TWI360584B - Apparatus for fabrication of carbon nanotubes - Google Patents

Description

1360584 _ 100 years U month 08 day shuttle replacement page six, invention description: [Technology of the invention] [0001] The present invention relates to a sputum type carbon nanotube preparation device, especially a thermal chemical vapor deposition nano Pipe breaking preparation device. [Prior Art] [0002] Nano carbon tube is a new type of one-dimensional nano carbon material, by the researcher

Iijima Chengo (S. Π jha) was first discovered in 丨 991. The carbon nanotubes have excellent properties such as high tensile strength and high thermal stability, and the carbon nanotubes can exhibit metallic or semiconducting properties as the carbon nanotube spirals. Since the carbon nanotubes have an ideal one-dimensional structure and excellent properties in fields such as force, electricity, and heat, they have shown broad application prospects in the fields of materials science, chemistry, and physics. Therefore, the realization of controlled growth of carbon nanotubes is the key to pushing carbon nanotubes into applications. [0003] At present, there are three main methods for preparing relatively mature carbon nanotubes: electrical isolation, electrical discharge, laser ablation, and chemical vapor deposition. Its A' vapor deposition (CVD) method has been widely studied and applied due to its simple process, low cost, and mass growth. [0004] 094137885 The chemical vapor deposition method uses a carbon-containing gas as a carbon source gas to grow a multi-wall or single-walled carbon nanotube on a stone substrate of Shi Xi or # , , 馇 / 图. However, as shown by the younger brother, the conventional thermal CVD carbon nanotube preparation apparatus 1 includes a reaction furnace 17 which includes an air inlet 13 and an air outlet 15 opposite to the air inlet 13. In the preparation process of the carbon nanotubes, the substrate 2 on which the catalyst layer 22 is formed on the surface of the crucible is loaded in the reaction furnace I7. The reaction gas is the gas with the carbon nanotubes 1〇〇3412〇86-〇11. The mouth 13 is blown horizontally to the air outlet 15 Form No. A0101 1360584 100 years. On November 08, the growth direction of the shuttle replacement page is vertical. For the fine carbon nanotubes, even if the flow rate of the reaction gas is slow, it will cause poor collimation of the finally grown carbon nanotubes. [0005] In view of this, a collimable neat can be provided. The preparation device for the carbon nanotubes is really necessary. SUMMARY OF THE INVENTION [0006] Hereinafter, an embodiment of a carbon nanotube preparation apparatus which can realize collimated growth of a carbon nanotube can be described by way of examples.

[0007] A carbon nanotube preparation apparatus for introducing a reaction gas for carbon nanotube growth to prepare a carbon nanotube, which comprises a reaction furnace, a flow guiding chamber, and an air delivery tube. The reaction furnace includes a first air inlet and an air outlet; the flow guiding chamber is disposed in the reaction furnace, and includes a top portion and a second air inlet, the top portion is provided with a plurality of openings; the gas conveying tube The first port is sealed with the first air inlet, the second port is sealed with the second air inlet, and the reaction gas for the carbon nanotube growth is located at the first The second port on one side of the air inlet enters the gas delivery tube, and is introduced into the flow guiding cavity via the second port, and the reaction gas is guided by the guiding cavity to be perpendicular to the top surface. From the plurality of openings, the reactor is entered. [0008] Compared to the prior art, the carbon nanotube preparation device changes the flow direction of the reaction gas required for the growth of the carbon nanotube by using a flow guiding cavity, and the flow direction is perpendicular to the nano carbon. The tube growth direction is parallel to the growth direction of the carbon nanotubes, and this arrangement can provide better collimation of the carbon nanotubes. 094137885 Form No. A0101 Page 5 of 14 1003412086-0 1360584 Revised replacement page of November 08, 100 [Embodiment] The embodiments of the present invention will be further described in detail below with reference to the accompanying drawings. [0010] Referring to the second figure, the carbon nanotube preparation apparatus 10 provided in this embodiment includes a reaction furnace 20, a flow guiding chamber 30, a gas delivery tube 40, and a heating device 12. [0011] The reaction furnace 20 includes a first intake port 22 and an air outlet port 24. [0012] The flow guiding cavity 30 is disposed in the reaction furnace 20, and the flow guiding cavity 30 is substantially in the shape of an inverted funnel, and includes a top portion 32 and a bottom portion 38, and a cavity is formed therein. Referring to the third figure, the top portion 32 is formed with a plurality of openings 34 that are regularly arranged. The shape of the plurality of openings 34 is preferably circular, and other planar geometries such as squares or triangles may be used. The opening 34 has a diameter of the order of millimeters. The bottom portion 38 is provided with a second air inlet 36. Of course, the second air inlet 36 can also be disposed on the side wall of the flow guiding cavity 30, which can be used for the growth of the carbon nanotubes in the flow chamber 30. The reaction gas is sufficient. The material of the flow guiding cavity 30 can be selected from stainless steel, ceramic, quartz, etc. [0013] The gas conveying pipe 40 is used for conveying the reaction gas in the cavity formed inside the guiding flow chamber 30, and includes a first port 42. With a second port 44. The first port 42 is sealingly sleeved with the first air inlet 22, and the second port 44 is sealed with the second air inlet 36. The carbon nanotube growth reaction gas enters the gas delivery tube 40 from the second port 42 on the side of the first inlet 22, and is introduced into the flow guiding chamber 30 via the second port 44, and then through the guide The flow chamber 30 is guided such that the reaction gas enters the reaction furnace 20 from the plurality of openings 34 in a direction perpendicular to the surface of the top portion 32.

094137885 Form No. A0101 Page 6 of 14 1003412086-0 1360.584 100 years.11. Month 8th Shuttle Right ¥00 [0014] The carbon nanotube preparation apparatus 10 further includes a substrate 50 for the substrate 50 The carbon nanotubes are grown on the surface of the top 32 of the flow guiding cavity 30. The material of the substrate 50 may be selected from quartz, tantalum, alumina, magnesia or the like. A catalyst layer 52 is formed on the surface of the substrate 50, and the catalyst layer 52 may be composed of a material such as Ming, Zhen, Iron, or an alloy thereof. [0015] The heating device 12 is disposed around the reaction furnace 20 for heating the carbon nanotube growth catalyst layer 52 loaded in the reaction furnace 20. The heating device 12 can be selected from a heating device such as a high temperature furnace or a high frequency furnace. J [0016] The method of using the carbon nanotube preparation apparatus 10 provided in the present embodiment will be described in detail below in conjunction with the preparation process of the carbon nanotubes. [0017] First, the substrate 50 having the catalyst layer 52 formed thereon is placed over the top 32 of the flow guiding cavity 30 and in direct contact with the surface of the top portion 32. The substrate 50 can also be placed in direct contact with the flow guiding cavity 30, such as by overhead, at a distance above the top 32 of the flow guiding cavity 30. The substrate 50 is preferably a substrate having a porous structure, the pore size of which is preferably on the order of micrometers to facilitate gas permeation from the pores and flow out perpendicular to the substrate 50. The flow guiding cavity 30 is then placed in the reaction furnace 20 and the gas delivery pipe 40 is connected. [0018] Then, a carrier gas is introduced from the first air inlet 22 under normal pressure, and the carrier gas can enter the flow guiding cavity 30 through the gas delivery pipe 40 and the second air inlet 36, and Outflow from the flow guiding cavity 30 into the reaction furnace 20 is made by the opening 34. The opening 34 can be formed by machining, such as drilling a drill or punching a punch. The carrier gas may be selected from hydrogen, nitrogen, ammonia or other inert gas. The catalyst layer 52 in the reaction furnace 20 is heated by the heating device 12 094137885 Form No. A0101 Page 7 of 14 1003412086-0 1360584 100. November 8th Nuclear replacement page

Heat up. After the temperature of the catalyst layer 52 is raised to a predetermined temperature, it is generally 500 to 900 degrees, and a reaction gas is introduced from the first gas inlet port 22. The reaction gas may be selected from a carbon source gas such as decane, ethane, ethylene or acetylene. The reaction gas enters the flow guiding cavity 30 through the gas delivery pipe 40 and the second inlet 36, and is vertically blown toward the substrate 50 through the opening 34, that is, perpendicular to the surface of the top 32, enters the reaction furnace through the plurality of openings 34. 20 inside. Due to the catalytic action of the catalyst, the carbon source gas introduced into the reaction furnace 20 is thermally decomposed into carbon units and hydrogen; the carbon unit is adsorbed on the surface of the catalyst particles formed by the catalyst layer 52, and the carbon unit adsorbed in the catalyst particles is saturated. Precipitation allows the carbon nanotubes to grow at the catalyst particle sites. The carrier gas and the exhaust gas generated after the reaction can be discharged through the gas outlet 24. [0019] Referring to the fourth figure, in another embodiment, the catalyst layer 60 may be formed directly on the surface of the top portion 32 of the flow guiding cavity 30 for the growth of the carbon nanotubes. [0020] Forming the top 32 of the flow chamber 30 having the catalyst layer 60 on its surface can be made by the following steps:

[0021] First, a plurality of regularly arranged plurality of openings 34 may be formed in the top portion 32 of the flow guiding cavity 30 by mechanical processing such as drilling or punching punching, etc., and then formed on the top surface 32 of the flow guiding cavity 30. A mask corresponding to the plurality of openings 34. In this embodiment, a photoresist process may be employed. The specific step may be: applying a photoresist layer on the surface of the top portion 32 of the flow guiding cavity 30; and placing a photomask having a pattern corresponding to the plurality of openings 34 in the light. The resist layer is exposed to ultraviolet light for a certain period of time; the alkaline solution such as potassium hydroxide is used as a developer, and the exposed photoresist material is removed by wet etching to form a surface of the top surface 32 of the flow guiding cavity 30. The mask of the plurality of openings 34 is masked. Among them, the photoresist material can be polymethyl methacrylate, polyvinyl chloride or polycarbonate 094137885 Form No. A0101 Page 8 / 14 pages 1003412086-0 100 years. November 08 revised replacement page 1360584 Cool and so on. [0022] Thereafter, a catalyst layer 60 is formed on the surface of the top portion 32 of the flow guiding cavity 30 without a mask region. The catalyst layer 60 can be formed by an ion plating method, a radio frequency magnetron sputtering, a vacuum evaporation method, a chemical vapor deposition method, or the like.

[0023] Finally, the mask of the surface of the top 32 of the flow guiding cavity 30 is removed. In this embodiment, the mask is removed using an organic solvent (e.g., acetone) to obtain a top portion 32 of the flow guiding cavity 30 having a plurality of openings 34 and having a catalyst layer 60 formed on the surface. [0024] The carbon nanotube preparation device provided by the embodiment of the invention changes the flow direction of the reaction gas for the growth of the carbon nanotube by the flow guiding cavity to be parallel with the growth direction of the carbon nanotube, and further The preparation of collimated carbon nanotubes is achieved. [0025] In addition, those skilled in the art may also make other changes within the spirit of the present invention, such as appropriately changing the position of the first air inlet and the air outlet, the shape and setting position of the air guiding cavity, or changing the second. The position of the air inlet, the shape of the opening, its size, and the like, as long as it does not deviate from the effects of the present invention. In summary, the present invention has indeed met the requirements of the invention patent, and has filed a patent application according to law. However, the above description is only the preferred embodiment of the present invention, and equivalent modifications or variations made by those skilled in the art of the present invention should be included in the following claims. BRIEF DESCRIPTION OF THE DRAWINGS [0027] The first figure is a schematic view of the structure of a carbon nanotube preparation apparatus in the prior art. 094137885 Form No. A0101 Page 9 of 14 1003412086-0 1360584 On November 08, 100, the shuttle is being replaced. [0028] The second drawing is a schematic structural view of a carbon nanotube preparation apparatus according to a first embodiment of the present invention. [0029] The third figure is a schematic top view of the flow guiding cavity of the embodiment of the present invention. [0030] The fourth drawing is a schematic view showing the structure of a carbon nanotube preparing apparatus of a second embodiment of the present invention. [Main component symbol description]

[0031] Nano Carbon Tube Preparation Apparatus 10 Heating Apparatus 12 [0032] Reaction Furnace 20 First Air Inlet 22 [0033] Air Outlet 24 Diversion Cavity 30 [0034] Top 32 Opening 34 [0035] Second Intake Port 36 bottom 38 [0036] gas delivery tube 40 first port 42

[0037] Second Port 44 Substrate 50 [0038] Catalyst Layer 52, 60 1003412086-0 094137885 Form No. A0101 Page 10 of 14

Claims (1)

1360584 Seven, the scope of application for patents: 100 years. November 8th, according to the replacement page 1. A carbon nanotube preparation device for introducing a reaction gas for carbon nanotube growth to prepare a carbon nanotube, comprising: a reactor comprising a first An air inlet and an air outlet; a flow guiding cavity disposed in the reaction furnace, the guiding cavity comprises a top portion and a second air inlet, the top portion is formed with a plurality of openings, each opening The central axis and the central axis of the second air inlet are both perpendicular to the central axis of the first air inlet; a gas delivery tube includes a first port and a second port, the first port is sealed with the first air inlet, and the second port is sealed with the second air inlet; a substrate for the tube, the substrate being located in the reaction furnace and placed on a top surface of the flow guiding cavity; The carbon nanotube growth reaction gas enters the gas delivery tube from the second port on the first inlet side, and is introduced into the flow guiding cavity via the second port, and then guided through the guiding cavity The reaction gas is introduced into the reaction furnace from the plurality of openings in a direction perpendicular to the top surface. 2. The carbon nanotube preparation apparatus according to claim 1, wherein the material of the flow guiding cavity comprises stainless steel, ceramics, and quartz. 3. The carbon nanotube preparation apparatus according to claim 1, wherein the second air inlet is disposed at a bottom of the flow guiding cavity. 4. The carbon nanotube preparation apparatus according to claim 1, wherein the second air inlet is disposed at a side wall of the flow guiding cavity. 5. The carbon nanotube preparation apparatus according to claim 1, wherein the flow guiding cavity is in the shape of a funnel. 094137885 Form No. A0101 Page 11 of 14 1003412086-0 1360584 _^ </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; The openings are circular in shape and are regularly arranged at the top of the flow guiding cavity. 7. The carbon nanotube preparation apparatus according to claim 6, wherein the circular opening has a diameter of a millimeter. 8. The carbon nanotube preparation apparatus according to claim 1, wherein the substrate has a porous structure and has a pore size of a micron order. 9. The carbon nanotube preparation apparatus according to claim 1, wherein the base material is quartz, tantalum, alumina, or magnesium oxide. 10. The carbon nanotube preparation apparatus according to claim 1, wherein a catalyst layer for growing a carbon nanotube is formed on the surface of the substrate. The carbon nanotube preparation apparatus according to claim 10, wherein the catalyst layer is formed of a material, an alloy, an iron, or an alloy thereof. 094137885 Form No. A0101 Page 12 of 14 1003412086-0