JP2003277033A - Method for growing carbon nanotube - Google Patents
Method for growing carbon nanotubeInfo
- Publication number
- JP2003277033A JP2003277033A JP2002084173A JP2002084173A JP2003277033A JP 2003277033 A JP2003277033 A JP 2003277033A JP 2002084173 A JP2002084173 A JP 2002084173A JP 2002084173 A JP2002084173 A JP 2002084173A JP 2003277033 A JP2003277033 A JP 2003277033A
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- JP
- Japan
- Prior art keywords
- metal pattern
- layer
- catalytic metal
- growing
- carbon nanotubes
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電子デバイスに応
用が期待されるカーボンナノチューブの成長方法に関す
る。TECHNICAL FIELD The present invention relates to a method for growing carbon nanotubes, which is expected to be applied to electronic devices.
【０００２】[0002]
【従来の技術】カーボンナノチューブは、炭素６員環が
連なったグラファイトの一層を丸めた直径約数ｎｍの円
筒状の物質である。所望の構造のカーボンナノチューブ
を作り、これをつなげることができれば、ナノメートル
サイズのデバイスが実現可能となるため、近年注目され
る素材の一つである。2. Description of the Related Art Carbon nanotubes are cylindrical substances each having a diameter of about several nm obtained by rolling a single layer of graphite in which carbon 6-membered rings are connected. If carbon nanotubes having a desired structure can be produced and connected to each other, a nanometer-sized device can be realized.
【０００３】このようなカーボンナノチューブの成長方
法としては、例えばアーク放電法及びＣＶＤ法があげら
れる。Examples of methods for growing such carbon nanotubes include an arc discharge method and a CVD method.
【０００４】アーク放電法では、やや減圧下で、例えば
アルゴン、水素等の雰囲気中、炭素棒の間に２０Ｖ５０
Ａ程度のアーク放電を行うと、炉の内側に煤として付着
する物質の中にカーボンナノチューブが見られる。In the arc discharge method, under a slightly reduced pressure, for example, in an atmosphere of argon, hydrogen or the like, a voltage of 20V50 is applied between carbon rods.
When an arc discharge of about A is performed, carbon nanotubes are found in the substance that adheres as soot inside the furnace.
【０００５】また、ＣＶＤ法では、炭素源となる炭素化
合物を５００ないし１０００℃で触媒金属微粒子と接触
させることにより、カーボンナノチューブが得られる。In the CVD method, carbon nanotubes can be obtained by bringing a carbon compound serving as a carbon source into contact with catalytic metal fine particles at 500 to 1000 ° C.
【０００６】しかしながら、これらの方法では、炉及び
触媒に付着したカーボンナノチューブを含む粉塵を集め
て精製する必要があり、また、これにより得られるもの
はカーボンナノチューブの束である。このため、カーボ
ンナノチューブをトランジスタ等の電子素子に応用する
場合に、基板上の所望の位置に単一のカーボンナノチュ
ーブを配置することは極めて困難であった。However, in these methods, it is necessary to collect and purify the dust containing the carbon nanotubes attached to the furnace and the catalyst, and the product obtained by this is a bundle of carbon nanotubes. Therefore, when the carbon nanotube is applied to an electronic device such as a transistor, it is extremely difficult to dispose a single carbon nanotube at a desired position on the substrate.
【０００７】[0007]
【発明が解決しようとする課題】本発明は、上記事情に
鑑みてなされたもので、高品質なカーボンナノチューブ
を所望の位置に成長する方法を提供することを目的とす
る。The present invention has been made in view of the above circumstances, and an object thereof is to provide a method for growing high-quality carbon nanotubes at desired positions.
【０００８】[0008]
【課題を解決するための手段】本発明のカーボンナノチ
ューブの成長方法は、基板上に、２種以上の異なる触媒
金属層が積層された多層触媒金属パターンを形成する工
程、及び該多層触媒金属パターンを加熱処理する工程、
及び加熱処理された該多層触媒金属パターン上に、ＣＶ
Ｄ法により、カーボンナノチューブを成長させる工程を
具備することを特徴とする。The carbon nanotube growth method of the present invention comprises a step of forming a multilayer catalytic metal pattern in which two or more different catalytic metal layers are laminated on a substrate, and the multilayer catalytic metal pattern. Heat treatment step,
And CV on the heat-treated multi-layer catalytic metal pattern.
The method is characterized by including a step of growing carbon nanotubes by the D method.
【０００９】[0009]
【発明の実施の形態】本発明のカーボンナノチューブの
成長方法は、基板上に、触媒金属パターンを形成し、こ
の基板を、炭素または炭素原料を使用してＣＶＤ（Ｃｈ
ｅｍｉｃａｌＶａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ）法に
供することにより、触媒金属パターン上にカーボンナノ
チューブを製造する方法において、触媒金属パターン
は、２種以上の異なる触媒金属層が積層された多層触媒
金属パターンからなり、この多層触媒金属パターンは、
ＣＶＤ法に供される前に加熱処理されることを特徴とす
る。BEST MODE FOR CARRYING OUT THE INVENTION The carbon nanotube growth method of the present invention comprises forming a catalytic metal pattern on a substrate, and then subjecting this substrate to CVD (Ch
In the method of producing carbon nanotubes on a catalyst metal pattern by subjecting the catalyst metal pattern to an electrical vapor deposition method, the catalyst metal pattern comprises a multilayer catalyst metal pattern in which two or more different catalyst metal layers are laminated. The pattern is
It is characterized in that it is heat-treated before being subjected to the CVD method.
【００１０】本発明によれば、多層触媒金属パターンを
形成する基板上の位置を選択することにより、基板上の
所望の位置にカーボンナノチューブを形成することがで
きる。また、本発明によれば、２種以上の異なる触媒金
属層を積層した多層金属触媒パターンを使用し、かつＣ
ＶＤ法を行う前に加熱処理をすることにより、曲がりが
少なく、十分な長さを有するカーボンナノチューブを成
長させることができる。According to the present invention, the carbon nanotube can be formed at a desired position on the substrate by selecting the position on the substrate where the multilayer catalytic metal pattern is formed. Also, according to the present invention, a multilayer metal catalyst pattern in which two or more different catalyst metal layers are laminated is used, and C
By performing the heat treatment before performing the VD method, it is possible to grow carbon nanotubes having a small bend and a sufficient length.
【００１１】基板としては、半導体基板、金属基板、ガ
ラス基板、及びアルミナ基板等を使用することができ
る。As the substrate, a semiconductor substrate, a metal substrate, a glass substrate, an alumina substrate or the like can be used.
【００１２】ＣＶＤ法としては、例えば熱化学的気相成
長法（熱ＣＶＤ法）またはプラズマ化学的気相成長法
（プラズマＣＶＤ法）を用いることができる。As the CVD method, for example, a thermochemical vapor deposition method (thermal CVD method) or a plasma chemical vapor deposition method (plasma CVD method) can be used.
【００１３】多層触媒金属パターンの各層は、白金、コ
バルト、鉄、ニッケル、及びパラジウムのうち少なくと
も１種の金属、またはこれらの２種以上を用いた合金等
であることが好ましい。上述の金属は、カーボンナノチ
ューブの成長に使用される触媒として好適である。Each layer of the multilayer catalytic metal pattern is preferably made of at least one metal selected from platinum, cobalt, iron, nickel and palladium, or an alloy using two or more of these metals. The metals mentioned above are suitable as catalysts used for the growth of carbon nanotubes.
【００１４】より好ましくは、多層触媒金属パターン
は、白金及びコバルトのうち少なくとも１種を含む。さ
らにまた好ましくは、多層触媒金属パターンは、白金を
含有する触媒金属層とコバルトを含有する触媒金属層と
を含む。例えば多層触媒金属パターンとして、白金層と
コバルト層とを積層することができる。この場合、白金
層上にコバルト層を形成することが望ましく、その厚さ
の比は、例えば白金層１に対し、コバルト層０．００１
ないし１であることが好ましい。More preferably, the multilayer catalytic metal pattern comprises at least one of platinum and cobalt. Still more preferably, the multilayer catalytic metal pattern comprises a catalytic metal layer containing platinum and a catalytic metal layer containing cobalt. For example, a platinum layer and a cobalt layer can be laminated as a multilayer catalytic metal pattern. In this case, it is desirable to form a cobalt layer on the platinum layer, and the thickness ratio is, for example, 0.001 cobalt layer to 1 platinum layer.
It is preferably from 1 to 1.
【００１５】また、加熱処理の温度は、好ましくは、５
００℃ないし１０００℃であり、この範囲であると触媒
活性がより高まる。５００℃未満であると、カーボンナ
ノチューブの成長が少なくなる傾向があり、また、１０
００℃を超えると、多層触媒金属パターンの変形等が発
生する傾向がある。より好ましくは、７００ないし９０
０℃である。The temperature of the heat treatment is preferably 5
The temperature is from 00 ° C to 1000 ° C, and in this range, the catalytic activity is further enhanced. If the temperature is lower than 500 ° C., the growth of carbon nanotubes tends to decrease,
If the temperature exceeds 00 ° C, the multilayer catalytic metal pattern may be deformed. More preferably 700 to 90
It is 0 ° C.
【００１６】また、ＣＶＤ法として熱ＣＶＤ法を用いる
場合、上記加熱処理の温度はカーボンナノチューブの成
長温度よりも１００ないし３００℃高いことが好まし
い。When the thermal CVD method is used as the CVD method, the temperature of the heat treatment is preferably 100 to 300 ° C. higher than the growth temperature of the carbon nanotubes.
【００１７】この加熱処理は、例えば常圧下、及び窒素
または希ガス雰囲気下で、あるいは真空下で行われるこ
とが好ましい。This heat treatment is preferably carried out, for example, under normal pressure and under a nitrogen or rare gas atmosphere, or under vacuum.
【００１８】多層触媒金属パターンは、少なくとも２つ
の独立した多層触媒層を有することが好ましい。例えば
複数の多層触媒層をアレイ状に形成することができる。
１つの多層触媒層の大きさは、その最大長さが１０ｎｍ
以上であることが好ましい。例えばトランジスタ等の電
子デバイスに使用する場合には、例えば１０ｎｍないし
数十μｍであることが好ましい。The multilayer catalytic metal pattern preferably has at least two independent multilayer catalytic layers. For example, a plurality of multilayer catalyst layers can be formed in an array.
The maximum length of one multilayer catalyst layer is 10 nm.
The above is preferable. For example, when used in an electronic device such as a transistor, the thickness is preferably, for example, 10 nm to several tens of μm.
【００１９】個々の多層触媒層の形状としては、ドッ
ト、円形、及び四角等があげられる。The shape of each multilayer catalyst layer includes dots, circles, squares and the like.
【００２０】多層触媒金属パターンの形成方法として
は、例えばフォトリソグラフィー法あるいは電子リソグ
ラフィー法によるレジストパターン形成後、真空蒸着法
により触媒金属を蒸着し、レジストパターン溶解してリ
フトオフを行う方法などがあげられる。As a method of forming the multilayer catalytic metal pattern, for example, after forming a resist pattern by a photolithography method or an electron lithography method, a catalytic metal is vapor-deposited by a vacuum vapor deposition method, and the resist pattern is dissolved to perform lift-off. .
【００２１】本発明によれば、曲がりが少なく、十分な
長さを有するカーボンナノチューブを基板上の所望の位
置に形成することができるので、トランジスタのチャネ
ル及びゲート電極、論理回路及び集積回路の配線とし
て、使用可能である。According to the present invention, since carbon nanotubes having a small amount of bending and having a sufficient length can be formed at desired positions on a substrate, channel and gate electrodes of transistors, wiring of logic circuits and integrated circuits are formed. Can be used as
【００２２】[0022]
【実施例】以下、実施例を示し、本明を具体的に説明す
る。EXAMPLES The present invention will be specifically described below with reference to examples.
【００２３】実施例
例えば２ｃｍ×２ｃｍの大きさの半導体基板上に、フォ
トリソグラフィーにより、５μｍ径のドット状の多層触
媒層を５μｍ間隔でアレイ状に配列した多層触媒金属パ
ターンを形成した。EXAMPLE A multi-layer catalytic metal pattern in which dot-shaped multi-layer catalytic layers each having a diameter of 5 μm were arranged in an array at intervals of 5 μm was formed on a semiconductor substrate having a size of 2 cm × 2 cm, for example, by photolithography.
【００２４】得られた多層触媒金属パターンの電子顕微
鏡写真を図１に示す。An electron micrograph of the obtained multilayer catalytic metal pattern is shown in FIG.
【００２５】多層金属層は、白金３０ｎｍとコバルト１
０ｎｍの２層構造とした。The multilayer metal layer is composed of platinum 30 nm and cobalt 1
It has a two-layer structure of 0 nm.
【００２６】多層触媒金属パターンを形成した半導体基
板を、真空加熱装置内に載置し、常圧下、窒素雰囲気、
８００℃で５分間加熱処理を行った。The semiconductor substrate on which the multilayer catalytic metal pattern is formed is placed in a vacuum heating device, and under normal pressure, in a nitrogen atmosphere,
Heat treatment was performed at 800 ° C. for 5 minutes.
【００２７】その後この半導体基板を熱ＣＶＤ装置管状
炉内に載置し、管状炉を６００℃に加熱して、常圧下
で、原料ガスとして流量２０ｍｌ／分のアセチレンガス
と流量１５０ｍｌ／分のアルゴンガスの混合ガスを使用
し、３０分間蒸着を行い、カーボンナノチューブ成長さ
せた。Then, this semiconductor substrate is placed in a tubular furnace of a thermal CVD apparatus, the tubular furnace is heated to 600 ° C., and acetylene gas having a flow rate of 20 ml / min and argon having a flow rate of 150 ml / min are used as a source gas under normal pressure. Using a mixed gas of gases, vapor deposition was performed for 30 minutes to grow carbon nanotubes.
【００２８】得られたカーボンナノチューブの電子顕微
鏡写真を図２に示す。An electron micrograph of the obtained carbon nanotube is shown in FIG.
【００２９】図示するように、直径約２０ｎｍの曲がり
の少ないカーボンナノチューブが、一方の多層触媒層
と、他方の触媒層との間を橋渡しするように、基板表面
に沿って成長していた。As shown in the drawing, carbon nanotubes having a diameter of about 20 nm and less bending were grown along the surface of the substrate so as to bridge between the multilayer catalyst layer on one side and the catalyst layer on the other side.
【００３０】比較例
なお、比較として、多層触媒金属パターンの代わりに、
白金の単層金属パターンを形成した場合、コバルトの単
層金属パターンを形成した場合、及び加熱処理を行わな
い場合について、各々実施例と同様にしてカーボンナノ
チューブを成長させた。Comparative Example As a comparison, instead of the multilayer catalyst metal pattern,
Carbon nanotubes were grown in the same manner as in each of the examples in which the platinum single-layer metal pattern was formed, the cobalt single-layer metal pattern was formed, and the heat treatment was not performed.
【００３１】しかしながら、白金の単層金属パターンを
形成した場合、カーボンナノチューブは成長せず、コバ
ルトの単層金属パターンを形成した場合、カーボンナノ
チューブは成長したが、得られたカーボンナノチューブ
は曲がりが多く、例えば２μｍ程の短いものであり、及
び加熱処理を行わない場合、カーボンナノチューブが成
長しなかった。However, when the platinum single-layer metal pattern was formed, the carbon nanotubes did not grow. When the cobalt single-layer metal pattern was formed, the carbon nanotubes grew, but the obtained carbon nanotubes had many bends. The carbon nanotubes did not grow when the heat treatment was not performed, for example, as short as 2 μm.
【００３２】[0032]
【発明の効果】本発明のカーボンナノチューブの成長方
法によれば、曲がりが少なく、十分な長さを有する高品
質なカーボンナノチューブを、所望の位置に成長するこ
とができる。According to the method of growing a carbon nanotube of the present invention, it is possible to grow a high-quality carbon nanotube having little bending and a sufficient length at a desired position.
【図１】多層触媒パターンの電子顕微鏡写真1] Electron micrograph of multilayer catalyst pattern
【図２】カーボンナノチューブの電子顕微鏡写真[Fig. 2] Electron micrograph of carbon nanotube
─────────────────────────────────────────────────────
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【手続補正書】[Procedure amendment]
【提出日】平成１５年３月１７日（２００３．３．１
７）[Submission date] March 17, 2003 (2003.3.1)
7)
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】特許請求の範囲[Name of item to be amended] Claims
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【特許請求の範囲】[Claims]
【手続補正２】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００８[Correction target item name] 0008
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【０００８】[0008]
【課題を解決するための手段】本発明カーボンナノチュ
ーブの成長方法は、基板上に、２種以上の異なる触媒金
属層が積層された多層触媒金属パターンを形成する工
程、及び該多層触媒金属パターンを加熱処理する工程、
及び加熱処理された該多層触媒金属パターン上に、ＣＶ
Ｄ法によりカーボンナノチューブを成長させる工程を具
備するカーボンナノチューブの成長方法であって、前記
多層触媒金属パターンは、コバルトを含有する触媒金属
層と、白金、鉄、ニッケルからなる群から選択される少
なくとも１種を含有する触媒金属層とが積層されたこと
を特徴とする。The carbon nanotube growth method of the present invention comprises a step of forming a multi-layer catalyst metal pattern in which two or more different catalyst metal layers are laminated on a substrate, and the multi-layer catalyst metal pattern. Process of heat treatment,
And CV on the heat-treated multi-layer catalytic metal pattern.
A method for growing carbon nanotubes, comprising the step of growing carbon nanotubes by method D , comprising:
The multilayer catalyst metal pattern is a catalyst metal containing cobalt.
Layers and a small number selected from the group consisting of platinum, iron and nickel.
It is characterized in that a catalyst metal layer containing at least one kind is laminated .
フロントページの続き Ｆターム(参考） 4G069 AA03 AA08 BB02A BB02B BC67A BC67B BC75A BC75B CB81 EA11 EC28 EC29 EE06 FA01 FB29 FC07 4G146 AA11 AB08 BA12 BC09 BC23 BC33A BC33B BC43 BC48 4K030 AA09 AA16 BA27 BB01 BB14 CA04 DA02 FA01 FA10 Continued front page F-term (reference) 4G069 AA03 AA08 BB02A BB02B BC67A BC67B BC75A BC75B CB81 EA11 EC28 EC29 EE06 FA01 FB29 FC07 4G146 AA11 AB08 BA12 BC09 BC23 BC33A BC33B BC43 BC48 4K030 AA09 AA16 BA27 BB01 BB14 CA04 DA02 FA01 FA10
Claims (7)
が積層された多層触媒金属パターンを形成する工程、及
び該多層触媒金属パターンを加熱処理する工程、及び加
熱処理された該多層触媒金属パターン上に、ＣＶＤ法に
よりカーボンナノチューブを成長させる工程を具備する
ことを特徴とするカーボンナノチューブの成長方法。1. A step of forming a multi-layer catalyst metal pattern in which two or more different catalyst metal layers are laminated on a substrate, a step of heat-treating the multi-layer catalyst metal pattern, and the heat-treated multi-layer catalyst. A method of growing carbon nanotubes, comprising a step of growing carbon nanotubes on a metal pattern by a CVD method.
有する触媒金属層を含むことを特徴とする請求項１に記
載のカーボンナノチューブの成長方法。2. The method of growing a carbon nanotube according to claim 1, wherein the multilayer catalytic metal pattern includes a catalytic metal layer containing platinum.
有する触媒金属層とコバルトを含有する触媒金属層とを
含むことを特徴とする請求項１に記載のカーボンナノチ
ューブの成長方法。3. The method of growing a carbon nanotube according to claim 1, wherein the multi-layer catalytic metal pattern includes a catalytic metal layer containing platinum and a catalytic metal layer containing cobalt.
も２つの独立した多層触媒金属層を含むことを特徴とす
る請求項１に記載のカーボンナノチューブの成長方法。4. The method of claim 1, wherein the multilayer catalytic metal pattern includes at least two independent multilayer catalytic metal layers.
ることを特徴とする請求項４に記載のカーボンナノチュ
ーブの成長方法。5. The method for growing carbon nanotubes according to claim 4, wherein the multi-layer catalyst layer is formed in an array.
００℃で行われる請求項１に記載のカーボンナノチュー
ブの成長方法。6. The heat treatment step comprises 500 to 10
The method for growing a carbon nanotube according to claim 1, which is performed at 00 ° C.
程は、熱ＣＶＤ法またはプラズマＣＶＤ法を用いて行わ
れることを特徴とする請求項１に記載のカーボンナノチ
ューブの成長方法。7. The method of growing a carbon nanotube according to claim 1, wherein the step of forming the carbon nanotube is performed using a thermal CVD method or a plasma CVD method.
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