Electric component production method

Description of equivalent WO 2005005317 A1

0001Specification

0002A carbon nanotube, a manufacturing method for the same, and carbon nanotube Manufacture device

0003Technical field

0004[0001] The manufacture device with which the present invention is used for the manufacturing method of the suitable carbon nanotube for electric field effect Emitter material, the sheet material for electromagnetic-wave-disorder prevention, etc., and it, for example, and That It is related with the carbon nanotube manufactured by Re and others.

0005Background art

0006[0002] Carbon nanotube (CNT; Carbon Nanotubes), a quality-of-the-material defect -- few Age the so-called field of Leave and nanoelectronics drops off also until it says -- for example, electric field effect Emitter and the suitable outstanding electrical property for the very high reinforced composite of mechanical strength, etc. -- As the material which has Mechanical properties In recent years, it is observed (for example, G. S. Choi, K. H. *on and D.J. Kim). t abrication of high periormance ca rbon nanotube field emitters, "Microelectronic EngineeringJ, April, 2003, 66 The, and The 1 -- No. 4 and p.206 -- 212 and Cho YR, Lee] H, Hwang C S, et al., Characterizations of fine -- pitched carbonnanotube pixel s for field emitter arrays_lambda"Japanese Journal of Applied Physics Par tl", March, 2002, 41 The, a The 3A item, p.1532 -- 1535 references. .

0007[0003] A two-layer carbon nanotube (DWCNT; Double_Walled Carbon Nan otubes) especially, Monolayer carbon nanotube (SWCNT;) The electrical property and mechanical property superior to Single--Walled Carbon Na notubes or the multiwalled carbon nanotube (MWCNT; Multi -- Walled Ca rbon Nanotubes) of three or more layers It becomes the material which it had. Since a possibility of obtaining is carried out, it is observed especially in recent years.

0008[0004] It is DWCNT if the case where a carbon nanotube is applied to electric field effect Emitter is considered as an example, It is possible for the endurance to consider it as a high thing on a par with MWCNT of three or more layers so that it is possible to make threshold voltage of the electronic discharge by the electric field effect in Emitter into the following low voltages equivalent to SWC NT. [0005] carrying out -- power While -- DWCNT -- in order [ for example, ] to utilize for the above electric field effect Emitter It is required to reduction-ize further the defective rate of incidence as the quality of the material of DWCNT. This When DWCNT has a quality-of-the-material defect, it is electric Lack of as electric field effect Emitter. It is because it becomes a serious factor which produces Recess. The quality-of-the-material defect of DWCNT is endurance. It becomes a factor of a fall. Namely, oxygen of the high temperature [ portion / quality of the material / defective ] for example, in the air If it touches, these artificers are various experiments about concentrating on the portion and degradation arising. Confirmation is carried out.

0009[0006] Since what is called mass-production art is not established, DWCNT is long production time. Extensive [ in a short time ] in the thing of the quality quality of the material [ be / no defect ], since it applies and only a small quantity can be generated Producing is in the difficult present condition.

0010[0007] Power in which it was discovered that DWCNT is generated by an arc discharge method at the beginning The heat treatment method of heat-treating and generating in recent years using fullerene C and SWCNT, Touch

001160

0012CVD using intermediation -- law (Chemical Vapor Deposition: chemical vapor phase epitaxy) -- or -- It is possible to generate DWCNT by the arc discharge method in the atmosphere containing hydrogen. it is -- things are proposed -- Les and To. carrying out -- power While -- generating applying a long time can only do a little D WCNT, but each of those manufacturing methods can realize mass-production Something technical Helmet and The were proposed, were Les(ed), and there were. [ no ]

0013[0008] in which it is difficult to realize the throughput which can respond to mass-production in heat treatment method. It is difficult to mass-produce DWCNT with high purity in a CVD method or an arc discharge method. There is a problem of being. power is also like [ according to / carry out and / these artificers' various experiments ] hydrogen gas -- anti- -- The former using reactive gas DWCNT generated in the CVD method or the arc discharge method -- the -- There is a problem that the probability that therefore a defect will occur in response to damage in reactant gas is high. To carry out or and use reactant gas like hydrogen gas in such a CVD method and an arc discharge method since DWCNT is ungenerable in practice if it kicks -- it is reduction about a defective rate of incidence ---izing -- To -- things were very difficult.

0014[0009] Incidentally, in order to generate DWCNT alternatively by the conventional arc discharge method, it is hydrogen. It was advocated that existence of reactant gas like gas is indispensable (Utchins on, J. L. et al, Carbon2001). Atmosphere of pure inactive gas like gaseous helium In the inside of The atmosphere, There was also a report that DWCNT was not generated (Saito, Y et al, "The Journal of Physical Chemistry B", 2003, 107 The, The No. 4, and p. 93 11 934). According to such a report, existence of hydrogen gas by the conventional arc discharge method I will hear that DWCNT cannot be generated, if it kicks.

0015[0010] It was very difficult to have made a defective rate of incidence reduction-ize in the conventional manufacturing method in this way. the manufacturing method which can respond to mass-production substantially should be proposed -- and -- It was.

0016The indication of an invention

0017[0011] It was made in view of power or Problems, and the present invention is the object, It is high Sour about DWCNT. Manufacture of the carbon nanotube which makes it possible to mass-produce by one put and a low defective rate of incidence It is in providing the carbon nanotube manufactured by the manufacture device and them which are used for a method and it.

0018[0012] A manufacturing method of the carbon nanotube by the present invention, A catalyst is arranged to the inside of the electrode of The 1 which has a hollow part, and the tip is the hollow circles of the electrode of The 1 about the electrode of The 2. It arranges so that it may be located, between the electrode of The 1, and the electrodes of The 2 -- arc discharge -- generating -- It is a thing which makes a carbon nanotube generate with a catalyst as the starting point by To and this arc discharge. It is.

0019[0013] A manufacture device of the carbon nanotube by the present invention, It has a hollow part and the electrode of The 1 in which a catalyst is arranged at an inside, and a tip are located in the hollow circles of the electrode of The 1. Vacuum room which has an electrode of The 2 by which way arrangement was carried out, Gas which introduces inactive gas into the vacuum interior of a room Predetermined voltage is impressed between an introduction means, and the electrode of The 1 and the electrode of The 2, and arc discharge is generated. It has a voltage applying means to carry out.

0020[0014] the carbon nanotube of The 1 by the present invention -- length -- the power 1 Bonnano tube of more than 1 mu m, below lmm, and The 2 -- length -- the carbon nanotube of more than lmm, below lcm, and The 3 -- long -- To are more than lcm and below lm. The length of the carbon nanotube of The 4 is more than lm and below 1 km. all break off -- or -- extension -- Les and one continuous filar car It is a Bonnano tube and can manufacture by the manufacture device or method of the present invention. To. [0015] With a manufacturing method or a manufacture device of a carbon nanotube by the present invention, it has a hollow part arc discharge occurs the 1st electrode of To, the electrode of The 2, and in between -- a carbon nanotube is generation Power carried out -- heat which arose by this arc discharge, The temperature of the catalyst moderately arranged near the inside of the electrode of *Ri and The 1 (i.e., the electrode of The 1) is maintained at the hollow circles of the electrode of The 1 by temperature suitable for generation of a carbon nanotube. Thereby, arc discharge is continued. One continued between To without a carbon nanotube breaking off with a catalyst as the starting point It continues being generated filar.

0021[0016] Moreover, with the manufacturing method or manufacture device by the present invention, even if it is among the atmosphere which contains neither hydrogen nor oxygen gas by considering it as the atmosphere of only inactive gas, for example, a helium, nitrogen, or argon gas, a carbon nanotube is generated by the high throughput. Inside of the atmosphere which contains neither hydrogen nor oxygen gas in particular in the case of the carbon nanotube of the two-layer structure It sets and is generated by a low defective rate of incidence.

0022Brief explanation of the drawings

0023[0017] [Drawing 1] It is a figure showing the outline composition of the manufacture device of DWCNT concerning the 1 embodiment of the present invention, and is Ah. To.

0024[figure 2] It is a figure which expresses typically the state where filar DWCNT is generated.

0025[figure 3] It is a figure showing an example of the recovery subsystem of DWCNT.

0026[figure 4] It is a figure showing other examples of the recovery subsystem of DWCNT.

0027[figure 5] It is a graph showing the result of TGA (TG analysis) refining before of filar DWCNT manufactured by the example, and after refining.

0028[figure 6] It is a graph showing the rate of change of TG as a result of TGA (TG analysis) refining before of filar DWCNT manufactured by the example, and after refining.

0029[figure 7] From the surface of the electrode of The 1, it is an enlargement by TEM of DWCNT generated filar, and is Ah. To.

0030[figure 8A] It is an enlargement by SEM of DWCNT generated from the surface of the electrode of The 1.

0031[figure 8B] a figure -- it is a photograph of DWCNT which made magnifying power higher than 8A.

0032[figure 9A] It is TEM after carrying out acetone treatment of the filar DWCNT manufactured by the example. It is the enlargement which carried out intermediary photography. [figure 9B] a figure -- it is an enlargement of one DWCNT in 9A.

0033[figure 9C] a figure -- it is a section enlargement of the bunch of DWCNT of 9A.

0034The best form for inventing

0035[0018] Hereinafter, describe an embodiment of the invention in detail with reference to drawings.

0036[0019] a figure -- 1 is a thing showing the outline composition of the device used for manufacture of the carbon nanotube concerning the 1 embodiment of the present invention, for example, the carbon nanotube of the two-layer structure, (DWCNT) -- is there.

0037[0020] The manufacture device of the carbon nanotube (DWCNT) of this two-layer structure is provided with electrode 2 of The 1 which has hollow part 2a in arc discharge, and electrode 3 of cylindrical The 2 into vacuum room (Chang Ba) 1. The Electrode of 1 2 is a hollow part here. 2a is a ball. (bowl) A state It is making. The hollow part. 2a is used as the upper surface and it is installed. Electrode 3 of The 2 is the point. It is perpendicularly arranged so that end 3a may be located in hollow part 2a of electrode 2 of The 1. the power supply (direct-current power supply) for impressing predetermined voltage to the exterior of vacuum room 1 between the 1st electrode 2 and electrode 3 of The 2 -- 4 is installed. the exhaust air pump which does not illustrate this vacuum room 1 -- decompression it being carried out and leading gas inlet 5 -- inactive gas, for example, gaseous helium, and nitrogen Guth -- being certain -- it is -- argon gas is introduced.

0038[0021] It is decompressed after filling up with the inactive gas which consists only of heliums (helium) first within vacuum chamber 1, when manufacturing DWCNT in this embodiment, and it is the decompression. Intermediary To have [ as ] to which arc discharge is performed in atmosphere. That is, in this embodiment, it becomes Not included and atmosphere about hydrogen and oxygen, and they are Les and To.

0039[0022] Kaso [ in / electrode 2 of The 1 is formed with carbon (C), and / direct-current arc discharge ] It is used as Do. This The Electrode of 1 In 2, it is that hollow part. Catalyst used as a starting point of generation of DCNT on the surface (wall surface) of 2a 6 distributes, and it is intermingled or supported. The catalyst. It is The at a wall surface by which 6 was distributed. Two electrodes Three tip parts 3a is surrounded. Although the metal particulates which consist of metallic sulfide like FeS (iron sulfide) as catalyst 6, for example are used, this catalyst 6 may be made intermingled in electrode 3 of The 2.

0040[0023] By this embodiment, electrode 2 of The 1 surrounds tip part 3a of electrode 3 of The 2 in this way. The temperature of the surface by the heat which arose by the arc discharge can be maintained now from Les and To to the temperature which can generate DWCNT, and they are Les and To.

0041[0024] In addition, electrode 2 of The 1 should just be the shape which can make filled with the heat which arose by arc discharge the fixed space area near the catalyst which has hollow sections and is arranged in an electrode surface. Therefore, closed music to which the shape not only of ball state but a corn (cone) has an opening only in one side It may be a field-like thing. In addition, if only the whole surface is made into an opening, it is applicable also by the shape of a rectangular parallelepiped (box-like), and the shape (dugout) of a cylinder.

0042[0025] On the other hand, electrode 3 of The 2 is also formed with carbon (C), and can be set to direct-current arc discharge. It is used as a To anode and used as a source of supply of the material (carbon) for generating DWCNT. The outside of electrode 3 of this The 2 is cylindrical, for example, or the shape of a square pillar, etc. are possible for it. It is.

0043[0026] Perform direct-current arc discharge between electrode 2 of The 1, and the 2nd electrode 3 as buffer gas in the manufacture device of this embodiment for example, in vacuum room 1 maintained at the atmosphere which does not contain hydrogen and oxygen using helium (helium) gas. By the direct-current arc discharge, Direct-current A - KPlasma 7 occurs, and the electric energy of direct-current arc discharge is thermal energy. It changes and the surface of electrode 2 of The 1 is supplied as a material for the carbon of electrode 3 of The 2 to generate DWCNT.

0044[0027] the surface of electrode 2 of The 1 -- a figure -- it was typically shown in 2 -- as -- direct-current arc discharge -- For The supplied carbon is set to DWCNT8 [ filar as a starting point ] in catalyst 6. Direct-current Oh my by which space inside electrode 2 of The 1 (hollow part 2a) will be covered with DW CNT8, for example, and arc discharge is prevented from supply or carbonaceous sufficient direct-current arc discharge while The electric discharge is continued If it does not grind, generation of DWCNT8 continues stably, without breaking off. therefore, way a piece -- or -- extension -- Les and continuous filar one DWCNT8 are obtained easily.

0045[0028] Les [ have ] which limits especially the length of DWCNT8 manufactured by doing in this way, More than lmm, the following [ lcm ], and length are obtained for more than 1 mu m, the following [ lmm ], and length, and more than lm and the following [ lkm ] are obtained [ But, for example length, ] for more than lcm, the following [ lm ], or length. Length It is also possible to cut beyond power im and the following [ lkm ] and to obtain the thing of shorter length.

0046[0029] DWCNT8 more than 1 mu m and below lmm has useful length as a paint substrate used for FED (Field Emission Display; field-electron-emission display) etc., for example. [0030] DWCNT8 more than lmm and below lcm is [ length ] an electromagnetic-wave-absorption agent or Nano de, for example. It is useful as a substrate of vice.

0047[0031] A nanowire ring is possible for DWCNT8 more than lcm and below lm for length, for example.

0048[0032] the wire and crane with which, as for DWCNT8 more than lm and below lkm, length supports a bridge, for example Consider it as construction and engineering-works materials including rope material, structure material, machinery material, an equipment component, etc. The -- extensive application is expectable. This kind of structure is supported conventionally, or it is used for some devices. The diameter became large and the To wire has also enlarged the whole structure or the whole device. It was. On the other hand, since rigidity is high, DWCNT8 of the present invention is the smallness of a structure or a device. It is advantageous to a type weight saving. It is if it is in DWCNT8 which has conductivity, Electric power is transmitted. It is nano Chu with a small path by bundling a nanotube, if it uses for the cable to carry out. While being able to transmit large electric power also by Bewire, lightweight [ of DWCNT8 ] -- and tough To -- therefore, thing for which the interval of the steel tower which supports a power transmission cable is also made into an interval with a long lkm grade It can do.

0049[0033] This corresponding to the mass production of DWCNT since filar DWCNT8 can be continuously generated stably by this embodiment in this way, without breaking off with catalyst 6 as the starting point It becomes possible. It continues by controlling the continuation time of direct-current arc discharge. He is further merit also at lmm, lcm, or lm about the length of filar DWCNT8 generated. Even if it is To lkm and more than it, it is possible to use the desired length.

0050[0034] It is possible to generate filar DWCNT8 by this embodiment moreover in the atmosphere which does not contain hydrogen and oxygen gas. Hydrogen gas with high reactivity to DWCNT8 In the rate of incidence of the defect resulting from existence of reactant gas like oxygen gas, the former is common. Compared with the case of the manufacturing method by CVD method, an arc discharge method, etc., it decreases by leaps and bounds, Trust DWCNT8 with Dependability and high endurance can be manufactured.

0051[0035] [Modification 1]

0052Drawing 3 expresses modification 1 of the present invention. the reticulate member (mesh) as a recovery subsystem which collects DWCNT8 by which the manufacture device of this modification is generated -- removing having had 9 It has the same composition as the manufacture device of the above-mentioned embodiment. Therefore, the same style The same numerals are given to Component and the explanation is omitted. [0036] Gas pressure Gl which this reticulate member 9 produces by the convection of atmosphere gas, G2 is made to generate DWCN T8 in the shape of an approximately straight line along the surface of reticulate member 9, without becoming entangled mutually, and it is recovery. It is for making it easy. if it is the material which does not change even if put to the high temperature atmosphere about 1000"C as a material of reticulate member 9, especially limitation will drop off -- for example tungsten and iron Or gold, such as an alloy containing at least one of sorts of these, ceramics, or iron Cerami who compounded Genus -- TASS is mentioned. the fineness of the net of reticulate member 9, DWCNT8, and Tangle It is preferred that it is the fineness which is easy to see. that is, atmosphere gas is reticulated so that it may mention below while pressing DWCNT8 to reticulate member 9 by passing member 9 -- DWCNT8 passing the meshes of a net of reticulate member 9 -- Les -- being set up like -- Les and To -- good -- better -- Les, For example, the diameter of and a mesh can be chosen for example, from 100 mu m as the range of 5 cm.

0053[0037] As for reticulate member 9, it is preferred to be estranged and allocated from electrode 2 of The 1. Mesh texture Distance of member 9 and the opening of electrode 2 of The 1, it is the distance to which electric discharge by an electric field does not arise between reticulate member 9 and the opening of electrode 2 of The 1, and gas pressure Gl and G2 act on reticulate member 9 -- good -- better -- they are more than Tooth, for example, lcm, and 50 cm or less. Reticulate member 9 is good also as movement being possible suitably in connection with the increase in the quantity of DW CNT8. in addition -- certainly carrying out reticulate member 9 a figure -- as shown in 3, for example, the necessity of being installed horizontally drops off, it becomes section V character-like -- as -- Installation may be carried out.

0054[0038] At this modification, it is Ah between electrode 2 of The 1, and electrode 3 of The 2 like the above-mentioned embodiment. While generating The electric discharge, if DWCNT8 is made to generate continuously -- a figure -- the arrow of 3 showed Gas pressure Gl and G2 arise by the convection of atmosphere gas through reticulate member 9 to obtain. DWCNT8 is pressed on the surface of reticulate member 9 by gas pressure G 1. The power pulled with gas pressure G2 in the direction which separates from electrode 3 of The 2 to DW CNT8 works. DWCNT8 [ therefore, ] it is extended in the shape of an approximately straight line along the surface of reticulate member 9 -- being involved with DWCNT8 of self or others -- Synthesis It obtains and things are lost. Therefore, as the above-mentioned embodiment explained, DWCNT8 of the length of lcm thru/or lm is generated easily and certainly.

0055[0039] It is DWCNT8 which grew along with reticulate member 9 in order to have maintained the abbreviated straight line state and to have collected DWCNT8 generated in the state where it extended such in the shape of an approximately straight line to the outside of electrode 2 of The 1. It is more desirable if it is made to collect. vacuum room 1, capacity, a size of electrode 2 of The 1, etc. being restrained -- continuation of generation of DWCNT8 -- on the way -- can generating of the situation where DWCNT8 in which a possibility that it may be come out and barred drops off becomes entangled with DWCNT8 of self and others be prevented? , -- it is .

0056[0040] In this modification, since it had reticulate member 9 as a recovery subsystem, D WCNT8 [ very long ] is easily and certainly generable, and recovery of DWC NT8 becomes easy by metal mesh 9, and it is advantageous to mass production. Capacity of vacuum room 1 or electrode 2 of The 1 It is lost that generation continuation time is restrained with a size etc., and it is filar DWCNT8. It becomes easy to carry out continuously in time, without suspending generation on the way.

0057[0041] Les [ have ] which will be restricted in addition to Well reticulate member 9 if the recovery subsystem of this modification has a crevice through which atmosphere gas can pass, For example, the thing of the shape of a stick, the shape of a crosspiece, or the shape of a lattice may be used.

0058[0042] [Modification 2]

0059Drawing 4 expresses other examples of the recovery subsystem. Roller-type recovery subsystem collected while making adsorb and twisting around the surface of The mouth which rotates DWCNT8 in this modification - La 9A It uses. Thereby, even if it is lm thru/or lkm, and DWCNT8 [ very long ], it is a time easily. Yield can be carried out and also it is advantageous to mass production.

0060[0043] more than lcm and below 50 cm make distance of roller 9A and the opening of electrode 2 of The 1 be the same as that of modification 1, for example -- good -- better -- Les, In connection with the increase in the quantity of rolled DWCNT8, it is good also as movement being possible suitably. The guide member or guide roller which is not illustrated between roller 9A and electrode 2 of The 1 may be formed. roller 9A -- a figure -- it is not restricted to the example shown in 4, but three or more may be provided. Reticulate member 9 and roller 9A are combined, and it is about reticulate member 9. It is considered as a guide member and may be made to lead DWCNT8 to the direction of roller 9A.

0061[0044] [Example]

0062Next, it is above. The manufacture device of the carbon nanotube of two-layer structure and it are used. It was The concrete example of the manufacturing method of the carbon nanotube of two-layer structure is described.

0063[0045] Filar DWCNT8 is generated considering inside electrode 2 of The 1, and catalyst 6 of the surface facing the 2nd electrode 3 as a starting point, as the above-mentioned embodiment explained. [0046] At this example, it is as the 1st electrode 2, Figure Vo who tolerates electrode 3 of The 2 as shown in 1 At the shape of Ur, they are NiS (sulfuration Nick window), CoS (sulfuration cobalt), and FeS (iron sulfide) as catalyst 6 1 : 1 : It contained by the ratio of 1 and used the thing containing very-small-quantity (1 % of the weight) Sn (tin). The 2 They are nickel (nickel) with a section size ofX[ 15 ] 15 mm and a length of 250 mm as electrode 3, Co (cobalt), and FeS (iron sulfide) 12 : 3 : The carbon stick included 4.5% of the weight by the ratio of 5 was used. Electricity The current in the case of the direct-current arc discharge by source 6 maintained 180A.

0064[0047] Arrange metal mesh 9 in the position which the opening power of electrode 2 of The 1 also left 30 cm perpendicularly as a recovery subsystem, and collect filar DWCNT8 generated from electrode 2 of The 1. It was. as buffer gas -- purity 99. 9999% of helium (helium) -- business -- Please and DWCNT8 The atmosphere in vacuum room 1 at the time of generating was kept at 80 [kPa].

0065[0048] By such manufacturing conditions, DWCNT8 was actually generated. And it refined to DWCN T8 generated.

0066[0049] Specifically, it was generated. It is at room temperature about DWCNT8. It is Across in 24 hours. 3N nitrogen oxide solution It agitates in inside. then -- applying to a centrifuge and an ultrasonic cleaner two or more times -- un--- . A pure thing was removed. And Across dryness was made to carry out in 10 hours by 60 degreeC.

0067[0050] In order to observe DWCNT8 manufactured by doing in this way with a TEM device (HRTEM, HF2000, product made from Hitachi), acetone treatment and supersonic treatment were performed. To and TEM Observation and photography were performed. TGA device (Perkin-Elmer, Phylisl)

0068TGA (temperature weight analysis) was performed using TGA. It was considered as 5 degrees of measurement run pin great Is C/min (minute) of the TGA.

0069[0051] Next, explain DWCNT8 produced by performing it above.

0070[0052] a figure -- 7 is an enlargement by TEM of DWCNT8 generated filar from the surface of electrode 2 of The 1. This photograph is an object for observation of vacuum room 1 in 10 minutes, after starting direct-current arc discharge. The state where it is observed from a window is photoed. smoke with filar DWCNT8 [ white ] -- like -- the power which is in sight -- this is based on powerful UV line (outside of purple) which arises by high temperature or direct-current arc discharge It is assumed that it originates in Brilliance.

0071[0053] After starting direct-current arc discharge, in several minutes, DWCNT8 of the length about number cm is the shape of a bunch. It becomes and it is begun as a starting point to generate catalyst 6 of the surface of electrode 2 of The 1. These filar DW(s) Many of CNT8 grow and go to being rapid and a length of 30 or more cm. and -- soon -- the -- It comes to be filled to the space between an intermediary with much quantity, and electrode 2 of The 1 and mesh 9 for recovery. Article When an affair is prepared, after starting direct-current arc discharge, it is 300 in 20 minutes. -- DW CNTof 500 mg8 were collected. This is the conventional catalyst. To the manufacturing method of DWCNT by a CVD method According to the manufacturing method of this example, it progresses rapidly compared with the case where DWCNT of an intermediary equivalent amount is manufactured. It means that DWCNT8 can be manufactured at Quick lever and speed-like, and they are Les and To.

0072[0054] a figure -- enlargement by SEM of DWCNT8 by which 8A was generated from the surface of electrode 2 of The 1 It is. The diameter of one filar duty of DWCNT8 shown in this enlargement serves as 1 1 100 z m. Manufacturing method in which DWCNT8 by this example is common as for the former Compared with DWCNT8 obtained, mechanical strength is high by leaps and bounds. Drawing 8B -- a figure -- it is an enlargement by S EM which made magnifying power higher than 8A further, and photoed DWCNT8 by this example. According to this photograph, it is a diameter of many numbers nm to 10 nm of numbers. It turns out that filar DWCNT8 and its bunch are coarsely located in a line.

0073[0055] a figure -- 9A is the enlargement taken by TEM, after carrying out acetone treatment of the filar DWCNT8 manufactured by this example. At an example of this specimen, metal particles etc. are Conspicuous. Strength Also after amorphous carbon treats with ultrasonic waves, only a small quantity exists extremely. It is absent. In the case of DWCNT8 from which this is obtained by the conventional general arc discharge method It is very contrastive.

0074[0056] a figure -- one of filar DWCNT8 by which 9B was manufactured by this example -- TEM It is the enlargement which carried out intermediary photography. a figure -- bunch by which 9C was manufactured by this example Ivy -- it is the enlargement which photoed the section of filar DWCNT8 by TEM. This expansion copy The former with DWCNT8 shown truly and one common diameter CVD method and arc Release The 2 [ same ] as DWCNT8 manufactured by the Electricity method etc. They are seven nm. This Expansion It is shown in close-up truth. Inside and outside in DWCNT8 An interval between two-layer is 0.36--0.42 nm. Graphite carbon. It is a typical value in MWCNT. About 0.34 nm It compares and is a little large intermediary To have.

0075[0057] yield of filar DWCNT8 manufactured to the carbonaceous amount of raw materials is as it is 50% or more. It is presumed. [0058] Drawing 5 and a figure -- refining before and the energy of filar DWCNT8 by which 6 was manufactured by this example It is a characteristic figure showing the result of TGA (TG analysis) after make. these figure 5 and a figure -- in 6, a expresses oxidation treatment before and b expresses the oxidation treatment back, respectively -- Les and To.

0076[0059] Filar DWCNT8 manufactured by this example, It is an unrefined thing and is 60 % of the weight. Even if the metal catalyst ingredient is included, it is near destruction-by-fire start temperature power S600-degreeC, this example if compared with 300 degreeC which is a classic example of the destruction-by-fire start temperature of DWCNT manufactured by the conventional general arc discharge method using used electrode 3 of The 2 -- very -- high Les, destruction-by-fire start temperature, and Being -- things were understood. this power -- being contained in DWCNT8 manufactured by this example at the time of un-refining -- Les and a Metal catalyst ingredient are falls about the destruction-by-fire start temperature of this DWCNT8 It became clear that it is not what is carried out.

0077[0060] It is the simple oxidation treatment in room temperature to filar DWCNT8 manufactured by this example. After giving, the metal catalyst ingredient fell to 6.8% of the weight. gold in which this was contained It can be contained in DWCNT8 by it and it comes out to such an extent that most Classification catalyst ingredients are easily removable. Are and were not taken into DWCNT8 so firmly that it is unremovable. It has suggested.

0078[0061] The peak of the rate of a weight change of a TGA analysis result has become near 720 degreeC also after oxidation treatment filar DWCNT8 manufactured by this example, and it is about oxidation resistance. It turned out that it hardly changes also after oxidation treatment.

0079[0062] here, these artificers change and catalyst 6 into the thing for generating SWCNT using the same manufacture device as what manufactured above DWCNT8 -- experiment which generates SWCNT It carried out. As a result, it was presumed to be that there was seemingly an operation which carries out self-recovery of it even if SW CNT generated produces a defect in the manufacturing method using electrode 2 of above The 1. what is generated in atmosphere without reactant gas like hydrogen gas or oxygen gas -- Lack of of SWCNT generated by using electrode 2 of The 1 which calls and has hollow part 2a It was checked that Incidence rate can be held down to a low thing by leaps and bounds.

0080[0063] The conventional general cylindrical Casso - Do is conversely used as a comparative example, without using electrode 2 of The 1, Mostly of CNT obtained when the experiment of having set up conditions, such as other catalysts, like this example, having performed direct-current arc discharge, and generating DWCNT8 was tried When is SWCNT -- small deer generation of DWCNT8 was not carried out very much.

0081[0064] Electrode 2 of The 1 which was used in this example from the thing of these, hydrogen gas -- oxygen gas -- Performing-in atmosphere without Something reactant gas-direct-current arc discharge power Filar DWCNT8 In order to generate continuously stably, it is presumed that it is what contributes greatly.

0082[0065] although the embodiment and the example were given and the present invention was explained above, the present invention is limited to the above-mentioned embodiment and an example -- it can change variously. For example, on When manufacturing DWCNT8 of two-layer structure in an account embodiment and an example, they are Helmet and The. Although explained, The manufacturing method or manufacture device of a carbon nanotube by the present invention is manufacture of the carbon nanotube of not only two-layer structure but monolayer structure or the structure of three or more layers, etc. It is applicable.

0083[0066] Mention the composition of a manufacture device concretely in the above-mentioned embodiment and an example, and it is an opinion. Although revealed, it has all the components explained in the above-mentioned embodiments, such as a recovery subsystem. Necessity is further extrinsically dropped off and provided with other components, such as a required window for maintenance. Ah is good.

0084[0067] According to the manufacturing method or manufacture device of a carbon nanotube of this embodiment or this example as mentioned above About defective rates of incidence, such as DWCNT, it is a conventional manufacturing method or Made. It can reduction-ize by leaps and bounds than what is manufactured by Construction equipment, and is A low about it. It can manufacture succeeding a constant target.

0085[0068] It is a catalyst to the inside of the electrode of The 1 which has a hollow part according to the manufacturing method of the carbon nanotube of the present invention, or the manufacture device of the power 1 Bonnano tube of the present invention as explained above. While arranging, About the electrode of The 2, the tip is the hollow circles of the electrode of above-mentioned The 1, or That. It arranges so that it may be located close, and it is arc discharge between the electrode of above-mentioned The 1, and the electrode of above-mentioned The 2. Since it was made to make it generate, The heat which arose by arc discharge is in the hollow part of the electrode of The 1. To the temperature to which the temperature of the surface where Indignation and a catalyst are arranged was suitable for generation of the carbon nanotube It is maintained. Therefore, a carbon nanotube is a bag while continuing direct-current arc discharge. One continued without breaking off with the catalyst of the A state electrode as the starting point and which continues being generated filar. This becomes possible to mass-produce a carbon nanotube stably.

0086[0069] If it is made to carry out in the state where hydrogen gas and oxygen gas are not included in inactive gas atmosphere, such as a helium, especially, it will be the conventional method of manufacture about the defective rate of incidence of a carbon nanotube. It can reduction-ize by leaps and bounds rather than what is manufactured by the method or a manufacture device. moreover -- according to the carbon nanotube of the present invention -- the length -- 1 or more mm -- more -- Desire -- better As for To, still more desirably, it breaks off more than lm or more than lcm does not have extension. Since it was made like For example, the use which needs a fibrous long carbon nanotube and a request It is [ nano / carbon ] to various uses etc. as which cutting and using for length is requested. It becomes possible to utilize a tube.