KR20050121426A - Method for preparing catalyst for manufacturing carbon nano tubes - Google Patents

Method for preparing catalyst for manufacturing carbon nano tubes Download PDF

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KR20050121426A
KR20050121426A KR1020040046552A KR20040046552A KR20050121426A KR 20050121426 A KR20050121426 A KR 20050121426A KR 1020040046552 A KR1020040046552 A KR 1020040046552A KR 20040046552 A KR20040046552 A KR 20040046552A KR 20050121426 A KR20050121426 A KR 20050121426A
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catalyst
metal precursor
catalyst metal
substrate
precursor solution
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KR1020040046552A
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Korean (ko)
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한인택
김하진
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삼성에스디아이 주식회사
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Priority to KR1020040046552A priority Critical patent/KR20050121426A/en
Priority to CNA2005100794134A priority patent/CN1883807A/en
Priority to JP2005180590A priority patent/JP2006007213A/en
Priority to US11/158,047 priority patent/US20070020167A1/en
Publication of KR20050121426A publication Critical patent/KR20050121426A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y99/00—Subject matter not provided for in other groups of this subclass

Abstract

본 발명에서는, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 기판 위에 더욱 균일하게 형성시킬 수 있는 새로운 방법과, 균일도가 향상된 카본나노튜브 합성 방법을 제공한다. 본 발명에서 제공하는 촉매 미립자 형성 방법은, 촉매금속 전구체 용액을 기판 위에 도포하는 단계; 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조하는 단계; 및 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시키는 단계를 포함한다. 본 발명의 촉매 미립자 형성 방법은, 촉매금속 전구체 용액을 냉동건조하므로써, 촉매 미립자 형성 과정에서의 촉매 미립자의 응집 및/또는 재결정을 최소화시킬 수 있다. 그리하여, 본 발명의 방법으로 형성된 촉매 미립자는, 매우 균일한 입자크기를 가지며, 또한 기판 위에 매우 균일하게 분포된다. The present invention provides a novel method for more uniformly forming catalyst fine particles, which are the basis of carbon nanotube growth, on a substrate, and a method for synthesizing carbon nanotubes with improved uniformity. The catalyst fine particle forming method provided by the present invention comprises the steps of applying a catalyst metal precursor solution on a substrate; Freeze-drying the catalyst metal precursor solution applied on the substrate; And reducing the lyophilized catalyst metal precursor to the catalyst metal. The catalyst fine particle formation method of the present invention can minimize the aggregation and / or recrystallization of the catalyst fine particles in the catalyst fine particle formation process by freeze-drying the catalyst metal precursor solution. Thus, the catalyst fine particles formed by the method of the present invention have a very uniform particle size and are distributed very uniformly on the substrate.

Description

탄소나노튜브 제조용 촉매의 제조 방법{Method for preparing catalyst for manufacturing carbon nano tubes}Method for preparing catalyst for manufacturing carbon nanotubes

본 발명은 탄소나노튜브 제조용 촉매의 제조 방법과, 이를 이용한 탄소나노튜브 제조 방법에 관한 것이다.The present invention relates to a method for producing a carbon nanotube catalyst and a method for producing carbon nanotubes using the same.

탄소나노튜브는 보통 수 nm 정도의 매우 미세한 직경과 약 10 내지 약 1,000 정도의 매우 큰 종횡비를 갖는 원통형 재료이다. 탄소나노튜브에 있어서, 일반적으로, 탄소원자들은 육각형 벌집구조로 배열되어 있으며, 각각의 탄소원자는 인접하는 3 개의 탄소원자와 결합하고 있다. 탄소나노튜브는, 그 구조에 따라서, 도체의 성질 또는 반도체의 성질을 가질 수 있다. 도체의 성질을 띠는 탄소나노튜브의 전기전도도는 매우 우수한 것으로 알려져 있다. 또한, 탄소나노튜브는 매우 강한 기계적 강도, 테라 단위의 영률(Young's modulus), 우수한 열전도도 등의 특성을 갖는다. 이러한 우수한 특성을 갖는 탄소나노튜브는, 예를 들면, FED의 에미터, 2차전지용 음극 재료, 연료 전지의 촉매 담지체, 고강도 복합소자, 등과 같은 다양한 기술분야에 매우 유리하게 사용될 수 있다. Carbon nanotubes are usually cylindrical materials having very fine diameters on the order of several nm and very large aspect ratios on the order of about 10 to about 1,000. In carbon nanotubes, in general, carbon atoms are arranged in a hexagonal honeycomb structure, and each carbon atom is bonded to three adjacent carbon atoms. Carbon nanotubes may have properties of a conductor or properties of a semiconductor, depending on their structure. It is known that the electrical conductivity of carbon nanotubes having a conductor property is very excellent. In addition, carbon nanotubes have very strong mechanical strength, Young's modulus in tera units, and excellent thermal conductivity. Carbon nanotubes having such excellent properties can be very advantageously used in various technical fields such as, for example, emitters of FEDs, anode materials for secondary batteries, catalyst carriers for fuel cells, high strength composite devices, and the like.

탄소나노튜브의 제조 방법으로서는, 전기방전법, 레이저증착법, 플라즈마 화학기상증착법, 화학기상증착법, 기상합성법, 전기분해법 등이 알려져 있다. As a method of producing carbon nanotubes, an electric discharge method, a laser deposition method, a plasma chemical vapor deposition method, a chemical vapor deposition method, a gas phase synthesis method, an electrolysis method and the like are known.

기상합성법은, 기판을 사용하지 않고, 반응로 안에 반응가스와 촉매금속을 직접 공급하여 기상에서 합성하는 방법으로서 탄소나노튜브를 벌크 형태로 합성하기에 적합한 방법이다. 전기방전법과 레이저증착법은 탄소나노튜브의 합성 수율이 비교적 낮다. 전기방전법과 레이저증착법으로는, 탄소나노튜브의 직경과 길이를 조절하는 것이 용이하지 않다. 또한, 전기방전법과 레이저증착법을 사용하면, 탄소나노튜브 뿐만아니라 비정질 탄소 덩어리가 다량으로 생성되기 때문에, 반드시 복잡한 정제과정이 수반되어야 한다. The gas phase synthesis method is a method for synthesizing carbon nanotubes in bulk form by directly supplying a reaction gas and a catalyst metal into a reactor without using a substrate and synthesizing it in the gas phase. Electro discharge and laser deposition have relatively low yields of carbon nanotubes. In the electric discharge method and the laser deposition method, it is not easy to control the diameter and length of the carbon nanotubes. In addition, when the electric discharge method and the laser deposition method are used, since a large amount of amorphous carbon as well as carbon nanotubes are generated, a complicated purification process must be accompanied.

기판 위에 탄소나노튜브를 형성시키기 위해서는 일반적으로, 예를 들면, 열화학기상증착법, 저압 화학기상증착법 및 플라즈마 화학기상증착법과 같은 화학기상증착법이 이용된다. 플라즈마 화학기상증착법의 경우, 플라즈마를 이용하여 가스를 활성화시키기 때문에, 저온에서 탄소나노튜브를 합성할 수 있다. 또한, 플라즈마 화학기상증착법은 탄소나노튜브의 직경, 길이, 밀도 등을 비교적 용이하게 조절할 수 있다. In order to form carbon nanotubes on a substrate, chemical vapor deposition methods such as, for example, thermochemical vapor deposition, low pressure chemical vapor deposition, and plasma chemical vapor deposition are generally used. In the case of the plasma chemical vapor deposition method, since the gas is activated by using plasma, carbon nanotubes can be synthesized at a low temperature. In addition, the plasma chemical vapor deposition method can relatively easily control the diameter, length, density and the like of the carbon nanotubes.

화학기상증착법의 경우에, 기판 위에 형성되는 탄소나노튜브의 밀도를 균일하게 하기 위하여, 미리, 기판 위에, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 분산시킨다. In the case of the chemical vapor deposition method, in order to make the density of the carbon nanotubes formed on the substrate uniform, catalyst fine particles, which are the basis of carbon nanotube growth, are dispersed on the substrate in advance.

예를 들면, 대한민국 공개특허공보 2001-0049398호에는, 기판 위에 촉매금속막을 형성한 후, 상기 촉매금속막을 식각 가스로 식각하여 복수의 촉매 미립자를 형성시키는 방법이 개시되어 있다. For example, Korean Patent Laid-Open Publication No. 2001-0049398 discloses a method of forming a plurality of catalyst fine particles by forming a catalyst metal film on a substrate and then etching the catalyst metal film with an etching gas.

다른 예를 들면, "Chemical physics letter, vol.377 p. 49, 2003"에는, 촉매금속 전구체 용액을 기판 위에 도포하고 건조시킨 후 열처리하므로써, 촉매 미립자를 기판위에 형성시키는 방법이 개시되어 있다. 그러나, 이 경우에, 건조 및 열처리 과정에서, 촉매금속의 재결정 및 응집이 발생하여, 기판 위에 형성되는 촉매금속 미립자의 균일도가 저하되는 문제점이 발생할 수 있다. 기판 위에 형성되는 촉매 미립자의 균일도가 저하되면, 그것을 기초로 하여 성장되는 카본나노튜브의 직경과 생성밀도의 균일성도 저하된다. In another example, "Chemical physics letter, vol. 377 p. 49, 2003" discloses a method of forming catalyst fine particles on a substrate by applying a catalyst metal precursor solution onto a substrate, drying and heat treatment. In this case, however, recrystallization and agglomeration of the catalyst metal may occur during drying and heat treatment, thereby causing a problem that the uniformity of the catalyst metal fine particles formed on the substrate is lowered. When the uniformity of the catalyst fine particles formed on the substrate is lowered, the uniformity of the diameter and the production density of the carbon nanotubes grown on the basis of the lowered particles is also reduced.

기판 위에 형성되는 촉매 미립자의 균일도는 촉매 미립자의 입자크기의 균일성과 촉매 미립자의 생성밀도의 균일성으로 평가될 수 있다. 지금 까지 알려진 방법들에 의하여 형성된 촉매 미립자의 균일도는 그다지 만족스럽지 않은 것으로 알려져 있다. 그리하여, 기판 위에 형성되는 촉매 미립자의 균일도를 향상기키기 위한 촉매 미립자의 새로운 형성 방법이 여전히 요구되고 있다.The uniformity of the catalyst fine particles formed on the substrate can be evaluated by the uniformity of the particle size of the catalyst fine particles and the uniformity of the production density of the catalyst fine particles. It is known that the uniformity of the catalyst fine particles formed by the methods known to date is not very satisfactory. Thus, there is still a need for a new method of forming catalyst fine particles for improving the uniformity of the catalyst fine particles formed on the substrate.

본 발명에서는, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 기판 위에 더욱 균일하게 형성시킬 수 있는 새로운 방법을 제공한다.The present invention provides a novel method for forming the catalyst fine particles, which are the basis for carbon nanotube growth, to be more uniformly formed on a substrate.

본 발명에서는 또한, 균일도가 향상된 카본나노튜브 합성 방법을 제공한다.The present invention also provides a method for synthesizing carbon nanotubes having improved uniformity.

본 발명에서 제공하는 촉매 미립자 형성 방법은, 촉매금속 전구체 용액을 기판 위에 도포하는 단계; 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조하는 단계; 및 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시키는 단계를 포함한다.The catalyst fine particle forming method provided by the present invention comprises the steps of applying a catalyst metal precursor solution on a substrate; Freeze-drying the catalyst metal precursor solution applied on the substrate; And reducing the lyophilized catalyst metal precursor to the catalyst metal.

본 발명의 촉매 미립자 형성 방법은, 촉매금속 전구체 용액을 냉동건조하므로써, 촉매금속 미립자 형성 과정에서의 촉매금속 미립자의 응집 및/또는 재결정을 최소화시킬 수 있다. 그리하여, 본 발명의 방법으로 형성된 촉매금속 미립자는, 매우 균일한 입자크기를 가지며, 또한 기판 위에 매우 균일하게 분포된다. The catalyst fine particle formation method of the present invention can minimize the aggregation and / or recrystallization of the catalyst metal fine particles in the catalyst metal fine particle formation process by freeze-drying the catalyst metal precursor solution. Thus, the catalytic metal fine particles formed by the method of the present invention have a very uniform particle size and are distributed very uniformly on the substrate.

본 발명의 탄소나노튜브 제조 방법은, 촉매금속 전구체 용액을 기판 위에 도포한 후, 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조한 다음 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시켜서, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 기판 위에 형성시키는 단계; 및 상기 촉매 미립자에 탄소원천을 공급하여, 상기 촉매 미립자 위에 탄소나노튜브를 성장시키는 단계를 포함한다. In the carbon nanotube manufacturing method of the present invention, the catalyst metal precursor solution is coated on a substrate, and the catalyst metal precursor solution applied on the substrate is lyophilized, and then the lyophilized catalyst metal precursor is reduced to the catalyst metal. Forming catalyst fine particles on the substrate on which growth is based; And supplying a carbon source to the catalyst fine particles to grow carbon nanotubes on the catalyst fine particles.

이하에서는, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 기판 위에 형성시키기 위한 본 발명의 방법을 상세히 설명한다. 본 발명의 촉매 미립자 형성 방법은, 촉매금속 전구체 용액을 기판 위에 도포하는 단계; 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조하는 단계; 및 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시키는 단계를 포함한다.Hereinafter, the method of the present invention for forming catalyst fine particles, which are the basis of carbon nanotube growth, on a substrate will be described in detail. The catalyst fine particle forming method of the present invention comprises the steps of applying a catalyst metal precursor solution on a substrate; Freeze-drying the catalyst metal precursor solution applied on the substrate; And reducing the lyophilized catalyst metal precursor to the catalyst metal.

상기 촉매금속 전구체 용액은 촉매금속 전구체;와 촉매금속 전구체를 용해시킬 수 있는 용매를 포함한다. The catalyst metal precursor solution includes a catalyst metal precursor; and a solvent capable of dissolving the catalyst metal precursor.

상기 촉매금속 전구체로서는, 탄소나노튜브 성장의 기초가 될 수 있는 미립자의 금속 형태로 전환될 수 있는 임의의 재료가 사용될 수 있다. 상기 촉매금속 전구체로서는, 예를 들면, 유기금속화합물(organo-metallic compound)이 사용될 수 있다. 상기 유기금속화합물은, 예를 들면, Fe, Co, Ni, Y, Mo, Cu, Pt, V 및 Ti 중에서 선택되는 적어도 하나의 금속원자를 함유할 수 있다. 상기 유기금속화합물의 구체적인 예로서는, 아세트산철(iron acetate), 옥살산철(iron oxalate), 아세트산코발트(cobalt acetate), 아세트산니켈(nickel acetate), 페로센(ferrocene), 또는 이들의 혼합물이 있다.As the catalyst metal precursor, any material that can be converted into a metal form of particulates which can be the basis of carbon nanotube growth can be used. As the catalyst metal precursor, for example, an organo-metallic compound may be used. The organometallic compound may contain, for example, at least one metal atom selected from Fe, Co, Ni, Y, Mo, Cu, Pt, V, and Ti. Specific examples of the organometallic compound include iron acetate, iron oxalate, cobalt acetate, nickel acetate, ferrocene, or mixtures thereof.

상기 용매로서는, 상기 촉매금속 전구체를 용해할 수 있는 임의의 액상 물질이 사용될 수 있다. 예를 들면, 상기 용매로서는, 에탄올(ethanol), 에틸렌글리콜(ethylene glycol), 폴리에틸렌글리콜(polyethylene glycol), 폴리비닐알콜(poly vinyl alcohol), 이들의 혼합물 등이 사용될 수 있다.As the solvent, any liquid substance capable of dissolving the catalyst metal precursor may be used. For example, ethanol, ethylene glycol, polyethylene glycol, polyvinyl alcohol, mixtures thereof, and the like may be used as the solvent.

상기 촉매금속 전구체 용액 중의 상기 촉매금속 전구체의 함량은 특별히 제한되지 않는다. 상기 촉매금속 전구체 용액 중의 상기 촉매금속 전구체의 함량이 너무 작으면, 추후의 탄소나노튜브 제조 공정에서, 탄소나노튜브가 생성되지 않을 수 있고, 너무 많으면, 추후의 탄소나노튜브 제조 공정에서, 생성되는 탄소나노튜브의 직경이 매우 굵어지거나, 생성되는 탄소나노튜브 또는 탄소나노파이버의 결정성이 저하될 수 있다. 상기 촉매금속 전구체 용액 중의 상기 촉매금속 전구체의 농도는 전형적으로 약 10 mM 내지 약 200 mM 일 수 있다.The content of the catalyst metal precursor in the catalyst metal precursor solution is not particularly limited. If the content of the catalyst metal precursor in the catalyst metal precursor solution is too small, carbon nanotubes may not be produced in a subsequent carbon nanotube manufacturing process, and if too much, in a subsequent carbon nanotube manufacturing process, The diameter of the carbon nanotubes may be very thick, or the crystallinity of the resulting carbon nanotubes or carbon nanofibers may be reduced. The concentration of the catalyst metal precursor in the catalyst metal precursor solution may typically be about 10 mM to about 200 mM.

상기 기판은 촉매 미립자가 그 표면 위에 부착될 수 있는 임의의 재료가 사용될 수 있다. 예를 들면, 상기 기판으로서는, 예를 들면, Mo, Cr 및 W 와 같이 높은 융점을 갖는 금속, 실리콘, 유리, 플라스틱, 석영, 등이 사용될 수 있다. The substrate may be any material to which the catalyst fine particles can be attached on its surface. For example, as the substrate, for example, metal having high melting point such as Mo, Cr and W, silicon, glass, plastic, quartz, or the like can be used.

상기 촉매금속 전구체 용액을 상기 기판 위에 도포하는 방법으로서는, 기판의 표면에 용액을 고르게 코팅할 수 있는 임의의 방법이 사용될 수 있다. 예를 들면, 상기 촉매금속 전구체 용액을 상기 기판 위에 도포하는 방법으로서, 침지법(dip coating), 증발법(evaporation coating), 스크린프린팅(screen printing), 스핀코팅(spin coating) 등이 사용될 수 있다. 또한, 이러한 방법들을 조합한 방법이 사용될 수도 있다.As a method of applying the catalyst metal precursor solution on the substrate, any method capable of evenly coating the solution on the surface of the substrate may be used. For example, a dip coating, evaporation coating, screen printing, spin coating, or the like may be used as a method of coating the catalyst metal precursor solution on the substrate. . Also, a method combining these methods may be used.

촉매금속 전구체 용액은 기판의 전표면에 도포될 수도 있고, 기판의 일부 표면에만 도포될 수도 있다. The catalyst metal precursor solution may be applied to the entire surface of the substrate, or may be applied only to some surfaces of the substrate.

이와 같이 기판 위에 도포된 촉매금속 전구체 용액은 냉동건조 과정을 거치게 된다. 냉동건조라 함은, 기판 위에 도포된 촉매금속 전구체 용액을, 상기 촉매금속 전구체 용액의 어는점 이하로 냉각한 후, 감압조건 하에서 상기 촉매금속 전구체 용액 중의 용매를 기화시키는 과정을 의미한다.The catalyst metal precursor solution applied on the substrate is subjected to a freeze drying process. Freeze-drying refers to a process of vaporizing a solvent in the catalyst metal precursor solution under reduced pressure after cooling the catalyst metal precursor solution applied on the substrate to below the freezing point of the catalyst metal precursor solution.

촉매금속 전구체 용액의 어는점은 촉매금속 전구체 용액의 조성에 따라 달라질 수 있다. 즉, 촉매금속 전구체의 성분, 용매의 성분, 촉매금속 전구체의 함량 등과 같은 조건에 의하여 촉매금속 전구체 용액의 어는점이 결정될 수 있다. 이러한 촉매금속 전구체 용액의 어는점은 열역학적 계산 또는 시행착오법에 의하여 당업자에 의하여 용이하게 측정될 수 있다. 또한, 촉매금속 전구체 용액의 조성을 조절하므로써 촉매금속 전구체 용액의 어는점을 선택할 수도 있다.The freezing point of the catalyst metal precursor solution may vary depending on the composition of the catalyst metal precursor solution. That is, the freezing point of the catalyst metal precursor solution may be determined by conditions such as the component of the catalyst metal precursor, the component of the solvent, and the content of the catalyst metal precursor. The freezing point of such catalyst metal precursor solutions can be readily determined by those skilled in the art by thermodynamic calculation or trial and error. It is also possible to select the freezing point of the catalyst metal precursor solution by adjusting the composition of the catalyst metal precursor solution.

기판 위에 도포된 촉매금속 전구체 용액을 촉매 용액의 어는점 이하로 냉각하는 과정은 촉매금속 전구체 용액의 어는점에 적합한 냉각방법을 사용하므로써 수행될 수 있다. 예를 들면, 냉동기, 액체질소, 등이 사용될 수 있다. 액체질소를 사용하는 경우에, 촉매금속 전구체 용액으로 도포된 기판을 액체질소에 담그므로써, 기판 위에 도포된 촉매금속 전구체 용액을 촉매금속 전구체 용액의 어는점 이하로 냉각할 수 있다.The cooling of the catalyst metal precursor solution applied on the substrate below the freezing point of the catalyst solution may be performed by using a cooling method suitable for the freezing point of the catalyst metal precursor solution. For example, freezers, liquid nitrogen, and the like can be used. In the case of using liquid nitrogen, the catalyst metal precursor solution applied on the substrate can be cooled below the freezing point of the catalyst metal precursor solution by immersing the substrate coated with the catalyst metal precursor solution in liquid nitrogen.

이와 같이, 기판 위에 도포된 촉매금속 전구체 용액을 냉동시킨 후 냉동된 촉매금속 전구체 용액 중의 용매 성분을 기화시키기 위하여, 냉동된 촉매금속 전구체 용액이 도포되어 있는 기판을 감압환경으로 보낸다. 예를 들면, 냉동된 촉매금속 전구체 용액이 도포되어 있는 기판을 진공챔버에 넣은 후, 진공챔버의 내부를 감압시킨다. As described above, in order to freeze the catalyst metal precursor solution applied on the substrate and to vaporize the solvent component in the frozen catalyst metal precursor solution, the substrate on which the frozen catalyst metal precursor solution is applied is sent to a reduced pressure environment. For example, the substrate on which the frozen catalyst metal precursor solution is applied is put in a vacuum chamber, and the inside of the vacuum chamber is depressurized.

감압은 냉동된 촉매금속 전구체 용액 중의 용매 성분이 기화되기에 충분한 정도이어야 한다. 이하에서는, 냉동된 촉매금속 전구체 용액 중의 용매 성분이 기화되기에 충분한 정도로 감압된 압력을 간단하게 "기화압력(evaporation pressure)"이라 부른다. 기화압력은 사용된 촉매금속 전구체 용액의 조성에 따라 달라질 수 있다. 즉, 촉매금속 전구체의 성분, 용매의 성분, 촉매금속 전구체의 함량, 냉동온도 등과 같은 조건에 의하여 촉매금속 전구체 용액의 기화압력이 결정될 수 있다. 이러한 촉매금속 전구체 용액의 기화압력은 열역학적 계산 또는 시행착오법에 의하여 당업자에 의하여 용이하게 측정될 수 있다. 또한, 촉매금속 전구체 용액의 조성, 냉동온도 등을 조절하므로써 촉매금속 전구체 용액 중의 용매의 기화압력을 선택할 수도 있다.The reduced pressure should be sufficient to allow the solvent component in the frozen catalyst metal precursor solution to vaporize. Hereinafter, the pressure reduced to a degree sufficient for the solvent component in the frozen catalyst metal precursor solution to vaporize is simply referred to as "evaporation pressure". The vaporization pressure may vary depending on the composition of the catalyst metal precursor solution used. That is, the vaporization pressure of the catalyst metal precursor solution may be determined by conditions such as the component of the catalyst metal precursor, the component of the solvent, the content of the catalyst metal precursor, and the freezing temperature. The vaporization pressure of the catalyst metal precursor solution can be easily measured by those skilled in the art by thermodynamic calculation or trial and error. In addition, the vaporization pressure of the solvent in the catalyst metal precursor solution may be selected by adjusting the composition, the freezing temperature, and the like of the catalyst metal precursor solution.

이러한 기화를 통하여 냉동된 촉매금속 전구체 용액 중의 용매 성분이 제거된다. 그 결과, 기판의 표면에는 촉매금속 전구체 성분이 미립자 형태로 형성된다. 주목할 점은, 본 발명의 방법으로 형성된 촉매금속 전구체 미립자는, 비교적 균일한 입자크기를 가지며, 또한 기판 위에 균일하게 분포된다는 점이다. This vaporization removes the solvent components in the frozen catalyst metal precursor solution. As a result, the catalyst metal precursor component is formed in the form of fine particles on the surface of the substrate. Note that the catalyst metal precursor fine particles formed by the method of the present invention have a relatively uniform particle size and are uniformly distributed on the substrate.

그 다음에, 기판의 표면에 형성된 촉매금속 전구체 미립자를 촉매금속 미립자로 환원시킨다. 촉매금속 전구체 미립자를 촉매금속 미립자로 환원시키는 과정은 예를 들면, 다음과 같이 수행될 수 있다. 먼저, 산화분위기 내에서의 열처리를 통하여 촉매금속 전구체를 산화물로 전환시킨 다음, 이렇게 형성된 산화물을, 환원분위기에서 열처리 또는 플라즈마 처리하여, 금속으로 환원시킨다. 촉매금속 전구체의 환원과정은 당업계에 알려진 다양한 방법에 의하여 수행될 수 있으므로, 여기에서는 더 이상 자세히 설명하지 않는다.Then, the catalytic metal precursor fine particles formed on the surface of the substrate are reduced to the catalytic metal fine particles. The process of reducing the catalytic metal precursor fine particles to the catalytic metal fine particles may be performed, for example, as follows. First, the catalytic metal precursor is converted to an oxide through heat treatment in an oxidizing atmosphere, and the oxide thus formed is heat-treated or plasma-treated in a reducing atmosphere to reduce the metal. The reduction of the catalytic metal precursor may be carried out by various methods known in the art, and thus will not be described in further detail here.

도 1은, 본 발명의 일 실시예에 따라 제조된 촉매금속 미립자의 전자현미경 사진이다. 도 1을 보면, 촉매금속 미립자가 기판 위에 고르게 분포되어 있을 뿐만아니라, 촉매금속 미립자의 입자크기가 비교적 균일하다는 것을 알 수 있다. 1 is an electron micrograph of catalyst metal particles prepared according to an embodiment of the present invention. 1, it can be seen that the catalyst metal fine particles are not only uniformly distributed on the substrate, but also the particle size of the catalyst metal fine particles is relatively uniform.

이하에서는, 본 발명의 탄소나노튜브 제조 방법을 상세히 설명한다.Hereinafter, the carbon nanotube manufacturing method of the present invention will be described in detail.

본 발명의 탄소나노튜브 제조 방법은, 촉매금속 전구체 용액을 기판 위에 도포한 후, 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조한 다음 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시켜서, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 기판 위에 형성시키는 단계; 및 상기 촉매 미립자에 탄소원천을 공급하여, 상기 촉매 미립자 위에 탄소나노튜브를 성장시키는 단계를 포함한다.In the carbon nanotube manufacturing method of the present invention, the catalyst metal precursor solution is coated on a substrate, and the catalyst metal precursor solution applied on the substrate is lyophilized, and then the lyophilized catalyst metal precursor is reduced to the catalyst metal. Forming catalyst fine particles on the substrate on which growth is based; And supplying a carbon source to the catalyst fine particles to grow carbon nanotubes on the catalyst fine particles.

기판 위에 촉매 미립자를 형성시키는 단계는 앞에서 설명한 본 발명의 촉매 미립자 형성 방법과 같다.Forming the catalyst fine particles on the substrate is the same as the catalyst fine particle formation method of the present invention described above.

촉매 미립자에 탄소원천을 공급하여, 상기 촉매 미립자 위에 탄소나노튜브를 성장시키는 단계는, 탄소나노튜브의 제조에 사용될 수 있는 다양한 방법에 의하여수행될 수 있다. Supplying a carbon source to the catalyst fine particles to grow carbon nanotubes on the catalyst fine particles may be performed by various methods that may be used to prepare carbon nanotubes.

예를 들면, 상기 탄소나노튜브 성장 단계에서는, 반응챔버 내에, 탄소나노튜브 성장의 기초가 되는 촉매 미립자가 부착되어 있는 기판을 위치시키고, 상기 반응챔버 내에 탄소전구체가스를 공급한 후, 상기 반응챔버 내에서 상기 탄소전구체가스를 분해하여 상기 촉매 미립자에 탄소를 공급하므로써, 상기 촉매 미립자 위에서 탄소나노튜브가 성장하게 된다.For example, in the carbon nanotube growth step, a substrate on which a catalyst fine particle, which is the basis of carbon nanotube growth, is attached is placed in the reaction chamber, and the carbon precursor gas is supplied into the reaction chamber, followed by the reaction chamber. The carbon nanotubes are grown on the catalyst fine particles by decomposing the carbon precursor gas and supplying carbon to the catalyst fine particles.

더욱 구체적인 예를 들면, 상기 탄소나노튜브 성장 단계는, 저압 화학기상증착법, 열화학기상증착법, 플라즈마 화학기상증착법에 의하여 수행될 수 있으며, 또는 이들 방법을 조합한 방법에 의해서도 수행될 수 있다.More specifically, the carbon nanotube growth step may be performed by low pressure chemical vapor deposition, thermochemical vapor deposition, plasma chemical vapor deposition, or by a combination of these methods.

탄소전구체가스로서는, 예를 들면, 아세틸렌, 메탄, 프로판, 에틸렌, 일산화 탄소, 이산화탄소, 알코올, 벤젠 등과 같은 탄소함유화합물이 사용될 수 있다. As the carbon precursor gas, for example, carbon-containing compounds such as acetylene, methane, propane, ethylene, carbon monoxide, carbon dioxide, alcohols, benzene and the like can be used.

상기 반응챔버 내의 온도가 너무 낮으면 생성되는 탄소나노튜브의 결정성이 저하될 수 있고, 너무 높으면 탄소나노튜브가 잘 형성되지 않을 수 있다. 이러한 점을 고려하여, 상기 반응챔버 내의 온도는 전형적으로 약 450 내지 약 1100 ℃ 일 수 있다.If the temperature in the reaction chamber is too low, the crystallinity of the resulting carbon nanotubes may be lowered. If the temperature is too high, the carbon nanotubes may not be well formed. In view of this, the temperature in the reaction chamber may typically be about 450 to about 1100 ° C.

상기 탄소나노튜브 성장 단계에서의 다른 공정 조건은, 탄소나노튜브의 성장에 적합한 통상적인 것들이 사용될 수 있으며, 또한, 당업자에 의하여 구체적인 적용목적에 따라 용이하게 선택될 수 있다. 그리하여, 여기에서는, 상기 탄소나노튜브 성장 단계에서의 다른 공정 조건에 대하여 더 이상 자세히 설명하지 않는다.Other process conditions in the carbon nanotube growth step, conventional ones suitable for the growth of carbon nanotubes can be used, and can also be easily selected by those skilled in the art according to a specific application. Therefore, here, no other process conditions in the carbon nanotube growth step will be described in detail any further.

본 발명의 탄소나노튜브 제조 방법에서는, 앞에서 설명한 바와 같이, 균일한 입자크기를 가지며 또한 기판 위에 균일하게 분포되어 있는 촉매 미립자를 기초로 하여 탄소나노튜브를 성장시키므로, 그 결과 합성된 탄소나노튜브의 균일도 역시 매우 향상된다. 탄소나노튜브의 균일도는, 탄소나노튜브의 길이와 직경의 균일도에 의해 평가된다. 탄소나노튜브의 길이는 전자 현미경에 의해 측정될 수 있으며, 직경은 투과 전자 현미경에 의해 측정될 수 있다.In the method for producing carbon nanotubes of the present invention, as described above, carbon nanotubes are grown on the basis of catalyst particles having a uniform particle size and uniformly distributed on a substrate. Uniformity is also greatly improved. The uniformity of the carbon nanotubes is evaluated by the uniformity of the length and diameter of the carbon nanotubes. The length of the carbon nanotubes can be measured by an electron microscope, and the diameter can be measured by a transmission electron microscope.

더우기, 본 발명의 방법으로 제조된 탄소나노튜브의 수직배향성도 매우 우수하다. 이는 도 2의 전자현미경 사진으로부터 확인될 수 있다. 도 2는 본 발명의 일 실시예에서 제조된 탄소나노튜브 군집의 측면을 보여주는 사진이다. 도 2에 나타난 바와 같이, 본 발명의 방법으로 제조된 탄소나노튜브는 엉킴현상을 보이지 않으며,수직방향으로 잘 배열되어 있다. Moreover, the vertical orientation of the carbon nanotubes produced by the method of the present invention is also very excellent. This can be confirmed from the electron micrograph of FIG. 2. Figure 2 is a photograph showing the side of the carbon nanotube community prepared in one embodiment of the present invention. As shown in FIG. 2, the carbon nanotubes prepared by the method of the present invention do not exhibit entanglement and are well arranged in the vertical direction.

도 3은 본 발명의 일 실시예에서 제조된 탄소나노튜브 군집의 표면을 보여주는 사진이다. 도 3으로부터, 본 발명의 방법으로 제조된 탄소나노튜브의 생성밀도는 매우 균일하다. Figure 3 is a photograph showing the surface of the carbon nanotube community prepared in one embodiment of the present invention. 3, the production density of the carbon nanotubes produced by the method of the present invention is very uniform.

<실시예><Example>

에탄올을 용매로 사용한 40 mM 농도의 아세트산철 용액을 제조하였다. 아세트산철 분말 0.1 g에 에탄올 20 ml 및 에틸렌글리콜 20 ml 를 첨가하여 적절한 점도의 용액을 얻었다. 이렇게 얻은 용액을 직경 8 인치의 실리콘 기판 위에 침지법을 이용하여 도포하였다. 코팅된 기판을 즉시 액체질소로 냉각한 후 진공 챔버로 옮긴 다음, 0.1 mmHg 이하의 진공을 가하여 용매를 증발시켰다. 용매의 잔류량을 최소화하기 위하여, 추가적으로, 100℃ 에서 상기 기판을 가열하였다. An iron acetate solution having a concentration of 40 mM was prepared using ethanol as a solvent. 20 ml of ethanol and 20 ml of ethylene glycol were added to 0.1 g of iron acetate powder to obtain a solution having an appropriate viscosity. The solution thus obtained was applied on a silicon substrate of 8 inches in diameter by dipping. The coated substrate was immediately cooled with liquid nitrogen and then transferred to a vacuum chamber, and then a vacuum of 0.1 mmHg or less was added to evaporate the solvent. In order to minimize the residual amount of solvent, the substrate was additionally heated at 100 ° C.

이와 같이 냉동건조된 기판을, 300 ℃의 공기 분위기에서 10 분간 열처리하여, 아세트산철 성분을 산화시켰다. 그 다음에, 600 ℃ 의 수소 분위기에서 기판을 환원처리하였다. The freeze-dried substrate was heat-treated for 10 minutes in an air atmosphere of 300 ° C to oxidize the iron acetate component. Next, the substrate was reduced in a hydrogen atmosphere at 600 ° C.

결과적으로, 기판에는 철(iron) 입자들이 균일하게 형성되었다. 도 1은, 본 실시예에 따라, 실리콘 기판위에 형성된 철 미립자의 전자현미경 사진이다. 도 1을 보면, 철 미립자가 기판 위에 고르게 분포되어 있을 뿐만아니라, 철 미립자의 입자크기가 비교적 균일하다는 것을 알 수 있다. As a result, iron particles were uniformly formed on the substrate. 1 is an electron micrograph of iron fine particles formed on a silicon substrate according to this embodiment. 1, it can be seen that the iron particles are not only uniformly distributed on the substrate, but also the particle size of the iron particles is relatively uniform.

이와 같은 철 미립자가 형성되어 있는 기판을, 600 ℃의 내부온도를 갖는 화학기상증착용 반응챔버에 넣은 후, 상기 반응챔버에 일산화탄소와 수소의 중량비가 1:2 인 혼합기체를 20분간 공급하여, 철 미립자를 기초로한 탄소나노튜브를 합성하였다. The substrate on which such iron fine particles were formed was placed in a chemical vapor deposition reaction chamber having an internal temperature of 600 ° C., and then a mixed gas having a weight ratio of carbon monoxide and hydrogen of 1: 2 was supplied to the reaction chamber for 20 minutes. Carbon nanotubes based on iron fine particles were synthesized.

도 2는 본 실시예에서 제조된 탄소나노튜브 군집의 측면을 보여주는 사진이다. 도 2에 나타난 바와 같이, 본 실시예에서 제조된 탄소나노튜브는 엉킴현상을 보이지 않으며, 수직방향으로 잘 배열되어 있다. 도 3은 본 실시예에서 제조된 탄소나노튜브 군집의 표면을 보여주는 사진이다. 도 3으로부터, 본 실시예에서 제조된 탄소나노튜브의 생성밀도가 매우 균일하다는 것을 알 수 있다. Figure 2 is a photograph showing the side of the carbon nanotube community prepared in this embodiment. As shown in FIG. 2, the carbon nanotubes prepared in this example do not show entanglement and are well arranged in the vertical direction. Figure 3 is a photograph showing the surface of the carbon nanotube community prepared in this embodiment. From Figure 3, it can be seen that the production density of the carbon nanotubes produced in this example is very uniform.

이와 같이 형성된 탄소나노튜브의 균일도를 평가하기 위해, 9 등분된 기판 각각에 대하여, 전자현미경을 이용한 탄소나노튜브의 길이 측정 및, 투과전자현미경을 이용한 탄소나노튜브의 직경 측정을 수행하였다. 그 결과, 9 등분된 기판의 탄소나노튜브는 +/- 5% 이내의 균일도를 갖는다는 것을 확인하였다. In order to evaluate the uniformity of the carbon nanotubes formed as described above, the length of the carbon nanotubes using the electron microscope and the diameter of the carbon nanotubes using the transmission electron microscope were measured on each of the nine equal substrates. As a result, it was confirmed that the carbon nanotubes of the nine equal substrates had a uniformity within +/- 5%.

<비교예>Comparative Example

기판 위에 도포된 아세트산철 용액을 냉동건조시키는 대신에 대기 중에서 자연 건조시킨 것을 제외하고는, 상기 실시예와 동일한 방법으로 탄소나노튜브를 합성하였다. Carbon nanotubes were synthesized in the same manner as in the above example, except that the iron acetate solution applied on the substrate was freeze-dried and air-dried.

도 4는 비교예에서 제조된 철 미립자를 보여주는 광학현미경 사진이다. 도 5는 도 4의 일부분을 확대한 도면이다. 도 4 및 도 5로부터, 비교예에서 형성된 철 미립자는 매우 불균일하다는 것을 알 수 있다.4 is an optical micrograph showing the iron fine particles prepared in the comparative example. 5 is an enlarged view of a portion of FIG. 4. 4 and 5, it can be seen that the iron fine particles formed in the comparative example is very nonuniform.

도 6은 비교예에서 합성된 탄소나노튜브 군집의 성상을 보여주는 전자현미경 사진이다. 도 6 에 나타난 바와 같이, 비교예에서 합성된 탄소나노튜브는 기판 위에 부분적으로 뭉쳐있으며, 수직으로 배향되지 않고 엉켜있다.6 is an electron micrograph showing the properties of the carbon nanotube community synthesized in the comparative example. As shown in FIG. 6, the carbon nanotubes synthesized in the comparative example are partially agglomerated on the substrate and entangled without being vertically oriented.

본 발명의 촉매 미립자 형성 방법은, 촉매금속 전구체 용액을 냉동건조하므로써, 촉매 미립자 형성 과정에서의 촉매 미립자의 응집 및/또는 재결정을 최소화시킬 수 있다. 그리하여, 본 발명의 방법으로 형성된 촉매 미립자는, 매우 균일한 입자크기를 가지며, 또한 기판 위에 매우 균일하게 분포된다. The catalyst fine particle formation method of the present invention can minimize the aggregation and / or recrystallization of the catalyst fine particles in the catalyst fine particle formation process by freeze-drying the catalyst metal precursor solution. Thus, the catalyst fine particles formed by the method of the present invention have a very uniform particle size and are distributed very uniformly on the substrate.

본 발명의 탄소나노튜브 제조 방법에서는, 앞에서 설명한 바와 같이, 균일한 입자크기를 가지며 또한 기판 위에 균일하게 분포되어 있는 촉매 미립자를 기초로 하여 탄소나노튜브를 성장시키므로, 그 결과 합성된 탄소나노튜브의 균일도 역시 매우 향상된다.In the method for producing carbon nanotubes of the present invention, as described above, carbon nanotubes are grown on the basis of catalyst particles having a uniform particle size and uniformly distributed on a substrate. Uniformity is also greatly improved.

도 1은 본 발명의 실시예에 따라 제조된 탄소나노튜브 제조용 촉매 미립자를 보여주는 광학현미경 사진이다.1 is an optical micrograph showing the catalyst fine particles for producing carbon nanotubes prepared according to an embodiment of the present invention.

도 2는 본 발명의 실시예에 따라 제조된 탄소나노튜브 군집의 측면을 보여주는 전자현미경 사진이다.Figure 2 is an electron micrograph showing the side of the carbon nanotube community prepared in accordance with an embodiment of the present invention.

도 3은 본 발명의 실시예에 따라 제조된 탄소나노튜브 군집의 표면을 보여주는 전자현미경 사진이다.3 is an electron micrograph showing the surface of the carbon nanotube community prepared according to an embodiment of the present invention.

도 4는 비교예에 따라 제조된 탄소나노튜브 제조용 촉매 미립자를 보여주는 광학현미경 사진이다.Figure 4 is an optical micrograph showing the catalyst fine particles for producing carbon nanotubes prepared according to a comparative example.

도 5는 도 4의 일부분을 확대한 도면이다.5 is an enlarged view of a portion of FIG. 4.

도 6은 비교예에 따라 제조된 탄소나노튜브 군집의 성상을 보여주는 전자현미경 사진이다.Figure 6 is an electron micrograph showing the appearance of the carbon nanotube community prepared according to the comparative example.

Claims (6)

촉매금속 전구체 용액을 기판 위에 도포하는 단계; Applying a catalyst metal precursor solution onto the substrate; 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조하는 단계; 및 Freeze-drying the catalyst metal precursor solution applied on the substrate; And 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시키는 단계를 포함하는, 탄소나노튜브 성장의 기초가 되는 촉매 미립자제조 방법.A method for producing catalyst particulates, which is the basis of carbon nanotube growth, comprising reducing a lyophilized catalyst metal precursor to a catalyst metal. 제 1 항에 있어서, 상기 촉매금속 전구체는 유기금속화합물인 것을 특징으로 하는 방법.The method of claim 1, wherein the catalytic metal precursor is an organometallic compound. 제 2 항에 있어서, 상기 촉매금속 전구체는 Fe, Co, Ni, Y, Mo, Cu, Pt, V 및 Ti 중에서 선택되는 적어도 하나의 금속원자를 함유하는 유기금속화합물인 것을 특징으로 하는 방법.The method of claim 2, wherein the catalyst metal precursor is an organometallic compound containing at least one metal atom selected from Fe, Co, Ni, Y, Mo, Cu, Pt, V, and Ti. 제 1 항에 있어서, 상기 용매는 에탄올, 에틸렌글리콜, 폴리에틸렌글리콜, 폴리비닐알콜, 또는 이들의 혼합물인 것을 특징으로 하는 방법.The method of claim 1, wherein the solvent is ethanol, ethylene glycol, polyethylene glycol, polyvinyl alcohol, or a mixture thereof. 제 1 항에 있어서, 상기 촉매금속 전구체 용액 중의 상기 촉매금속 전구체의 농도는 10 mM 내지 200 mM 인 것을 특징으로 하는 방법.The method of claim 1, wherein the concentration of the catalyst metal precursor in the catalyst metal precursor solution is 10 mM to 200 mM. 촉매금속 전구체 용액을 기판 위에 도포한 후, 상기 기판 위에 도포된 촉매금속 전구체 용액을 냉동건조한 다음 냉동건조된 촉매금속 전구체를 촉매금속으로 환원시켜서, 탄소나노튜브 성장의 기초가 되는 촉매 미립자를 기판 위에 형성시키는 단계; 및 After the catalyst metal precursor solution is applied onto the substrate, the catalyst metal precursor solution applied on the substrate is lyophilized, and then the lyophilized catalyst metal precursor is reduced to the catalyst metal so that the catalyst fine particles, which are the basis of carbon nanotube growth, are deposited on the substrate. Forming; And 상기 촉매 미립자에 탄소원천을 공급하여, 상기 촉매 미립자 위에 탄소나노튜브를 성장시키는 단계를 포함하는, 탄소나노튜브 제조 방법.Supplying a carbon source to the catalyst microparticles, and growing carbon nanotubes on the catalyst microparticles.
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