JP2002097008A - Method for perforating monolayered carbon nanotube - Google Patents

Method for perforating monolayered carbon nanotube

Info

Publication number
JP2002097008A
JP2002097008A JP2000286095A JP2000286095A JP2002097008A JP 2002097008 A JP2002097008 A JP 2002097008A JP 2000286095 A JP2000286095 A JP 2000286095A JP 2000286095 A JP2000286095 A JP 2000286095A JP 2002097008 A JP2002097008 A JP 2002097008A
Authority
JP
Japan
Prior art keywords
swnt
carbon nanotube
walled carbon
opening
carbon nanotubes
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.)
Pending
Application number
JP2000286095A
Other languages
Japanese (ja)
Inventor
Sumio Iijima
澄男 飯島
Toshiharu Bando
俊治 坂東
Kazutomo Suenaga
和知 末永
Yoshiori Hirahara
佳織 平原
Toshiya Okazaki
俊也 岡崎
Hisanori Shinohara
久典 篠原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nagoya University NUC
Japan Science and Technology Agency
NEC Corp
Original Assignee
Nagoya University NUC
NEC Corp
Japan Science and Technology Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nagoya University NUC, NEC Corp, Japan Science and Technology Corp filed Critical Nagoya University NUC
Priority to JP2000286095A priority Critical patent/JP2002097008A/en
Priority to PCT/JP2001/008195 priority patent/WO2002024573A1/en
Publication of JP2002097008A publication Critical patent/JP2002097008A/en
Pending legal-status Critical Current

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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C01B32/168—After-treatment
    • 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
    • C01B2202/02—Single-walled nanotubes

Abstract

PROBLEM TO BE SOLVED: To provide a new method for simply perforating a monolayered carbon nanotube, which is useful for developing a high performance material, a device material and the like, by using the monolayered carbon nanotube, and can perforate even on the wall of the tube. SOLUTION: The perforations of 1-2 nm in diameter are made in the monolayered carbon nanotube by keeping the carbon nanotube in a dry reactive gas at 200-600 degree C for 1 minute and more.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】この出願の発明は、単層カー
ボンナノチューブの開孔方法に関するものである。さら
に詳しくは、この出願の発明は、デバイス材料等の高機
能材料の開発および製造に有用で、管壁にも開孔でき
る、簡便で新しい単層カーボンナノチューブの開孔方法
に関するものである。The present invention relates to a method for opening single-walled carbon nanotubes. More specifically, the invention of this application relates to a simple and new method for perforating single-walled carbon nanotubes, which is useful for the development and production of high-performance materials such as device materials, and can also perforate a tube wall.

【０００２】[0002]

【従来の技術とその課題】カーボンナノチューブは、エ
ネルギー分野を始め、情報通信、航空・宇宙、生体・医
療等の幅広い分野で、次世代の高機能材料として注目さ
れている物質であり、近年になって、新しい素子あるい
は材料等の研究および開発がさらに活発に行われてい
る。このカーボンナノチューブには、チューブを形成す
るグラファイトシートが一層である、いわゆる単層カー
ボンナノチューブ（ＳＷＮＴ：Single- walled carbon
nanotube）と、グラファイトシートの円筒が多数入れ子
状に重なった多層カーボンナノチューブ（ＭＷＮＴ：Mu
lti - walled carbon nanotube）とがある。カーボンナ
ノチューブの持つ電子放出機能、水素吸蔵機能、磁気機
能等を効率よく応用するための研究および開発において
は、カーボンナノチューブの構造の単純化が必要である
ため、主にＳＷＮＴが用いられている。2. Description of the Related Art Carbon nanotubes have attracted attention as next-generation high-performance materials in a wide range of fields, including the energy field, information and communication, aviation and space, and biological and medical fields. As a result, research and development of new devices or materials are being actively conducted. This carbon nanotube has a single layer of graphite sheet forming a tube, a so-called single-walled carbon nanotube (SWNT).
nanotubes) and multi-walled carbon nanotubes (MWNT: Mu) in which a number of graphite sheet cylinders are nested.
lti-walled carbon nanotube). In research and development for efficiently applying the electron emission function, the hydrogen storage function, the magnetic function, and the like of the carbon nanotube, SWNT is mainly used because the structure of the carbon nanotube needs to be simplified.

【０００３】ＳＷＮＴは、その生成機構に関連して、チ
ューブの終端がキャップと呼ばれるフラーレンの半球で
閉じた状態で生成されている。したがって、ＳＷＮＴの
中の中空に何らかの物質を内包させる場合には、このキ
ャップを取る必要が生じる。また、ＳＷＮＴ同士や、Ｓ
ＷＮＴと他の分子とを繋ぐ等の加工を施す場合には、Ｓ
ＷＮＴのキャップあるいは管壁を開孔する必要がある。[0003] In relation to its production mechanism, SWNT is produced with the end of the tube closed with a fullerene hemisphere called a cap. Therefore, it is necessary to take off this cap when enclosing any substance in the hollow of the SWNT. In addition, SWNTs, S
When processing such as connecting WNT to other molecules, S
It is necessary to open the WNT cap or tube wall.

【０００４】ＳＷＮＴの終端のキャップを取る方法とし
ては、従来より、酸素雰囲気条件を注意深く制御する方
法や、エタノール中に分散させて超音波をかけること
で、キャップ部分の５員環の弱い結合を切る方法が知ら
れている。しかし、この方法では開孔条件が確立されて
おらず、またＳＷＮＴの管壁に開孔することはできなか
った。[0004] Conventionally, as a method of removing the end cap of SWNT, a method of carefully controlling the oxygen atmosphere condition or a method of dispersing in ethanol and applying ultrasonic waves to weaken the five-membered ring of the cap portion. A method of cutting is known. However, in this method, the opening conditions have not been established, and it has not been possible to open the SWNT tube wall.

【０００５】また、ＳＷＮＴの管壁を開孔する方法とし
ては、適当な質量とエネルギーのイオンをＳＷＮＴに照
射する方法が提案されている。しかしながら、この方法
は、大掛かりな装置と細かな作業を必要とし、大量のＳ
ＷＮＴの管壁を開孔することは困難であった。[0005] As a method of opening the SWNT tube wall, a method of irradiating SWNTs with ions having an appropriate mass and energy has been proposed. However, this method requires extensive equipment and detailed work, and requires a large amount of S
It was difficult to open the WNT tube wall.

【０００６】そこで、この出願の発明は、以上の通りの
事情に鑑みてなされたものであり、従来技術の問題点を
解消し、単層カーボンナノチューブを用いたデバイス材
料等の高機能材料の開発に有用で、その管壁にも開孔で
きる、簡便で新しい単層カーボンナノチューブの開孔方
法を提供することを課題としている。Accordingly, the invention of this application has been made in view of the above circumstances, and solves the problems of the prior art, and develops high-performance materials such as device materials using single-walled carbon nanotubes. It is an object of the present invention to provide a simple and new method for opening single-walled carbon nanotubes, which is useful for forming a single-walled carbon nanotube.

【０００７】[0007]

【課題を解決するための手段】そこで、この出願の発明
は、上記の課題を解決するものとして、以下の通りの発
明を提供する。Accordingly, the invention of this application provides the following invention to solve the above problems.

【０００８】すなわち、まず第１には、この出願の発明
は、単層カーボンナノチューブを２００〜６００℃の温
度範囲の乾燥反応性ガス中に１分以上保持することで、
単層カーボンナノチューブに直径１〜２ｎｍの孔を開孔
することを特徴とする単層カーボンナノチューブの開孔
方法を提供する。That is, first of all, the invention of this application is to hold single-walled carbon nanotubes in a dry reactive gas in a temperature range of 200 to 600 ° C. for 1 minute or more.
Provided is a method for forming a single-walled carbon nanotube, characterized in that a hole having a diameter of 1 to 2 nm is formed in the single-walled carbon nanotube.

【０００９】そして第２には、この出願の発明は、上記
第１の発明において、保持温度を、３００〜４５０℃の
温度範囲とすることを特徴とする単層カーボンナノチュ
ーブの開孔方法を、第３には、開孔部が、単層カーボン
ナノチューブの端部あるいは管壁であることを特徴とす
る単層カーボンナノチューブの開孔方法を提供する。Secondly, the invention of this application is directed to a method for opening single-walled carbon nanotubes according to the first invention, wherein the holding temperature is in a temperature range of 300 to 450 ° C. Thirdly, the present invention provides a method for opening a single-walled carbon nanotube, wherein the opening is an end portion or a tube wall of the single-walled carbon nanotube.

【００１０】[0010]

【発明の実施の形態】この出願の発明は、上記の通りの
特徴を持つものであるが、以下にその実施の形態につい
て説明する。BEST MODE FOR CARRYING OUT THE INVENTION The invention of this application has the features as described above, and embodiments thereof will be described below.

【００１１】まず、この出願の発明が提供する単層カー
ボンナノチューブ（ＳＷＮＴ）の開孔方法は、ＳＷＮＴ
を２００〜６００℃の温度範囲の乾燥反応性ガス中に１
分以上保持することで、ＳＷＮＴに直径１〜２ｎｍの孔
を開孔することを特徴としている。First, the method of opening single-walled carbon nanotubes (SWNT) provided by the invention of this application is based on the SWNT
In a dry reactive gas in a temperature range of 200 to 600 ° C.
By holding for at least a minute, a hole having a diameter of 1 to 2 nm is formed in the SWNT.

【００１２】ＳＷＮＴは、一般に知られている各種の方
法で作製されたものを対象とすることができる。例え
ば、アーク放電法や、高温レーザ蒸発法、さらにはＣＶ
Ｄ（化学蒸着法）による合成方法等が例示される。ＳＷ
ＮＴは、精製されたものを用いてもよいし、未精製のも
のを用いてもよい。精製法としては、例えば、ＳＷＮＴ
を硝酸等の酸化性強酸中に入れ、１００〜２００℃で数
時間処理した後水洗する方法等がある。[0012] The SWNTs can be those manufactured by various generally known methods. For example, arc discharge method, high-temperature laser evaporation method, and CV
A synthesis method by D (chemical vapor deposition) is exemplified. SW
As the NT, a purified one or an unpurified one may be used. As a purification method, for example, SWNT
Is placed in a strong oxidizing acid such as nitric acid, treated at 100 to 200 ° C. for several hours, and then washed with water.

【００１３】このＳＷＮＴを、２００〜６００℃の温度
範囲の乾燥反応性ガス中に１分以上保持する。この様な
熱処理における保持温度は、２００〜６００℃の温度範
囲とすることができ、より好ましくは、３００〜４５０
℃の温度範囲とすることが示される。The SWNT is kept in a dry reactive gas at a temperature in the range of 200 to 600 ° C. for one minute or more. The holding temperature in such a heat treatment can be in a temperature range of 200 to 600 ° C, more preferably 300 to 450 ° C.
The temperature range is shown in ° C.

【００１４】熱処理の際の雰囲気は、乾燥反応性ガスと
する。反応性ガス中に水分が含まれている場合には、高
温での化学反応性が高められ、湿度の変化によりＳＷＮ
Ｔ開孔時の熱処理温度を大きく変化させてしまうため好
ましくない。乾燥反応性ガスとしては、乾燥空気、乾燥
酸素ガスあるいは酸素を２０％程度含んだ乾燥窒素ガス
（不活性ガス）等を使用することができ、なかでも乾燥
空気を用いることが好ましい。乾燥反応性ガスは、空気
等の反応性ガス中の水分を取り除いたものであり、たと
えば、一般に各種の高純度ガスとして入手できるもの等
を使用することができる。The atmosphere during the heat treatment is a dry reactive gas. When moisture is contained in the reactive gas, the chemical reactivity at high temperature is increased, and the change in humidity causes the SWN to change.
It is not preferable because the heat treatment temperature at the time of opening T is greatly changed. As the dry reactive gas, dry air, dry oxygen gas, dry nitrogen gas (inert gas) containing about 20% of oxygen, or the like can be used, and among them, dry air is preferably used. The dry reactive gas is a gas obtained by removing moisture in a reactive gas such as air, and for example, those generally available as various high-purity gases can be used.

【００１５】この様な条件下でのＳＷＮＴの保持時間を
調整することで、ＳＷＮＴの開孔数を制御することがで
きる。保持時間は、ＳＷＮＴの量や、保持温度および雰
囲気条件により異るが、１分以上、より具体的には、１
分〜数時間程度とすることができる。The number of SWNT holes can be controlled by adjusting the holding time of the SWNT under such conditions. The holding time varies depending on the amount of SWNT, the holding temperature, and the atmospheric conditions, but is 1 minute or more, more specifically, 1 minute.
It can be from minutes to several hours.

【００１６】なお、以上の熱処理は、上記温度範囲内の
一定の温度で保持する一段階処理であってもよいし、上
記温度範囲内の複数の温度で保持する多段階処理であっ
てもよいし、さらには、上記温度範囲内で処理温度を随
時変化させる処理方法等も考慮することができる。The above heat treatment may be a one-step treatment in which the temperature is maintained at a constant temperature within the above-mentioned temperature range, or a multi-step treatment in which the heat treatment is maintained at a plurality of temperatures within the above-mentioned temperature range. Further, a processing method or the like in which the processing temperature is changed as needed within the above temperature range can be considered.

【００１７】これによって、通常ＳＷＮＴの端部に形成
されているキャップをとるか、あるいは、管壁のカーボ
ン結合を切断することで、チューブ径と同じで直径１〜
２ｎｍの孔をＳＷＮＴに開けることができる。Thus, by taking the cap usually formed at the end of the SWNT, or by cutting the carbon bond of the tube wall, the diameter of the tube is reduced to 1 to 1 mm.
A 2 nm hole can be drilled in the SWNT.

【００１８】以上のような、この出願の発明のＳＷＮＴ
の開孔方法では、ＳＷＮＴの端部だけでなく、管壁にも
開孔することができる。そのため、この発明によって得
られたＳＷＮＴは、より多彩なＳＷＮＴの加工を可能と
し、単層カーボンナノチューブを用いたデバイス材料等
の高機能材料の開発に有用である。As described above, the SWNT of the invention of the present application
In the opening method described above, not only the end of the SWNT but also the tube wall can be opened. Therefore, the SWNTs obtained according to the present invention enable more versatile processing of SWNTs and are useful for the development of high-functional materials such as device materials using single-walled carbon nanotubes.

【００１９】また、この出願の発明のＳＷＮＴの開孔方
法では、レーザー等の大掛かりな装置や細かな作業を必
要とせず、簡便に多量のＳＷＮＴを開孔できるため、経
済的にも優れている。In addition, the method for opening SWNTs of the present invention does not require a large-scale device such as a laser or the like, and can easily open a large amount of SWNTs, which is economically excellent. .

【００２０】以下、添付した図面に沿って実施例を示
し、この発明の実施の形態についてさらに詳しく説明す
る。Hereinafter, embodiments of the present invention will be described in more detail with reference to the accompanying drawings.

【００２１】[0021]

【実施例】（実施例１）レーザー蒸発法によって、すす
状生成物質としてのＳＷＮＴを得た。得られたＳＷＮＴ
を硝酸等の酸化性強酸中に入れ、１００〜２００℃で数
時間処理した後水洗して精製することで、主として長さ
１〜１０μｍ，チューブ径１〜２ｎｍで、チューブの両
端がキャップで閉じた構造のＳＷＮＴを得た。EXAMPLES (Example 1) SWNT as a soot-like substance was obtained by a laser evaporation method. Obtained SWNT
Is placed in a strong oxidizing acid such as nitric acid, treated at 100-200 ° C. for several hours, washed with water and purified, mainly with a length of 1-10 μm, a tube diameter of 1-2 nm, and both ends of the tube are closed with caps. SWNT having the above structure was obtained.

【００２２】このＳＷＮＴを、乾燥空気を導入した容器
に入れ、４５０℃で３０時間保持した。処理後のＳＷＮ
Ｔを電子顕微鏡で観察した結果、ほぼすべてのＳＷＮＴ
の端部あるいは管壁に、直径１〜２ｎｍの孔が開孔して
いるのが確認された。 （実施例２）実施例１と同様の方法で得たすす状物質の
ＳＷＮＴを、精製せずに、乾燥空気を導入した容器に入
れ、４００℃で１時間保持した。その結果、実施例１の
場合と同様に、ほぼすべてのＳＷＮＴの端部あるいは管
壁に、直径１〜２ｎｍの孔が開孔しているのが確認され
た。 （実施例３）実施例１で得られた開孔を有するＳＷＮＴ
内に、Ｃ60分子を導入した際のＳＷＮＴを電子顕微鏡で
観察した。図１に、ＳＷＮＴの電子顕微鏡像を示した。This SWNT was placed in a container into which dry air had been introduced, and kept at 450 ° C. for 30 hours. SWN after processing
As a result of observing T with an electron microscope, almost all SWNTs
It was confirmed that a hole having a diameter of 1 to 2 nm was formed in the end portion or the tube wall. (Example 2) SWNT as a soot-like substance obtained in the same manner as in Example 1 was put in a container into which dry air was introduced without purification, and kept at 400 ° C for 1 hour. As a result, as in the case of Example 1, it was confirmed that holes having a diameter of 1 to 2 nm were formed in almost all the ends or the tube walls of the SWNTs. (Example 3) SWNT having an opening obtained in Example 1
Within, and the SWNT when introducing the C 60 molecule was observed with an electron microscope. FIG. 1 shows an electron microscope image of SWNT.

【００２３】図中の▼で示した部分のＳＷＮＴ端部ある
いは管壁に、開孔が確認された。An opening was confirmed at the end of the SWNT or the tube wall at the portion indicated by ▼ in the figure.

【００２４】もちろん、この発明は以上の例に限定され
るものではなく、細部については様々な態様が可能であ
ることは言うまでもない。Of course, the present invention is not limited to the above-described example, and it goes without saying that various aspects are possible in detail.

【００２５】[0025]

【発明の効果】以上詳しく説明した通り、この発明によ
って、単層カーボンナノチューブを用いたデバイス材料
等の高機能材料の開発に有用で、その管壁にも開孔でき
る、簡便で新しい単層カーボンナノチューブの開孔方法
が提供される。As described in detail above, the present invention is useful for the development of high-performance materials such as device materials using single-walled carbon nanotubes, and is simple and new single-walled carbon which can be opened in the tube wall. A method for opening nanotubes is provided.

【００２６】[0026]

【図面の簡単な説明】[Brief description of the drawings]

【００２７】[0027]

【図１】実施例において、チューブ内にＣ60分子を導入
したＳＷＮＴの電子顕微鏡像を例示した図である。[1] In the embodiment, a diagram illustrating an electron microscope image of SWNT was introduced C 60 molecules in the tube.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 坂東 俊治 愛知県日進市赤池５−1305 アクトピア赤 池ＩＩ−201 (72)発明者 末永 和知 愛知県名古屋市天白区中平１−603 アム ール中平601 (72)発明者 平原 佳織 愛知県日進市梅森台１−45 コーポ梅五 203 (72)発明者 岡崎 俊也 愛知県名古屋市昭和区神村町１−31−１ ユーハウスドーム四ツ谷1004 (72)発明者 篠原 久典 愛知県名古屋市天白区植田本町３−917 Ｆターム(参考） 4G046 CB01 CC03  ────────────────────────────────────────────────── ─── Continued on the front page (72) Inventor Shunji Bando 5-1305 Akaike, Nisshin City, Aichi Prefecture Actopia Akaike II-201 (72) Inventor Kazuchi Suenaga 1-603 Nakadaira, Tenpaku-ku, Nagoya City, Aichi Prefecture Nakadaira 601 (72) Inventor Kaori Hirahara 1-45 Umemoridai, Nisshin-shi, Aichi Prefecture Corp. Umego 203 (72) Inventor Toshiya Okazaki 1-31-1 Kamimuracho, Showa-ku, Nagoya-shi, Aichi U-House Dome Yotsuya 1004 (72) Inventor Hisanori Shinohara 3-917 Uedahonmachi, Tenpaku-ku, Nagoya-shi, Aichi F-term (reference) 4G046 CB01 CC03

Claims (3)

【特許請求の範囲】[Claims] 【請求項１】 単層カーボンナノチューブを２００〜６
００℃の温度範囲の乾燥反応性ガス中に１分以上保持す
ることで、単層カーボンナノチューブに直径１〜２ｎｍ
の孔を開孔することを特徴とする単層カーボンナノチュ
ーブの開孔方法。1. A method for preparing single-walled carbon nanotubes from 200 to 6
By holding in a dry reactive gas within a temperature range of 00 ° C. for 1 minute or more, the single-walled carbon nanotubes have a diameter of 1-2 nm.
A method for opening single-walled carbon nanotubes, comprising the steps of: 【請求項２】 保持温度を、３００〜４５０℃の温度範
囲とすることを特徴とする単層カーボンナノチューブの
開孔方法。2. A method for opening single-walled carbon nanotubes, wherein the holding temperature is in a temperature range of 300 to 450 ° C. 【請求項３】 開孔部が、単層カーボンナノチューブの
端部あるいは管壁であることを特徴とする請求項１記載
の単層カーボンナノチューブの開孔方法。3. The method for opening single-walled carbon nanotubes according to claim 1, wherein the opening is an end portion or a tube wall of the single-walled carbon nanotube.
JP2000286095A 2000-09-20 2000-09-20 Method for perforating monolayered carbon nanotube Pending JP2002097008A (en)

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