JP6234298B2 - Carbon nanotube production equipment - Google Patents

Description

  The present invention relates to a carbon nanotube production apparatus.

  As a conventionally known high-performance battery, an electrode in which an amorphous layer is grown on the outer surface of the carbon nanotube on the electrolyte membrane can be used to support more battery catalysts and the battery. There is known a fuel cell in which the catalyst is prevented from aggregating on the surface of the carbon nanotube and the power generation efficiency is further improved (for example, see Patent Document 1).

JP 2007-257886 A

  In the prior art, the length of the carbon nanotube and the thickness of the amorphous layer are controlled by the concentration of the source gas supplied, but even if a sufficiently high concentration of source gas is supplied, depending on the thickness of the resulting amorphous layer In some cases, aggregation of the battery catalyst on the surface of the carbon nanotube is not suppressed.

  In order to solve this problem, for example, a temperature suitable for growth of carbon nanotubes having high crystallinity (so-called length growth) and growth of amorphous carbon formed on the outer surface of the carbon nanotubes (so-called growth) It seems that the length and the thickness of the amorphous layer can be individually controlled by growing the carbon nanotubes in two stages with a temperature suitable for the growth of the amorphous layer. However, in such a manufacturing apparatus that continuously generates carbon nanotubes, a region provided in one reaction vessel that performs the first-stage growth and a region that performs the second-stage growth, A section is required to transition from a temperature suitable for the growth of the length to a temperature suitable for the growth of the amorphous layer, but the length of the carbon nanotubes is excessively extended due to the material gas flowing into this section by mistake. It is considered that there are cases where the length of the carbon nanotube cannot be accurately controlled.

  Therefore, an object of the present invention is to provide a carbon nanotube production apparatus capable of accurately controlling the length of a carbon nanotube and the thickness of an amorphous layer.

The carbon nanotube production apparatus according to the present invention introduces a substrate on which a catalyst is supported and is moved in a predetermined direction, and heats the substrate surface to a first CVD temperature along the direction of movement of the substrate. There is provided a first CVD temperature region in which carbon nanotubes are grown to a predetermined length, and a second CVD region in which the substrate surface is heated to a second CVD temperature higher than the first CVD temperature to deposit carbon on the surface of the carbon nanotubes. An apparatus for producing carbon nanotubes having a reduced pressure reaction vessel for continuously producing carbon nanotubes using chemical vapor deposition,
In the reaction vessel, the first CVD temperature region and the second CVD temperature region are connected to the source gas supply pipe for supplying the source gas to the substrate and cover the surface of the substrate over a predetermined range. The first space partition and the second space partition that limit the reaction space by being arranged, respectively,
A heat shielding member is provided between the first space partition and the second space partition.

The heat shielding member is preferably made of steel coated with ceramics or silicon carbide.
The second CVD temperature may be set higher by 50 to 200 degrees than the first CVD temperature.

  In the reaction vessel, it is preferable that a heat shielding member is further provided on the rear side in the movement direction of the substrate with respect to the first space partition and on the front side in the movement direction of the substrate with respect to the second space partition.

  More preferably, the heat shielding member is composed of a plurality of plates, and a gas exhaust pipe for exhausting the raw material gas discharged from between the plates to the outside is connected to the wall portion of the reaction vessel.

  According to the carbon nanotube manufacturing apparatus of the present invention, between the first CVD temperature region heated to a temperature suitable for the growth of the length and the second CVD temperature region heated to a temperature suitable for the growth of the amorphous layer. By providing the heat shielding member, the heat transfer between the first CVD temperature region and the second CVD temperature region is prevented, the inflow of the source gas is prevented, and the length of the carbon nanotube and the thickness of the amorphous layer are accurately controlled. Carbon nanotubes can be produced.

It is a side view which shows the schematic structure of the whole carbon nanotube manufacturing apparatus which concerns on Example 1 of this invention. It is a perspective view which shows schematic structure in the pressure reduction chamber of the manufacturing apparatus. It is a longitudinal cross-sectional view which shows schematic structure in the pressure reduction chamber. It is the elements on larger scale in the heat shielding member and formation part in the decompression chamber. It is BB sectional drawing shown in FIG. It is the elements on larger scale in the heat shielding member and formation part of the manufacturing apparatus of the carbon nanotube which concerns on Example 2 of this invention.

[Example 1]
A carbon nanotube production apparatus according to Example 1 of the present invention will be described with reference to FIGS.

  As shown in FIGS. 2 and 3, the processing space 4 includes a pre-processing unit 10 that raises the temperature of the substrate 2 to a predetermined temperature along the moving direction of the substrate 2, and a predetermined temperature at the pre-processing unit 10. Forming the carbon nanotube 3 by the chemical vapor deposition method (Chemical Vapor Deposition method: CVD method) while supplying the raw material gas G2 to the substrate 2 that has risen up to, and the carbon nanotube 3 formed in the forming portion 20 And a post-processing unit (also referred to as a cooling unit) 30 for lowering the temperature of the substrate 2. Depending on the surface temperature of the substrate 2, the processing space 4 includes a temperature rising region X corresponding to the preprocessing unit 10, a CVD temperature region Y corresponding to the forming unit 20, and post-processing, as indicated by a virtual line in FIG. It is divided into a temperature fall region Z corresponding to the part 30. A heat insulating material 9 is provided on the inner wall surface of the decompression chamber 5.

  First, the pretreatment unit 10 is provided in the decompression chamber 5 on the feeding unit 6 side, and increases the temperature of the substrate 2 to a temperature equivalent to the heating temperature (CVD temperature) in the formation unit 20 on the lower side. At least one heating device is provided. In the present embodiment, since the temperature of the substrate 2 is raised in three stages in the temperature raising region X, the first temperature region A1 and the second temperature are increased from the upstream side to the downstream side as shown by the phantom line in FIG. A temperature region A2 and a third temperature region A3 are provided. The pretreatment unit 10 includes a first heating device 11 provided in the first temperature region A1, a second heating device 12 provided in the second temperature region A2, and a third heating device 13 provided in the third temperature region A3. The three heating devices are provided. The heating temperature of the 1st heating apparatus 11, the 2nd heating apparatus 12, and the 3rd heating apparatus 13 is each set to the temperature from which the board | substrate 2 surface becomes the range of 450 to 600 degreeC. In this embodiment, the temperature of the surface of the substrate 2 is measured by inserting a thermometer such as a thermocouple near the surface of the substrate 2 in the decompression chamber 5 and calculating the temperature of the surface of the substrate 2 from the measured temperature. Thus, the heating temperature by the heating device is maintained or controlled.

  The pretreatment unit 10 includes a duct 14 that guides the substrate 2 while covering the periphery of the substrate 2 having a predetermined width sent from the feeding unit 6. In this embodiment, as shown in FIGS. 2 and 3, the duct 14 is rectangular in cross section and hollow, and the duct 14 is used from the front end to the rear end, that is, the first end of the pretreatment unit 10 (temperature rising region X). The temperature region A1 extends from the third temperature region A3. In general, as shown in FIG. 4, the duct 14 may have a size that allows at least the substrate 2 to be inserted. In the roll-to-roll manufacturing apparatus 1 as in this embodiment, the thickness of the substrate 2 is, for example, 0.03 mm to 0.100 mm. Further, as shown in FIG. 3, in the present embodiment, the upstream end of the duct 14 of the pretreatment unit 10 protrudes into the connecting member 8 that connects the feeding unit 6 and the decompression chamber 5, An insertion port 15 for inserting the duct 14 is formed in the chamber 5. Between the insertion port 15 and the duct 14, for example, an O-ring (O-ring) 16 is provided as a seal member that prevents the gas in the pretreatment unit 10 from flowing into the connection member 8.

The pretreatment gas G <b> 1 is supplied to the duct 14 of the pretreatment unit 10 from the supply unit 6 side via the connection member 8. As the pretreatment gas G1, for example, an inert gas such as nitrogen (N ₂ ) or argon (Ar) and an atomized gas such as hydrogen (H ₂ ) that atomizes the catalyst on the surface of the substrate 2 are used. Note that the atomization gas may be supplied together with the inert gas.

  In the present embodiment, as shown in FIGS. 3 and 4, the downstream end of the duct 14 of the pretreatment unit 10 is located in the vicinity of the boundary between the pretreatment unit 10 and the forming unit 20. At the downstream end of the duct 14 of the pretreatment unit 10, the pretreatment gas G1 supplied to the pretreatment unit 10 and the raw material gas G2 supplied to the forming unit 20 (precisely, the raw material generated by a chemical reaction) An exhaust opening 40 for exhausting the mixed gas G3 mixed with the source gas G2 and the decomposed component may be referred to as source gas G4). It has been. In the present embodiment, the exhaust opening 40 is an opening end on the upstream side of the duct 14 of the pretreatment unit 10.

  Further, in order to prevent the source gas G2 from flowing into the duct 14 of the pretreatment unit 10 in the vicinity of the boundary between the pretreatment unit 10 and the formation unit 20, the mixed gas exhausted from the exhaust opening 40. A mixed gas exhaust pipe 41 for flowing G3 out of the decompression chamber 5 and a mixed gas exhaust port 41a for connecting the mixed gas exhaust pipe 41 are provided. In the present embodiment, as shown in FIG. 4, the mixed gas exhaust pipe 41 and the mixed gas exhaust port 41 a are disposed below the substrate 2 in the decompression chamber 5.

  In this way, by supplying the pretreatment gas G1 to the duct 14 provided in the pretreatment unit 10, the raw material gas G2 can be prevented from flowing into the duct 14 from the formation unit 20. Therefore, the raw material gas G2 is prevented from coming into contact with the catalyst on the surface of the substrate 2, and the substrate 2 is sent to the forming unit 20 without impairing the activity of the catalyst supported on the surface. Will improve.

  When the pretreatment unit 10 includes the exhaust opening 40, the raw material gas G2 can be more reliably prevented from flowing into the duct 14 of the pretreatment unit 10, and the production rate of the carbon nanotubes 3 can be improved.

  Next, as shown in FIGS. 3 and 4, the formation portion 20 provided at the downstream side of the pretreatment portion 10 that is the gist of the present invention, that is, the CVD temperature region Y, is a carbon whose surface of the substrate 2 is highly crystalline. A first CVD temperature region (fourth temperature region) A4 that is heated to a first CVD temperature suitable for nanotube growth (so-called growth in the length direction) and the surface of the substrate 2 are formed on the outer surface of the carbon nanotube. And a second CVD temperature region (fifth temperature region) A5 that is heated to a second CVD temperature suitable for the growth of amorphous carbon (so-called amorphous layer growth). Specifically, the first CVD temperature is preferably in the range of 600 ° C to 700 ° C, and the second CVD temperature is in the range of 650 ° C to 900 ° C, which is 50 ° C to 200 ° C higher than the first CVD temperature. Is preferred.

  A fourth heating device 25 provided below the substrate 2 is provided in the upstream first CVD temperature region A4, and a fifth heating device 26 provided below the substrate 2 is provided in the downstream second CVD temperature region A5. Are arranged respectively. The fourth heating device 25 and the fifth heating device 26 mainly heat the substrate 2 and the first CVD temperature region A4 and the second CVD temperature region A5 in the decompression chamber 5 together.

As shown in FIGS. 3 and 4, in the forming unit 20, that is, the first CVD temperature region A4 and the second CVD temperature region A5, hydrocarbons such as methane (CH ₄ ) and acetylene (C ₂ H ₂ ) are contained in the decompression chamber 5. The source gas supply pipe 21 for supplying the source gas G2 of the system, the source gas supply port 21a for connecting the source gas supply pipe 21, and the source gas supply pipe 21 are connected to the surface of the substrate 2. A first space partition 22A and a second space partition 22B that limit the reaction space in which the supplied source gas G2 is chemically reacted on the substrate 2 to generate the carbon nanotubes 3 by covering over a predetermined range are provided. It is done. The first space partition 22A mainly controls the length of the carbon nanotubes, and the second space partition 22B mainly controls the thickness of the amorphous layer (more specifically, the thickness of the carbon nanotubes).

  As shown in FIGS. 3 and 4, the space partitions 22 </ b> A and 22 </ b> B are provided in the hollow rectangular parallelepiped reaction main body 23 and the lower end thereof and extend along the moving direction of the substrate 2 to surround the substrate 2. And a substrate guide protrusion 24 for guiding the substrate 2. Specifically, as shown in FIGS. 3 and 4, the cross section of the substrate guiding protrusion 24 has the same shape as the duct 14, in other words, the shape in which the duct 14 is connected to the reaction main body 23. doing. Hereinafter, the board guide protrusion is referred to as a duct portion 24. The reaction main body 23 is formed by welding five plates made of quartz glass having low thermal conductivity and low thermal expansion by engaging the stepped portions provided at each joint. The reaction main body 23 has a supply pipe connection port 21 b for connecting the source gas supply pipe 21. That is, the source gas supply pipe 21 is inserted into the source gas supply port 21a of the decompression chamber 5 and provided to the supply pipe connection port 21b. In this embodiment, as shown in FIG. 4, the height H1 of the opening end of the duct 14 of the pretreatment unit 10 and the pretreatment unit 10 side (upstream side) of the duct unit 24 of the formation unit 20 are illustrated. The height H2 of the opening end is the same (H1 = H2).

  At this time, if heat transfer such as heat conduction, heat transfer, and radiation occurs between the first CVD temperature region A4 and the second CVD temperature region A5, the length and thickness of the carbon nanotube cannot be accurately controlled. , Production efficiency decreases. Therefore, as shown in FIG. 4, the formation part 20 is provided with a heat shielding member 27 between the first space partition 22A and the second space partition 22B. Here, in order to simplify the configuration of the manufacturing apparatus 1, the duct portion 24 is not provided between the first space partition 22A and the second space partition 22B.

  The heat shielding member 27 is made of a material that can withstand high temperatures such as the first CVD temperature and the second CVD temperature, and examples thereof include ceramics and steel coated with silicon carbide. In addition, examples of the shape of the heat shielding member 27 include a block shape, a plate shape, and a film shape. Specifically, the shape is preferably a plate shape as shown in FIG. Hereinafter, this heat shielding member is referred to as a heat shielding plate 27. Further, the heat shield plate 27 is formed with a slit 27a through which the substrate 2 can be inserted as shown in FIG. The width and height of the slit 27a are preferably the same as the height and width of the duct portion 24.

  The heat shielding plate 27 is fixed in the decompression chamber 5 with the side end portion and the upper end portion being supported by the heat insulating material 9. Specifically, as shown in FIGS. 4 and 5, the heat insulating material 9 is provided with the same number of grooves as the number of the heat shielding plates 27, and the heat shielding plates 27 are inserted and fixed in the grooves. However, the lower end of the heat shielding plate 27 is open. Therefore, a gap is formed between the heat shield plates 27 through which gas can pass.

  The thickness of the heat shield plate 27 and the number of sheets to be used may be appropriately determined depending on the values of the first CVD temperature and the second CVD temperature and the size of the interval between the first space partition 22A and the second space partition 22B. In particular, since heat transfer due to radiation is large under reduced pressure, it is necessary to provide a sufficient number of heat shielding plates 27 so that the second CVD temperature does not affect the first CVD temperature. Therefore, for example, a configuration may be adopted in which a plurality of heat shielding plates 27 having a predetermined thickness (for example, 50 μm thickness) are arranged in a predetermined section (for example, 20 mm section) at a predetermined interval (1 mm interval). Specifically, in Example 1, it is possible to suppress heat transfer due to radiation at 50 ° C. per sheet.

  The source gas supply port 21 a is provided above the substrate 2 of the reaction main body 23, and the source gas G 4 and the like supplied into the first space partition 22 A and the second space partition 22 B are supplied to the decompression chamber 5. A gas exhaust port 28 a for connecting a gas exhaust pipe 28 for exhausting to the outside is provided on the lower side of the substrate 2 in the decompression chamber 5. Specifically, the gas exhaust port 28a for discharging the source gas G4 or the like is preferably arranged corresponding to each space partition 22A, 22B, but in this embodiment, the configuration of the manufacturing apparatus 1 is simplified. Therefore, as shown in FIG. 4, the mixed gas exhaust port 41a is also used as the gas exhaust port 28a disposed with respect to the first space partition 22A, and the mixed gas exhaust port 41a is connected to the mixed gas exhaust port 41a. The connected mixed gas exhaust pipe 41 is also used. Further, with respect to the second space partition 22 </ b> B, in the decompression chamber 5, the downstream side of the duct portion 24, which is a boundary between the formation unit 20 and the post-processing unit 30 (a boundary between the CVD temperature region Y and the temperature decrease region Z). A gas exhaust port 28a is provided at a position directly below the end, and a gas exhaust pipe 28 is connected thereto. Furthermore, the gas exhaust pipe 28 is more preferably provided at a position corresponding to the space between the first space partition 22A and the second space partition 22B, that is, directly below the heat shield plate 27.

  Further, as shown in FIG. 4, the formation portion 20 has a reaction main body portion 23 on the upper surface of the surface of the substrate 2 on the inner surface of the duct portion 24 in each of the space partitions 22 </ b> A and 22 </ b> B, that is, on the inner surface of the ceiling of the duct portion 24. A gas deflection unit 29 is provided for directing the source gas G2 flowing in from the substrate 2 toward the surface of the substrate 2. Specifically, as shown in FIG. 4, the gas deflection unit 29 is a plurality of protrusion members 29 extending in a direction intersecting the moving direction of the substrate 2 (specifically, the width direction of the substrate 2). They are arranged at a predetermined interval in the moving direction of the substrate 2.

  As described so far, in the formation unit 20, the heat shield plate 27 is provided between the first CVD temperature region A4 and the second CVD temperature region A5, so that the first CVD temperature region A4 and the second CVD temperature region A5 are separated. Heat transfer between them can be prevented.

  Further, in the forming unit 20, the source gas supply port 21 a is provided on the upper side of the substrate 2, and the gas exhaust port 28 a is provided on the lower side of the substrate 2. Therefore, the flow of the source gas G2 in the first space partition 22A and the second space partition 22B is directed from the upper side to the lower side of the substrate 2. Therefore, the source gas G2 is likely to come into contact with the catalyst on the surface of the substrate 2, and the generation rate of the carbon nanotubes 3 is improved. In particular, when the gas exhaust pipe 28 is provided directly below the heat shielding plate 27, for example, when the concentration of the source gas G2 supplied to the first space partition 22A and the second space partition 22B is different, the respective spaces The source gas G2 supplied to the partitions 22A and 22B can be prevented from being mixed with each other, and the length and thickness of the carbon nanotubes 3 can be controlled more precisely.

  By providing the gas deflecting portion 29 on the inner surface of the ceiling of the duct portion 24, the source gas G2 flowing into the duct portion 24 collides with the gas deflecting portion (projection member) 29 and heads toward the substrate 2 side. Since the flow of the raw material gas G2 can be made and the raw material gas G2 can be brought into contact with the catalyst on the surface of the substrate 2 more reliably, the production rate of the carbon nanotubes 3 is improved.

  Finally, in the cooling unit 30 provided on the downstream side of the forming unit 20, that is, the temperature drop region Z, as shown in FIG. 3, the substrate 2 and the generated carbon nanotube 3 (hereinafter referred to as the substrate 2 or the like) may be used. ) At least one heating device for lowering the temperature from the second CVD temperature in the forming unit 20 to room temperature. In the present embodiment, in the temperature lowering region Z, the temperature of the substrate 2 and the like is decreased in three stages. Therefore, as shown by the phantom line in FIG. It has area | region A7 and 8th temperature area A8. The post-processing unit 30 includes a sixth heating device 31 provided in the sixth temperature region A6, a seventh heating device 32 provided in the seventh temperature region A7, and an eighth heating device 33 provided in the eighth temperature region A8. The three heating devices are provided. The heating temperature of the sixth heating device 31, the seventh heating device 32, and the eighth heating device 33 is such that the surface temperature of the substrate 2 is 500 in order to prevent thermal deformation of the substrate 2 when cooling from the heating temperature in the forming unit 20. The temperature is set so as to gradually decrease to room temperature after passing through the temperature of 600C to 600C.

  In the present embodiment, as the heating device, a heating element (for example, a filament) is placed in a quartz cylinder and filled with silicon carbide in any of the pretreatment unit 10, the formation unit 20, and the posttreatment unit 30. A so-called quartz tube heater is used in which a plurality of such are arranged in the moving direction of the substrate 2 and connected to a power supply device.

  Furthermore, the temperature of the decompression chamber 5 may be kept constant by applying cold air to the decompression chamber 5 from the outside or providing a cooling water pipe on the outer periphery of the decompression chamber 5. By such cooling, for example, the temperature of the O-ring 16 is kept constant, so that the sealing performance is maintained. As a result, the pressure in the decompression chamber 5 can be kept constant.

Hereinafter, the manufacturing method using the manufacturing apparatus 1 of the carbon nanotube 3 which concerns on Example 1 of this invention is demonstrated using FIGS. 1-3.
As shown in FIGS. 1 and 2, the substrate 2 is introduced from the feeding unit 6 into the processing space 4 in the decompression chamber 5 and moved to the winding unit 7. As shown in FIG. 3, in the pretreatment unit 10 of the treatment space 4, the substrate 2 having a catalyst applied to the surface of the substrate 2 in advance is introduced into the duct 14 to which the pretreatment gas G1 is supplied. When heated by the first heating device 11 to the third heating device 13, the temperature is raised in the temperature raising region X and the catalyst on the surface of the substrate 2 is atomized. Next, the substrate 2 is introduced from the pretreatment unit 10 to the formation unit 20, and is set to the first CVD temperature by the fourth heating device 25 in the first reaction space P <b> 1 of the first space partition 22 </ b> A and to the second space partition. The source gas G2 is reacted on the substrate 2 while being heated to the second CVD temperature by the fifth heating device 26 in the second reaction space P2 of the body 22B. Accordingly, the length of the carbon nanotube 3 is grown on the substrate 2 in the first reaction space P1, and the thickness of the carbon nanotube 3 is grown on the substrate 2 in the second reaction space P2. The substrate 2 is introduced from the forming unit 20 to the post-processing unit 30 and heated by the sixth heating device 31 to the eighth heating device 33, so that the carbon nanotubes 3 generated on the substrate 2 and the substrate 2 are formed. The temperature is lowered. At this time, in the forming unit 20, the source gas G4 and the like discharged from the forming unit 20 is discharged from the decompression chamber 5 through the gas exhaust pipe 28 provided below the substrate 2, particularly immediately below the heat shielding plate 27. Has been exhausted.

Thus, according to the carbon nanotube production apparatus 1 of the present invention, the first CVD temperature region A4 heated to a temperature suitable for the growth of the length of the carbon nanotube 3 and the growth of the amorphous layer of the carbon nanotube 3 are suitable. By providing the heat shielding plate 27 between the second CVD temperature region A5 heated to a predetermined temperature, heat transfer between the first CVD temperature region A4 and the second CVD temperature region A5 is prevented, and the mutual temperature regions It is possible to produce carbon nanotubes in which the raw material gas G2 is prevented from being mixed and the length of the carbon nanotubes and the thickness of the amorphous layer are precisely controlled.
[Example 2]
A second embodiment will be described with reference to FIG. The same components as those in the first embodiment are denoted by the same names and reference numerals, and the description thereof is omitted. In the first embodiment, the heat shielding plate 27 is provided between the first space partition 22A and the second space partition 22B of the forming unit 20, but in the second embodiment, the first space partition 22A is further provided. On the upstream side, more specifically on the boundary between the pre-processing unit 10 and the forming unit 20, and on the downstream side of the second space partition 22 </ b> B, more specifically on the boundary between the forming unit 20 and the post-processing unit 30. A heat shielding plate 27 was provided.

  Further, as shown in FIG. 6, an exhaust opening 40 of the duct 14 is provided in the vicinity of the heat shielding plate 27 provided at the boundary between the pretreatment unit 10 and the forming unit 20, and immediately below the heat shielding plate 27. The mixed gas exhaust port 41a and the mixed gas exhaust pipe 41 are provided. A gas exhaust port 28 a and a gas supply pipe 28 were provided immediately below the heat shielding plate 27 provided at the boundary between the forming unit 20 and the post-processing unit 30. In addition, in order to simplify the structure of the manufacturing apparatus 1, each space partition 22A, 22B is not provided with the duct part 24, respectively.

  In addition to between the first CVD temperature region A4 and the second CVD temperature region A5, the heat shielding plate 27 is also formed at the boundary between the pretreatment unit 10 and the formation unit 20 and the boundary between the formation unit 20 and the posttreatment unit 30. Are provided between the substrate 2 heated by the pre-processing unit 10 and the substrate 2 heated to the first CVD temperature, and the substrate 2 heated to the second CVD temperature and the substrate cooled by the post-processing unit 30 Heat transfer is also suppressed between the two.

  In addition, an exhaust opening 40 is provided in the duct 14, and a mixed gas exhaust port 41 a and a mixed gas exhaust pipe 41 are provided directly below the heat shielding plate 27 provided at the boundary between the pretreatment unit 10 and the forming unit 20. Thus, the mixed gas G3 can be exhausted out of the decompression chamber 5 through the heat shielding plate 27 more reliably.

  Then, by providing a gas exhaust port 28a and a gas supply pipe 28 immediately below the heat shielding plate 27 provided at the boundary between the forming unit 20 and the post-processing unit 30, the source gas G4 and the like are transferred between the heat shielding plates 27. It is possible to evacuate out of the decompression chamber 5 more reliably.

DESCRIPTION OF SYMBOLS 1 Carbon nanotube manufacturing apparatus 2 Substrate 3 Carbon nanotube 4 Processing space 5 Depressurization chamber (reaction vessel)
6 Feeding section 7 Winding section 10 Pretreatment section 11 First heating device 12 Second heating device 13 Third heating device 14 Duct X Temperature rising area A1 First temperature area A2 Second temperature area A3 Third temperature area 20 Forming section 21 Source gas supply pipe 22A 1st space partition 22B 2nd space partition P1 1st reaction space P2 2nd reaction space 23 Reaction main-body part 24 Protrusion part for substrate guidance (duct part)
25 4th heating device 26 5th heating device 27 Heat shielding plate (heat shielding member)
28 Gas exhaust pipe 29 Gas deflection part (projection part)
Y CVD temperature region A4 First CVD temperature region (fourth temperature region)
A5 2nd CVD temperature range (5th temperature range)
30 Post-processing section 31 6th heating device 32 7th heating device 33 8th heating device 40 Exhaust opening 41 Mixed gas exhaust pipe Z Temperature drop region A6 6th temperature region A7 7th temperature region A8 8th temperature region G1 Inactive Gas G2 Raw material gas G3 Mixed gas G4 Raw material gas, etc.

Claims (5)

A substrate on which a catalyst is supported and which is moved in a predetermined direction is introduced, and a carbon nanotube is grown to a predetermined length by heating the substrate surface to a first CVD temperature along the moving direction of the substrate. Using a chemical vapor deposition method, in which a 1 CVD temperature region and a second CVD region for heating the substrate surface to a second CVD temperature higher than the first CVD temperature to deposit carbon on the surface of the carbon nanotube are provided. An apparatus for producing carbon nanotubes having a reduced-pressure reaction vessel for continuously producing carbon nanotubes,
In the reaction vessel, the first CVD temperature region and the second CVD temperature region are connected to the source gas supply pipe for supplying the source gas to the substrate and cover the surface of the substrate over a predetermined range. The first space partition and the second space partition that limit the reaction space by being arranged, respectively,
A carbon nanotube manufacturing apparatus, wherein a heat shielding member is provided between the first space partition and the second space partition.   The carbon nanotube manufacturing apparatus according to claim 1, wherein the heat shielding member is made of steel coated with ceramics or silicon carbide.   The apparatus for producing carbon nanotubes according to claim 1 or 2, wherein the second CVD temperature is set to be higher by 50 to 200 degrees than the first CVD temperature.   In the reaction container, a heat shielding member is further provided on the rear side in the movement direction of the substrate with respect to the first space partition and on the front side in the movement direction of the substrate with respect to the second space partition. The carbon nanotube manufacturing apparatus according to any one of claims 1 to 3.   2. The heat shielding member is composed of a plurality of plate members, and a gas exhaust pipe for exhausting the source gas discharged from between the plate members to the outside is connected to a wall portion of the reaction vessel. The manufacturing apparatus of the carbon nanotube as described in any one of thru | or 4.

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