WO2004096705A1 - ナノカーボン製造装置およびナノカーボンの製造方法 - Google Patents
ナノカーボン製造装置およびナノカーボンの製造方法 Download PDFInfo
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- WO2004096705A1 WO2004096705A1 PCT/JP2004/006048 JP2004006048W WO2004096705A1 WO 2004096705 A1 WO2004096705 A1 WO 2004096705A1 JP 2004006048 W JP2004006048 W JP 2004006048W WO 2004096705 A1 WO2004096705 A1 WO 2004096705A1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Definitions
- the present invention relates to a nanocarbon production apparatus and a nanocarbon production method.
- Nanocarbon refers to a carbon material having a nanoscale microstructure, such as carbon nanotubes and carbon nanohorns.
- the carbon nanohorn has a tubular structure in which one end of a carbon nanotube in which the graphite sheet is rounded into a cylindrical shape has a conical shape.
- the application to the field is expected.
- the carbon nanohorns are usually assembled by van der Waalska acting between the cones, with the cones protruding like horns from the surface around the tube.
- Non-Patent Document 1 describes rotating a columnar graphite target along an axis and irradiating a side surface thereof with a laser beam vertically.
- Non-Patent Document 1 S. Iijima, 6 others, ChemiCalPhyssicsLetterrs, ELSEVIER, 1991, No. 3909, p. 165-170
- the irradiation position of the laser light sometimes shifted.
- the surface of the graphe target once irradiated with the laser light is roughened, so if the roughened part is irradiated again with the laser light, the light irradiation area on the side surface of the graphe target changes.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a technique for stably mass-producing carbon nanohorn aggregates. Another object of the present invention is to provide a technique for stably mass-producing nanocarbon.
- a target holding means for holding a sheet-like or rod-like graph-eye target, a light source for irradiating light to the surface of the graph-eye target, and the target held by the target holding means
- a moving means for moving one of the graph target and the light source relative to the other, and moving the light irradiation position on the surface of the graph target; and irradiating the graph eye with the light.
- a recovery device for recovering carbon vapor evaporated from the target to obtain nanocarbon is provided, and a nanocarbon production apparatus is provided.
- the nanocarbon production apparatus includes target holding means for holding a sheet-like or rod-like graphite target. Also, there is a moving means for moving one of the graph eye target and the light source relative to the other. Therefore, it is possible to irradiate the surface of the graph target with light while moving these relative positions.
- the term “power density” hereinafter refers to the power density of light actually illuminating the surface of the graph target 1, that is, the power density at the light-irradiated portion of the surface of the graph eye target.
- the surface of the graphic target can be a flat surface. This makes it possible to more reliably suppress a change in the power density due to a shift in the light irradiation position.
- a step of obtaining nanocarbon and a method for producing nanocarbon.
- the method for producing nanocarbon according to the present invention since the surface of a sheet-like or rod-like graphite target is irradiated with light, it is possible to suppress deviation in power density due to displacement of a light-irradiated portion. Therefore, the quality of nanocarbon can be stabilized. In addition, the yield of nanocarbon can be improved. Therefore, it is possible to stably mass-produce nanocarbon.
- the moving unit may be configured to move the light irradiation position while making the light irradiation angle at the irradiation position on the surface of the graphite target substantially constant. Good.
- the method for producing nanocarbon of the present invention may include a step of irradiating the light such that an irradiation angle of the light on the surface of the graphite target is substantially constant.
- the moving means may be configured to move the light irradiation position while erasing the graphite target at the position irradiated with the light.
- the light irradiation position may be moved on the surface of the graphite target while erasing the graphite target at the position irradiated with the light. Good.
- the light irradiation is performed while moving the graph eye target to the light irradiation position, and the graph eye target disappears from the light-irradiated portion.
- the disappearance of the graphite target does not mean that only the region at a predetermined depth from the surface of the graph target is evaporated and removed, but the irradiated region is completely removed in the depth direction. Re-irradiation of light is unnecessary.
- the supply and consumption of the graph-eye target can be linked to efficiently use the graph-eye target.
- the graphite target can be eliminated without re-irradiating the once irradiated area on the graphite target surface, it is possible to use up the graphite target by one light irradiation. it can. Once the light is illuminated, the surface has four convexities, so the power density tends to fluctuate when irradiating the light again.However, in this way, the power of the light illuminating the graphe target surface Variation in density can be suppressed more reliably. For this reason, the quality of nanocarbon can be stabilized. Further, the yield of nanocarbon can be further improved.
- the nanocarbon producing apparatus further includes a control unit that controls an operation of the moving unit or the light source such that a power density of the light applied to a surface of the graphite target is substantially constant. Is also good. In this way, the power density of the light illuminating the surface of the graph target is improved. Control can be performed more reliably. For this reason, it is possible to adopt a configuration capable of producing a stable quality of nano force in high yield.
- the moving means may be configured to translate the graphite target held by the target holding means.
- the graph target By adopting a configuration in which the graph target is translated, there is no need to provide a rotation mechanism for rotating the graph target, and the device configuration can be simplified.
- the rod-shaped or sheet-shaped graphite target in translation it becomes easy to suppress the fluctuation of the power density of the light applied to the surface of the graphite target. For this reason, the quality of nanocarbon can be further stabilized. In addition, the yield of nanocarbon can be improved.
- the endless belt-shaped graph eye target is provided between a pair of rollers, and the moving means drives the graph eye target by rotating the rollers. You can. By doing so, the graph eye target can be efficiently transmitted to the light irradiation position. In addition, it becomes easy to control the power density of the light irradiated at this time.
- the apparatus can be downsized by arranging an endless belt-shaped graph-eye target between a pair of rollers. In the present invention, the number of rollers included in the “pair of rollers” may be two, or may be three or more.
- the graph eye target is a sheet-like graph eye target wound on a rotating body, and the moving means drives the rotating body to rotate, and simultaneously moves the rotating body from the rotating body.
- the released graphite target may be configured to be pushed in the direction of the light irradiation position.
- the size of the apparatus can be further reduced.
- the part that is released from the rotating body and unwound and spreads is pushed out in the direction of the light irradiation position, thereby forming a sheet-shaped target. Can be continuously supplied to the light irradiation position.
- the amount of graphite targets used in one production can be increased, a configuration suitable for mass production can be obtained.
- the nanocarbon may be a carbon nanohorn aggregate.
- the step of collecting nanocarbon may include a step of collecting a carbon nanohorn aggregate.
- the force constituting the carbon nanohorn aggregate can be a single-layer carbon nanohorn or a multi-layer carbon nanohorn.
- the step of light irradiation may include a step of irradiating the lasers one light.
- the wavelength and direction of the light can be kept constant, so that the conditions for irradiating the surface of the graph-ite target with light can be controlled accurately. Therefore, it is possible to selectively produce desired nanocarbon.
- nanocarbon can be stably mass-produced.
- carbon nanohorn aggregates can be stably mass-produced.
- FIG. 1 is a side view showing a configuration of a nanocarbon production apparatus according to an embodiment.
- FIG. 2 is a diagram showing a configuration of a nanocarbon production apparatus according to the embodiment.
- C is a side view showing a configuration of the nanocarbon production apparatus according to the embodiment.
- FIG. 4 is a side view showing the configuration of the nanocarbon production apparatus according to the embodiment.
- FIG. 5 is a side view showing the configuration of the nanocarbon production apparatus according to the embodiment.
- FIG. 6 is a diagram exemplifying a shape of a graphite target applicable to the nanocarbon manufacturing apparatus according to the embodiment.
- FIG. 7 is a diagram illustrating a shape of a graphite target applicable to the nanocarbon manufacturing apparatus according to the embodiment.
- FIG. 8 is a diagram for explaining a method of process management in the nanocarbon manufacturing apparatus according to the embodiment.
- FIG. 9 is a diagram for explaining the method for producing nanocarbon according to the embodiment.
- FIG. 10 is a diagram for explaining the irradiation angle of laser light. BEST MODE FOR CARRYING OUT THE INVENTION
- FIG. 1 is a side view showing an example of a configuration of a nanocarbon production apparatus.
- FIG. 1 and the drawings used for describing other manufacturing apparatuses are schematic views, and the sizes of the respective components do not always correspond to actual dimensional ratios.
- the nanocarbon production apparatus 125 of FIG. 1 includes two chambers, a production chamber 107 and a nano-force recovery chamber 119.
- An inert gas supply unit 127 is connected to the production chamber 107 via a flow meter 127.
- Ma the laser beam emitted from the laser light source 1 1 1 held by the light source holding unit 1 1 2 1 0 3 force Z ii S e through the plano-convex lens 13 1 and the Z n Se window 13
- the surface of the graphite target 139 installed in the manufacturing chamber 107 is irradiated.
- Graphite target 1339 is a solid carbon simple substance that is a target of laser beam 103 irradiation.
- the graph target 13 is held in a target holding section 15 3 on the target supply plate 13 5.
- the plate holding section 135 moves the target supply plate 135 horizontally in the horizontal direction. For this reason, when the target supply plate 13 5 moves, the graph eye target 13 9 placed thereon moves, and the irradiation position of the laser beam 103 and the surface of the graph eye target 13 9 move.
- the configuration is such that the relative position with respect to moves.
- FIGS. 2 (a) and 2 (b) are diagrams for explaining the configurations of the target supply plate 135 and the plate holding portion 135 in more detail.
- FIG. 2A is a top view
- FIG. 2B is a cross-sectional view taken along line AA ′ of FIG. 2A.
- Threads are formed on the bottom surface of the target supply plate 1 35 and the surface of the plate holding section 1 37, and the target supply plate 1 35 is a rack and pinion type as shown in FIG. 2 (b). It is configured to be able to move in the left-right direction.
- the target holding portion 153 and the target holding portion 153 are held.
- the graph eye target 1 39 held in the section 15 3 is configured to be able to move up and down in FIG. 2 (a). With such a configuration, the sheet-like graph eye target 1339 can be moved in the P l — direction and the P i — pn direction. For this reason, the graph target 13 can be moved two-dimensionally in the plane. Therefore, it can be supplied to the irradiation position of the laser beam 103 emitted from the laser light source 111.
- the graph object target 13 The irradiation position of the laser beam 103 on the graph target target 1339 is moved so that the power density of the irradiation light becomes substantially constant. For example, the irradiation angle or irradiation light intensity of the laser beam 103 is adjusted. For example, if the surface of the Graphite Target 1339 is flat, the laser light source 111 is installed so that the irradiation angle of the laser light 103 is constant, and the laser light 103 is emitted at a constant intensity.
- the graph eye target 1339 can be translated while irradiating.
- the transfer tube 14 1 communicates with the nanocarbon recovery chamber 1 19.
- the transfer pipe 141 is provided in the direction of the generation of the plume 109 when the laser light 103 is emitted from the laser light source 111 to the surface of the graphite target 133. ing.
- the plume 109 is perpendicular to the surface of the graphite target 1339 because the laser beam 103, which forms a 45 ° angle with the surface of the graphite target 1339, is irradiated. Occurs in the direction.
- the transport pipe 141 has a configuration in which its length direction is arranged in the vertical direction on the surface of the graphite target 13. In this way, the carbon nanohorn assembly 1 17 generated by cooling the evaporated carbon vapor is guided from the transfer pipe 14 1 to the nano carbon recovery chamber 1 19, and is reliably transferred to the nano carbon recovery channel 1 19. Collected.
- the shape of the solid carbon substance used as the graphite target 1339 is not particularly limited, but may be, for example, a sheet shape or a rod shape.
- the length of the graph-eye target 13 9 The laser beam 103 can be irradiated at a constant power density in the vertical direction.
- the irradiation angle at this time is preferably 30 ° or more and 60 ° or less.
- the irradiation angle is an angle between a perpendicular to the surface of the graphite target 13 9 at the irradiation position of the laser beam 103 and the laser beam 103.
- FIG. 10 is a diagram for explaining this irradiation angle. FIG.
- FIG. 10 (a) is a cross-sectional view of the Daraite target 1339 when the surface of the Graphite target 1339 is flat
- FIG. 10 (b) is a cross-sectional view of the graphite target 13
- FIG. 31 is a cross-sectional view of the graph eye target 13 9 when the surface of 39 is a curved surface.
- the irradiation angle By setting the irradiation angle to 30 ° or more, it is possible to prevent reflection of the irradiation laser beam 103, that is, generation of return light. Further, the generated plume 109 is prevented from directly hitting the ZnSe plano-convex lens 131 through the ZnSe window 1333. For this reason, the ZnSe plano-convex lens 13 1 can be protected. In addition, it is possible to prevent the carbon nanohorn aggregates 117 from adhering to ZnSe e window 133.
- the irradiation angle By controlling the irradiation angle to 60 ° or less, the formation of amorphous carbon is suppressed, and the ratio of the carbon nanohorn aggregates 117 in the product, that is, the yield of the carbon nanohorn aggregates 117, is reduced. Can be improved.
- the irradiation angle was 45 as shown in Fig. 1. Les, especially preferred. 4 5.
- the ratio of the carbon nanohorn aggregate 11 ⁇ in the product can be further increased, and the yield can be improved.
- the irradiation position of the laser beam 103 on the surface of the graph electrode target 139 can be continuously changed, so that the carbon nanohorn assembly It is possible to produce bodies 1 17 continuously.
- the power density of the laser beam 103 applied to the surface of the graphite target 1339 constant, it is possible to stably produce the carbon nanohorn aggregate in a high yield.
- a method for producing the carbon nanohorn aggregate 117 using the production apparatus of FIG. 1 will be specifically described.
- the graphite target 1339 high-purity graphite, for example, sheet-like or rod-like sintered carbon or compression-molded carbon can be used.
- the laser beam 1 0 3 for example, using a laser beam, such as a high output C_ ⁇ 2 gas laser beam.
- a r, reaction inert gas atmosphere including a rare gas such as H e, for example 1 0 3 P a than on 1 0 5 Perform in an atmosphere of Pa or less.
- the output of the laser light 103 is, for example, 1 kW or more and 50 kW or less, and more specifically, for example, 3 kW or more and 5 kW or less.
- the pulse width of the laser beam 103 is, for example, at least 0.02 seconds, preferably at least 0.5 seconds, and more preferably at least 0.75 seconds. By doing so, the accumulated energy of the laser beam 103 irradiated on the surface of the graph eye rod 101 can be sufficiently secured. For this reason, the carbon nanohorn aggregate 117 can be manufactured efficiently.
- the pulse width of the laser beam 103 is, for example, 1.5 seconds or less, and preferably 1.25 seconds or less.
- the pulse width of the laser beam 103 is more preferably 0.75 seconds or more and 1 second or less. In this case, both the production rate and the yield of the carbon nanohorn aggregate 117 can be improved.
- the pause width in the irradiation of the laser beam 103 can be, for example, 0.1 seconds or more, and preferably 0.25 seconds or more. By doing so, overheating of the graph eye rod 101 surface can be suppressed more reliably. Can be.
- the preferable irradiation angle of the laser beam 103 can be set to 30 ° or more and 60 ° or less, and is preferably set to 45 °.
- the spot diameter of the laser beam 103 irradiated on the surface of the graph target 13 can be, for example, not less than 0.5 mm and not more than 5 mm.
- the graph eye target 13 9 is translated. At this time, it is possible to move the graph target 139 so that the spot of the laser beam 103 is moved at a speed of, for example, 0.01 mm / sec or more and 100 mm / sec or less. preferable.
- the moving speed of the graph object target 13 9 is, for example, not less than 2.5 mm / sec and not more than 50 mm / sec.
- the soot-like substance produced by using the nanocarbon production apparatus 125 mainly includes the carbon nanohorn aggregates 117, and for example, is collected as a substance containing 90 wt% or more of the carbon nanohorn aggregates 117. You. As described above, by using the nanocarbon production apparatus 125, a carbon nanohorn assembly 117 can be obtained with a high yield. Further, the quality of the obtained carbon nanohorn aggregate 117 can be stabilized.
- the position of the graphite target 13 9 can be moved in the plane direction, so that the laser beam 10 3 exhausts the graphite target 13 9 It is possible.
- the carbon nanohorns that constitute the carbon nanohorn assembly 1 17 The shape, size of the diameter, length, shape of the tip, the distance between the carbon molecules and the carbon nanohorn, and the like can be variously controlled by the irradiation conditions of the laser beam 103 and the like.
- the present embodiment relates to another configuration of the nanocarbon production device.
- the same components as those of the nanocarbon producing apparatus 125 described in the first embodiment are denoted by the same reference numerals, and the description thereof will not be repeated.
- FIG. 3 is a side view showing the configuration of the nanocarbon production apparatus according to the present embodiment.
- the nanocarbon production apparatus 149 of FIG. 3 has a configuration in which the graphite target 139 is sent out by a belt conveyor system.
- an annular sheet of graphite target 139 is mounted on the side surface of a cylindrical roller 161 via a target holding plate 159.
- the roller 16 1 By rotating the roller 16 1 in a predetermined direction, the irradiation position of the laser beam 103 on the surface of the graph eye target 13 9 moves.
- Irradiation with the laser beam 103 is preferably performed on a portion of the graphite target 139 supported by the target holding plate 159.
- the surface of the irradiation site is flat, whereas in the corners not supported by the target holding plate 159, the target holding plate 15 This is because the curvature of the surface of the graphite target 13 9 is larger than that of the portion supported by 9.
- an endless belt-shaped graph eye target 13 9 is attached to the side surface of the roller 16 1, and an endless belt-shaped graph eye target 13 9 is installed between the pair of rollers 16 1.
- it is configured so that the roller fight target 1 39 is driven by rotating the roller 16 1. Therefore, with a simple configuration, a smooth graph target is applied to the irradiation position of the laser beam 103.
- the surface of 139 can be supplied stably and continuously. Therefore, the configuration is more suitable for mass production.
- a groove (not shown in FIG. 3) is formed in the target holding plate 159.
- the present embodiment relates to another configuration of the nanocarbon production device. Also in this embodiment, the same components as those of the nanocarbon production apparatus 125 or the nanocarbon production apparatus 149 described in the first or second embodiment are denoted by the same reference numerals, and will be appropriately described. Is omitted.
- FIG. 4 is a side view showing the configuration of the nanocarbon production apparatus according to the present embodiment.
- the basic configuration of the nanocarbon production system 15 1 shown in Fig. 4 is the same as that of the nanocarbon production system 125 shown in Fig. 1, but the rotatable target support column 1 79 has a graphite target 13 The difference is that 9 is wound.
- the sheet-shaped or bar-shaped graphite target 139 is wound around the target support column 179 as a roll.
- the end area of the graph eye target 13 9 released from the winding around the target support column 17 9 is placed on the target supply plate 13 5, and is placed in the light irradiation direction. Be guided.
- Graphite targets 13 9 are sequentially sent out in the direction of the laser beam 10 3, so that the graphite targets are continuously supplied to the light irradiation position and carbon nanohorn aggregates 11 17 are obtained. It has a configuration.
- One end of the graphite target 13 9 is set on the target supply plate 13 5.
- the target support column 1 79 rotates about its central axis, and the target supply plate 1 3 5 translates on the plate holding section 1 3 7, so that the graph targets 1 and 3 9 move.
- the laser beam 103 is supplied to the irradiation position.
- the groove (not shown in FIG. 4) is formed in the target supply plate 135 in the same manner as the configuration described with reference to FIG. 2 in the first embodiment.
- the graph eye target 1339 can also be moved in a direction perpendicular to the paper surface of FIG. It is possible.
- FIG. 5 is a side view showing the configuration of an apparatus having a different configuration for sending out the roll of the graph object target 1339.
- the nanocarbon production apparatus 163 of FIG. 5 has two pairs of rollers 165 that hold the graphite target 139 from both sides. By rotating the target support columns 1-9 and the rollers 1659, the graphite targets 1339 are sent out in the direction of the laser beam 103 irradiation.
- the graphite target 139 is formed on a substrate such as a Cu plate. By doing so, it is possible to suppress cracking or breakage that occurs in the graph eye target 13 when the roll-shaped graph eye target 13 is fed.
- a winding portion for winding the substrate after evaporating the graphite item 1339 may be provided in the manufacturing chamber 107.
- the laser beam 103 is irradiated a plurality of times. For example, when the laser beam 103 is irradiated twice, the graph eye target 1 39 of the irradiated portion is used up. You can adjust the thickness of 3 9
- a method of producing a carbon nanohorn aggregate 117 by applying a sheet-like graphite target 139 to the nanocarbon production apparatus 125 of FIG. 1 will be described as an example.
- the thickness of the graph target 13 is about 3 mm from the surface. Therefore, in this case, the thickness of the graph target 13 is set to about 6 mm.
- the irradiated surface may become rougher and the power density may fluctuate, but the graph-eye target 1 By setting the thickness of 39 in this way, it is possible to suppress the fluctuation of the power density. For this reason, the yield of the carbon nanohorn aggregate 117 can be improved.
- the adjustment of the thickness of the graph target 139 is not limited to the case where the laser beam 103 disappears when the laser beam 103 is irradiated twice, but for example, the laser beam 103 is irradiated three times with the laser beam 103. May be lost.
- the graph target 13 may be moved in the vertical direction in FIG. 2 (a) every 1.5 reciprocations.
- the pulse width and pause width of the laser beam 103 and the moving speed of the graph target 1 39 were adjusted, and the graph eye target 1 39 disappeared.
- the carbon nanohorn aggregate 117 may be manufactured under the condition that the irradiation of the laser beam 103 is not performed. This way. The disappearance of the graph eye target 13 9 causes the laser beam 103 Irradiation to members other than the target 13 can be suppressed. For this reason, the carbon nanohorn aggregate 117 can be produced more stably with a high yield.
- a target supply plate is provided at a lower portion of the graphite target 1339 at a portion irradiated with the laser beam 103, for example, as in the nanocarbon production apparatus shown in FIG. 1 or FIG.
- a configuration without 1 3 5 is also acceptable.
- a target supply plate 135 is provided below the graph target 133 at the irradiation position of the laser beam 103. There can be no configuration. This makes it possible to prevent the laser beam 103 from being directly irradiated onto the target supply plate 135 when the graphite target 139 just disappears.
- a buffering graphite target may be provided in an area where the laser beam 103 is irradiated. This makes it possible to more reliably suppress the deterioration of the manufacturing chamber 107 due to the direct irradiation of the wall of the manufacturing chamber 107 with the laser beam.
- the graphite target 1339 may be formed on a sheet of a material that is not excited by the irradiation of the laser beam 103. In this way, when the graphite target 1339 has just disappeared, the carbon nanohorn assembly 117 is directly irradiated with the laser beam 103 to the target supply plate 135, etc. Can be suppressed from decreasing.
- the thickness of the graph target 13 is adjusted so that when the laser beam 103 is irradiated once, the graph target 133 of the irradiated portion is used up. You may.
- the graphite target 1339 When the graphite target 1339 is formed in a sheet shape, for example, it can be formed into a shape having a surface as shown in FIG. 6 (a) or FIG. 6 (b).
- FIG. 6A is a flat plate, which is preferable because it is easy to make the power density of the laser beam 103 constant.
- a regular repeating structure is formed at a predetermined pitch on the surface of the graphite target 13.
- the laser beam 1 0 3 e.g. P l - when moving the qi direction, it is possible to suppress the vibration of the power density definitive irradiation position.
- the width w of the repeating structure be substantially equal to the spot diameter of the laser beam 103.
- the light-irradiated part of the graph target 13 9 is moved in the p! -C direction, and then in the p 2 -q 2 direction, and the irradiation position is set in the direction P i_ P 5
- the power density of the laser beam 103 irradiated on the surface of the graph target 139 can be kept constant. Therefore, the power density of the laser beam 103 applied to one graphite target 1339 is suppressed from varying, and the carbon nanohorn aggregate 117 having desired properties can be stably produced at a high yield. Obtainable.
- the surface shape of the graph-it target may be any repetitive structure having a predetermined repetitive structure width w (pitch), and is not particularly limited to the configuration shown in FIG. 6 (b), and may be selected as appropriate. it can.
- the thickness h of the graphite target 13 9 is set to such a value as to evaporate in one irradiation of the laser beam 103 as described above. I do.
- the thickness of the graphite target 1339 that evaporates when irradiated once with the laser beam 103 Is about 3 mm from the surface, the thickness h can be about 3 mm.
- the width of the graph target 139 may be a rod shape substantially equal to the spot diameter of the laser beam 103.
- the movement direction of the graph eye target 1339 can be limited to the A—A ′ direction in FIG. 2 (a). For this reason, it is not necessary to form a movable mechanism by combining the groove portion 150 and the convex portion 157 between the target supply plate 135 and the target holding portion 153. It is possible to further simplify.
- FIG. 7 is a diagram showing an example of the shape of a bar-shaped graph eye target 139.
- Fig. 7 (a) is a square pillar
- Fig. 7 (b) is a cylindrical graph target.
- the shape of the graphite target 139 is not limited to these, but preferably has a constant cross-sectional shape. By keeping the cross-sectional shape constant, it is possible to suppress the fluctuation of the power density of the laser beam 103 applied to the surface of the graphite target 13.
- the maximum width w of the graphite target 1319 is equal to or smaller than the spot diameter of the laser beam 103. By doing so, it is only necessary to move the graph item target 1339 in the length direction, and the manufacturing process can be simplified. Further, the thickness h of the graphite target 139 is preferably not more than the spot diameter of the laser beam 103. By doing so, it is possible to surely erase the graph-it target at the irradiation position by a single irradiation of the laser beam 103.
- both w and h are smaller than the spot diameter of the laser beam 103.
- the laser beam is applied to the surface along the length of the bar-shaped graph eye 1, target 1, and 139.
- the graphite target 139 can be used up in one irradiation.
- This embodiment is also applicable to the nanocarbon manufacturing apparatus shown in FIGS. 3 and 4, as in the fourth embodiment.
- FIG. 8 is a diagram for explaining a method of process management in the above-described nanocarbon production apparatus.
- a process management unit 167 manages the schedule of each process based on the time information input from the clock unit 169. This schedule management will be described with reference to the flowchart of FIG. 9 taking as an example the case of using the nanocarbon manufacturing apparatus 125 of the first embodiment (FIGS. 1 and 2) in the fourth embodiment.
- the pump control unit 171 drives the vacuum pump 143 to evacuate and exhaust the nanocarbon collection chamber 119 and the production champ 107 connected thereto (S101).
- the vacuum pump 144 is stopped, and the inert gas control unit 173 supplies the inert gas from the inert gas supply unit 127 to the manufacturing chamber 107 in a constant manner. Supply (S102).
- the laser light controller 175 irradiates a laser beam 103 (not shown in FIG. 8) with a predetermined intensity from the laser light source 111 (S103).
- Step 104 corresponds to the movement of the graph eye target 1339 in the p--q direction in FIG. 2 (a).
- the laser beam 103 on the surface of the graph eye target 1339 Move the graphite target 1 39 so that the irradiation position makes one round trip between pt and qi.
- Each of the above steps is managed by the process management unit 167.
- the moving means controller 177 moves one of the graphite target 1339 and the laser light source 111 relative to the other, and What is necessary is just to move the irradiation position of the laser beam 103 on the surface of the target 1339.
- a configuration may be adopted in which the irradiation angle of the laser light source 111 for irradiating the laser light 103 to the surface of the moving means control unit 177 force S and the graph object target 139 is also possible.
- the laser-light control unit 175 may be configured to irradiate the laser beam 103 while changing the intensity of the emitted light of the laser beam 103. This makes it possible to more precisely adjust the power density of the laser beam 103 applied to the Daraite target 1319.
- the carbon nanohorn aggregate is manufactured as the nanocarbon
- the nanocarbon manufactured using the nanocarbon manufacturing apparatus according to the present embodiment is the carbon nanohorn aggregate. It is not limited to the body.
- a carbon nanotube can be manufactured using the nanocarbon manufacturing apparatus according to the present embodiment.
- graphite Totage' sheet 1 3 9 substantially constant power density of the laser beam 1 0 3 at the surface of, for example 5 0 ⁇ 1 0 k W / cm 2 and so as to output a laser beam 1 0 3 It is preferable to adjust the diameter, spot diameter, and irradiation angle.
- a catalyst metal is added to the graphite target 1339, for example, in an amount of 0.0001 wt% or more and 5% or less.
- the metal catalyst for example, metals such as Ni and Co can be used.
- the nanocarbon manufacturing apparatus By using the nanocarbon manufacturing apparatus according to the present embodiment, it is possible to continuously send out the graphite target 139 to the irradiation position of the laser beam 103. Large-scale production is possible.
- the soot-like substance obtained by the irradiation of the laser beam 103 is recovered in the nanocarbon recovery chamber 119.
- it can also be collected by depositing it on an appropriate substrate, or by a method of collecting fine particles using a dust bag.
- an inert gas can be circulated in the reaction vessel to recover soot-like substances by the flow of the inert gas.
- the irradiation position of the laser beam 103 is kept constant, and the relative position of the laser beam 103 is moved by moving the graph item target 39.
- the relative position may be changed by moving the laser beam 103 by holding the laser light source 111 in the moving means.
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Abstract
Description
Claims
Priority Applications (2)
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JP2005505910A JP4581997B2 (ja) | 2003-04-30 | 2004-04-27 | ナノカーボン製造装置およびナノカーボンの製造方法 |
US10/555,064 US20070003468A1 (en) | 2003-04-30 | 2004-04-27 | Nanocarbon producing device and nanocarbon producing method |
Applications Claiming Priority (2)
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JP2003125844 | 2003-04-30 | ||
JP2003-125844 | 2003-04-30 |
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WO2004096705A1 true WO2004096705A1 (ja) | 2004-11-11 |
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PCT/JP2004/006048 WO2004096705A1 (ja) | 2003-04-30 | 2004-04-27 | ナノカーボン製造装置およびナノカーボンの製造方法 |
Country Status (5)
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US (1) | US20070003468A1 (ja) |
JP (1) | JP4581997B2 (ja) |
CN (1) | CN100340478C (ja) |
TW (1) | TWI254029B (ja) |
WO (1) | WO2004096705A1 (ja) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2009536917A (ja) * | 2006-05-12 | 2009-10-22 | 本田技研工業株式会社 | ドライパウダー注入装置、および、単層カーボンナノチューブの生産方法 |
WO2019026275A1 (ja) * | 2017-08-04 | 2019-02-07 | 日本電気株式会社 | カーボンナノホーン集合体の製造装置 |
WO2019026274A1 (ja) * | 2017-08-04 | 2019-02-07 | 日本電気株式会社 | カーボンナノホーン集合体の製造装置 |
WO2019030890A1 (ja) * | 2017-08-10 | 2019-02-14 | 日本電気株式会社 | カーボンナノホーン集合体の製造部材及び製造装置 |
WO2020158665A1 (ja) * | 2019-01-29 | 2020-08-06 | 日本電気株式会社 | カーボンナノブラシの連続製造用部材および製造方法 |
US11511998B2 (en) | 2018-05-29 | 2022-11-29 | Nec Corporation | Continuous production method of fibrous carbon nanohorn aggregate |
Families Citing this family (5)
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JP4982320B2 (ja) * | 2007-09-27 | 2012-07-25 | 大日本スクリーン製造株式会社 | 基板処理装置 |
US8237677B2 (en) * | 2008-07-04 | 2012-08-07 | Tsinghua University | Liquid crystal display screen |
CN104760953B (zh) * | 2015-04-13 | 2016-08-24 | 北京化工大学 | 一种激光隧道全反射轴心聚焦碳纤维石墨化炉 |
EP3587347A4 (en) * | 2017-02-27 | 2020-01-22 | Nec Corporation | PROCESS FOR PRODUCING CARBON NANOCORNET AGGREGATES |
CN107416799A (zh) * | 2017-07-31 | 2017-12-01 | 江苏大学 | 一种提高石墨烯制备效率的装置与方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62224669A (ja) * | 1986-03-27 | 1987-10-02 | Mitsubishi Electric Corp | レ−ザセラミツクスコ−テイング方法 |
JPH0633237A (ja) * | 1992-07-17 | 1994-02-08 | Kobe Steel Ltd | 昇華性材料の蒸着めっき方法 |
JPH08268705A (ja) * | 1995-03-28 | 1996-10-15 | Toho Rayon Co Ltd | フラーレンの製造方法及びその製造装置 |
JP2001064004A (ja) * | 1998-07-25 | 2001-03-13 | Japan Science & Technology Corp | 単層カーボンナノホーン構造体とその製造方法 |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3284372A (en) * | 1965-09-14 | 1966-11-08 | Great Lakes Carbon Corp | Apparatus and process for continuously making baked and graphitized carbon bodies |
JPS6033237A (ja) * | 1983-08-04 | 1985-02-20 | 武州興業株式会社 | 水硬性低強度セメントの製法 |
US4816293A (en) * | 1986-03-27 | 1989-03-28 | Mitsubishi Denki Kabushiki Kaisha | Process for coating a workpiece with a ceramic material |
US5411797A (en) * | 1988-04-18 | 1995-05-02 | Board Of Regents, The University Of Texas System | Nanophase diamond films |
DE69424917T2 (de) * | 1993-11-03 | 2000-10-12 | Bridgestone Corp | Verfahren und Vorrichtung zur ablativen Behandlung von elastomerischen Produkten |
WO2000022184A1 (en) * | 1998-10-12 | 2000-04-20 | The Regents Of The University Of California | Laser deposition of thin films |
-
2004
- 2004-04-27 CN CNB2004800116341A patent/CN100340478C/zh not_active Expired - Lifetime
- 2004-04-27 JP JP2005505910A patent/JP4581997B2/ja not_active Expired - Fee Related
- 2004-04-27 US US10/555,064 patent/US20070003468A1/en not_active Abandoned
- 2004-04-27 WO PCT/JP2004/006048 patent/WO2004096705A1/ja active Application Filing
- 2004-04-29 TW TW093112018A patent/TWI254029B/zh not_active IP Right Cessation
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62224669A (ja) * | 1986-03-27 | 1987-10-02 | Mitsubishi Electric Corp | レ−ザセラミツクスコ−テイング方法 |
JPH0633237A (ja) * | 1992-07-17 | 1994-02-08 | Kobe Steel Ltd | 昇華性材料の蒸着めっき方法 |
JPH08268705A (ja) * | 1995-03-28 | 1996-10-15 | Toho Rayon Co Ltd | フラーレンの製造方法及びその製造装置 |
JP2001064004A (ja) * | 1998-07-25 | 2001-03-13 | Japan Science & Technology Corp | 単層カーボンナノホーン構造体とその製造方法 |
Non-Patent Citations (1)
Title |
---|
IIJIMA S. ET AL: "Nano-aggregates of single-walled graphitic carbon nano-horns", CHEMICAL PHYSICS LETTERS, vol. 309, 13 August 1999 (1999-08-13), pages 165 - 170, XP002909062 * |
Cited By (14)
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JP2009536917A (ja) * | 2006-05-12 | 2009-10-22 | 本田技研工業株式会社 | ドライパウダー注入装置、および、単層カーボンナノチューブの生産方法 |
WO2019026275A1 (ja) * | 2017-08-04 | 2019-02-07 | 日本電気株式会社 | カーボンナノホーン集合体の製造装置 |
WO2019026274A1 (ja) * | 2017-08-04 | 2019-02-07 | 日本電気株式会社 | カーボンナノホーン集合体の製造装置 |
US11485641B2 (en) | 2017-08-04 | 2022-11-01 | Nec Corporation | Production apparatus for carbon nanohorn aggregate |
JPWO2019026274A1 (ja) * | 2017-08-04 | 2020-07-02 | 日本電気株式会社 | カーボンナノホーン集合体の製造装置 |
JPWO2019026275A1 (ja) * | 2017-08-04 | 2020-07-09 | 日本電気株式会社 | カーボンナノホーン集合体の製造装置 |
JPWO2019030890A1 (ja) * | 2017-08-10 | 2020-07-09 | 日本電気株式会社 | カーボンナノホーン集合体の製造部材及び製造装置 |
US11208329B2 (en) | 2017-08-10 | 2021-12-28 | Nec Corporation | Production member and production apparatus for carbon nanohorn aggregate |
WO2019030890A1 (ja) * | 2017-08-10 | 2019-02-14 | 日本電気株式会社 | カーボンナノホーン集合体の製造部材及び製造装置 |
US11511998B2 (en) | 2018-05-29 | 2022-11-29 | Nec Corporation | Continuous production method of fibrous carbon nanohorn aggregate |
WO2020158665A1 (ja) * | 2019-01-29 | 2020-08-06 | 日本電気株式会社 | カーボンナノブラシの連続製造用部材および製造方法 |
JPWO2020158665A1 (ja) * | 2019-01-29 | 2021-12-02 | 日本電気株式会社 | カーボンナノブラシの連続製造用部材および製造方法 |
JP7156407B2 (ja) | 2019-01-29 | 2022-10-19 | 日本電気株式会社 | カーボンナノブラシの連続製造用部材および製造方法 |
US11981568B2 (en) | 2019-01-29 | 2024-05-14 | Nec Corporation | Member for continuous production of carbon nanobrush, and method for continuous production of carbon nanobrush |
Also Published As
Publication number | Publication date |
---|---|
TW200424124A (en) | 2004-11-16 |
US20070003468A1 (en) | 2007-01-04 |
JPWO2004096705A1 (ja) | 2006-07-13 |
CN100340478C (zh) | 2007-10-03 |
TWI254029B (en) | 2006-05-01 |
CN1780790A (zh) | 2006-05-31 |
JP4581997B2 (ja) | 2010-11-17 |
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