 탄소나노튜브를 합성한 후, 암모니아 가스또는 수소가스를 사용하여 상기 탄소나노튜브의 표면에 부착된 전이금속덩어리와 탄소파티클을 제거하는 방법을 구비하는 상기 화학기상증착장치를 이용한 탄소나노튜브의 대량합성법.The method of claim 2, wherein the method comprises forming fine grains on the surface of the transition metal film and synthesizing the carbon nanotubes in a vertical direction by using carbonization gas such as acetylene at low pressure on the fine grains of the transition metal film. After synthesizing the nanotubes, a mass synthesis method of carbon nanotubes using the chemical vapor deposition apparatus comprising a method for removing transition metal masses and carbon particles attached to the surface of the carbon nanotubes using ammonia gas or hydrogen gas. . 제2항에 있어서, 전이금속막은 코발트-니켈 합금, 코발트, 니켈, 철, 이트륨, 코발트-니켈-철 합금, 코발트-철 합금, 니켈-철 합금, 코발트-니켈-이트륨 합금, 코발트-이트륨 합금등을 포함하는 방법.The transition metal film of claim 2, wherein the transition metal film is cobalt-nickel alloy, cobalt, nickel, iron, yttrium, cobalt-nickel-iron alloy, cobalt-iron alloy, nickel-iron alloy, cobalt-nickel-yttrium alloy, cobalt-yttrium alloy And the like.
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