JP2003160319A - Method and apparatus for synthesizing single-wall carbon nanotube - Google Patents
Method and apparatus for synthesizing single-wall carbon nanotubeInfo
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- JP2003160319A JP2003160319A JP2001356514A JP2001356514A JP2003160319A JP 2003160319 A JP2003160319 A JP 2003160319A JP 2001356514 A JP2001356514 A JP 2001356514A JP 2001356514 A JP2001356514 A JP 2001356514A JP 2003160319 A JP2003160319 A JP 2003160319A
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- Prior art keywords
- carbon nanotube
- raw material
- synthesis chamber
- nanotube raw
- inert gas
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、プラズマにより
原料を蒸発させることにより、高い収率で大量合成を可
能にした単層カーボンナノチューブの合成方法及び合成
装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and apparatus for synthesizing single-walled carbon nanotubes, which enables large-scale synthesis with high yield by evaporating raw materials with plasma.
【０００２】[0002]
【従来の技術】単層カーボンナノチューブの合成法とし
ては、アーク放電法、レーザ蒸発法、化学気相成長法
（ＣＶＤ法）等が一般に知られている図２は、従来のア
ーク放電法の一例を示す図である。同図において、１は
合成チャンバ、３は不活性ガス供給装置（ボンベ）、９
は排気ポンプ、１６はアーク放電用のカーボン電極、１
７はカーボン電極１６に電力を供給する電源である。2. Description of the Related Art As a method for synthesizing a single-walled carbon nanotube, an arc discharge method, a laser evaporation method, a chemical vapor deposition method (CVD method), etc. are generally known. FIG. 2 shows an example of a conventional arc discharge method. FIG. In the figure, 1 is a synthesis chamber, 3 is an inert gas supply device (cylinder), 9
Is an exhaust pump, 16 is a carbon electrode for arc discharge, 1
Reference numeral 7 is a power source for supplying electric power to the carbon electrode 16.
【０００３】次に、動作について説明する。不活性ガス
供給装置３から合成チャンバ１内に不活性ガスを供給
し、カーボン電極１６に電力を供給してアーク放電１５
を行う。これにより、カーボン電極１６の一部を蒸発さ
せ、合成チャンバ１内でカーボンナノチューブ１２が合
成される。Next, the operation will be described. The inert gas is supplied from the inert gas supply device 3 into the synthesis chamber 1 to supply electric power to the carbon electrode 16 to cause the arc discharge 15
I do. As a result, a part of the carbon electrode 16 is evaporated and the carbon nanotubes 12 are synthesized in the synthesis chamber 1.
【０００４】図３は、従来のレーザ蒸発法の一例を示す
図である。同図において、１は合成チャンバ、３は不活
性ガス供給装置（ボンベ）、９は排気ポンプ、１８は合
成チャンバ１に取付けられたレーザ発振器、１９はカー
ボンナノチューブ回収部、２０は合成チャンバ１内に設
置されたカーボンペレットである。FIG. 3 is a diagram showing an example of a conventional laser evaporation method. In the figure, 1 is a synthesis chamber, 3 is an inert gas supply device (cylinder), 9 is an exhaust pump, 18 is a laser oscillator attached to the synthesis chamber 1, 19 is a carbon nanotube recovery section, and 20 is inside the synthesis chamber 1. Is a carbon pellet installed in.
【０００５】次に、動作について説明する。レーザ発振
器１８からレーザビーム２１をカーボンペレット２０に
照射する。これにより、カーボンペレット２０が蒸発
し、カーボンナノチューブ１２が合成される。Next, the operation will be described. The carbon pellet 20 is irradiated with the laser beam 21 from the laser oscillator 18. As a result, the carbon pellets 20 are evaporated and the carbon nanotubes 12 are synthesized.
【０００６】[0006]
【発明が解決しようとする課題】従来の単層カーボンナ
ノチューブの合成法は上記のように構成されていたの
で、以下のような問題があった。すなわち、図２のアー
ク放電法では、カーボン電極１６の一部を蒸発させるた
め、多量の蒸発生成物が合成されるが、この蒸発生成物
は合成チャンバ１内で散乱するのみで単層カーボンナノ
チューブ１２の成長に必要な反応場が長時間持続できな
いため、蒸発生成物中に含まれる単層カーボンナノチュ
ーブ１２の割合が低く、まとまった量を得ることが困難
である。また、図３のレーザ蒸発法では、レーザビーム
２１によるカーボンペレット２０の蒸発量はごく微量で
あり、したがって、大量の単層カーボンナノチューブの
の生産は困難である。この発明は、上記ような課題を解
決するためになされたもので、単層カーボンナノチュー
ブが高収率で大量に合成可能な単層カーボンナノチュー
ブの合成方法及び合成装置を提供することを目的とす
る。Since the conventional method for synthesizing single-walled carbon nanotubes is configured as described above, it has the following problems. That is, in the arc discharge method of FIG. 2, since a part of the carbon electrode 16 is evaporated, a large amount of evaporation product is synthesized, but this evaporation product is only scattered in the synthesis chamber 1 and is a single-wall carbon nanotube. Since the reaction field required for growth of 12 cannot be maintained for a long time, the ratio of the single-walled carbon nanotubes 12 contained in the evaporation product is low, and it is difficult to obtain a large amount. Further, in the laser evaporation method of FIG. 3, the evaporation amount of the carbon pellets 20 by the laser beam 21 is very small, so that it is difficult to produce a large amount of single-walled carbon nanotubes. The present invention has been made to solve the above problems, and an object of the present invention is to provide a method and an apparatus for synthesizing single-wall carbon nanotubes capable of synthesizing a large number of single-wall carbon nanotubes in a high yield. .
【０００７】[0007]
【課題を解決するための手段】この発明に係る単層カー
ボンナノチューブの合成方法は、合成チャンバに粉末状
又はガス状のカーボンナノチューブ原料を不活性ガスに
より送り込む工程と、前記合成チャンバ内で放電させて
プラズマを生成し、このプラズマで前記カーボンナノチ
ューブ原料を蒸発させることにより単層カーボンナノチ
ューブを得る工程と、を具備することを特徴とする。A method for synthesizing single-walled carbon nanotubes according to the present invention comprises a step of feeding a powdery or gaseous carbon nanotube raw material into a synthesis chamber by an inert gas, and discharging in the synthesis chamber. Plasma to generate a single-walled carbon nanotube by evaporating the carbon nanotube raw material with this plasma.
【０００８】この発明に係る単層カーボンナノチューブ
の合成方法は、合成チャンバ内に筒状の反応生成場維持
部材が配置され、カーボンナノチューブ原料の蒸発物質
を該反応生成場維持部材の内外で循環させることを特徴
とする。In the method for synthesizing single-walled carbon nanotubes according to the present invention, a tubular reaction product field maintaining member is arranged in the synthesis chamber, and vaporized substances of carbon nanotube raw materials are circulated inside and outside the reaction product field maintaining member. It is characterized by
【０００９】この発明に係る単層カーボンナノチューブ
の合成装置は、合成チャンバと、前記合成チャンバに連
結され、粉末状又はガス状のカーボンナノチューブ原料
を収容するカーボンナノチューブ原料収容部と、前記カ
ーボンナノチューブ原料収容部に不活性ガスを供給して
前記原料収容部に収容されたカーボンナノチューブ原料
を前記合成チャンバ内に送り込む不活性ガス供給装置
と、前記合成チャンバ内に設けられた放電電極と、前記
放電電極に開口部を対向させて前記合成チャンバ内に配
置された筒状の反応生成場維持部材と、を備えたことを
特徴とする。The single-walled carbon nanotube synthesizing apparatus according to the present invention comprises a synthesizing chamber, a carbon nanotube raw material storage unit which is connected to the synthetic chamber and stores powdery or gaseous carbon nanotube raw material, and the carbon nanotube raw material. An inert gas supply device that supplies an inert gas to the storage unit to feed the carbon nanotube raw material stored in the raw material storage unit into the synthesis chamber, a discharge electrode provided in the synthesis chamber, and the discharge electrode And a tubular reaction product field maintaining member disposed in the synthesis chamber with the opening facing each other.
【００１０】この発明に係る単層カーボンナノチューブ
の合成装置の放電電極は、ノズル状の開口部を有する筒
状体からなる外側電極と、該外側電極内に配置された内
側電極とで構成され、前記外側電極内に前記単層カーボ
ンナノチューブ原料を送り込むようにしたことを特徴と
する。The discharge electrode of the apparatus for synthesizing single-walled carbon nanotubes according to the present invention comprises an outer electrode made of a tubular body having a nozzle-shaped opening, and an inner electrode arranged inside the outer electrode. The single-walled carbon nanotube raw material is fed into the outer electrode.
【００１１】[0011]
【発明の実施の形態】以下、この発明の実施の一形態を
図面と共に説明する。なお、図２及び図３と同一部材又
は同一機能のものは同一符号で示している。図１におい
て、１は合成チャンバ、２は合成チャンバ１の上部に設
けられたカーボンナノチューブ原料収容部、３はこのカ
ーボンナノチューブ原料収容部２に不活性ガスを供給す
る不活性ガス供給装置、４は合成チャンバ１の下部に設
けられたカーボンナノチューブ回収部である。合成チャ
ンバ１内の右端部には、放電電極Ｐが設けられている。
この放電電極Ｐは、先端にノズル部５ａが形成された円
筒状の外側電極５と、その内部に設けられたピン状の内
側電極６とで構成され、この外側電極５と内側電極６と
の間に直流又は交流の電源７が接続されている。外側電
極５にはカーボンナノチューブ原料１０を収容するカー
ボンナノチューブ原料収容部２の管２ａが接続されてい
る。合成チャンバ１内には、筒状の反応生成場維持部材
８が前記外側電極５のノズル部５ａに対向して配設され
ている。なお、９は合成チャンバ１の上部に設けられた
排気装置である。BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the present invention will be described below with reference to the drawings. The same members or functions as those in FIGS. 2 and 3 are designated by the same reference numerals. In FIG. 1, reference numeral 1 is a synthesis chamber, 2 is a carbon nanotube raw material storage portion provided above the synthesis chamber 1, 3 is an inert gas supply device for supplying an inert gas to the carbon nanotube raw material storage portion 2, and 4 is It is a carbon nanotube recovery unit provided in the lower part of the synthesis chamber 1. A discharge electrode P is provided at the right end of the synthesis chamber 1.
The discharge electrode P is composed of a cylindrical outer electrode 5 having a nozzle portion 5a formed at its tip and a pin-shaped inner electrode 6 provided therein. The outer electrode 5 and the inner electrode 6 are A DC or AC power supply 7 is connected between them. The outer electrode 5 is connected to the tube 2 a of the carbon nanotube raw material storage portion 2 that stores the carbon nanotube raw material 10. In the synthesis chamber 1, a tubular reaction product field maintaining member 8 is arranged so as to face the nozzle portion 5a of the outer electrode 5. Reference numeral 9 is an exhaust device provided above the synthesis chamber 1.
【００１２】次に、動作について説明する。カーボンナ
ノチューブ原料収容部２に粉末状のカーボンナノチュー
ブ原料１０を収容し、不活性ガス供給装置３から不活性
ガスをカーボンナノチューブ原料収容部に供給し、カー
ボンナノチューブ原料１０を不活性ガスと共に外側電極
６と内側電極５の間に送り込む。電源７から両電極５，
６に交流又は直流の電力を供給する。これにより、電極
５，６間で放電し、不活性ガスによりプラズマ１１が生
成され、プラズマ１１中に単層カーボンナノチューブ原
料１０が供給される。カーボンナノチューブ原料１０は
プラズマ１１中で蒸発されて分解、再構成され、反応生
成場維持部材８内を通過しつつ単層カーボンナノチュー
ブ１２となってカーボンナノチューブ回収部４に回収さ
れる。なお、合成チャンバ１内の圧力は排気装置９によ
り調整されるようになっている。単層カーボンナノチュ
ーブ１２は、蒸発したカーボンが高温中で緩やかに成長
することにより生成される。反応生成場維持部材８は、
加熱ガスの拡散を抑制し、プラズマ１１による高温領域
を長く保つためのものである。Next, the operation will be described. The carbon nanotube raw material storage unit 2 stores the powdery carbon nanotube raw material 10 and an inert gas supply device 3 supplies an inert gas to the carbon nanotube raw material storage unit to supply the carbon nanotube raw material 10 together with the inert gas to the outer electrode 6 Between the inner electrode 5 and the inner electrode 5. Power source 7 to both electrodes 5,
6 is supplied with AC or DC power. As a result, electric discharge is generated between the electrodes 5 and 6, plasma 11 is generated by the inert gas, and the single-walled carbon nanotube raw material 10 is supplied into the plasma 11. The carbon nanotube raw material 10 is vaporized in the plasma 11, decomposed and reconstituted, and passes through the inside of the reaction production site maintaining member 8 to be converted into the single-walled carbon nanotubes 12 and recovered in the carbon nanotube recovery part 4. The pressure in the synthesis chamber 1 is adjusted by the exhaust device 9. The single-walled carbon nanotubes 12 are generated by slowly growing vaporized carbon at high temperature. The reaction production site maintaining member 8 is
This is for suppressing the diffusion of the heating gas and for keeping the high temperature region by the plasma 11 long.
【００１３】プラズマ１１により分解、再構成された原
料粉末の蒸発物質の一部は、単層カーボンナノチューブ
１２以外の物質となっているため、反応生成場維持部材
８の内外を循環するガス流１３によりプラズマ１１中に
再循環され、これにより、単層カーボンナノチューブの
回収率を高めている。Since a part of the vaporized substance of the raw material powder decomposed and reconstituted by the plasma 11 is a substance other than the single-walled carbon nanotube 12, a gas flow 13 circulating inside and outside the reaction product field maintaining member 8 is formed. Is recirculated into the plasma 11 by this, thereby increasing the recovery rate of the single-walled carbon nanotubes.
【００１４】なお、単層カーボンナノチューブ原料１０
は粉末状のもののほか、例えば、鉄ペンタカルボニル等
のガス状のものを使用してもよい。The single-walled carbon nanotube raw material 10
In addition to the powdery form, a gaseous form such as iron pentacarbonyl may be used.
【００１５】以上のように、本実施の形態によれば、合
成チャンバ１に粉末状又はガス状のカーボンナノチュー
ブ原料１０を不活性ガス供給装置３からの不活性ガスに
より送り込み、合成チャンバ１内で放電電極Ｐにより放
電させてプラズマ１１を生成し、このプラズマ１１でカ
ーボンナノチューブ原料１０を蒸発させると共に、合成
チャンバ１内に設けられた筒状の反応生成場維持部材８
の内外で蒸発物質を循環させるようにしたので、プラズ
マ１１により形成された高温反応場が反応生成場維持部
材８により長い時間維持されることになり、その結果単
層カーボンナノチューブ１２の収率を向上させることが
できる。As described above, according to the present embodiment, the powdery or gaseous carbon nanotube raw material 10 is fed into the synthesis chamber 1 by the inert gas from the inert gas supply device 3 and the inside of the synthesis chamber 1 is fed. The discharge electrode P discharges plasma 11 to generate the carbon nanotube raw material 10. The plasma 11 causes the carbon nanotube raw material 10 to evaporate, and the tubular reaction production site maintaining member 8 provided in the synthesis chamber 1
Since the evaporation material is circulated inside and outside the reactor, the high temperature reaction field formed by the plasma 11 is maintained for a long time by the reaction product field maintaining member 8, and as a result, the yield of the single-walled carbon nanotube 12 is increased. Can be improved.
【００１６】また、単層カーボンナノチューブ原料１０
として粉末状あるいはガス状のものを用いたので、原料
が効率的に蒸発され、これにより多量の単層カーボンナ
ノチューブを合成することが可能となる。Further, the single-wall carbon nanotube raw material 10
Since a powder or gas is used as the material, the raw material is efficiently evaporated, and a large amount of single-walled carbon nanotubes can be synthesized.
【００１７】また、円筒ノズル状の外側電極５と、ピン
状の内側電極６とで放電電極Ｐを構成し、外側電極５内
にカーボンナノチューブ原料１０を送り込むようにした
ので、原料がノズル部５ａから効率よく反応生成場維持
部材８に送り込まれ、収率をより高めることができる。
なお、放電電極Ｐは、例えば外側、内側ともに円筒体で
ある構成、あるいはピン相互を並設又は突き合わせた構
成でも実施は可能であり、放電電極Ｐの構成を図示の構
成に限定するものではない。Further, since the discharge electrode P is constituted by the cylindrical nozzle-shaped outer electrode 5 and the pin-shaped inner electrode 6, and the carbon nanotube raw material 10 is fed into the outer electrode 5, the raw material is the nozzle portion 5a. It can be efficiently sent to the reaction product field maintaining member 8 from the above, and the yield can be further improved.
The discharge electrode P can be implemented by, for example, a structure in which the outer side and the inner side are cylindrical bodies, or a structure in which pins are arranged side by side or abutted with each other, and the structure of the discharge electrode P is not limited to the illustrated structure. .
【００１８】[0018]
【発明の効果】以上のように、この発明によれば、合成
チャンバに粉末状又はガス状のカーボンナノチューブ原
料を不活性ガスにより送り込み、合成チャンバ内で放電
電極により放電させてプラズマを生成し、このプラズマ
でカーボンナノチューブ原料を蒸発させると共に、筒状
の反応生成場維持部材の内外で蒸発物質を循環させるよ
うにしたので、高温反応場が反応生成場維持部材により
長い時間維持されることになり、その結果単層カーボン
ナノチューブの収率を向上させることができると共に、
単層カーボンナノチューブ原料として粉末状あるいはガ
ス状のものを用いたので、原料が効率的に蒸発され、こ
れにより多量の単層カーボンナノチューブを合成するこ
とが可能となる効果がある。また、円筒ノズル状の外側
電極内に単層カーボンナノチューブ原料を送り込むよう
にしたので、原料がノズル部から効率よく反応生成場維
持部材に送り込まれ、収率をより高めることができる。As described above, according to the present invention, powdery or gaseous carbon nanotube raw material is fed into the synthesis chamber by an inert gas, and is discharged by a discharge electrode in the synthesis chamber to generate plasma, This plasma evaporates the carbon nanotube raw material and circulates the vaporized material inside and outside the tubular reaction product field maintaining member, so that the high temperature reaction field is maintained by the reaction product field maintaining member for a long time. As a result, the yield of single-walled carbon nanotubes can be improved, and
Since the powdery or gaseous material is used as the single-walled carbon nanotube raw material, there is an effect that the raw material is efficiently evaporated, whereby a large amount of single-walled carbon nanotube can be synthesized. Further, since the single-walled carbon nanotube raw material is fed into the cylindrical nozzle-shaped outer electrode, the raw material can be efficiently fed from the nozzle portion to the reaction product field maintaining member, and the yield can be further increased.
【図１】この発明の実施の形態による単層カーボンナノ
チューブの合成装置の縦断側面図である。FIG. 1 is a vertical side view of a single-wall carbon nanotube synthesizing apparatus according to an embodiment of the present invention.
【図２】従来のアーク放電法による単層カーボンナノチ
ューブの合成装置の一例を示す縦断側面図である。FIG. 2 is a vertical cross-sectional side view showing an example of a conventional apparatus for synthesizing single-walled carbon nanotubes by an arc discharge method.
【図３】従来のレーザ蒸発法による単層カーボンナノチ
ューブの合成装置の一例を示す縦断側面図である。FIG. 3 is a vertical sectional side view showing an example of a conventional apparatus for synthesizing single-walled carbon nanotubes by a laser evaporation method.
１ 合成チャンバ ２ カーボンナノチューブ原料収容部 ３ 不活性ガス供給装置 ４ カーボンナノチューブ回収部 ５ 外側電極 ５ａ ノズル部 ６ 内側電極 ７ 電源 ８ 反応生成場維持部材 ９ 排気装置 １０ 単層カーボンナノチューブ原料 Ｐ 放電電極 1 synthesis chamber 2 Carbon nanotube raw material storage 3 Inert gas supply device 4 Carbon nanotube recovery section 5 Outer electrode 5a nozzle part 6 inner electrode 7 power supply 8 Reaction production site maintenance member 9 exhaust system 10 Raw material for single-walled carbon nanotubes P discharge electrode
───────────────────────────────────────────────────── フロントページの続き (72)発明者 熊谷 幹郎 千葉県柏市高田1201 財団法人 産業創造 研究所内 Ｆターム(参考） 4G046 CA00 CA01 CB02 CC02 CC10 4L037 CS03 CT05 CT40 FA02 FA04 FA20 PA08 PA10 PA19 PA24 PA28 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Mikiro Kumagai 1201 Takada, Kashiwa City, Chiba Prefecture Industrial Creation In the laboratory F-term (reference) 4G046 CA00 CA01 CB02 CC02 CC10 4L037 CS03 CT05 CT40 FA02 FA04 FA20 PA08 PA10 PA19 PA24 PA28
Claims (4)
ボンナノチューブ原料を不活性ガスにより送り込む工程
と、 前記合成チャンバ内で放電させてプラズマを生成し、こ
のプラズマで前記カーボンナノチューブ原料を蒸発させ
ることにより単層カーボンナノチューブを得る工程と、
を具備することを特徴とする単層カーボンナノチューブ
の合成方法。1. A step of feeding a powdery or gaseous carbon nanotube raw material into the synthesis chamber by an inert gas, and causing discharge in the synthesis chamber to generate plasma, and the plasma to vaporize the carbon nanotube raw material. The step of obtaining a single-walled carbon nanotube by
A method for synthesizing single-walled carbon nanotubes, which comprises:
部材が配置され、カーボンナノチューブ原料の蒸発物質
を該反応生成場維持部材の内外で循環させることを特徴
とする請求項１記載の単層カーボンナノチューブの合成
方法。2. The cylindrical reaction product field maintaining member is arranged in the synthesis chamber, and the evaporated material of the carbon nanotube raw material is circulated inside and outside the reaction product field maintaining member. Method for the synthesis of single-walled carbon nanotubes.
ボンナノチューブ原料を収容するカーボンナノチューブ
原料収容部と、 前記カーボンナノチューブ原料収容部に不活性ガスを供
給して前記原料収容部に収容されたカーボンナノチュー
ブ原料を前記合成チャンバ内に送り込む不活性ガス供給
装置と、 前記合成チャンバ内に設けられた放電電極と、 前記放電電極に開口部を対向させて前記合成チャンバ内
に配置された筒状の反応生成場維持部材と、を備えたこ
とを特徴とする単層カーボンナノチューブの合成装置。3. A synthesis chamber, a carbon nanotube raw material storage unit which is connected to the synthesis chamber and stores a powdery or gaseous carbon nanotube raw material, and an inert gas is supplied to the carbon nanotube raw material storage unit to supply the carbon nanotube raw material. An inert gas supply device for feeding the carbon nanotube raw material stored in the raw material storage portion into the synthesis chamber, a discharge electrode provided in the synthesis chamber, and an inside of the synthesis chamber with an opening facing the discharge electrode. 1. A device for synthesizing single-walled carbon nanotubes, comprising:
筒状体からなる外側電極と、該外側電極内に配置された
内側電極とで構成され、前記外側電極内に単層カーボン
ナノチューブ原料を送り込むようにしたことを特徴とす
る請求項１記載の単層カーボンナノチューブの合成装
置。4. The discharge electrode is composed of an outer electrode made of a tubular body having a nozzle-shaped opening and an inner electrode arranged in the outer electrode, and the single-walled carbon nanotube raw material is provided in the outer electrode. 2. The apparatus for synthesizing single-wall carbon nanotubes according to claim 1, wherein
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| JP3863009B2 JP3863009B2 (en) | 2006-12-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100665993B1 (en) | 2005-01-04 | 2007-01-10 | 삼성전자주식회사 | Apparatus for producing nano-particles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100665993B1 (en) | 2005-01-04 | 2007-01-10 | 삼성전자주식회사 | Apparatus for producing nano-particles |
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| Publication number | Publication date |
|---|---|
| JP3863009B2 (en) | 2006-12-27 |
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