CN108046237B - Device for preparing carbon nano material by arc plasma - Google Patents
Device for preparing carbon nano material by arc plasma Download PDFInfo
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- CN108046237B CN108046237B CN201711346947.8A CN201711346947A CN108046237B CN 108046237 B CN108046237 B CN 108046237B CN 201711346947 A CN201711346947 A CN 201711346947A CN 108046237 B CN108046237 B CN 108046237B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a device for preparing carbon nano-materials by arc plasma, which relates to the technical field of carbon nano-material preparation, and comprises: a gas supply unit; an arc reaction unit comprising: the device comprises a tube body, a cathode driving mechanism and an anode driving mechanism, wherein an annular cavity is formed in the side wall of the tube body, a first opening and a second opening which are communicated with the annular cavity are formed in the tube body, a gas outlet tube and a gas inlet are connected to the side wall of the tube body, the gas inlet is communicated with a gas mixing device, and a plurality of magnets are arranged on the side wall of the gas outlet tube; a sample heating unit including a sample placing member disposed in the gas outlet pipe, a heating device for heating the sample placing member; the cooling system is used for introducing cooling liquid through the first opening and the second opening so as to cool the pipe body; and the vacuum system is used for vacuumizing the tube body. The method and the device can produce the carbon nano material in various environments, realize dynamic preparation of the carbon nano material and accelerate the output speed.
Description
Technical Field
The invention relates to the technical field of carbon nano-material preparation, in particular to a device for preparing a carbon nano-material by arc plasma.
background
The nano-material is defined by the european commission as a powdery or agglomerated natural or artificial material consisting of elementary particles having one or more three-dimensional dimensions between 1nm and 100nm, and this elementary particle accounts for more than 50% of the total number of particles of the material. The nano material shows unique properties such as surface effect, quantum effect and quantum size effect due to the special structure, and is widely applied to various fields such as microelectronic devices, high-performance composite materials, medicine and the like; among them, carbon nanomaterials (fullerenes, carbon nanotubes, graphene) are called "king of nanometers", which is at the front of the scientific research of nanomaterials and is always the key field of research in various countries. The preparation method of the carbon nano material also draws wide attention; in recent years, carbon nanomaterial preparation methods have been greatly developed and enriched, and mainly include arc methods, mechanical ball milling methods, chemical vapor deposition methods, laser evaporation methods, in-situ synthesis methods, sol-gel methods, and the like. The arc method, that is, arc discharge is performed under a specific atmosphere (inert gas or reducing gas) and pressure to generate arc plasma, the anode is continuously consumed, and carbon nano materials are generated on the cathode, the wall of the reaction chamber or a specific substrate, so that the method has the potential of mass production and industrialization of the carbon nano materials. The fourth state of plasma, which is a substance widely existing in the universe, is a substance set composed of charged particles (electrons and cations) and neutral particles and showing overall charge neutrality, and has high molecular activity; meanwhile, the plasma science is combined with a plurality of industrial technologies, so that the processing on an atomic level is realized, and the production and manufacturing modes of modern industry are influenced.
However, in the existing equipment, the deposition temperature of the carbon nano-material can be greatly reduced by combining the low-temperature plasma technology and the chemical vapor deposition technology. However, the synthesis rate of the carbon nanomaterial is low, and the waste of raw materials is easily caused.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide an apparatus for preparing a carbon nanomaterial using arc plasma, which can produce a carbon nanomaterial in various environments, achieve dynamic preparation of the carbon nanomaterial, and increase the output speed.
The specific technical scheme of the embodiment of the invention is as follows:
An apparatus for preparing carbon nanomaterial by arc plasma, comprising:
a gas supply unit comprising: the gas mixing device is communicated with the gas storage devices, and the mass flow meter is connected between the gas storage devices and the gas mixing device;
An arc reaction unit comprising: the utility model provides a pipe body, set up at pipe body one end negative pole actuating mechanism, set up the positive pole actuating mechanism at the pipe body other end, annular cavity has in the pipe body lateral wall, have on the pipe body with first opening, the second opening of annular cavity intercommunication, be connected with gas outlet pipe on the lateral wall of pipe body and have gas inlet, gas inlet with gas mixing arrangement is linked together, positive pole actuating mechanism includes the positive pole, is used for pressing from both sides and establishes positive pole first clamping device, connect the lead screw in first clamping device one end, with the lead screw stepper motor that the lead screw is connected, negative pole actuating mechanism includes: the distance between the anode and the cathode can be adjusted under the action of the lead screw stepping motor, a plurality of magnets are arranged on the side wall of the gas outlet pipe and are circumferentially arranged around the axis of the gas outlet pipe, the N pole of each magnet faces the pipe body, and the S pole of each magnet is far away from the pipe body;
A sample heating unit including a sample placing member disposed in the gas outlet pipe, a heating device for heating the sample placing member;
A cooling system for introducing a cooling fluid through the first opening and the second opening to cool the tube;
A vacuum system for evacuating the interior of the tube.
in a preferred embodiment, the side wall of the tube body is provided with an observation port, and the observation port is provided with a sealing ring and quartz glass through bolt connection.
in a preferred embodiment, the vacuum system comprises a vacuum pump and a vacuum gauge in communication with the gas outlet pipe and/or the gas inlet.
In a preferred embodiment, a first ceramic tube is arranged between the tube body and the first clamping device, the first ceramic tube has an external thread, one end of the tube body has an internal thread, the external thread of the first ceramic tube is connected with the internal thread at one end of the tube body, and a circular ring-shaped sealing ring is arranged at a port of the first ceramic tube; the body with be provided with the second ceramic pipe between the second clamping device, the second ceramic pipe has the external screw thread, the other end of body has the internal thread, the external screw thread of second ceramic pipe with the internal thread of the body other end is connected, the port department of second ceramic pipe is provided with the ring form sealing washer.
In a preferred embodiment, the cathode and the anode are made of an electrode-like material, and have a diameter of between 2mm and 13mm, and the distance between the cathode and the anode is between 1mm and 2 mm.
In a preferred embodiment, the spindle is made of an insulating, high-temperature-resistant material.
In a preferred embodiment, the first clamping device has a positive terminal and the second clamping device has a negative terminal.
In a preferred embodiment, the first clamping device has an external thread, the first ceramic tube has an internal thread, and the external thread of the first clamping device is connected with the internal thread of the first ceramic tube; the second ceramic tube has an internal thread, the second clamping device has an external thread, and the internal thread of the second ceramic tube is connected with the external thread of the second clamping device.
In a preferred embodiment, the first opening is an inlet for the cooling fluid, which is located at the upper end of the tube, and the second opening is an outlet for the cooling fluid, which is located at the lower end of the tube; the gas outlet pipe and the gas inlet are oppositely arranged, and the axes of the gas outlet pipe and the gas inlet are positioned in the same plane.
In a preferred embodiment, the sample placing member is a quartz boat, the sample placing member is in contact with a wall surface of the gas outlet pipe, and the heating means is a thermocouple.
the technical scheme of the invention has the following remarkable beneficial effects:
The device for preparing the carbon nano material by the arc plasma can achieve the purpose of introducing gas raw materials with different proportions and different components through the gas supply unit according to the preparation requirement of the carbon nano material, generate high-temperature plasma under different reaction conditions in the arc reaction unit, and generate the carbon nano material on a sample placed on a sample placing piece below a fluid under the guidance of the fluid and a magnetic field generated by a magnet by the high-temperature plasma. The application can prepare the carbon nano material under various environments; the dynamic preparation of the material is realized, and the output speed of the carbon nano material on the sample can be accelerated through the magnetic field generated by the magnet.
specific embodiments of the present invention are disclosed in detail with reference to the following description and drawings, indicating the manner in which the principles of the invention may be employed. It should be understood that the embodiments of the invention are not so limited in scope. The embodiments of the invention include many variations, modifications and equivalents within the spirit and scope of the appended claims. Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.
Drawings
The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way. In addition, the shapes, the proportional sizes, and the like of the respective members in the drawings are merely schematic for facilitating the understanding of the present invention, and do not specifically limit the shapes, the proportional sizes, and the like of the respective members of the present invention. Those skilled in the art, having the benefit of the teachings of this invention, may choose from the various possible shapes and proportional sizes to implement the invention as a matter of case.
FIG. 1 is a schematic system diagram of an apparatus for producing carbon nanomaterials using arc plasma according to an embodiment of the present invention;
FIG. 2 is a schematic partial structural view of an apparatus for producing carbon nanomaterials using arc plasma according to an embodiment of the present invention;
FIG. 3 is a cross-sectional view of a tube in an apparatus for producing carbon nanomaterial using arc plasma according to an embodiment of the present invention;
Fig. 4 is a schematic diagram illustrating a plasma moving direction when a magnet is provided in the apparatus for preparing a carbon nanomaterial by arc plasma according to the embodiment of the present invention.
reference numerals of the above figures:
1. A screw rod stepping motor; 2. a screw rod; 3. a first clamping device; 4. a positive electrode interface; 5. a pipe body; 6. a first opening; 7. a gas inlet; 8. an observation port; 9. a bolt; 10. a gasket; 11. quartz glass; 12. a seal ring; 13. a ring-shaped sealing ring; 14. a first ceramic tube; 15. a negative electrode interface; 16. a second clamping device; 17. a cathode; 18. a second opening; 19. a gas outlet pipe; 20. a sample; 21. a coolant flow passage; 22. a heating device; 23. a sample placement member; 24. a magnet; 25. an anode; 26. a gas storage device; 27. a third on-off valve; 28. a first on-off valve; 29. a mass flow meter; 30. a gas mixing device; 31. a second on-off valve; 32. a nut; 33. a power supply; 34. a power switch; 35. a vacuum pump; 36. a vacuum gauge; 37. a second ceramic tube; 38. an annular cavity.
Detailed Description
The details of the present invention can be more clearly understood in conjunction with the accompanying drawings and the description of the embodiments of the present invention. However, the specific embodiments of the present invention described herein are for the purpose of illustration only and are not to be construed as limiting the invention in any way. Any possible variations based on the present invention may be conceived by the skilled person in the light of the teachings of the present invention, and these should be considered to fall within the scope of the present invention. It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "mounted," "connected," and "connected" are to be construed broadly and may include, for example, mechanical or electrical connections, communications between two elements, direct connections, indirect connections through intermediaries, and the like. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In order to produce carbon nanomaterials under various environments, achieve dynamic preparation of the carbon nanomaterials, and increase the output speed, the applicant has proposed a device for preparing carbon nanomaterials by using arc plasma through research, fig. 1 is a system schematic diagram of the device for preparing carbon nanomaterials by using arc plasma in the embodiment of the present invention, fig. 2 is a schematic diagram of a partial structure of the device for preparing carbon nanomaterials by using arc plasma in the embodiment of the present invention, as shown in fig. 1 and 2, the device for preparing carbon nanomaterials by using arc plasma in the present application includes: a gas supply unit including: a plurality of gas storage devices 26, a gas mixing device 30 communicated with the gas storage devices 26, and a mass flow meter 29 connected between the gas storage devices 26 and the gas mixing device 30; an arc reaction unit, the arc reaction unit comprising: body 5, the setting is at 5 one end negative pole 17 actuating mechanism of body, the setting is at the positive pole 25 actuating mechanism of the 5 other ends of body, annular cavity 38 has in the 5 lateral walls of body, first opening 6 with annular cavity 38 intercommunication has on the body 5, second opening 18, be connected with gas outlet pipe 19 and have gas inlet 7 on the lateral wall of body 5, positive pole 25 actuating mechanism includes positive pole 25, be used for pressing from both sides the first clamping device 3 who establishes positive pole 25, connect at the lead screw 2 of first clamping device 3 one end, lead screw step motor 1 who is connected with lead screw 2, negative pole 17 actuating mechanism includes: the cathode 17 and the second clamping device 16 are used for clamping the cathode 17, and the distance between the anode 25 and the cathode 17 can be adjusted under the action of the screw rod stepping motor 1; a sample heating unit including a sample placing member 23 provided in the gas outlet pipe 19, a heating device 22 for heating the sample placing member 23; a cooling system for introducing a cooling fluid through the first opening 6 and the second opening 18 to cool the tubular body 5; and a vacuum system for evacuating the interior of the tube 5.
The device for preparing the carbon nano material by the arc plasma can achieve the purpose of introducing gas raw materials with different proportions and different components through the gas supply unit according to the preparation requirement of the carbon nano material, generate high-temperature plasma under different reaction conditions in the arc reaction unit, and generate the carbon nano material on the sample 20 placed on the sample placing piece 23 below the fluid under the guidance of the fluid and the magnetic field generated by the magnet 24 by the high-temperature plasma. The application can prepare the carbon nano material under various environments; the dynamic preparation of the material is realized, and the production speed of the carbon nano-material on the sample 20 can be accelerated by the magnetic field generated by the magnet 24.
in order to better understand the device for preparing carbon nano-materials by arc plasma in the present application, it will be further explained and illustrated below. As shown in fig. 2, the arc reaction unit may include: the tube body 5, set up at 5 one ends of tube body 17 actuating mechanism of negative pole, set up the 25 actuating mechanism of positive pole at the other end of tube body 5, tube body 5 is roughly the pipe form, and its both ends are open state. The inside of the tube 5 is an arc reaction region.
Fig. 3 is a cross-sectional view of a tube 5 in an apparatus for preparing carbon nanomaterial by arc plasma according to an embodiment of the present invention, as shown in fig. 3, an annular cavity 38 is formed in a sidewall of the tube 5, and the tube 5 has a first opening 6 and a second opening 18 which are communicated with the annular cavity 38. First opening 6 can be the entry of coolant liquid, and it can be located the upper end of body 5, and second opening 18 can be the export of coolant liquid, and it is located the lower extreme of body 5, so, can flow into the annular cavity 38 back of body 5 by the coolant liquid, thereby can follow both sides around annular cavity 38 half cycle and flow out from second opening 18 again, above-mentioned in-process, the contact body 5 wall that the coolant liquid can be fully even to can be better reach refrigerated purpose. In general, the cooling liquid may be chosen to be water, although other liquid media for cooling may be chosen. The cooling system is used to introduce a cooling fluid through the first opening 6 and the second opening 18 to cool the tubular body 5. Thereby reach the purpose of cooling down to body 5 through letting in the coolant liquid in the first opening 6 to body 5, simultaneously according to the degree of cooling, steerable body 5's temperature range roughly to reach the purpose that produces carbon nano-material under the different environment.
As shown in fig. 2 and 3, the side wall of the tube body 5 is connected with a gas outlet tube 19 and has a gas inlet 7, and the gas inlet 7 is used for communicating with a gas mixing device 30. The gas outlet tube 19 and the gas inlet 7 are arranged opposite each other, and the axes of both can be in the same plane. In a more preferred embodiment, the axes of the gas outlet tube 19 and the gas inlet 7 may be substantially aligned, so that the reaction gas flowing in from the gas inlet 7 after the reaction in the arc reaction region can flow more easily to the gas outlet tube 19 and flow the high temperature plasma generated by the reaction into the gas outlet tube 19.
As shown in fig. 2, the anode 25 driving mechanism includes an anode 25, a first clamping device 3 for clamping the anode 25, a screw rod 2 connected to one end of the first clamping device 3, and a screw rod stepping motor 1 connected to the screw rod 2, wherein the distance between the anode 25 and the cathode 17 can be adjusted by the screw rod stepping motor 1. The anode 25 may be made of an electrode-like material, such as a carbon rod, having a diameter of between 2mm and 13 mm. The first clamping device 3 has a positive terminal 4. The first clamping device 3 has three ports, the first port is used for clamping the anode 25, the second port is the positive electrode interface 4 and is used for connecting the positive electrode of the power supply 33, the third port is used for connecting the lead screw 2, and the lead screw can be made of insulating high-temperature resistant materials. The connection part of the screw rod, the pipe body 5 and the first clamping device 3 can be made of insulating materials. Because the cathode 17 and the anode 25 can generate partial consumption in the process of generating arc light, the screw rod stepping motor 1 can push the anode 25, and the distance between the cathode and the anode in the reaction process is ensured. A first ceramic tube 14 can be arranged between the tube body 5 and the first clamping device 3, the first ceramic tube 14 has an external thread, one end of the tube body 5 has an internal thread, the external thread of the first ceramic tube 14 is connected with the internal thread at one end of the tube body 5, and a circular ring-shaped sealing ring 13 is arranged at the port of the first ceramic tube 14. The first clamping device 3 has an external thread and the first ceramic tube 14 has an internal thread, the external thread of the first clamping device being connected to the internal thread of the first ceramic tube 14. Can guarantee the leakproofness between first ceramic tube 14 and body 5, the first clamping device 3 through above-mentioned mode, simultaneously, first ceramic tube 14 can play insulating and bear the effect of high temperature, prevents that electric current from directly flowing through from body 5, leads to unable production arc plasma between negative pole 17, the positive pole 25.
as shown in fig. 2, the cathode 17 driving mechanism may include: a cathode 17, a second clamping device 16 for clamping the cathode 17. The second clamping device 16 has two ports, the first port for holding the cathode 17 and the second port being a negative interface 15 for connecting to the negative pole of a power supply 33. The cathode 17 is made of an electrode-like material, such as a carbon rod, having a diameter of between 2mm and 13 mm. The cathode 17 and the anode 25 are positioned on the same line and at a distance of between 1mm and 2 mm. When the cathode 17 and the anode 25 generate arc light, the temperature between the cathode 17 and the anode 25 is more than 3000 ℃. A second ceramic tube 37 can be arranged between the tube body 5 and the second clamping device 16, the second ceramic tube 37 has an external thread, the other end of the tube body 5 has an internal thread, the external thread of the second ceramic tube 37 is connected with the internal thread at the other end of the tube body 5, and a circular ring-shaped sealing ring 13 is arranged at the port of the second ceramic tube 37. The second ceramic tube 37 has an internal thread, the second clamping device 16 has an external thread, and the internal thread of the second ceramic tube 37 is connected to the external thread of the second clamping device 16. In a similar way, the tightness between the second ceramic tube 37 and the tube body 5 and between the second ceramic tube 37 and the second clamping device 16 can be ensured in the above manner, and meanwhile, the second ceramic tube 37 can play a role of insulation and bearing high temperature, so that the current is prevented from directly flowing from the tube body 5, and arc plasma cannot be generated between the cathode 17 and the anode 25.
as shown in fig. 2, a side wall of the pipe body 5 may be provided with an observation port 8, and the observation port 8 may be provided with a seal ring 12 and a quartz glass 11 connected by a bolt 9. The reaction between the cathode 17 and the anode 25 in the tube 5 is observed through the quartz glass 11. The sealing ring 12 is used for ensuring the sealing performance between the quartz glass 11 and the tube body 5, and when the tube body 5, the sealing ring 12 and the quartz glass 11 are connected through the bolt 9, a plurality of through holes at different positions can be formed in the tube body 5, the sealing ring 12 and the quartz glass 11, and then the tube body 5, the gasket 10 and the nut 32 are connected to ensure the sealing performance in the tube body 5.
Fig. 4 is a schematic diagram showing a plasma moving direction when the magnet 24 is provided in the apparatus for preparing the carbon nanomaterial by using the arc plasma in the embodiment of the present invention, as shown in fig. 2 and 4, a plurality of magnets 24 are provided on a side wall of the gas outlet pipe 19, the magnets 24 are circumferentially arranged around an axis of the gas outlet pipe 19, an N pole of the magnet 24 faces the tube 5, and an S pole of the magnet 24 is far from the tube 5. The sample heating unit may comprise a sample placing member 23 arranged in the gas outlet tube 19, heating means 22 for heating the sample placing member 23. The sample placing member 23 may be a quartz boat for placing the sample 20, the sample placing member 23 is in contact with the wall surface of the gas outlet tube 19, and the heating means 22 is a thermocouple. When the thermocouple heats the tube 5 which the sample holder 23 contacts, the heat is transferred to the sample holder 23, thereby heating the sample holder 23. After the plurality of magnets 24 are arranged on the side wall of the gas outlet pipe 19, the magnetic field generated by the magnets 24 can control the plasma generated between the cathode 17 and the anode 25 in the pipe body 5 to a certain extent, so that the plasma generated in the pipe body 5 is accelerated and flows into the gas outlet pipe 19, and the production speed of the carbon nano-material on the sample 20 on the sample placing member 23 is accelerated. A cooling liquid flow passage 21 is further provided at the sample placing member 23 of the gas outlet pipe 19, and the sample placing member 23 is rapidly cooled by feeding a cooling liquid into the cooling liquid flow passage 21.
As shown in fig. 1, the gas supply system may include: a plurality of gas storage devices 26, a gas mixing device 30 communicated with the gas storage devices 26, and a mass flow meter 29 connected between the gas storage devices 26 and the gas mixing device 30. The gas storage device 26 stores therein a protective gas, a reducing gas, a carbon-containing gas, and the like. The mass flow meter 29 can precisely control the flow rate of different gases in the gas storage device 26 flowing into the gas mixing device 30, thereby controlling the mixing ratio of the gases. A first on-off valve 28 may be provided between the gas mixing device 30 and the gas inlet 7 to control the gas mixing device 30 to deliver gas into the tube 5. A third on-off valve 27 is provided between the gas storage device 26 and the mass flow meter 29. The gas supply system can be used for introducing gas raw materials with different proportions and different components into the tube body 5, so that the carbon nano-material is generated in various environments, and the purpose of dynamically preparing the material is achieved. The various environments may include atmospheric pressure, low pressure, different temperatures, a static environment, and a dynamic environment. The dynamic environment specifically means that when the cathode 17 and the anode 25 are electrified to perform reaction, the gas introduced into the tube 5 is always in a flowing state, and the static environment specifically means that when the cathode 17 and the anode 25 are electrified to perform reaction, the gas in the tube 5 is kept unchanged and is not continuously introduced any more.
As shown in fig. 1, a vacuum system may be used to draw a vacuum within tube 5. Specifically, the vacuum system may include a vacuum pump 35 and a vacuum gauge 36 in communication with the gas outlet tube 19 and/or the gas inlet 7. Second switch valve 31 can be provided with between vacuum pump 35 and gas outlet pipe 19 or the gas feed 7, after vacuum pump 35 finishes to the evacuation of body 5, can close second switch valve 31 to be vacuum state in the assurance body 5.
The device for preparing the carbon nano material by the arc plasma in the application dynamically prepares the carbon nano material by the following process: first, the pretreated sample is placed on the sample placing member 23; next, the cathode 17 and the anode 25 are mounted on the first clamping device 3 and the second clamping device 16, respectively; secondly, the sample holder 23 holding the sample 20 may be finally put into the gas outlet tube 19 after connecting the respective parts in the apparatus for preparing carbon nanomaterial by arc plasma to prevent the surface of the sample 20 from being damaged during the installation process. Then, carrying out primary vacuum pumping on the interior of the tube body 5 through a vacuum system, carrying out vacuum pumping again after introducing protective gas, and circulating for many times in such a way to discharge air possibly remaining in the tube body 5; then, heating the sample to the required reaction temperature by a sample heating unit; starting a power switch 34 of a power supply 33 under the condition of introducing protective gas, forming arc light between a cathode 17 and an anode 25 in the tube body 5 to generate high-temperature plasma, and simultaneously starting the screw rod stepping motor 1 and a cooling system; after the high-temperature arc is stabilized, the required mixed gas is introduced into the tube body 5 through the gas supply unit. And finally, continuing for a period of time, closing the experimental device after the reaction is finished, and collecting a reaction product, namely the carbon nano material, on the sample 20 after cooling.
the device for preparing the carbon nano material by the arc plasma in the application statically prepares the carbon nano material by the following process: a baffle (not shown) is placed above the inside of the gas outlet pipe 19; next, the cathode 17 and the anode 25 are mounted on the first clamping device 3 and the second clamping device 16, respectively; secondly, connecting all parts in the device for preparing the carbon nano material by the arc plasma; then, carrying out primary vacuum pumping on the interior of the tube body 5 through a vacuum system, carrying out vacuum pumping again after introducing protective gas, and circulating for many times in such a way to discharge air possibly remaining in the tube body 5; then, the required gas raw material is introduced into the pipe body 5 through the gas supply unit to reach the ideal pressure, and the tail ends of the gas inlet 7 and the gas outlet pipe 19 are closed; turning on a power switch 34 of a power supply 33 so that an arc is formed between the cathode 17 and the anode 25 in the tube 5 to generate high-temperature plasma, and simultaneously turning on the lead screw stepping motor 1 and the cooling system; and finally, continuing for a period of time, closing the experimental device after the reaction is finished, and collecting a test product, namely the carbon nano material, on the baffle after cooling.
All articles and references disclosed, including patent applications and publications, are hereby incorporated by reference for all purposes. The term "consisting essentially of …" describing a combination shall include the identified element, ingredient, component or step as well as other elements, ingredients, components or steps that do not materially affect the basic novel characteristics of the combination. The use of the terms "comprising" or "including" to describe combinations of elements, components, or steps herein also contemplates embodiments that consist essentially of such elements, components, or steps. By using the term "may" herein, it is intended to indicate that any of the described attributes that "may" include are optional. A plurality of elements, components, parts or steps can be provided by a single integrated element, component, part or step. Alternatively, a single integrated element, component, part or step may be divided into separate plural elements, components, parts or steps. The disclosure of "a" or "an" to describe an element, ingredient, component or step is not intended to foreclose other elements, ingredients, components or steps.
The embodiments in the present specification are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. an apparatus for preparing carbon nano-materials by arc plasma, which is characterized by comprising:
a gas supply unit comprising: the gas mixing device is communicated with the gas storage devices, and the mass flow meter is connected between the gas storage devices and the gas mixing device;
an arc reaction unit comprising: the utility model provides a pipe body, set up at pipe body one end negative pole actuating mechanism, set up the positive pole actuating mechanism at the pipe body other end, annular cavity has in the pipe body lateral wall, have on the pipe body with first opening, the second opening of annular cavity intercommunication, be connected with gas outlet pipe on the lateral wall of pipe body and have gas inlet, gas inlet with gas mixing arrangement is linked together, positive pole actuating mechanism includes the positive pole, is used for pressing from both sides and establishes positive pole first clamping device, connect the lead screw in first clamping device one end, with the lead screw stepper motor that the lead screw is connected, negative pole actuating mechanism includes: the distance between the anode and the cathode can be adjusted under the action of the lead screw stepping motor, a plurality of magnets are arranged on the side wall of the gas outlet pipe and are circumferentially arranged around the axis of the gas outlet pipe, the N pole of each magnet faces the pipe body, and the S pole of each magnet is far away from the pipe body;
A sample heating unit including a sample placing member disposed in the gas outlet pipe, a heating device for heating the sample placing member;
A cooling system for introducing a cooling fluid through the first opening and the second opening to cool the tube;
A vacuum system for evacuating the interior of the tube.
2. the apparatus for preparing carbon nanomaterial according to claim 1, wherein the side wall of the tube body is provided with an observation port, and the observation port is provided with a sealing ring and quartz glass by bolt connection.
3. The apparatus of claim 1, wherein the vacuum system comprises a vacuum pump and a vacuum gauge in communication with the gas outlet pipe and/or the gas inlet.
4. The apparatus for preparing carbon nanomaterial by using arc plasma according to claim 1, wherein a first ceramic tube is arranged between the tube body and the first clamping device, the first ceramic tube has external threads, one end of the tube body has internal threads, the external threads of the first ceramic tube are connected with the internal threads at one end of the tube body, and a circular ring-shaped sealing ring is arranged at a port of the first ceramic tube; the body with be provided with the second ceramic pipe between the second clamping device, the second ceramic pipe has the external screw thread, the other end of body has the internal thread, the external screw thread of second ceramic pipe with the internal thread of the body other end is connected, the port department of second ceramic pipe is provided with the ring form sealing washer.
5. The apparatus of claim 1, wherein the cathode and the anode are made of an electrode-based material and have a diameter of 2mm to 13mm, and the distance between the cathode and the anode is 1mm to 2 mm.
6. The apparatus of claim 1, wherein the screw rod is made of an insulating and high temperature resistant material.
7. the apparatus of claim 1, wherein the first clamping device has a positive interface thereon and the second clamping device has a negative interface thereon.
8. The apparatus for preparing a carbon nanomaterial according to claim 4, wherein the first clamping means has an external thread, the first ceramic tube has an internal thread, and the external thread of the first clamping means is connected to the internal thread of the first ceramic tube; the second ceramic tube has an internal thread, the second clamping device has an external thread, and the internal thread of the second ceramic tube is connected with the external thread of the second clamping device.
9. The apparatus of claim 1, wherein the first opening is an inlet of the cooling fluid at an upper end of the tube, and the second opening is an outlet of the cooling fluid at a lower end of the tube; the gas outlet pipe and the gas inlet are oppositely arranged, and the axes of the gas outlet pipe and the gas inlet are positioned in the same plane.
10. The apparatus of claim 1, wherein the sample holder is a quartz boat, the sample holder is in contact with a wall surface of the gas outlet pipe, and the heating means is a thermocouple.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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