KR100477506B1 - Method for the growth of vertically aligned single carbon nanotube by electron beam - Google Patents
Method for the growth of vertically aligned single carbon nanotube by electron beam Download PDFInfo
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- KR100477506B1 KR100477506B1 KR10-2002-0073749A KR20020073749A KR100477506B1 KR 100477506 B1 KR100477506 B1 KR 100477506B1 KR 20020073749 A KR20020073749 A KR 20020073749A KR 100477506 B1 KR100477506 B1 KR 100477506B1
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Abstract
본 발명은 전자빔에 의해 국부적으로 열을 인가하여 수직 정렬 성장된 단일 탄소 나노튜브를 제조하는 방법에 관한 것이다. The present invention relates to a method for producing vertically grown single carbon nanotubes by applying heat locally by an electron beam.
본 발명의 전자빔을 이용한 단일 탄소 나노튜브의 수직 정렬 성장 제조방법은 Si 웨이퍼 또는 유리기판 위에 촉매물질인 나노 입자 혼합용액을 도포하는 단계(10); 상기 혼합용액의 나노 입자물질이 기판에 접착되도록 열처리하는 단계(20); 상기 열처리된 기판을 전자빔 발생장치의 챔버에 넣는 단계(30); 상기 챔버를 메탄과 수소의 혼합기체 분위기로 만들어 주는 단계; 및 탄소 나노튜브가 성장할 위치를 찾은 다음, 원하는 탄소 나노튜브의 성장 길이만큼의 시간동안 전자빔을 조사하여 단일 탄소 나노튜브를 성장시키는 단계(40)를 포함하여 이루어짐에 기술적 특징이 있다.Method for producing a vertical alignment growth of a single carbon nanotube using an electron beam of the present invention comprises the steps of applying a nanoparticle mixed solution as a catalyst material on a Si wafer or a glass substrate (10); Heat treating the nanoparticle material of the mixed solution to adhere to the substrate (20); Placing the heat-treated substrate in a chamber of an electron beam generator (30); Making the chamber a mixed gas atmosphere of methane and hydrogen; And finding 40 a position to grow the carbon nanotubes, and then irradiating the electron beam for a time as long as the desired growth length of the carbon nanotubes to grow a single carbon nanotube 40.
따라서, 본 발명의 전자빔을 이용한 단일 탄소 나노튜브의 수직 정렬 성장 제조방법은 촉매물질에 열을 인가할 때 전자빔을 이용함으로써 기판 전체가 아니라 탄소 나노튜브가 성장될 곳에 국부적으로 열반응이 일어나기 때문에 열이 약한 소재에도 탄소 나노튜브를 성장시킬 수 있고 원하는 특정 위치에만 단일 탄소 나노튜브를 성장시킬 수 있다는 장점이 있다.Therefore, the vertical alignment growth production method of a single carbon nanotube using the electron beam of the present invention is because the thermal reaction occurs locally where the carbon nanotubes are grown, not the entire substrate, by using the electron beam when heat is applied to the catalyst material. This weak material has the advantage of growing carbon nanotubes and growing single carbon nanotubes only at specific locations.
Description
본 발명은 전자빔을 이용한 단일 탄소 나노튜브의 수직 정렬 성장 제조방법에 관한 것으로, 보다 자세하게는 Si 웨이퍼나 유리와 같은 기판에 촉매물질을 도포하고, 전자빔을 조사하여 원하는 위치에 탄소 나노튜브를 수직 정렬 성장시키는 기술에 관한 것이다.The present invention relates to a method for manufacturing vertically aligned growth of a single carbon nanotube using an electron beam, and more particularly, to apply a catalytic material to a substrate such as a Si wafer or glass, and irradiate the electron beam to vertically align the carbon nanotube at a desired position. It is about growing technology.
종래에는 탄소 나노튜브를 수직 성장시키기 위하여 CH4, C2H2와 같은 탄화수소기체를 사용하여 900℃이상의 고온에서 기판 위에 탄소 나노튜브를 형성하는 것으로서, 성장온도가 높다는 단점이 있었다. 미국 등록특허 제6,350,488호에서는 열 화학기상증착(Thermal CVD, CVD:Chemical Vapor Deposition)에 의한 탄소 나노튜브의 수직 정렬 성장에 대한 연구를 개시하고 있고, Science 282(1998) 1105에서는 촉매금속을 기판위에 증착시킨 후 암모니아와 수소기체로 식각시켜 나노 입자를 형성하고, 여기에 열을 인가한 후 CH4, C2H2, C2H6 ,CO 등의 반응가스를 공급하면서 양전극에 고주파 전원을 인가하여 글로우 방전을 일으킴으로써 탄소 나노튜브를 합성하는 연구에 대한 것이다.Conventionally, in order to vertically grow carbon nanotubes, carbon nanotubes are formed on a substrate at a high temperature of 900 ° C. or more using a hydrocarbon gas such as CH 4 , C 2 H 2, and the growth temperature is high. U.S. Patent No. 6,350,488 discloses a study on the vertical alignment growth of carbon nanotubes by thermal CVD (Chemical Vapor Deposition), and Science 282 (1998) 1105 discloses catalytic metal on a substrate. After deposition, the nanoparticles are formed by etching with ammonia and hydrogen gas, heat is applied thereto, and high frequency power is applied to both electrodes while supplying a reaction gas such as CH 4 , C 2 H 2 , C 2 H 6 , and CO. To synthesize carbon nanotubes by causing a glow discharge.
그러나, 상기와 같은 종래의 탄소 나노튜브를 성장시키는 기술은 기판 전체에 열을 인가하여 촉매물질을 반응시켜야 하기 때문에, 열에 약한 기판 소재의 물리적, 화학적 변형이 일어나게 되고, 또한 열이 기판전체에 인가되기 때문에 온도의 균일성이 떨어져서 균일한 크기의 탄소 나노튜브를 성장시킬 수 없다는 문제점이 있다.However, the conventional carbon nanotube growth technique requires applying a heat to the entire substrate to react the catalyst material, so that physical and chemical deformation of the substrate material that is weak to heat occurs, and heat is applied to the entire substrate. Because of this, there is a problem in that the uniformity of temperature is inferior so that carbon nanotubes of uniform size cannot be grown.
따라서, 본 발명은 상기와 같은 종래 기술의 제반 단점과 문제점을 해결하기 위한 것으로, 탄소 나노튜브를 성장시킬 때 기판 전체에 열을 인가하지 않고 전자빔에 의해 국부적으로 열을 인가함으로써 원하는 위치에 원하는 성장길이 만큼의 단일 탄소 나노튜브를 수직 정렬되도록 성장시킬 수 있는 방법을 제공함에 본 발명의 목적이 있다. Accordingly, the present invention is to solve the above disadvantages and problems of the prior art, and when growing carbon nanotubes, the desired growth at a desired position by applying heat locally with an electron beam without applying heat to the entire substrate. It is an object of the present invention to provide a method capable of growing a single carbon nanotube by length in vertical alignment.
본 발명의 상기 목적은 Si 웨이퍼나 유리와 같은 기판(1)에 촉매물질(2)이 도포되고 여기에 국부적으로 전자빔(4)을 조사하여 성장되는 전자빔을 이용한 단일 탄소 나노튜브(3)의 수직 정렬 성장 제조방법에 의해 달성된다.The above object of the present invention is the verticality of a single carbon nanotube (3) using an electron beam which is grown by irradiating an electron beam (4) on a catalyst material (2) applied to a substrate (1), such as a Si wafer or glass. Achievement is achieved by an alignment growth manufacturing method.
본 발명의 전자빔을 이용한 단일 탄소 나노튜브의 수직 정렬 성장 제조방법은 Si 웨이퍼 또는 유리기판 위에 촉매물질인 나노 입자 혼합용액을 도포하는 단계(10); 상기 혼합용액의 나노 입자물질이 기판에 접착되도록 열처리하는 단계(20); 상기 열처리된 기판을 전자빔 발생장치의 챔버에 넣는 단계(30); 상기 챔버를 메탄과 수소의 혼합기체 분위기로 만들어 주는 단계; 및 탄소 나노튜브가 성장할 위치를 결정하여 원하는 탄소 나노튜브의 성장 길이만큼의 시간동안 전자빔을 조사하여 단일 탄소 나노튜브를 성장시키는 단계(40)를 포함하여 이루어진 제조방법으로서, 촉매물질에 열을 인가할 때 전자빔을 이용함으로써 기판 전체가 아니라 탄소 나노튜브가 성장될 곳에 국부적으로 열반응이 일어나기 때문에 열이 약한 소재에도 탄소 나노튜브를 성장시킬 수 있고 원하는 특정 위치에만 단일 탄소 나노튜브를 성장시킬 수 있는 제조방법이다.Method for producing a vertical alignment growth of a single carbon nanotube using an electron beam of the present invention comprises the steps of applying a nanoparticle mixed solution as a catalyst material on a Si wafer or a glass substrate (10); Heat treating the nanoparticle material of the mixed solution to adhere to the substrate (20); Placing the heat-treated substrate in a chamber of an electron beam generator (30); Making the chamber a mixed gas atmosphere of methane and hydrogen; And determining a location where the carbon nanotubes are to be grown to grow a single carbon nanotube by irradiating an electron beam for a time length corresponding to the growth length of the desired carbon nanotubes, wherein the heat is applied to the catalyst material. When the electron beam is used, the thermal reaction occurs locally where the carbon nanotubes are grown, not the entire substrate, so that the carbon nanotubes can be grown on a weak material and a single carbon nanotube can be grown only at a specific position. It is a manufacturing method.
본 발명의 상기 목적과 기술적 구성 및 그에 따른 작용효과에 관한 자세한 사항은 본 발명의 명세서에 첨부된 도면을 참조한 이하 상세한 설명에 의해 보다 명확하게 이해될 것이다.Details of the above object and technical configuration of the present invention and the effects thereof according to the present invention will be more clearly understood by the following detailed description with reference to the accompanying drawings.
먼저, 도 1은 본 발명에 의해 수직 정렬 성장된 단일 탄소 나노튜브의 개념도이다. 즉, Si 웨이퍼나 유리와 같은 기판(1)에 나노 입자의 촉매물질이 도포, 접착되어 있고, 여기에 전자빔(4)의 조사에 의하여 성장시키고자 하는 위치에 단일 탄소 나노튜브(3)가 수직 정렬 성장되어 있다.First, FIG. 1 is a conceptual diagram of a single carbon nanotube grown vertically by the present invention. That is, a nanoparticle catalyst material is applied and adhered to a substrate 1 such as Si wafer or glass, and a single carbon nanotube 3 is perpendicular to a position to be grown by irradiation of the electron beam 4. The alignment is growing.
다음, 도2는 본 발명에 의한 탄소 나노튜브의 제조방법을 나타낸 플로우 차트이다. Next, Figure 2 is a flow chart showing a method of manufacturing carbon nanotubes according to the present invention.
Si 웨이퍼 또는 유리기판 위에 촉매물질인 나노 입자 혼합용액을 도포하는 단계(10); 상기 혼합용액의 나노 입자물질이 기판에 접착되도록 열처리하는 단계(20); 상기 열처리된 기판을 전자빔 발생장치의 챔버에 넣는 단계(30); 상기 챔버를 메탄과 수소의 혼합기체 분위기로 만들어 주는 단계; 및 단일 탄소 나노튜브가 성장할 위치에 전자빔을 조사하여 단일 탄소 나노튜브를 성장시키는 단계(40)를 포함하는 본 발명의 전자빔을 이용한 단일 탄소 나노튜브의 수직 정렬 성장 제조방법을 나타내고 있다.Applying (10) a nanoparticle mixed solution that is a catalyst material on a Si wafer or a glass substrate; Heat treating the nanoparticle material of the mixed solution to adhere to the substrate (20); Placing the heat-treated substrate in a chamber of an electron beam generator (30); Making the chamber a mixed gas atmosphere of methane and hydrogen; And irradiating the electron beam to the position where the single carbon nanotubes are to be grown to grow a single carbon nanotube (40).
즉, 단일 탄소나노튜브를 성장시키고자 하는 기판 위에 탄소 나노튜브의 성장 촉매제인 나노 입자 혼합용액을 도포(10)하고, 탄소 나노튜브가 성장될 수 있도록 이 나노 입자의 혼합용액이 기판에 접착(20)되어 열처리 해주어야 하는데, 이 때의 상기 Si 웨이퍼 또는 유리기판 위에 도포되는 촉매물질인 나노 입자의 혼합 용액은 메탄올 15ml에 나노 사이즈의 알루미나(Alumina) 20mg과 Fe(NO3)3·9H 2O 20mg 및 MoO(acac)2 2mg으로 이루어져 있으며, 이러한 물질들을 혼합한 후 다시 초음파 처리하여 균질한 혼합 용액을 만들어 준다. 이 때 나노 입자 혼합용액이 혼합되는 시간은 바람직하게는 23∼25시간이며, 이 혼합된 용액을 다시 1시간 동안 초음파 처리한다.That is, a nanoparticle mixed solution, which is a carbon nanotube growth catalyst, is applied onto a substrate on which a single carbon nanotube is to be grown (10), and the mixed solution of the nanoparticles is adhered to the substrate so that the carbon nanotubes can be grown. 20) and heat treatment, wherein the mixed solution of nanoparticles, which is a catalyst material applied on the Si wafer or glass substrate, is 20 mg of alumina (Alumina) and Fe (NO 3 ) 3 · 9H 2 O It consists of 20mg and 2Omg of MoO (acac) 2 and mixes these materials and sonicates again to make a homogeneous mixture solution. At this time, the mixing time of the nanoparticle mixed solution is preferably 23 to 25 hours, and the mixed solution is sonicated again for 1 hour.
또한 상기 촉매물질인 혼합용액의 나노 입자물질이 기판에 접착되도록 열처리하는 단계(20)는 상기 기판에 도포된 나노 입자의 혼합 용액이 상온에서 용매 증발되도록 상온에서 기판을 방치하는 단계와 상기 용매증발된 기판을 열처리하는 단계로 다시 나뉘어 진다. 이때 용매증발된 나노 입자를 기판에 접착시키기 위한 열처리는 160℃∼180℃에서 3∼7분 동안 행해진다.In addition, the step (20) of heat treatment so that the nanoparticle material of the mixed solution as the catalyst material is adhered to the substrate, leaving the substrate at room temperature so that the mixed solution of the nanoparticles applied to the substrate is solvent evaporated at room temperature and the solvent evaporation. The substrate is divided into heat treatment steps. At this time, the heat treatment for bonding the solvent-evaporated nanoparticles to the substrate is performed for 3 to 7 minutes at 160 ℃ to 180 ℃.
이와 같이 탄소 나노튜브가 성장될 수 있도록 촉매물질을 도포하고 열처리를 통하여 기판에 촉매물질이 접착되면, 이 기판을 전자빔 발생장치의 챔버에 넣고(30) 챔버를 메탄과 수소의 혼합기체 분위기로 만들어 준다. 이 때의 혼합기체는 99.999%의 고순도의 메탄 기체를 포함하는 것으로 한다.When the catalyst material is applied to the carbon nanotubes to be grown and the catalyst material is adhered to the substrate through heat treatment, the substrate is placed in the chamber of the electron beam generator (30) and the chamber is made into a mixed gas atmosphere of methane and hydrogen. give. The mixed gas at this time is assumed to contain high purity methane gas of 99.999%.
최종적으로, 상기와 같이 준비된 기판에 전자빔을 조사하여 수직 정렬 성장되는 탄소 나노튜브를 얻게 되는데(40), 이 때 단일 탄소 나노튜브의 성장 길이는 전자빔의 강도 및 조사하는 시간에 따라 조절된다.Finally, the substrate prepared as described above is irradiated with an electron beam to obtain carbon nanotubes grown vertically aligned (40), wherein the growth length of the single carbon nanotubes is controlled according to the intensity of the electron beam and the irradiation time.
따라서, 본 발명의 전자빔을 이용한 단일 탄소 나노튜브의 수직 정렬 성장 제조방법은 기판 위에 탄소 나노튜브를 형성하기 위하여 촉매물질에 열을 인가할 때 전자빔을 이용함으로써 기판 전체가 아닌 국부적인 열반응을 일으켜 탄소 나노튜브를 수직 정렬 성장시키기 때문에 열이 약한 소재에도 탄소 나노튜브를 성장시킬 수 있고 원하는 특정 위치에만 단일 탄소 나노튜브를 성장시킬 수 있다는 장점이 있다.Accordingly, the method for producing vertically aligned growth of a single carbon nanotube using the electron beam of the present invention causes local thermal reactions rather than the entire substrate by using an electron beam when heat is applied to the catalyst material to form carbon nanotubes on the substrate. The vertical alignment growth of carbon nanotubes allows the growth of carbon nanotubes even on materials with low heat and the ability to grow single carbon nanotubes only at specific locations.
도 1은 본 발명에 의해 수직 정렬 성장된 단일 탄소 나노튜브의 개념도이다.1 is a conceptual diagram of a single carbon nanotube grown vertically by the present invention.
도 2는 본 발명에 의한 탄소 나노튜브의 제조방법을 나타낸 플로우 차트이다.2 is a flow chart showing a method for producing carbon nanotubes according to the present invention.
((도면의 주요부분에 대한 부호의 설명))((Explanation of symbols for main parts of drawing))
1. 기판 2. 촉매물질1. Substrate 2. Catalyst
3. 탄소 나노튜브 4. 전자빔3. Carbon Nanotubes 4. Electron Beams
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| JPH08217431A (en) * | 1995-02-09 | 1996-08-27 | Res Dev Corp Of Japan | Fullerene and method for producing the same |
| JPH11106208A (en) * | 1996-02-13 | 1999-04-20 | Agency Of Ind Science & Technol | Recovery of carbon nanotube |
| JPH11349307A (en) * | 1998-06-05 | 1999-12-21 | Osaka Gas Co Ltd | Production of functional carbonaceous material |
| KR20010091389A (en) * | 2000-03-15 | 2001-10-23 | 이영희 | Method for depositing a vertically aligned carbon nanotubes using thermal chemical vapor deposition |
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| JPH11106208A (en) * | 1996-02-13 | 1999-04-20 | Agency Of Ind Science & Technol | Recovery of carbon nanotube |
| JPH11349307A (en) * | 1998-06-05 | 1999-12-21 | Osaka Gas Co Ltd | Production of functional carbonaceous material |
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