JP3337313B2 - Method and apparatus for producing fullerenes - Google Patents
Method and apparatus for producing fullerenesInfo
- Publication number
- JP3337313B2 JP3337313B2 JP07534194A JP7534194A JP3337313B2 JP 3337313 B2 JP3337313 B2 JP 3337313B2 JP 07534194 A JP07534194 A JP 07534194A JP 7534194 A JP7534194 A JP 7534194A JP 3337313 B2 JP3337313 B2 JP 3337313B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- fullerenes
- carbonaceous electrode
- electrode rod
- switching
- 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.)
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Description
【０００１】[0001]
【産業上の利用分野】本発明は、Ｃ60、Ｃ70、Ｃ76、Ｃ
78等の物性を有するフラーレン類を効率よく製造するた
めの方法および装置に関する。The present invention relates to C 60 , C 70 , C 76 , C
The present invention relates to a method and an apparatus for efficiently producing fullerenes having physical properties such as 78 .
【０００２】[0002]
【従来の技術】フラーレンは、炭素原子が数十個集合し
た性状の炭素分子（カーボンクラスター）を指し、現
在、Ｃ60、Ｃ70、Ｃ76、Ｃ78などの物質が知られてい
る。このフラーレンは、１９８５年にクロト(Kuroto)と
スモーリー(Smalley) らによって炭素により構成された
サッカーボール状のクラスター分子の存在が実験的に確
認され、次いで１９９０年にクレッチマー(Kratschmer)
とハフマン(Huffman) らによりＣ60、Ｃ70の合成が発表
されて以来、黒鉛およびダイヤモンドに次ぐ第３の新規
な炭素物質として注目を集めている。分子構造が解明さ
れた当初は固体潤滑剤や触媒への応用が考えられていた
が、その後Ｃ60の結晶層間に微量のカリウムをドープす
ると超電導体（Tc＝18K)になることが実証され、用途面
での期待が一層高まっている。2. Description of the Related Art Fullerene is a carbon molecule (carbon cluster) in which several tens of carbon atoms are gathered, and substances such as C 60 , C 70 , C 76 and C 78 are currently known. This fullerene was experimentally confirmed in 1985 by Kuroto and Smallley et al. In the presence of a soccer-ball-like cluster molecule composed of carbon, and then in 1990 by Kratschmer.
Since the announcement of the synthesis of C 60 and C 70 by Huffman et al., It has attracted attention as the third new carbon material after graphite and diamond. Initially the molecular structure has been elucidated was considered to be applied to the solid lubricant and a catalyst, been demonstrated that subsequently become Doping potassium traces between crystal layers of C 60 superconductors (Tc = 18K), Expectations in applications are increasing.
【０００３】フラーレン類は、高温で気化させた炭素蒸
気を冷却再凝固する方法により生成されるが、炭素を蒸
発させる加熱手段として、燃焼法、抵抗加熱法、レーザ
ー加熱法、アーク放電法などが試みられている。このう
ち、燃焼法は減圧下でベンゼンを燃焼源として酸素およ
びアルゴン雰囲気下で燃焼させたり、内燃機関（化学工
業、2/25,1992)を用いて加熱する方法、抵抗加熱法は炭
素棒に通電して抵抗発熱する方法、そしてレーザー加熱
法は黒鉛板に高エネルギーのレーザー光を照射させる方
法である。アーク放電法は前記したクレッチマー(Krats
chmer)等により大量合成法として報告(Nature,347,354,
1990) された方法で、５０〜２００TorrのＨｅ雰囲気容
器内で陽極・陰極となる一対の黒鉛電極間にアーク放電
させて炭素を蒸発させることによりフラーレン類を含む
スート粉末として回収する方法である。[0003] Fullerenes are produced by a method of cooling and resolidifying carbon vapor vaporized at a high temperature. As a heating means for evaporating carbon, a combustion method, a resistance heating method, a laser heating method, an arc discharge method and the like are used. Attempted. Of these, the combustion method uses benzene as a combustion source under reduced pressure and burns in an atmosphere of oxygen and argon, or the heating method using an internal combustion engine (Chemical Industry, 2/25, 1992) .The resistance heating method uses a carbon rod. The method of generating heat by resistance when energized and the laser heating method are methods of irradiating a graphite plate with high-energy laser light. The arc discharge method is based on the aforementioned Kretschmer (Krats
chmer), etc. (Nature, 347, 354,
1990) in a 50-200 Torr He atmosphere container, by arc discharge between a pair of graphite electrodes serving as an anode and a cathode to evaporate carbon, thereby recovering soot powder containing fullerenes.
【０００４】[0004]
【発明が解決しようとする課題】上記方法のうちでは、
アーク放電法、とくに安定な直流アーク放電を用いて炭
素蒸気を気化させるプロセスが工業的に有利であるが、
従来技術では炭素蒸発量が高い割にはフラーレンの生成
効率が低く、また経時的に陽極炭素質電極棒からの炭素
蒸発速度が減退する現象があった。SUMMARY OF THE INVENTION Among the above methods,
The arc discharge method, in particular, the process of vaporizing carbon vapor using a stable DC arc discharge is industrially advantageous,
In the prior art, the efficiency of fullerene generation was low in spite of the high carbon evaporation amount, and the rate of carbon evaporation from the anode carbonaceous electrode rod declined with time.
【０００５】本発明者は、この現象について究明したと
ころ、直流アーク放電において陽極炭素質電極棒から気
化した炭素蒸気はその一部が陰極炭素質電極棒の上に炭
素塊として析出・堆積し、これが原因でフラーレンの生
成が阻害されるとともに、経時的に陽極炭素質電極棒か
らの炭素の蒸発速度を低下させることが解明された。こ
のため、一定時間ごとに陰極炭素質電極棒に析出・堆積
した炭素塊を除去するか、陰極炭素質電極棒を新たに交
換しない限り、長時間に亘り効率よくフラーレンの生成
させることが不可能となる。The inventor of the present invention has investigated this phenomenon. As a result, a part of the carbon vapor vaporized from the anode carbonaceous electrode rod in the DC arc discharge is deposited and deposited as a carbon mass on the cathode carbonaceous electrode rod. It has been clarified that this causes inhibition of fullerene production and a reduction in the evaporation rate of carbon from the anodic carbonaceous electrode rod with time. For this reason, it is impossible to efficiently generate fullerenes over a long period of time unless the carbon mass deposited and deposited on the cathode carbonaceous electrode rod is removed at regular intervals or the cathode carbonaceous electrode rod is replaced anew. Becomes
【０００６】かかる陰極炭素質電極棒に対する炭素塊の
析出・堆積現象は、アーク放電を交流電流により発生さ
せることにより低減させることができるが、交流アーク
放電では直流アーク放電に比べて単位電力当たりの炭素
蒸発量が低くなるほか、生成したスート中に含有するフ
ラーレン類の含有率が著しく少なくなって工業的な生産
手段としては不適となる。[0006] The precipitation and deposition of carbon lumps on the cathode carbonaceous electrode rod can be reduced by generating an arc discharge by using an alternating current. In addition to the low carbon evaporation, the content of fullerenes in the soot thus produced is extremely low, making it unsuitable for industrial production.
【０００７】本発明は、直流アーク法を適用する際に障
害となる上記の課題を解決するためになされたもので、
常に効率よくフラーレン類を生成することができる直流
アーク法によるフラーレン類の製造方法および製造装置
の提供を目的とする。SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problem which is an obstacle when applying the DC arc method.
An object of the present invention is to provide a method and an apparatus for producing fullerenes by a DC arc method that can always efficiently produce fullerenes.
【０００８】[0008]
【課題を解決するための手段】上記の目的を達成するた
めの本発明によるフラーレン類の製造方法は、カーボン
源となる炭素質電極棒間に直流アークを発生させて高温
気化させた炭素蒸気を冷却再凝固させてフラーレン類を
回収する方法において、炭素質電極棒相互の極性を一定
時間毎に連続的に切り換えながらアーク放電させること
を構成上の特徴とする。In order to achieve the above object, the method for producing fullerenes according to the present invention is directed to a method of producing a DC vapor between carbonaceous electrode rods serving as a carbon source to produce a high-temperature vaporized carbon vapor. The method of recovering fullerenes by cooling and re-solidifying is characterized in that arc discharge is performed while continuously switching the polarity of the carbonaceous electrode rods at regular intervals.
【０００９】従来技術においては、直流アーク放電させ
る対極の炭素質電極棒はそれぞれ陽極および陰極に固定
されており、炭素蒸気は専ら陽極炭素質電極棒から気化
させる機構が採られていたが、本発明においては定時的
な極性切り換えによって両極の炭素質電極棒が相互にカ
ーボン源となる点に機能的特徴がある。したがって、対
極とする炭素質電極棒はいずれも炭素蒸気が発生し易い
同一の炭素質材料で構成することが好ましい態様とな
る。In the prior art, the carbonaceous electrode rods of the counter electrode to be subjected to DC arc discharge are fixed to the anode and the cathode, respectively, and a mechanism is employed in which carbon vapor is exclusively vaporized from the anode carbonaceous electrode rods. The present invention is characterized in that the carbonaceous electrode rods of both poles mutually serve as a carbon source by periodic polarity switching. Therefore, it is preferable that all the carbonaceous electrode rods serving as counter electrodes are made of the same carbonaceous material that easily generates carbon vapor.
【００１０】好適な炭素質電極棒は、黒鉛化度の発達し
た黒鉛材料により構成される。例えば、Ｘ線回折により
求めた (002)面の面間隔(d002)が３．３７１オングスト
ローム以下で、Ｃ軸方向の結晶子の大きさ(Lc)が２９０
オングストローム以上の結晶性状を有し、電気抵抗率が
１２５０μΩcm以下の特性を備える黒鉛材料がカーボン
源として最適で、該黒鉛材料から形成した炭素質電極棒
を用いることによりフラーレン含有率の高いスートを得
ることができる。A preferred carbonaceous electrode is made of a graphite material having a high degree of graphitization. For example, the (002) plane spacing (d002) determined by X-ray diffraction is 3.371 Å or less, and the crystallite size (Lc) in the C-axis direction is 290
A graphite material having a crystalline property of Å or more and an electrical resistivity of 1250 μΩcm or less is optimal as a carbon source, and a soot having a high fullerene content is obtained by using a carbonaceous electrode rod formed from the graphite material. be able to.
【００１１】フラーレン類は、カーボン源となる炭素質
電極棒間に直流アークを発生させて高温気化した炭素蒸
気を冷却再凝固することにより含有スートとして回収さ
れるが、アーク放電過程を通じて炭素質電極棒相互の極
性（＋−）を一定時間毎に連続的に切り換えながら操作
することが重要な要件となる。極性の切り換えは、２〜
２４０秒の時間範囲でおこなうことが好適である。この
極性切り換え時間が２秒未満では炭素蒸発量が低下し
て、単位時間内に得られるフラーレン含有スート量およ
びフラーレン類の生成量が低下し、他方、切り換え時間
が２４０秒を上廻る場合にも同様に炭素蒸発量が減少す
るほか、徐々に陰極時の炭素質電極棒に炭素塊が析出・
堆積して単位時間内に得られるフラーレン含有スート量
およびフラーレン類の生成量が低下する。より好ましい
極性切り換え時間の範囲は、１０〜６０秒である。[0011] Fullerenes are recovered as contained soot by generating a direct current arc between carbonaceous electrode rods serving as a carbon source and cooling and resolidifying the high-temperature vaporized carbon vapor. An important requirement is to operate while continuously switching the polarity (+-) between the bars at regular intervals. The polarity can be switched between 2
It is preferable to carry out in a time range of 240 seconds. If the polarity switching time is less than 2 seconds, the amount of carbon evaporation decreases, and the amount of fullerene-containing soot and fullerenes produced in a unit time decreases. On the other hand, when the switching time exceeds 240 seconds, Similarly, the amount of carbon evaporation decreases, and carbon lumps are gradually deposited on the carbonaceous electrode during cathode operation.
The amount of fullerene-containing soot and the amount of fullerenes produced within a unit time after deposition are reduced. A more preferable range of the polarity switching time is 10 to 60 seconds.
【００１２】直流アーク放電により陽極になった炭素質
電極棒から交互に生成する炭素蒸気は冷却再凝固されて
フラーレン含有スートとして回収され、ついで例えばベ
ンゼンのような有機溶媒を用いて抽出処理することによ
りフラーレン類として分離される。The carbon vapor alternately generated from the carbonaceous electrode rod which has become an anode by the DC arc discharge is cooled and re-solidified to be recovered as fullerene-containing soot, and then subjected to an extraction treatment using an organic solvent such as benzene. To separate as fullerenes.
【００１３】上記の製造方法に用いる本発明の製造装置
は、真空排気管とヘリウムガス導入管を備えた加熱チャ
ンバーの内部に、炭素質電極棒の対極を先端部に放電ギ
ャップを設けた状態で対向装着してなる構造において、
前記炭素質電極棒の周囲を被包するように外周面に水冷
蛇管を巻設した回収用円筒を設置し、かつ各炭素質電極
棒を極性切換用スイッチング装置を介して直流電源と接
続してなる構造を特徴としている。The manufacturing apparatus of the present invention used in the above-described manufacturing method is a heating chamber provided with a vacuum exhaust pipe and a helium gas introducing pipe, in which a discharge gap is provided at the tip of a counter electrode of a carbonaceous electrode rod. In the structure that is mounted opposite,
By installing a collecting cylinder around which a water-cooled snake tube is wound on the outer peripheral surface so as to enclose the periphery of the carbonaceous electrode rod, and connecting each carbonaceous electrode rod to a DC power supply via a polarity switching device. It is characterized by the following structure.
【００１４】図１は本発明の製造装置を示した断面図
で、１は下部に系外の真空ポンプに連通する真空排気管
２と図示しないヘリウムボンベに連結するヘリウムガス
導入管３を備えた加熱チャンバー、４および５は前記加
熱チャンバー１の内部に所定の放電ギャップを置いて対
向装着された炭素質電極棒である。該炭素質電極棒４、
５の周囲にはその外周面を被包する状態に水冷蛇管６を
巻設した銅製の回収用円筒７が設置されており、炭素質
電極棒４、５は調整用保持部材８および９の基端部から
切換スイッチング装置１０を介して直流電源１１に導線
接続している。FIG. 1 is a cross-sectional view showing a manufacturing apparatus according to the present invention. In the lower part, 1 is provided with a vacuum exhaust pipe 2 communicating with a vacuum pump outside the system and a helium gas introducing pipe 3 connected to a helium cylinder (not shown). The heating chambers 4, 4 and 5 are carbonaceous electrode rods which are oppositely mounted inside the heating chamber 1 with a predetermined discharge gap. The carbonaceous electrode rod 4,
A copper recovery cylinder 7 around which a water-cooled snake tube 6 is wound so as to enclose the outer peripheral surface thereof is provided around the periphery of the carbon fiber electrode rod 5. An end is connected to a DC power supply 11 via a switching device 10 by conducting wires.
【００１５】切換スイッチング装置１０は、一定時間毎
に＋極と−極とが連続的に切り換えられる回路機構を備
えるものであれば装置の構造は問われない。例えば、図
２のように−側入力端子１２および＋側入力端子１３と
出力端子１４、１５との間に、パソコン１６と入出力イ
ンターフェース１７に接続する電流切換用のコントロー
ル回路を組み込んだ装置を用いることができる。The structure of the switching device 10 is not limited as long as the switching device 10 has a circuit mechanism capable of continuously switching between a positive pole and a negative pole at regular intervals. For example, as shown in FIG. 2, a device in which a control circuit for switching a current connected to a personal computer 16 and an input / output interface 17 is provided between a negative input terminal 12 and a positive input terminal 13 and output terminals 14 and 15 is provided. Can be used.
【００１６】操業に際しては、切換スイッチング装置１
０を作動させた状態で直流電源１１から通電し、炭素質
電極棒４、５の間に一定時間毎に極性が切り換わる状態
で直流アーク放電を発生させる。したがって、炭素蒸気
は極性が変わるたびに陽極側の炭素質電極棒から交互に
気化する。気化した炭素蒸気は水冷された回収用円筒７
の内面で再凝固しスートとして徐々に堆積する。アーク
放電終了後、回収用円筒７からフラーレンを含むスート
を回収し、これをソックスレー抽出器を用いてベンセン
抽出したのちベンゼンを蒸発させてフラーレン類を得
る。In operation, the switching device 1
0 is activated, DC power is supplied from the DC power supply 11, and DC arc discharge is generated in a state where the polarity is switched between the carbonaceous electrode rods 4 and 5 at regular intervals. Accordingly, the carbon vapor is alternately vaporized from the anode-side carbonaceous electrode rod every time the polarity changes. The vaporized carbon vapor is recovered by water-cooled recovery cylinder 7
Resolidifies on the inner surface of the steel and gradually deposits as soot. After the completion of the arc discharge, soot containing fullerene is collected from the collecting cylinder 7 and extracted with benzene using a Soxhlet extractor, and then benzene is evaporated to obtain fullerenes.
【００１７】[0017]
【作用】本発明によれば、対極となる炭素質電極棒相互
の極性（＋−）を一定時間毎（好適時間範囲：２〜２４
０秒）に連続的に切り換えながら直流アークを発生させ
るから、アーク放電により生じる炭素蒸気は極性が変わ
る毎に陽極側の炭素質電極棒から交互に気化する。この
切り換え機構により、陰極側に切り換えた際の短時間内
に炭素質電極棒に析出する炭素塊は陽極に切り換わった
際にカーボン源となって気化し、該相互作用は操作終了
時まで継続する。このため、極性を固定する場合に起き
る陰極炭素電極棒の表面に炭素塊が析出・堆積してフラ
ーレンの生成効率を低下させる現象は解消され、長時間
に亘り安定かつ効率的にフラーレン類を製造することが
可能となる。According to the present invention, the polarity (+-) of the carbonaceous electrode rods serving as counter electrodes is changed at regular time intervals (preferable time range: 2 to 24).
(0 seconds), the DC arc is generated while continuously switching, so that the carbon vapor generated by the arc discharge is alternately vaporized from the carbonaceous electrode rod on the anode side every time the polarity changes. By this switching mechanism, the carbon lump deposited on the carbonaceous electrode rod within a short time when switching to the cathode side becomes a carbon source when it is switched to the anode and evaporates, and the interaction continues until the end of the operation. I do. For this reason, the phenomenon that carbon mass is deposited and deposited on the surface of the cathode carbon electrode rod, which occurs when the polarity is fixed, and lowers the production efficiency of fullerenes is eliminated, and fullerenes are produced stably and efficiently over a long period of time. It is possible to do.
【００１８】[0018]
【実施例】次に、本発明の実施例を比較例と対比しなが
ら具体的に説明する。Next, examples of the present invention will be specifically described in comparison with comparative examples.
【００１９】実施例１〜９、比較例１〜４ 下部に真空ポンプに連通する真空排気管２とヘリウムボ
ンベと連結するヘリウムガス導入管３を備えた加熱チャ
ンバー１の内部に、切換スイッチング装置１０を介して
直流電源１１に接続する炭素質電極棒４、５を先端部に
放電ギャップを設けてセットし、該炭素質電極棒の周囲
を被包する状態に外周面に水冷蛇管６を巻設した銅製の
回収用円筒７を設置した図１に示す製造装置を設置し
た。炭素質電極棒４、５としては、Ｘ線回折により求め
た (002)面の面間隔(d002)が３．３６８オングストロー
ム、Ｃ軸方向の結晶子の大きさ(Lc)が３５０オングスト
ロームの結晶性状を有し、電気抵抗率が１２００μΩcm
の特性を備える黒鉛材料から形成した直径８mmの円柱を
用い、電極間ギャップ１〜２mm、放電電流１１０〜１２
０Ａ、チャンバー内のヘリウム圧力９８〜１０２Torrの
条件により、極性の切り換え時間を変えて３０分間直流
アーク放電を継続した。Examples 1 to 9 and Comparative Examples 1 to 4 A switching unit 10 is provided inside a heating chamber 1 provided with a vacuum exhaust pipe 2 connected to a vacuum pump and a helium gas introduction pipe 3 connected to a helium cylinder at the lower part. The carbonaceous electrode rods 4 and 5 connected to the DC power supply 11 are set by providing a discharge gap at the tip, and the water-cooled snake tube 6 is wound around the outer peripheral surface so as to enclose the periphery of the carbonaceous electrode rod. The manufacturing apparatus shown in FIG. 1 in which the collected copper recovery cylinder 7 was installed was installed. As the carbonaceous electrode rods 4 and 5, the crystallographic properties of the (002) plane spacing (d002) determined by X-ray diffraction of 3.368 angstroms and the crystallite size (Lc) in the C-axis direction of 350 angstroms were obtained. Having an electrical resistivity of 1200 μΩcm
Using a cylinder having a diameter of 8 mm formed of a graphite material having the following characteristics, a gap between electrodes of 1 to 2 mm, and a discharge current of 110 to 12
Under a condition of 0 A and a helium pressure of 98 to 102 Torr in the chamber, the DC arc discharge was continued for 30 minutes while changing the polarity switching time.
【００２０】アーク放電終了後に回収用円筒７からフラ
ーレンを含むスートを回収し、これをソックスレー抽出
器を用いてベンセン抽出したのちベンゼンを蒸発させて
フラーレン類を得た。各例における炭素蒸発量、得られ
たスート回収率（蒸発炭素重量に対する比率）およびス
ート中に含まれるカーボンクラスター含有率を測定し、
極性切換時間その他の変動条件と対比させて表１に示し
た。After the completion of the arc discharge, soot containing fullerene was recovered from the recovery cylinder 7, which was extracted with benzene using a Soxhlet extractor, and then benzene was evaporated to obtain fullerenes. In each case, the amount of carbon evaporation, the obtained soot recovery rate (ratio to the weight of evaporated carbon) and the carbon cluster content contained in the soot were measured.
The results are shown in Table 1 in comparison with the polarity switching time and other fluctuation conditions.
【００２１】比較例５ 直流電源を交流電源に代えたほかは、実施例と同一の製
造装置および条件により交流アーク放電によりフラーレ
ン類を製造した。交流電流の周波数は、５０Hzとした。
この場合の炭素蒸発量、得られたスート回収率（蒸発炭
素重量に対する比率）およびスート中に含まれるカーボ
ンクラスター含有率を測定し、結果を表１に併載した。Comparative Example 5 Fullerenes were produced by AC arc discharge using the same production equipment and conditions as in the example except that the DC power supply was replaced with an AC power supply. The frequency of the alternating current was set to 50 Hz.
In this case, the amount of carbon evaporation, the obtained soot recovery rate (ratio to the weight of evaporated carbon) and the content of carbon clusters contained in the soot were measured, and the results are shown in Table 1.
【００２２】[0022]
【表１】 [Table 1]
【００２３】表１の結果から、炭素質電極棒の極性を２
〜２４０秒の時間範囲で切り換えながら直流アーク放電
をおこなった実施例においては、比較例に比べて相対的
に炭素蒸発量、スート回収率が高く、フラーレン生成量
が大幅に向上していることが認められた。これに対し、
従来技術と同様に極性を固定した比較例１ではスート回
収率が低く、フラーレン生成量も少ない。また、極性切
り換え時間が本発明の要件を外れる比較例２〜４では、
炭素蒸発量、フラーレン生成量が共に少なく、生成効率
が悪い結果を示した。From the results shown in Table 1, the polarity of the carbonaceous electrode
In the example in which DC arc discharge was performed while switching in the time range of up to 240 seconds, the carbon evaporation amount and soot recovery rate were relatively high and the fullerene generation amount was significantly improved as compared with the comparative example. Admitted. In contrast,
In Comparative Example 1 in which the polarity was fixed as in the prior art, the soot recovery rate was low and the amount of fullerene produced was small. In Comparative Examples 2 to 4 in which the polarity switching time deviates from the requirements of the present invention,
Both the carbon evaporation amount and the fullerene production amount were small, and the production efficiency was poor.
【００２４】[0024]
【発明の効果】以上のとおり、本発明の製造方法および
製造装置を用いれば、炭素質電極棒相互の極性を一定時
間範囲で切り換えながら連続的に直流アーク放電させる
ことにより、長時間安定して効率よくフラーレン類を製
造することが可能となる。したがって、Ｃ60、Ｃ70、Ｃ
76、Ｃ78等のフラーレン類およびこれらフラーレン類を
含むスートを工業的に製造する手段として極めて有用で
ある。As described above, according to the manufacturing method and the manufacturing apparatus of the present invention, a continuous DC arc discharge is performed while switching the polarity of the carbonaceous electrode rods within a certain time range, so that the carbon electrode rods can be stably operated for a long time. Fullerenes can be efficiently produced. Therefore, C 60 , C 70 , C
76, C 78 fullerenes, and the like, and is very useful as means for industrial production of soot containing these fullerenes.
【図１】本発明に係るフラーレンの製造生成装置を示し
た断面図である。FIG. 1 is a cross-sectional view showing a fullerene production and production apparatus according to the present invention.
【図２】極性切り換えに使用する切換スイッチング装置
を例示した回路説明図である。FIG. 2 is a circuit diagram illustrating a switching device used for polarity switching.
１ 加熱チャンバー ２ 真空排気管 ３ ヘリウムガス導入管 ４ 炭素質電極棒 ５ 炭素質電極棒 ６ 水冷蛇管 ７ 回収用円筒 ８ 調整用保持部材 ９ 調製用保持部材 10 切換スイッチング装置 11 直流電源 12 −側入力端子 13 ＋側入力端子 14 出力端子 15 出力端子 16 パソコン 17 入出力インターフェース DESCRIPTION OF SYMBOLS 1 Heating chamber 2 Vacuum exhaust pipe 3 Helium gas introduction pipe 4 Carbonaceous electrode rod 5 Carbonaceous electrode rod 6 Water-cooled snake tube 7 Recovery cylinder 8 Adjustment holding member 9 Preparation holding member 10 Switching switching device 11 DC power supply 12-side input Terminal 13 + input terminal 14 output terminal 15 output terminal 16 PC 17 I / O interface
Claims (3)
アークを発生させて高温気化させた炭素蒸気を冷却再凝
固させてフラーレン類を回収する方法において、炭素質
電極棒相互の極性を一定時間毎に連続的に切り換えなが
ら直流アーク放電させることを特徴とするフラーレン類
の製造方法。1. A method of recovering fullerenes by generating a DC arc between carbonaceous electrode rods serving as a carbon source and cooling and resolidifying carbon vapor vaporized at a high temperature to obtain fullerenes. A method for producing fullerenes, wherein DC arc discharge is performed while continuously switching every time.
時間範囲で切り換えながら直流アーク放電させる請求項
１記載のフラーレン類の製造方法。2. The method for producing fullerenes according to claim 1, wherein the direct current arc discharge is performed while switching the polarity of the carbonaceous electrode rod in a time range of 2 to 240 seconds.
た加熱チャンバーの内部に、炭素質電極棒の対極を先端
部に放電ギャップを設けた状態で対向装着してなる構造
において、前記炭素質電極棒の周囲を被包するように外
周面に水冷蛇管を巻設した回収用円筒を設置し、かつ各
炭素質電極棒を極性切換用スイッチング装置を介して直
流電源と接続してなる構造を有するフラーレン類の製造
装置。3. A structure comprising a heating chamber provided with a vacuum exhaust pipe and a helium gas introduction pipe, wherein a counter electrode of a carbonaceous electrode is opposedly mounted with a discharge gap provided at a tip end thereof. A recovery cylinder with a water-cooled snake tube wound around the outer surface so as to enclose the periphery of the electrode rod is installed, and each carbonaceous electrode rod is connected to a DC power supply via a polarity switching device. Fullerene manufacturing equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07534194A JP3337313B2 (en) | 1994-03-22 | 1994-03-22 | Method and apparatus for producing fullerenes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07534194A JP3337313B2 (en) | 1994-03-22 | 1994-03-22 | Method and apparatus for producing fullerenes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07257916A JPH07257916A (en) | 1995-10-09 |
| JP3337313B2 true JP3337313B2 (en) | 2002-10-21 |
Family
ID=13573466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP07534194A Expired - Fee Related JP3337313B2 (en) | 1994-03-22 | 1994-03-22 | Method and apparatus for producing fullerenes |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3337313B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020189632A1 (en) | 2019-03-20 | 2020-09-24 | ビタミンＣ６０バイオリサーチ株式会社 | Molded article for use in production of carbon cluster, and method for producing same |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3047062B2 (en) * | 1996-09-20 | 2000-05-29 | 大阪府 | Gas sensor |
| CN100351174C (en) * | 2005-12-12 | 2007-11-28 | 西安交通大学 | Method for producing fullerene by temperature-controlling arc furnace |
| CN102001645B (en) * | 2010-12-16 | 2012-08-29 | 中国科学院高能物理研究所 | Rotating arc synthesizing furnace for preparing fullerene nanometer material |
| JP6386784B2 (en) * | 2014-05-16 | 2018-09-05 | 三重野 哲 | Carbon cluster manufacturing equipment and manufacturing method |
-
1994
- 1994-03-22 JP JP07534194A patent/JP3337313B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020189632A1 (en) | 2019-03-20 | 2020-09-24 | ビタミンＣ６０バイオリサーチ株式会社 | Molded article for use in production of carbon cluster, and method for producing same |
| RU2771121C1 (en) * | 2019-03-20 | 2022-04-26 | Витамин С60 Биорисёч Корпорейшен | Moulded product for application in production of carbon clusters and method for production thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07257916A (en) | 1995-10-09 |
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