JPH08188406A - Composite carbon nanotube whose ends are closed and its production and closing of opening of carbon nanotube - Google Patents
Composite carbon nanotube whose ends are closed and its production and closing of opening of carbon nanotubeInfo
- Publication number
- JPH08188406A JPH08188406A JP7002672A JP267295A JPH08188406A JP H08188406 A JPH08188406 A JP H08188406A JP 7002672 A JP7002672 A JP 7002672A JP 267295 A JP267295 A JP 267295A JP H08188406 A JPH08188406 A JP H08188406A
- Authority
- JP
- Japan
- Prior art keywords
- carbon nanotube
- composite carbon
- closed
- tube
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、螺旋状に炭素が結合
し、ストロー状になった炭素化合物であるカーボンナノ
チューブの内部中空部分に金属や金属化合物などを有す
る複合カーボンナノチューブに関するものであり、エレ
クトロニクス産業への応用が期待されている。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a composite carbon nanotube having a metal compound and a metal compound in the inner hollow part of a carbon compound which is a carbon compound in which carbon is spirally bound to form a straw. It is expected to be applied to the electronics industry.
【０００２】[0002]
【従来の技術】金属や金属化合物をカーボンナノチュー
ブの内部中空部分に有する複合カーボンナノチューブ
は、１９９３年にアジャヤン等によって合成された（１
９９３年、ネイチャー、３９２巻、５２２−５２５頁
（Ｎａｔｕｒｅ，ｖｏｌ３９２，５２２−５２５頁（１
９９３）））。この時に合成された複合カーボンナノチ
ューブは、合成の際に金属とカーボンナノチューブを混
合し、酸素中で加熱し、酸化反応を利用しカーボンナノ
チューブの両端を開口し、毛細管現象を利用して中空部
分に金属や金属化合物を導入するというものであった。2. Description of the Related Art A composite carbon nanotube having a metal or a metal compound in a hollow portion inside the carbon nanotube was synthesized by Ajayan et al.
993, Nature, 392, 522-525 (Nature, vol 392, 522-525 (1
993))). The composite carbon nanotubes synthesized at this time mixed metal and carbon nanotubes during synthesis, heated in oxygen, opened both ends of the carbon nanotubes using the oxidation reaction, and used the capillary phenomenon to create a hollow portion. It was to introduce metals and metal compounds.
【０００３】[0003]
【発明が解決しようとする課題】しかし、従来の方法に
より得られた複合カーボンナノチューブの両端は開口し
たままになっているため、大気中での安定性が低いこと
が問題となっている。両端の閉じた構造を有する安定性
の高い複合カーボンナノチューブの作製が待たれている
が、開口した複合カーボンナノチューブはこれまでには
作製されていなかった。However, since both ends of the composite carbon nanotube obtained by the conventional method remain open, there is a problem that the stability in the atmosphere is low. Although preparation of highly stable composite carbon nanotubes having a structure with both ends closed has been awaited, open composite carbon nanotubes have not been prepared so far.
【０００４】本発明はこのような状況から生まれたもの
であり、上記課題を解決し、メモリ素子材料への応用の
基礎となる複合カーボンナノチューブの安定性を高めた
材料と、その作製方法を提供することを目的とする。The present invention was born from such a situation, and provides a material which solves the above problems and has improved stability of a composite carbon nanotube which is a basis of application to a memory device material, and a manufacturing method thereof. The purpose is to do.
【０００５】[0005]
【課題を解決するための手段】本発明の特徴とするとこ
ろは、従来の合成方法で得られたカーボンナノチューブ
の内部中空部分に金属や金属化合物を有する複合カーボ
ンナノチューブと、炭素からなるサッカーボール状のク
ラスター分子Ｃ60やＣ70等の一連のＣn 系物質であるフ
ラーレン（Ｃn 群炭素分子化合物）類とを不活性ガス中
で混合加熱し、複合カーボンナノチューブの開口した両
端をフラーレン類と反応させることによって封管するこ
とにある。A feature of the present invention is that a carbon nanotube obtained by a conventional synthesis method has a composite carbon nanotube having a metal or a metal compound in an inner hollow portion thereof, and a soccer ball shape made of carbon. The fullerene (C n group carbon molecular compound), which is a series of C n -based substances such as the cluster molecules C 60 and C 70 , are mixed and heated in an inert gas, and both ends of the opening of the composite carbon nanotube are converted into fullerenes. It is to seal the tube by making it react.
【０００６】本発明の第１の発明は、カーボンナノチュ
ーブの内部中空部分に単体又は化合物を有し、前記チュ
ーブの端が閉じた構造を有することを特徴とする複合カ
ーボンナノチューブである。A first invention of the present invention is a composite carbon nanotube, characterized in that the carbon nanotube has a simple substance or a compound in an inner hollow portion thereof, and has a structure in which the end of the tube is closed.
【０００７】第２の発明は、カーボンナノチューブの内
部中空部分に金属又は金属化合物を有し、前記チューブ
の端が閉じた構造を有することを特徴とする複合カーボ
ンナノチューブである。A second aspect of the present invention is a composite carbon nanotube characterized in that it has a metal or metal compound in the hollow interior of the carbon nanotube and has a structure in which the end of the tube is closed.
【０００８】第３の発明は、カーボンナノチューブの内
部中空部分に金属又は金属化合物を有し前記チューブの
端が開口した複合カーボンナノチューブと、フラーレン
（Ｃn 群分子化合物）を混合し、不活性ガス中で加熱す
ることを特徴とするチューブ端の閉じた複合カーボンナ
ノチューブの作製方法である。A third aspect of the present invention is to mix a fullerene (C n group molecular compound) with a composite carbon nanotube having a metal or a metal compound in an inner hollow portion of the carbon nanotube and having an open end of the tube, and then producing an inert gas. It is a method for producing a composite carbon nanotube with closed tube ends, which is characterized by heating in a tube.
【０００９】第４の発明は、チューブの端が開口したカ
ーボンナノチューブと、フラーレン（Ｃn 群分子化合
物）を混合し、不活性ガス中で加熱することを特徴とす
るカーボンナノチューブの閉口方法である。A fourth aspect of the present invention is a method for closing carbon nanotubes, characterized in that carbon nanotubes having an open tube end are mixed with fullerenes (C n group molecular compounds) and heated in an inert gas. .
【００１０】第５の発明は、前記フラーレン（Ｃn 群分
子化合物）が、前記複合カーボンナノチューブの端の開
口径と同程度の径を有するものであることを特徴とする
第３の発明に記載のチューブ端の閉じた複合カーボンナ
ノチューブの作製方法である。A fifth invention is characterized in that the fullerene (C n group molecular compound) has a diameter similar to the opening diameter at the end of the composite carbon nanotube. This is a method for producing a composite carbon nanotube whose tube end is closed.
【００１１】第６の発明は、前記フラーレン（Ｃn 群分
子化合物）が、前記カーボンナノチューブの端の開口径
と同程度の径を有するものであることを特徴とする第５
の発明に記載のカーボンナノチューブの閉口方法であ
る。A sixth aspect of the invention is characterized in that the fullerene (C n group molecular compound) has a diameter approximately equal to the opening diameter of the end of the carbon nanotube.
The method for closing carbon nanotubes according to the invention of claim 1.
【００１２】[0012]
【作用】カーボンナノチューブは、炭素原子で構成され
る六員環の集合した炭素シートが円筒状になったもので
あり、その両端は六員環と五員環の組み合わせにより半
球状に丸まり完全に閉じた構造となっている。この両端
の五員環を有する部分はチューブ側面の六員環だけから
なる部分よりも反応性が高い。それを利用して酸素中で
カーボンナノチューブを加熱すると五員環部分が酸素と
反応し、カーボンナノチューブの五員環部分を有する両
端が開口する。この時、開口部の近くに溶融した金属等
が存在すると毛細管現象により、金属等がカーボンナノ
チューブ内に導入される。このようにして得られた複合
カーボンナノチューブの両端は開口したままになってい
るが、開口部は炭素原子間の結合が切れているために反
応性が高くなっている。また、カーボンナノチューブの
直径は数nm程度の大きさを持っており、Ｃ60などのフラ
ーレン類の直径とほぼ同じ大きさである。フラーレン類
は、直径１nm程度のＣ60から様々な直径の物が存在し、
フラーレン類にも開口前のカーボンナノチューブの両端
と同じように五員環部分が存在する。カーボンナノチュ
ーブの開口径と同程度の径を有するフラーレンを含む種
々の大きさのフラーレンと開口した複合カーボンナノチ
ューブを混合し、不活性ガス中で加熱すると、フラーレ
ン類の五員環部分と複合カーボンナノチューブの炭素原
子間の結合が切れた部分とが反応し、複合カーボンナノ
チューブの開口部を塞ぐことができる。[Function] A carbon nanotube is a carbon sheet in which a 6-membered ring composed of carbon atoms is assembled into a cylindrical shape. It has a closed structure. The portions having the 5-membered rings at both ends have higher reactivity than the portions having only the 6-membered rings on the side surface of the tube. When the carbon nanotube is heated in oxygen by utilizing it, the five-membered ring portion reacts with oxygen, and both ends of the carbon nanotube having the five-membered ring portion are opened. At this time, if a molten metal or the like exists near the opening, the metal or the like is introduced into the carbon nanotube due to a capillary phenomenon. Both ends of the thus obtained composite carbon nanotube remain open, but the opening has high reactivity because the bond between carbon atoms is broken. Further, the diameter of the carbon nanotube has a size of about several nm, which is almost the same as the diameter of fullerenes such as C 60 . Fullerenes have various diameters from C 60 with a diameter of about 1 nm,
Fullerenes also have a five-membered ring portion like both ends of the carbon nanotube before opening. When mixed open carbon nanotubes are mixed with fullerenes of various sizes including fullerenes having a diameter similar to that of carbon nanotubes and heated in an inert gas, the five-membered ring portion of fullerenes and composite carbon nanotubes Reacts with the part where the bond between the carbon atoms is broken, and can block the opening of the composite carbon nanotube.
【００１３】[0013]
【実施例】本発明の一実施例を以下に示す。An embodiment of the present invention will be described below.
【００１４】（実施例１）鉛化合物を中空部分に有する
複合カーボンナノチューブと、アーク放電法によって得
られた炭素すすをトルエン溶媒でソックスレー抽出した
フラーレン類を５０ｍｇずつ混合し、石英管に入れた。
石英管中の圧力が８００ｔｏｒｒになるようにアルゴン
ガスで満たしたあと石英管を封管した。封管した石英管
を電気炉の中に入れ５００℃に加熱して１ケ月間反応さ
せた。反応後、石英管から反応物を取り出し電子顕微鏡
により観察した結果、チューブの両端が閉口した複合カ
ーボンナノチューブの存在が確認された。反応性があま
り高くないので、開口した複合カーボンナノチューブと
フラーレン類の混合比はフラーレン類を量論比１：１よ
りも多く混合したほうが反応が進みやすい。反応時の加
熱温度は５００°以上、複合カーボンナノチューブ中に
含まれる物質の溶融温度未満であればよい。また、反応
時間もできる限り長くしたほうがより多くの閉口した複
合カーボンナノチューブが得られる。雰囲気ガスとして
アルゴンガス以外にもヘリウムガスでも作製可能であ
る。Example 1 A composite carbon nanotube having a lead compound in the hollow portion and 50 mg of fullerenes obtained by soxhlet-extracting carbon soot obtained by an arc discharge method with a toluene solvent were mixed and placed in a quartz tube.
After filling the quartz tube with argon gas so that the pressure in the quartz tube was 800 torr, the quartz tube was sealed. The sealed quartz tube was placed in an electric furnace and heated to 500 ° C. to react for one month. After the reaction, the reaction product was taken out from the quartz tube and observed by an electron microscope. As a result, it was confirmed that there were composite carbon nanotubes in which both ends of the tube were closed. Since the reactivity is not so high, the mixing ratio of the opened composite carbon nanotubes and the fullerenes is more likely to proceed when the fullerenes are mixed more than the stoichiometric ratio of 1: 1. The heating temperature during the reaction may be 500 ° C. or higher and lower than the melting temperature of the substance contained in the composite carbon nanotube. Further, the longer the reaction time is, the more closed carbon nanotubes can be obtained. Helium gas may be used as the atmosphere gas in addition to argon gas.
【００１５】（実施例２）ビスマス化合物を中空部分に
有する複合カーボンナノチューブと、アーク放電法によ
って得られた炭素すすをトルエン溶媒でソックスレー抽
出したフラーレン類を５０ｍｇずつ混合し、石英管に入
れた。石英管中の圧力が８００ｔｏｒｒになるようにア
ルゴンガスで満たしたあと石英管を封管した。封管した
石英管を電気炉の中に入れ６００℃に加熱して１ケ月間
反応させた。反応後、石英管から反応物を取り出し電子
顕微鏡により観察した結果、チューブの両端が閉口した
複合カーボンナノチューブの存在が確認された。反応性
があまり高くないので、開口した複合カーボンナノチュ
ーブとフラーレン類の混合比はフラーレン類を量論比
１：１よりも多く混合したほうが反応が進みやすい。反
応時の加熱温度は５００°以上、複合カーボンナノチュ
ーブ中に含まれる物質の溶融温度未満であればよい。ま
た、反応時間もできる限り長くしたほうがより多くの閉
口した複合カーボンナノチューブが得られる。雰囲気ガ
スとしてアルゴンガス以外にもヘリウムガスでも作製可
能である。(Example 2) Composite carbon nanotubes having a bismuth compound in the hollow portion and 50 mg of fullerenes obtained by soxhlet-extracting carbon soot obtained by the arc discharge method with a toluene solvent were mixed and placed in a quartz tube. After filling the quartz tube with argon gas so that the pressure in the quartz tube was 800 torr, the quartz tube was sealed. The sealed quartz tube was placed in an electric furnace and heated to 600 ° C. to react for one month. After the reaction, the reaction product was taken out from the quartz tube and observed by an electron microscope. As a result, it was confirmed that there were composite carbon nanotubes in which both ends of the tube were closed. Since the reactivity is not so high, the mixing ratio of the opened composite carbon nanotubes and the fullerenes is more likely to proceed when the fullerenes are mixed more than the stoichiometric ratio of 1: 1. The heating temperature during the reaction may be 500 ° C. or higher and lower than the melting temperature of the substance contained in the composite carbon nanotube. Further, the longer the reaction time is, the more closed carbon nanotubes can be obtained. Helium gas may be used as the atmosphere gas in addition to argon gas.
【００１６】[0016]
【発明の効果】以上述べたように、本発明の方法を用い
れば、金属や金属化合物を中空部分に有する複合カーボ
ンナノチューブの開口端を閉じることができ、チューブ
の両端を閉じることによって、酸素や水素の不純物に対
して耐性の高い複合カーボンナノチューブを得ることが
できる。金属化合物等を内部に有する複合カーボンナノ
チューブは、その螺旋構造の螺旋状態および内部に存在
する物質の種類によって導伝性などの各種特性を持つこ
とが期待されている物質であり、工業的応用が期待され
ている。本発明を用いると安定性の高い複合カーボンナ
ノチューブを得ることができるのでその意義は大きい。As described above, according to the method of the present invention, the open end of the composite carbon nanotube having a metal or metal compound in the hollow portion can be closed, and by closing both ends of the tube, oxygen or A composite carbon nanotube having high resistance to hydrogen impurities can be obtained. Composite carbon nanotubes having metal compounds inside are materials expected to have various properties such as conductivity depending on the spiral state of the spiral structure and the type of materials existing inside, and are not suitable for industrial applications. Is expected. The use of the present invention makes it possible to obtain a highly stable composite carbon nanotube, and therefore its significance is great.
Claims (6)
体又は化合物を有し、前記チューブの端が閉じた構造を
有することを特徴とする複合カーボンナノチューブ。1. A composite carbon nanotube, characterized in that the carbon nanotube has a simple substance or a compound in an inner hollow portion thereof, and has a structure in which an end of the tube is closed.
属又は金属化合物を有し、前記チューブの端が閉じた構
造を有することを特徴とする複合カーボンナノチュー
ブ。2. A composite carbon nanotube having a structure in which a metal or a metal compound is contained in an inner hollow portion of the carbon nanotube and the end of the tube is closed.
属又は金属化合物を有し前記チューブの端が開口した複
合カーボンナノチューブと、フラーレン（Ｃn 群分子化
合物）を混合し、不活性ガス中で加熱することを特徴と
するチューブ端の閉じた複合カーボンナノチューブの作
製方法。3. A composite carbon nanotube having a metal or a metal compound in an inner hollow portion of the carbon nanotube and having an open end of the tube, and fullerene (C n group molecular compound) are mixed and heated in an inert gas. A method for producing a composite carbon nanotube with a closed tube end, comprising:
ーブと、フラーレン（Ｃn 群分子化合物）を混合し、不
活性ガス中で加熱することを特徴とするカーボンナノチ
ューブの閉口方法。4. A method of closing a carbon nanotube, which comprises mixing a carbon nanotube having an open tube end with a fullerene (C n group molecular compound) and heating the mixture in an inert gas.
前記複合カーボンナノチューブの端の開口径と同程度の
径を有するものであることを特徴とする請求項３記載の
チューブ端の閉じた複合カーボンナノチューブの作製方
法。5. The fullerene (C n group molecular compound) is
The method for producing a composite carbon nanotube with a closed tube end according to claim 3, wherein the composite carbon nanotube has a diameter similar to the opening diameter at the end of the composite carbon nanotube.
前記カーボンナノチューブの端の開口径と同程度の径を
有するものであることを特徴とする請求項５記載のカー
ボンナノチューブの閉口方法。6. The fullerene (C n group molecular compound) is
The method for closing carbon nanotubes according to claim 5, wherein the carbon nanotubes have a diameter approximately equal to the diameter of the openings at the ends of the carbon nanotubes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7002672A JP2848258B2 (en) | 1995-01-11 | 1995-01-11 | Method for producing composite carbon nanotube having closed tube end and method for closing carbon nanotube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7002672A JP2848258B2 (en) | 1995-01-11 | 1995-01-11 | Method for producing composite carbon nanotube having closed tube end and method for closing carbon nanotube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08188406A true JPH08188406A (en) | 1996-07-23 |
| JP2848258B2 JP2848258B2 (en) | 1999-01-20 |
Family
ID=11535813
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7002672A Expired - Fee Related JP2848258B2 (en) | 1995-01-11 | 1995-01-11 | Method for producing composite carbon nanotube having closed tube end and method for closing carbon nanotube |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2848258B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7687801B2 (en) | 2005-01-06 | 2010-03-30 | National Institute Of Advanced Industrial Science And Technology | Dopant material, dopant material manufacturing method, and semiconductor device using the same |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8454923B2 (en) | 2009-06-10 | 2013-06-04 | Carbon Solutions, Inc. | Continuous extraction technique for the purification of carbon nanomaterials |
| US8449858B2 (en) | 2009-06-10 | 2013-05-28 | Carbon Solutions, Inc. | Continuous extraction technique for the purification of carbon nanomaterials |
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-
1995
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|---|---|---|---|---|
| JPH06227806A (en) * | 1992-12-22 | 1994-08-16 | Nec Corp | Carbon nanotube enclosing foreign substance and its production |
| JPH06271306A (en) * | 1993-03-17 | 1994-09-27 | Nec Corp | Rosary-like macromolecular cluster and formation thereof |
| JPH0768160A (en) * | 1993-06-22 | 1995-03-14 | Nippon Kasei Chem Co Ltd | Production of superfine particles of carbide or single element enhanced in carbon wall coating |
| JPH0729462A (en) * | 1993-07-14 | 1995-01-31 | Nec Corp | Carbon nano-tube fine line and switch |
| JPH07165406A (en) * | 1993-10-19 | 1995-06-27 | Sony Corp | Production of carbon tube |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7687801B2 (en) | 2005-01-06 | 2010-03-30 | National Institute Of Advanced Industrial Science And Technology | Dopant material, dopant material manufacturing method, and semiconductor device using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2848258B2 (en) | 1999-01-20 |
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