KR20070073396A - Reaction chamber and method used in producting carbon nano tube - Google Patents

Abstract

A reaction chamber used in production of carbon nanotubes, which can shorten a time required in the entire process, and a method for producing carbon nanotubes using the same are provided. A reaction chamber used in production of carbon nanotubes comprises: a reaction tube(120) in which the carbon nanotubes are produced; a heating part(140) for heating the reaction tube; a gas feeding pipe(184) for feeding a source gas into the reaction tube; and a heating member(186) for heating the source gas before the source gas is fed into the reaction tube. The reaction chamber further comprises synthetic substrates(10) coated with a catalyst, the synthetic substrates are provided into the reaction tube during the process proceeding, and the source gas includes at least one selected from the group consisting of acetylene, ethylene, methane, benzene, xylene, carbon monoxide and carbon dioxide. The heating member is installed on the gas feeding pipe.

Description

Reaction chambers and methods for producing carbon nanotubes used in the production of carbon nanotubes {REACTION CHAMBER AND METHOD USED IN PRODUCTING CARBON NANO TUBE}

1 is a view schematically showing a production system of carbon nanotubes to which the reaction chamber of the present invention is applied.

2 shows a cooling line for cooling an O-ring installed in a reaction chamber;

3 shows a heating member for heating a reactor;

4A is a cross-sectional view showing an example of a reaction chamber in which a support frame is installed;

4b is a sectional view showing another example of a reaction chamber in which a support frame is installed;

5 is a configuration diagram of the catalyst coating of FIG.

FIG. 6 is a plan view seen from above in a cut state along line A-A 'in FIG. 5;

7a to 7c are diagrams for explaining step by step the catalyst coating process in the catalyst coating unit;

FIG. 8 is a plan view illustrating the substrate storage part and the first transfer device of FIG. 1; FIG.

9 is a side view of the substrate storage portion.

10 is a perspective view showing a cassette of the substrate storage portion.

11 is a perspective view of the first transfer device.

12 is a view showing a cooling member for cooling the arm of FIG.

13 is a perspective view of the blade of FIG. 12;

14A-14C show various examples of protrusions formed on the blades;

FIG. 15 is a perspective view of a recovery part of FIG. 1; FIG.

16 is a plan view of the recovery part of FIG.

17 is a view for explaining a carbon nanotube recovery process in the recovery unit;

18 is a process flow diagram in a system for carbon nanotube production.

* Explanation of symbols for the main parts of the drawings *

100: reaction chamber 200: station portion

300: first transfer device 400: substrate storage unit

500: catalyst coating unit 600: recovery unit

700: second transfer device

The present invention relates to a reaction chamber used for the production of carbon nanotubes and a method for producing carbon nanotubes.

Carbon nano tubes (carbon nanotubes) is formed by combining three carbon atoms adjacent to one carbon atom to form a hexagonal ring, and the hexagonal ring is a honeycomb-shaped plane rolled to form a cylindrical or tube.

Carbon nanotubes are a material that can exhibit metallic conductivity or semiconducting conductivity depending on their structure, and thus can be widely applied in various technical fields. For example, carbon nanotubes are applicable to electrodes of electrochemical storage devices such as secondary cells, fuel cells or supercapacitors, electromagnetic shielding, field emission displays, or gas sensors.

Most of these carbon nanotubes consist of small quantities of hand-dependent production. In particular, a process of applying a catalyst to a synthetic substrate, loading / unloading a synthetic substrate into a reaction tube, and recovering carbon nanotubes from the synthetic substrate by unloading the synthetic substrate on which the carbon nanotubes are synthesized in the reaction tube It is difficult to carry out continuous process and mass production because the back is made by worker.

In general, the carbon nanotube production process is performed by supplying a source gas into a reactor provided with a synthetic substrate coated with a catalyst, and heating the reactor to a process temperature. However, since the source gas is supplied into the reaction chamber at room temperature and the process proceeds, it takes a long time for the source gas to be heated and activated in the reaction chamber.

It is an object of the present invention to provide a reaction chamber and a method for producing carbon nanotubes, which are used for producing carbon nanotubes, which can shorten the time required for the entire process.

The present invention provides a reaction chamber used for producing carbon nanotubes. The reaction chamber is made of carbon nanotubes, the reactor is heated to the process temperature during the process, the gas supply pipe for supplying the source gas into the reactor, and the source gas before the source gas is supplied into the reactor It includes a heating member for heating.

The present invention also provides a method of producing carbon nanotubes on a composite substrate by supplying a source gas into the reactor. According to the method, the source gas is supplied into the reactor in a state heated to a set temperature.

In one embodiment, the synthetic substrate is introduced into the reactor in the state where the catalyst is applied thereon, the source gas is at least one selected from the group consisting of acetylene, ethylene, methane, benzene, xylene, carbon monoxide and carbon dioxide It may include.

Hereinafter, a method of cooling a reaction chamber and a sealing member provided in the reaction chamber will be described in detail with reference to the accompanying drawings, FIGS. 1 to 18. Embodiment of the present invention may be modified in various forms, the scope of the present invention is not limited to the embodiments described below. This embodiment is provided to more completely explain the present invention to those skilled in the art. Accordingly, the shape of elements in the figures is exaggerated to emphasize clear explanation.

1 is a schematic view showing an example of a carbon nanotube production system. Referring to FIG. 1, the system 1 has a composite substrate 10, a reaction chamber 100, and a post-process chamber.

The synthetic substrate 10 is used as a base plate on which carbon nanotubes (30 in FIG. 7) are synthesized. The composite substrate 10 on which the carbon nanotubes 30 are synthesized includes a silicon wafer, an induim tin oxide (ITO) substrate, coated glass (ITO-coated glass), soda-lime glass, corning glass, alumina, and the like. This can be used. However, if the carbon nanotube 30 has sufficient rigidity for synthesizing (growing, producing), various kinds of synthetic substrates may be used in addition to the above-described substrates.

The reaction chamber 100 performs a process of generating carbon nanotubes 30 on the composite substrate 10, and the pre- and post-processing chambers are used for the composite substrate 10 loaded / unloaded from / to the reaction chamber 100. Pretreatment and post-treatment processes are carried out. The pretreatment process and the aftertreatment process include a process of applying the catalyst 20 to the substrate, a process of recovering the carbon nanotubes 30 generated on the synthetic substrate, and the like. The pre- and post-processing chamber includes a station unit 200, a first transfer device 300, a substrate storage unit 400, a catalyst coating unit 500, a recovery unit 600, and a second transfer device 700.

The station unit 200 prevents the composite substrate 10 unloaded from the reaction chamber 100 from being exposed to the atmosphere. The first transfer device 300 loads / unloads the composite substrate into / from the reaction chamber 100. The substrate storage 400 stores a composite substrate that is loaded or unloaded into / from the reaction chamber 100. The catalyst applicator 500 performs a process of applying the catalyst 20 on the synthetic substrate 10 before the synthetic substrate 10 is loaded into the reaction chamber 100. The recovery unit 600 performs a process of recovering the carbon nanotubes 30 generated on the synthetic substrate 10 unloaded from the reaction chamber 100 from the synthetic substrate 10. The second transfer device 700 transfers the synthetic substrate 10 between the substrate storage unit 400, the catalyst application unit 500, and the recovery unit 600.

According to an example, the station unit 200 is disposed side by side with the reaction chamber 100 on one side of the reaction chamber 100. The station unit 200 has a first area 240 and a second area 260. The first region 240 is disposed adjacent to the reaction chamber 100, and the substrate storage 400 is positioned in the first region 240. The second region 260 is provided in a direction opposite to the reaction chamber 100 with respect to the first region 240 and the first transfer device 300 is located. The reaction chamber 100 and the second region 260 are disposed in the same direction in the first direction 42. The first region 240 has an upper region 242 and a lower region 244. The upper region 242 is a region located on the same line as the reaction chamber 100 and the second region 260, and the lower region 244 is a second perpendicular to the first direction 42 from the upper region 244. It is an area extending in the direction 44. The first region 240 and the second region 260 are generally rectangular in shape. Due to the above structure, the station 200 has a generally '-' shape. The catalyst applicator 500, the recovery part 600, and the second transfer device 400 are positioned adjacent to the station part 200, and have a lower area based on the upper area 242 of the first area 240. It is disposed side by side in a direction parallel to the first direction 42 at a position opposite to the (244). The second transfer device 400 is disposed at a position opposite to the first area 240 of the station unit 200. In addition, the second transfer device 400 is located between the catalyst applicator 500 and the recovery part 600. The shape of the station unit 200 and the arrangement of the station unit 200, the first transfer device 300, the second transfer device 400, the catalyst applying unit 500, and the recovery unit 600 may vary. Can be changed.

Next, each component of the system of the present invention will be described in detail.

Referring to FIG. 1, the reaction chamber 100 includes a reaction tube 120, first and second flanges 132 and 134, and a heating member 140. , A cooling member 150, and a boat 160. The reactor 120 is made of a heat resistant material such as quartz or graphite. Reactor 120 may be provided in a substantially cylindrical shape. During the process, the reactor 120 may be maintained at approximately 500-1100 degrees Celsius by the heating unit 140.

The first flange 132 of a disc shape is coupled to the front end of the reactor 120, the second flange 134 is coupled to the rear end of the reactor (120). The first flange 132 has a generally disc shape. A gas supply member 180 for supplying a source gas into the reactor 120 is connected to the first flange 132. The gas supply member 180 has a gas supply source 182, a gas supply pipe 184, and a heating member 186. The gas supply pipe 184 is coupled to the first flange 132 to supply source gas from the gas supply source 182 into the reactor 120. Here, at least one selected from the group consisting of acetylene, ethylene, methane, benzene, xylene, carbon monoxide and carbon dioxide may be used as the source gas. The gas supply pipe 184 is provided with a valve 184a for opening and closing the inner passage or adjusting the flow rate of the source gas flowing therein. The heating member 186 is installed in the gas supply pipe 184. The heating member 186 heats the source gas to a set temperature before the source gas is supplied into the reactor 120. This shortens the time required for the source gas to be activated in the reactor 120 to reduce the total time required for the process. The source gas is activated by pyrolysis and carbon nanotubes are generated by reacting with the catalyst applied on the synthetic substrate 10. The second flange 134 has an annular ring shape, and the second flange is coupled to an exhaust line 189 for discharging residual gas in the reactor 120 after the reaction.

Sealing members 132a and 134a for sealing the inside of the reactor 120 from the outside are provided on the contact surface of the first flange 132 and the reactor 120 and the contact surface of the second flange 134 and the reaction chamber 120. Is installed. O-rings may be used as the sealing members 132a and 134a. The sealing member is cooled by the cooling member. The cooling member has a cooling line 152, a cooling water supply pipe 156, and a sensor 158. The cooling line 152 is formed in each of the inside of the first flange 132 and the second flange 134, the cooling fluid flows. Cooling water is used as the cooling fluid. Alternatively, inert gas may be used as the cooling fluid. Cooling water flowing through the cooling line 152 cools the sealing members 132a and 134a to prevent the sealing members 132a and 134a from being damaged by heat in the reactor.

Referring to Figure 2, the cooling line 152 is coupled to the cooling water supply pipe 156 and the cooling water recovery pipe (not shown). The cooling water supply pipe 156 is provided with a valve 156a for opening and closing the inner passage or adjusting the flow rate of the cooling water flowing therein. In addition, the cooling water supply pipe 156 is provided with a sensor 158 that measures the flow rate or temperature of the cooling water flowing therein, and the signal measured by the sensor 158 is transmitted to the controller 159 that controls the entire facility. . The controller 159 analyzes the signal transmitted from the sensor 158 and stops the system or notifies the operator through a display or a warning sound when the flow rate or temperature of the coolant is out of the set range for a set time. This allows the process to continue continuously within a predetermined time before the sealing members 132a and 134a are damaged even though the coolant does not flow at a temporarily set flow rate or set temperature through the coolant supply pipe 156. The set time described above is determined in consideration of the time taken until the sealing members 132a and 134a are affected when the cooling water is not continuously supplied smoothly.

The heating unit 140 heats the inside of the reactor 120 to a process temperature. The heating unit 140 is preferably installed to surround the outer wall of the reactor (120). As a method of heating the reactor 120, a method using a heating coil or a method using a heating lamp may be used.

3 is a view showing a reaction chamber 100 in which an example of the heating unit 140 of the present invention is shown. For ease of explanation, the regions adjacent to the first flange 132 and the second flange 134 in the reactor 120 are called edge regions 122a and 122b, and between edge regions 122a and 122b. The region located at is called the central region 124. When the entire region of the reactor 120 is heated by one heater, the edge regions 122a and 122b have a lower temperature than the central region 124. This is because the edge regions 122a and 122b of the reactor 120 are affected by the cooling line 152 installed in the flanges 132 and 134. Therefore, in order to process the composite substrate 10 at the same temperature state, the synthesis substrates have to be provided only in the central region 124 of the reactor, and thus the length of the reactor 120 becomes long.

In order to solve the above-described problem, referring to FIG. 3, the heating unit 140 has an edge heater 142, a central heater 144, and a heater controller 146. The edge heater 142 heats the edge regions 122a and 122b of the reactor 120, and the central heater 144 heats the central region 124 of the reactor 120. The heater controller 146 independently controls the central heater 144 and the edge heater 142, respectively. The edge heater 142 heats the reactor 120 to a higher temperature than the central heater 144 so that the process temperature is provided uniformly throughout the reactor 120. The edge heater 142 of the reactor 120 adjacent to the first heater 142a and the second flange 134 heats the edge region 122a of the reactor 120 adjacent to the first flange 132. It has a second heater 142b that heats the edge region 122b. This is useful when the temperature between the edge regions 122a and 122b of the reactor 120 is different. In this case, the heater controller 146 independently controls the first heater 142a and the second heater 142b.

Only one boat 160 may be provided in the reactor 120, or a plurality of boats 160 may be provided. The boat 160 is provided with a sufficiently large size so that a plurality of synthetic substrates 10 may be placed in one boat 160 along the longitudinal direction of the reactor 120 (the first direction 42 described above). . Optionally, the boat 160 may have a size and a structure capable of supporting the plurality of composite substrates 10 in the vertical direction and the longitudinal direction, respectively. According to an example, the boats 160 have a size and a structure capable of supporting the composite substrate 10 two vertically and two longitudinally. The boats 160 may be fixedly installed in the reactor 120 or may be provided to be loaded / unloaded.

In addition, the boat 160 may be provided in a size capable of supporting one composite substrate 10. In this case, one or more boats 160 may be provided. When a plurality of boats 160 are provided, a plurality of boats 160 may be disposed along the longitudinal direction of the reactor 120 (first direction 42 described above), or optionally perpendicular to the first direction 42. It can be stacked in one vertical direction.

Optionally, a support frame 160 ′ in which the composite substrate 10 is placed may be installed in the reactor 120 instead of the boat 160. 4A and 4B are cross-sectional views of the reactor 120 in which a support frame 160 'is installed therein, respectively. Referring to FIG. 4A, the support frame 160 ′ is provided with two frames 162 and 164 provided to protrude from the inner wall of the reactor 120 into the reactor 120 along the longitudinal direction of the reactor 120. ) The first frame 162 and the second frame 164 are disposed to face each other, and support the edges of the composite substrate 10, respectively. In order to stably support the composite substrate 10, guide ends 162a and 164a protruding upward are provided at the ends of the first frame 162 and the second frame 164, and the edge region of the composite substrate 10 is provided. A locking projection 10a protruding downward to be caught by the guide protrusions 162a and 164a may be provided.

The first frame 162 and the second frame 164 may be provided sufficiently long so that the plurality of composite substrates 10 are placed along the length of the reactor 120 in one support frame 160 ′. . The support frame 160 ′ may be provided in plural so as to be spaced apart by a predetermined distance up and down. When the reactor 120 is provided in a circular cross section, two support frames 160 ′ may be installed vertically. Optionally, by providing a wider width of the support frame 160 'toward the center, three or more support frames may be provided. Alternatively, as illustrated in FIG. 4B, the reactor 140a may be provided to have a rectangular cross section, and the support frame 160 ′ may be provided to be stacked up and down.

In the present embodiment, a reaction chamber 100 having a structure to which pyrolysis of hydrocarbon is applied by pyrolyzing hydrocarbons to produce carbon nanotubes 30 is described as an example, but this is only one example. In the system 100 of the present invention, a reaction chamber having a structure to which various generation methods such as laser deposition, plasma chemical vapor deposition, thermochemical vapor deposition, flame synthesis, and electric discharge is applied may be used.

Referring back to FIG. 1, the station unit 200 includes a chamber 200a isolated from the outside. A first gate valve 222 is installed between the station unit 200 and the reaction chamber 100 to open and close a passage through which the composite substrate 10 moves, and the station unit 200 and the second transfer device 700 are provided therebetween. The second gate valve 224, which opens and closes the passage through which the composite substrate 10 moves between them, is installed between them.

The station unit 200 is provided with a gas supply member 280 for supplying an inert gas such as nitrogen, argon, and the like into the station unit 200. The inert gas removes air (particularly oxygen) inside the station unit 200 and maintains an inert gas atmosphere inside the station unit 200. This prevents the hot carbon nanotubes 30 produced on the synthetic substrate 10 from contacting with oxygen when the composite substrate 10 is unloaded from the reaction chamber 100 in the station unit 200. . The gas supply member 280 is preferably provided in the first region 240 in which the substrate storage unit 400 is installed.

When the first gate valve 222 is disposed adjacent to the reaction chamber 100, the first gate valve 222 may be damaged by radiant heat in the reaction chamber 100. In order to prevent this, the length of the reaction chamber 100 may be sufficiently long so that the distance between the heating unit 140 and the first gate valve 222 is sufficiently maintained. In this case, however, the system 1 becomes larger due to the increase in the length of the reaction chamber 100.

According to the present embodiment, the heat between the first gate valve 222 and the reaction chamber 100 to prevent the system 1 from being enlarged and to prevent the first gate valve 222 from being damaged by radiant heat. The blocking member 190 is installed. The heat blocking member 190 blocks radiant heat transmitted from the reaction chamber 100 to the first gate valve 222. The heat blocking member 190 has a blocking plate 192 of a material having a low thermal conductivity, such as alumina, and a driver 194 driving the same. Optionally, the blocking plate 192 may be made of a general metal material. In this case, a cooling member (not shown) may be provided to prevent the blocking plate 192 from being damaged by heat in the reactor 120 and to cool the blocking plate 192 in order to increase the blocking efficiency.

The blocking plate 190 is positioned in front of the first gate valve 222 while the first gate valve 222 is closed to prevent the first gate valve 222 from being damaged by heat, and the first gate valve ( When the 222 is open, the 222 is moved to a position that does not obstruct the movement path of the composite substrate 10.

Before the synthetic substrate 10 is loaded into the reaction chamber 160, the catalyst 20 (metal film) is applied to the upper surface of the reaction chamber 160 in the catalyst applying unit 500. FIG. 5 is a configuration diagram of the catalyst applicator 500 shown in FIG. 1, and FIG. 6 is a plan view of the catalyst applicator 500 viewed from the top after cutting along the line A-A 'of FIG.

5 and 6, the catalyst applicator 500 includes a catalyst storage tank (hopper) 520, a metering supply 560, a brush unit 580, and a stage 590. During the process, the synthetic substrate 10 is placed on the stage 590. The catalyst storage tank 520 is disposed above the stage 590 and has a discharge port 526a for supplying a predetermined amount of the catalyst 20 to the upper surface of the synthetic substrate 10. The brush unit 580 spreads the catalyst 20 supplied to the upper surface of the synthetic substrate 10 to a uniform thickness on the upper surface of the synthetic substrate 10.

The stage 590 is installed to protrude inwardly to the side plates 592 and the respective side plates 592 which are spaced apart from each other so as to face each other so that the composite substrate 10 is positioned so as to face the edge region of the composite substrate 10. It has a plurality of support protrusions 594 for supporting. A plurality of support protrusions 594 may be installed on each side plate 592.

The brush unit 580 includes a guide rail 584, an application brush 587, and a movable body 588. The guide rails 584 are installed in the longitudinal direction on both sides of the stage 590 on which the composite substrate 10 is placed. The movable body 588 is movably installed on the guide rail 584, and the movable body 588 is linearly moved by a known linear movement driver 586 such as a linear motor drive method, a cylinder drive method, and a motor drive method. The coating brush 587 is positioned above the stage 590, and spreads the catalyst 20 in a uniform thickness on the entire surface of the synthetic substrate 10. Both ends of the coating brush 587 are connected to the movable body 588 and are moved in a slide manner together with the movable body 588. The coating brush 587 may be provided in a plate shape of a metal or nonmetal material having a specific inclined surface with respect to the traveling direction.

The coating brush 587 is moved up and down by the vertical mover 589 so that the coating brush 587 can be adjusted on the movable body 588. This makes it possible to adjust the coating thickness of the catalyst 20 applied to the upper surface of the synthetic substrate 10. The vertical mover 589 includes an upper plate 589a fixedly coupled to the upper end of the movable body 588, a lower plate 589b fixedly coupled to the lower end of the movable body 588 to face the upper plate 589a, and an upper plate 589a and the lower plate 589b. ) Has a guide shaft 589c disposed vertically. The guide shaft 589c is linearly moved up and down along the guide shaft 589c by a driver (not shown), and a bracket 589d to which the application brush 587 is fixedly mounted is provided.

The catalyst storage tank 520 supplies the catalyst 20 stored therein onto the synthetic substrate 10. Catalyst storage tank 520 has an upper surface 522, a side 524, and a lower surface 526 with an outlet 526a formed therein. Side 524 has a generally vertical upper portion 524a, an intermediate side portion 524b extending downwardly therefrom and inclined inwardly downward, and a lower portion 524c extending generally vertically downwardly therefrom. . Due to the above-described structure, a large amount of catalyst 20 is stored in the space provided by the upper portion 524a in a region corresponding to the same height as compared to the space provided by the lower portion 524c. Due to the shape of the intermediate side portion 524b described above, the catalyst 20 in the space provided by the upper portion 524a is smoothly supplied to the space provided by the lower portion 524c.

The catalyst storage tank 520 is provided with a quantitative supply unit 560 for supplying the catalyst 20 by the amount set to the upper surface of the synthetic substrate 10. The metered feeder 560 has an upper barrier plate 564 and a lower barrier plate 562 that can provide a quantitative space 568 in which a set amount of catalyst 20 can be contained. The upper blocking plate 564 and the lower blocking plate 562 are provided at the lower side 524c. The metering space 568 is located above the outlet 526a of the catalyst storage tank 520, the upper blocking plate 564 is provided to the top of the metering space 568, the lower blocking plate 562 is the metering space ( 568). The upper block plate 564 and the lower block plate 562 are operated by driving means such as the cylinder 566. When the upper block 564 is closed while the lower block 562 is closed, the quantitative space 568 filled with the amount of catalyst 20 set between the lower block 562 and the upper block 564 is filled. Is provided again.

When the lower blocking plate 562 is opened, the catalyst 20 contained in the metering space 568 is supplied to the upper surface of the synthetic substrate 10 through the discharge port 526a. On the other hand, an agitator 540 for stirring the catalyst 20 is installed in the middle side portion 524b of the catalyst storage tank 520. The stirring blade 542 of the stirrer 540 rotates before the catalyst 20 is supplied to the quantitative space to remove the empty space inside the catalyst storage tank 520 and at the same time, the catalyst 20 naturally moves to the quantitative space 568. Has a role of inducing supply.

7A to 7C are diagrams for explaining the catalyst application process in the catalyst applying unit 500 step by step. 7A to 7C, when the composite substrate 10 is placed on the stage 590 by the second transfer device 700, the lower blocking plate 562 is operated by the cylinder 566 to move laterally. While moving, the lower portion of the quantitative space 568 is opened, and the set amount of the catalyst 20 contained in the quantitative space 568 falls to the upper surface of the synthetic substrate 10 (FIG. 7A). Catalyst 20 piled up on the upper surface of the synthetic substrate 10 is applied to the entire surface of the synthetic substrate 10 by a brush unit 580 in a uniform thickness (Figs. 7b and 7c). That is, the application brush 587 uniformly applies the catalyst 20 to the entire surface of the synthetic substrate 10 while slidingly moving from one end to the other end of the synthetic substrate 10 together with the moving body 588. In this case, a vibrator (not shown) may be additionally provided to apply a fine vibration to the application brush 587 or the synthetic substrate 10 for uniform application of the catalyst 20.

Here, the catalyst 20 includes, for example, transition metals such as iron, platinum, cobalt, nickel, and yttrium, and alloys thereof, and magnesium oxide (Mg0), aluminum oxide (Al ₂ 0 ₃ ), and silicon oxide (Si0 ₂ ). It may be in the form of a powder mixed with a porous material. Or it may be a liquid catalyst 20 containing such a material. When the catalyst 20 is in a liquid phase, it may include a catalyst storage tank, a supply line, a pump for quantitative supply installed on the supply line, and a supply nozzle for supplying the liquid catalyst 20 to the upper surface of the synthetic substrate.

In the above-described example, it has been described that the catalyst 20 is uniformly coated on the synthetic substrate 10 while the application brush 587 moves. Alternatively, the application brush 587 may be fixed and the stage 590 may be moved. However, in order to reduce the space of the catalyst coating unit 500, it is preferable that the coating brush 587 is moved as in the above-described example.

In addition, in the above-described example, the catalyst 20 is applied on the synthetic substrate 10 separately from the catalyst applying unit 500, and in the reaction chamber 100 on the synthetic substrate 10 to which the catalyst 20 is applied. It has been described as producing the carbon nanotubes 30. Alternatively, however, the catalyst applicator may be removed, and the catalyst gas and the source gas may be supplied in the reaction chamber to apply the catalyst and generate carbon nanotubes on the synthetic substrate.

8 is a plan view of the substrate storage unit 400 and the first transfer device 300, Figure 9 is a side view of the substrate storage unit 400. 8 and 9, the substrate storage unit 400 may include a cassette 420, a vertical rails 442, a horizontal rail 444, and moving frames 446 for storing the composite substrate 10. Have The vertical rails 442 are disposed at corners of the first region 240, respectively. The vertical rails 442 have a long rod shape in the vertical direction and guide the vertical movement of the moving frame 446. Each vertical rail 442 is coupled with a bracket 448 that is moved up and down by a vertical drive (not shown) along the vertical rail 442. Each moving frame 446 is provided long along the first direction 42 and is disposed to face each other. The moving frame 446 is fixedly coupled to the bracket 448 and linearly moves up and down along the vertical rail 442 together with the bracket 448. Both ends of each moving frame 446 are fixedly installed on brackets 448 facing each other in the first direction 42, and the moving frames 446 are moved up and down together with the bracket 448. The horizontal rail 444 is fixedly installed on the moving frame 446. Each horizontal rail 444 is provided long along the second direction 44, and the horizontal rails 444 are disposed to face each other. The horizontal rail 444 is provided over the first area 240, and the cassette 420 is mounted on the horizontal rail 444 to be movable in the second direction 44 along the horizontal rail 444.

As shown in FIG. 8, the cassette 420 is moved horizontally between the standby position indicated by the dotted line and the loading / unloading position X2 indicated by the solid line (just before the first gate valve 222 connected to the reaction chamber). do. The standby position X1 is a position in the lower region 244 of the first region 240 and the loading / unloading position X2 is a position in the upper region 242 of the first region 240. The cassette 420 is loaded / unloaded position (X2) when loading / unloading the composite substrate 10 into / from the reaction chamber 100 and when transferring the composite substrate 10 by the second transfer device 700. Is moved to, and when waiting to lower the temperature of the composite substrate 10 is moved to the standby position (X1).

10 is a perspective view of the cassette 420. The composite substrate 10 to be loaded into the reaction chamber 100 and the composite substrates 10 unloaded from the reaction chamber 100 are stored in the cassette 420. Referring to FIG. 8, the cassette 420 has supports 422, an upper plate 424 and a lower plate 426, and vertical axes 428. The upper plate 424 and the lower plate 426 are generally provided in a rectangular shape and are disposed to face each other up and down. The vertical axes 428 connect four corner portions of the upper plate 424 and the lower plate 426 facing each other. Support portions 422 supporting the composite substrate 10 are installed on the vertical axis 428 so that the composite substrate 10 is stacked and stored in the cassette 420. Each support 422 has four support blocks 423 for supporting the edge of the composite substrate 10. The supports 422 are grouped into two groups. The supports 422a (hereinafter referred to as the first support) belonging to the first group support the composite substrates 10 to be loaded into the reaction chamber 100, and the supports 422b (hereinafter referred to as the second support) belonging to the second group react. The unloaded composite substrates 10 are supported from the chamber 100. In an example, four first supporting parts 422a and two second supporting parts 422b are provided, and the first supporting parts 422a are provided to be positioned above the second supporting parts 422b.

The vertical space between the second supports 422b is wider than the vertical space between the first supports 422a. Due to the structure described above, the total height of the cassette 420 is reduced while the carbon nanotubes 30 formed on the upper surface of the unloaded synthetic substrate 10 from the reaction chamber 100 do not come into contact with the adjacent synthetic substrate 10. It can provide enough space.

The composite substrates 10 stored in the first support portions 422 of the cassette 420 are loaded into the reaction chamber 100 by the first transfer device 300. Four synthetic substrates 10 are placed in the boat 160 of the reaction chamber 100. The first transfer device 300 sequentially loads and unloads the composite substrate into / from the reaction chamber 100 one by one.

When the loading of the synthetic substrates 10 is completed, a process for generating the carbon nanotubes 30 is performed in the reaction chamber 100. During the process in the reaction chamber 100, another four composite substrates 10 are waiting for the first support portion 422 of the cassette 420 after applying the catalyst in the catalyst coating portion 500.

When the production process of the carbon nanotubes 30 in the reaction chamber 100 is completed, the synthetic substrate 10 in a high temperature state is unloaded from the reaction chamber 100 by the first transfer device 300 to draw the cassette 420. The second support portion 422b is stored in the high temperature synthetic substrate 10 undergoes a cooling process for a predetermined time in the second support portion 422b. Cooling is achieved by natural cooling. Optionally, forced cooling may be achieved using cooling means such as cooling water.

On the other hand, when the composite substrates 10 that have completed the production of the carbon nanotubes 30 are quickly withdrawn from the reaction chamber 100 (without waiting for the temperature to drop to a certain temperature), the first support part 422a of the cassette 420 is atmospheric. Four synthetic substrates (synthetic substrates waiting to be produced for the carbon nanotubes 30) 10 are loaded into the reaction chamber 100. As such, in the reaction chamber 100, the temperature increase process for increasing the process temperature of the reactor 120 may be omitted by rapidly loading the composite substrates 10 while the temperature of the reactor 120 maintains the process temperature.

The composite substrates 10 on which the carbon nanotubes 30 are formed are waited at the second support portions 422b of the cassette 420 until they fall below a predetermined temperature. The cassette 420 on which the synthetic substrates 10 are located is located inside the station unit 200. Since the inside of the station part 200 is filled with inert gas, the synthetic substrates 10 waiting in the cassette 420 are not in contact with outside air (especially oxygen). For example, the synthesis substrate 10 that has been processed in the reaction chamber 100 may not be in a state where the temperature falls below a predetermined temperature. However, when the synthesis substrate 10 is exposed to the atmosphere at room temperature in a high temperature state, the surface of the synthesis substrate 10 The produced carbon nanotubes 30 react with oxygen in the atmosphere to cause deformation. In the present invention, in order to prevent such a problem, the unloaded synthetic substrate 10 in the reaction chamber 100 is provided with a station part 200 filled with an inert gas as described above so as not to come into contact with oxygen.

Meanwhile, the composite substrates 10 waited for a predetermined time in the second support parts 422b of the cassette 420 are transferred to the recovery part 600 by the second transfer device 700 through the second gate valve 224. Transferred. After the carbon nanotubes 30 have been recovered from the recovery part 600, the synthetic substrate 10 is coated with the catalyst 20 from the catalyst applicator 500, and again, the first support part 422a of the cassette 420. ) Is stored.

As described above, in the system of the present invention, a total of eight synthetic substrates are divided into two groups, and thus the carbon nanotube 30 synthesis process is continuously performed in the reaction chamber alternately, and thus the throughput can be expected to be improved, thereby allowing mass production. There is this.

11 is a perspective view of the first transfer device. Referring to FIG. 11, the first transfer apparatus 300 includes an arm 320, a blade 340, and a driver 360 that support the composite substrate 10. The driver 360 has vertical rails 362, horizontal rails 364, moving frames 366, and moving blocks 368. The vertical rails 362 are disposed at corners of the second region 260, respectively. The vertical rails 362 have a long rod shape in the vertical direction and guide the vertical movement of the moving frame 366. Each vertical rail 362 is coupled with a bracket 365 which is moved up and down by a vertical drive (not shown) along the vertical rail 362. Each moving frame 366 is elongated along the second direction 44 and is disposed to face each other. The moving frame 366 is fixedly coupled to the bracket 365 and linearly moved up and down along the vertical rail 362 together with the bracket 365. Both ends of each of the moving frames 366 are fixed to brackets 365 facing each other in the second direction 44, and the moving frames 366 are moved up and down together with the brackets 365. Horizontal rails 364 are fixedly installed on the moving frames 366. Each horizontal rail 364 is provided elongated in the first direction 42. The horizontal rail 364 is provided over the entire area of the second region 260, and the movable block 368 is mounted on the horizontal rail 364 to be movable in the second direction 44 along the horizontal rail 364. . The movable block 368 is provided with an arm 320 that is installed to extend along the first direction 42, and a blade 340 for supporting the composite substrate 10 is mounted at the end of the arm 320.

In addition, the first transfer device 300 is provided with a cooling member 330 for cooling the arm (320). When the length of the reactor 120 is long, a long arm 320 is used for loading / unloading the composite substrate 10. However, since the inside of the reactor 120 is maintained at a very high temperature, the arm 320 is elongated by heat as it enters the reactor 120, and thus, the composite substrate 10 is located at a position deviated from the set position on the blade 340. Is seated. This is because the composite substrate 10 may be separated from the blade 340 while the composite substrate 10 is moved by the blade 340, or the composite substrate 10 may be out of position and placed in the cassette 420.

The cooling member 330 prevents the arm 320 from being damaged by heat when the arm 320 is introduced into the reactor 120. 12 shows a first transfer device 300 provided with a cooling member 330. Referring to FIG. 12, the cooling member 330 has a cooling line 332, a cooling water supply pipe 334, and a cooling water recovery pipe 336. Cooling line 332 is provided in arm 320 along the longitudinal direction of arm 320. One end of the cooling line 332 is connected to the cooling water supply pipe 334 for supplying the cooling water to the cooling line 332 and the other end is connected to the cooling water recovery pipe 336 for recovering the cooling water from the cooling line 332. The cooling water supply pipe 334 is provided with a valve 334a for opening and closing the inner passage and adjusting the flow rate of the cooling water.

The synthetic substrate 10 having completed the process is heated to a high temperature. When the blade 340 waiting at the station unit 200 contacts the high temperature composite substrate 10 to unload it from the reactor 120, the composite substrate 10 may be damaged by a sudden temperature change. Therefore, the contact area between the blade 340 and the composite substrate 10 is preferably minimized.

FIG. 13 is a perspective view of the blade 340 of FIG. 11. Referring to FIG. 13, the blade 340 has a plate 342 having a flat upper surface and protrusions 344 protruding upward therefrom and contacting the composite substrate 10. Since the plate 342 is introduced into the reactor 120 for loading / unloading of the synthetic substrate 10 during the process, the plate 342 is made of a material having excellent heat resistance. The protrusions are intended to reduce the contact area between the blade and the composite substrate, and are provided uniformly in the corner region or the entire region of the plate.

As shown in FIGS. 14A and 14B, the protrusions 344a are each formed in the shape of a hemisphere, a polygonal pyramid, or the like, and are in point contact with the composite substrate 10, or as shown in FIG. 14C. It is formed in a polygonal column shape and is in surface contact with the composite substrate 10.

The shape of the protrusion 344 may be variously modified and changed, and is not limited due to the above-described embodiments. The protrusion 344 is for preventing the synthetic substrate 10 from being damaged by a sudden temperature change, and the shape, number, and arrangement of the protrusion 344 may be variously applied.

The composite substrates 10 that have been cooled for a predetermined time in the second support parts 444 of the cassette 420 are transferred to the recovery part 600 by the second transfer device 700 through the second gate valve 224. Transferred.

15 and 16 are respectively a perspective view and a plan view of the recovery portion, Figure 17 is a view for explaining the carbon nanotube 30 recovery process in the recovery portion.

15 to 17, the recovery unit 600 has a stage 620 on which the composite substrate 10 is placed. At the bottom of the stage 620 is a recovery container 660 in which the carbon nanotubes 30 recovered from the synthetic substrate 10 are stored. In addition, the stage 620 is provided with a recovery unit 640 for sweeping the carbon nanotubes 30 into the recovery container 660 on the upper surface of the synthetic substrate 10. The recovery unit 640 is provided with a guide rail 646 installed in the longitudinal direction of the composite substrate 10. The movable body 644 is installed in the guide rail 646, and the recovery brush 642 is installed in the movable body 644. The recovery brush 642 sweeps the carbon nanotubes 30 on the upper surface of the synthetic substrate 10 into the recovery container 660 while slidingly moving in one direction from one side of the synthetic substrate 10. The recovery brush 642 may be adjustable in height in the movable body 644.

In the above-described example, it has been described that the catalyst 20 is swept out on the synthetic substrate 10 while the recovery brush 642 is moved. Alternatively, however, the recovery brush 642 can be fixed and the stage can be moved. However, in order to reduce the space of the recovery unit 600, it is preferable that the recovery brush 642 is moved as in the above-described example.

The synthetic substrate 10 from which the carbon nanotubes 30 have been recovered is provided to the catalyst applying unit 500 by the second transfer device 700, and then passes through the aforementioned catalyst coating process. It is accommodated in 422a.

Referring to Figure 18, the process proceeds in the system for mass production of carbon nanotubes 30 having such a configuration is a catalyst coating step (S110), carbon nanotubes 30 production step (S120), cooling (wait) It has a step (S130), a recovery step (S140). In the catalyst application step S110, when the catalyst 20 corresponding to a single coating amount is supplied from the catalyst storage tank 520 to the upper surface of the synthetic substrate 10, the application brush 587 of the brush unit 580 is moved. The catalyst 20 is evenly distributed over the synthetic substrate 10. The composite substrate 10 having the catalyst 20 coated thereon is accommodated in the cassette 420 of the substrate storage unit 400 installed in the station unit 200 by the second transfer device 700. The composite substrate 10 accommodated in the first supporting portion 422a of the cassette 420 is formed by the first transfer device 300 immediately after the composite substrate 10 which has been processed from the reaction chamber 100 is unloaded. Loaded into boat 160 of 100. When the loading of the synthetic substrate 10 is completed, a process for generating the carbon nanotubes 30 is performed in the reaction chamber 100 (S120). Meanwhile, the synthetic substrates 10 unloaded from the reaction chamber 100 are accommodated in the second support part 422b of the cassette 420 and then cooled for a predetermined time (S130). After a certain time, the synthetic substrate 10 is drawn out of the station unit 400 and moved to the recovery unit 600 (S140). After the recovery of the carbon nanotubes 30 from the recovery unit 600, the synthetic substrate 10 is moved to the catalyst applying unit 500 again and is stored in the first support part 422a of the cassette 420 after the catalyst application. After completing the process in the reaction chamber 100, the synthetic substrate 10 is stored in the second support portion 422b of the cassette 420, and then repeats the above-described process.

According to the present invention, since the source gas is heated to a constant temperature and then introduced into the reactor, the time required for the process in the reactor can be shortened.

In addition, the present invention can automate the production process of carbon nanotubes.

In addition, according to the present invention, carbon nanotubes can be produced in large quantities.

In addition, according to the present invention, since the process temperature of the reaction chamber can be maintained continuously, the carbon nanotube synthesis of the composite substrate can be continuously performed, thereby improving the facility operation rate.

In addition, the present invention can ensure the process reliability through accurate and reliable automatic catalyst supply.

In addition, the present invention can be accurately calculated through the automatic recovery of carbon nanotubes.

Claims (5)

In the reaction chamber used to produce carbon nanotubes, A reactor for producing carbon nanotubes; A heating unit for heating the reactor; A gas supply pipe for supplying a source gas into the reactor, and And a heating member for heating the source gas before the source gas is supplied into the reactor. The method of claim 1, The reaction chamber further comprises a synthetic substrate coated with a catalyst, the synthetic substrate is provided in the reactor during the process, Wherein the source gas comprises at least one selected from the group consisting of acetylene, ethylene, methane, benzene, xylene, carbon monoxide and carbon dioxide. The method according to claim 1 or 2, The heating member is installed on the gas supply pipe. A method of producing carbon nanotubes on a composite substrate by supplying a source gas into the reactor, And the source gas is supplied into the reactor in a state of being heated to a set temperature. The method of claim 4, wherein The synthetic substrate is introduced into the reactor in the state where the catalyst is applied, The source gas is carbon nanotubes production method comprising at least one selected from the group consisting of acetylene, ethylene, methane, benzene, xylene, carbon monoxide and carbon dioxide.

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