CN114679832B - Sliding arc discharge plasma device and nano powder preparation method - Google Patents
Sliding arc discharge plasma device and nano powder preparation method Download PDFInfo
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- CN114679832B CN114679832B CN202210362740.4A CN202210362740A CN114679832B CN 114679832 B CN114679832 B CN 114679832B CN 202210362740 A CN202210362740 A CN 202210362740A CN 114679832 B CN114679832 B CN 114679832B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/48—Generating plasma using an arc
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/48—Generating plasma using an arc
- H05H1/482—Arrangements to provide gliding arc discharges
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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 relates to a sliding arc discharge plasma device and a preparation method of nano powder. Comprises a sliding arc plasma generator, a venturi tube with a preset proportion and a fluidized bed; the carrier gas, the precursor gas and the etching gas are introduced into a closed sliding arc plasma reactor after the proportion is adjusted; starting a power supply, an induced draft fan or a vacuum pump, adjusting the reaction pressure of a plasma region, and maintaining a sliding arc to perform discharge reaction in a stable state; the plasma cracks and nucleates the precursor and etching gas, the gas flow rate is increased in a venturi tube with a specific proportion, the precursor and etching gas further grow in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector. The invention can directly prepare nano powder materials in a gas phase environment, has the characteristics of less arcing limiting factors, simple operation, rapid and continuous production and the like, and the obtained nano powder has multiple types, small size and high quality, and can be used in various front edge fields.
Description
Technical Field
The invention belongs to the field of nano powder plasma preparation, and particularly relates to a sliding arc discharge plasma device and a nano powder preparation method.
Background
In recent years, with the continuous development of plasma technology, plasmas exhibit their unique advantages in the fields of nanomaterial science and technology. The Shenhua group Limited liability company discloses a preparation method of carbon black (patent grant publication No. CN 106543777B), which comprises the steps of cracking carbonaceous materials at 1400-1800 ℃ by high-temperature plasma to obtain a product rich in acetylene, and continuously decomposing the obtained product to obtain the carbon black. The method can simplify the step of purifying acetylene, shorten the production flow of carbon black and reduce the production cost.
The lithium battery is used as a new energy source to provide power sources for most portable electronic equipment and even electric automobiles, and the graphene is a good choice as a conductive material of the lithium ion battery because the special lamellar and stacking structure of the graphene powder enables lithium ions to be more easily intercalated and deintercalated. Xiang Yong to university of electronic technology et al discloses a method for preparing graphene (patent grant publication number: CN 108190864B). The invention adopts liquid metal tin as a carrier, saccharides as solid carbon sources, and carbon atoms are dissolved at high temperature. And after cooling, generating graphene on the surface of the metal tin, and then cleaning and separating to obtain the graphene. Compared with the mechanical stripping, liquid phase stripping and vapor deposition methods of graphene, the method has certain advantages, but other operations such as substrate, separation, drying and the like are also needed in the preparation process. In addition, silicon-carbon composite materials have many advantages over graphite materials, and are one of the most potential lithium ion battery anode materials at present. The doped graphene or the doped carbon has wide application prospect in the application fields of electrochemistry and electrocatalysts. Guan Naijia, et al, of the university of south-open discloses a preparation method of a nitrogen-doped graphene material, which comprises the following steps: adding small molecular fatty amine aqueous solution into the ultrasonic dispersion graphite oxide aqueous solution to carry out hydrothermal reaction 36-72 h, and separating, washing and drying to obtain the nitrogen-doped graphene material (patent grant publication number: CN 103691471B). The material prepared by the method has good catalytic activity in Michael addition reaction and transesterification reaction, but the whole preparation requires longer time, and the purposes of quick preparation and simple operation cannot be achieved.
The sliding arc can simultaneously meet the requirements of high electron temperature, high electron density and high unbalance required by thermal plasma and low-temperature plasma in the plasma chemical process, and most of input electric energy can greatly improve chemical reaction efficiency, so that the sliding arc is low-temperature plasma with high energy utilization rate. In addition, the sliding arc device has simple structure, low cost and convenient operation, and is not limited by pressure change. Thus, sliding arc discharge is widely used and studied in methane gas reforming, pollutant degradation, nanomaterial preparation, modification, and other fields. Zhang Baoshun of the asian silicon industry (green sea) incorporated discloses a method by which hydrogenated silicon tetrachloride materials can be obtained by introducing silicon tetrachloride and hydrogen into a sliding arc discharge reaction filled with an electromagnetic field adjusting material and a supported metal catalyst (patent grant No. CN 108439413B). However, there are few methods and patents for directly preparing nano-powder in a gas phase environment for a sliding arc discharge plasma process.
Disclosure of Invention
The invention aims at solving the problems of how to quickly, simply, continuously, effectively, controllably, with low cost and low energy consumption in the preparation process of nano powder materials, and provides a sliding arc discharge plasma device and a preparation method of nano powder.
In order to achieve the above purpose, the technical scheme of the invention is as follows: a sliding arc discharge plasma device comprises a sliding arc plasma generator, a venturi tube with a preset proportion and a fluidized bed; the sliding arc plasma generator comprises an insulating chassis, a cylindrical electrode and a conical electrode; the cylindrical electrode and the conical electrode are connected with a power supply, and the air inlet is tangential to the cylindrical electrode; the insulation chassis is connected with the bottom of the cylindrical electrode and the conical electrode, wherein the conical electrode is positioned in the cylindrical electrode, one surface of the insulation chassis is separated from the conical electrode through a ceramic plate, and a gap generated by connecting the other surface of the insulation chassis with the conical electrode is sealed through silicon rubber which can be solidified at room temperature; the venturi tube with the preset proportion is a pipeline with large outlet areas at two ends and small middle section, the outlet end of the venturi tube with the preset proportion is connected with the inlet of the fluidized bed, and the inlet end of the venturi tube with the preset proportion is connected with the top of the cylindrical electrode.
In one embodiment of the invention, the conical electrode, the ceramic sheet and the insulating chassis are connected through an electrode height adjusting hole in the center of the insulating chassis, the height is adjusted, and a gap generated by the conical electrode and the insulating chassis is filled by silicon rubber which can be solidified at room temperature; the insulation chassis is a polytetrafluoroethylene disc which is easy to process, short circuit of the high-voltage end and the low-voltage end can be prevented when the high-voltage end and the low-voltage end are electrified, and the thickness of the insulation chassis is 1/4-1/3 of the diameter of the disc; the ceramic plate is a concentric ring ceramic plate, so that the damage to the reactor chassis caused by the combustion phenomenon caused by stacking a small amount of powder materials in the electrode area can be reduced, an additional cooling medium and a device are not needed for cooling the electrode and the chassis, the inner circle is a conical electrode adjusting hole, the diameter of the outer circle is slightly smaller than that of the cylindrical electrode, and 1-2 mm of space between the ceramic plate and the bottom circular surface of the conical electrode is reserved.
In one embodiment of the invention, the air inlet is positioned below the cylindrical electrode at the same height as the bottom circular surface of the conical electrode so that the generated sliding arc slides upwards around the conical electrode and reduces damage to the ceramic wafer.
In an embodiment of the present invention, the ratio of the inlet pipe to the throat pipe of the venturi tube is 5:1 to 20:1, preferably 10:1, so that the conversion rate of the raw material is greater than 50%; the ratio of the length of the venturi tube to the inlet tube is 5:1-15:1, preferably 8:1, so that powder with the diameter smaller than 100 nm can be obtained.
The invention also provides a preparation method of the nano powder by adopting the device, which comprises the following steps:
(1) The proportion of the carrier gas, the precursor gas and the etching gas is adjusted by a mass flowmeter, and the carrier gas, the precursor gas and the etching gas are introduced into a closed sliding arc plasma generator;
(2) Starting a power supply, an induced draft fan or a vacuum pump, adjusting the reaction pressure of a plasma region, and maintaining a sliding arc to perform discharge reaction in a stable state;
(3) The plasma cracks the precursor and etching gas and nucleates, the gas flow rate is increased in a venturi tube with a preset proportion, the precursor and etching gas further grow in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector.
In one embodiment of the present invention, the carrier gas in the step (1) is one or more of air, argon, neon, helium, nitrogen or other ionizable gas (e.g. air and argon, nitrogen and argon); the precursor gas is a mixed gas of one or more of carbon precursor gas (gaseous hydrocarbon or vaporized alcohol), silicon precursor gas (gaseous or vaporized small molecule silane), nitrogen precursor gas, for example: silicon precursor and carbon precursor, carbon precursor and nitrogen precursor (ammonia or nitrogen); the etching gas is one or a mixture of more of hydrogen, carbon dioxide and water vapor; the temperature of the gas introduced into the gas inlet can be in the range from room temperature to 300 ℃, and the heated gas can enhance the effect of plasma pyrolysis.
In one embodiment of the present invention, when the pressure of the sealed plasma reactor in the step (1) is atmospheric pressure, the mass flow ratio of the carrier gas to the precursor gas is 6:1 to 16:1, and the mass flow ratio of the precursor gas to the etching gas is 1:1 to 10:1; when the pressure range is 20-90 kPa, the mass flow ratio of the carrier gas to the precursor gas is 0:1-10:1, and the mass flow ratio of the precursor gas to the etching gas is 2:1-5:1.
In one embodiment of the present invention, in the step (2), the induced draft fan is used to drive the air flow in the plasma reaction under the atmospheric pressure, and the vacuum pump is used to regulate the pressure in the plasma reaction under the reduced pressure so as to reduce the flow rate of the carrier gas, thereby achieving the purpose of reducing the production cost of the nano powder material. .
In one embodiment of the present invention, the power range of the power supply in step (2) is 1-50 kW, preferably 20 kW, the plasma generator can work for a long time, and the electrodes are not ablated; the no-load voltage is in the range of 20 kV-50 kV, preferably 30 kV, so that the multi-atomic gas can be promoted to generate plasma, arc interruption is avoided, and abnormal conditions of electric leakage are avoided.
In an embodiment of the present invention, the final nano powder in the step (3) is a silicon-carbon composite material, graphene, doped nano carbon or other composite nano powder material.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method can realize the preparation of various nano powder materials with different forms and structures, and the obtained powder material has great application potential in a plurality of front fields.
(2) The method of the invention is not limited by pressure, and the vacuum pump is used for providing the depressurized plasma reaction pressure, thereby greatly reducing the carrier gas flow and the power supply energy consumption and achieving the purpose of reducing the production cost of the nano powder material.
(3) The method of the invention can prevent the abnormal arc burning phenomenon generated by the accumulation of a small amount of nano powder material on the electrode from damaging the reactor chassis by adding the ceramic plate, and can prevent the abnormal discharge caused by the falling of the nano powder material on the plasma area from reducing the yield by adding a venturi-like device to increase the gas flow rate.
(4) The method has the advantages of one-step reaction in a gas-phase environment, simple operation and process, high reaction speed, high efficiency, controllability, continuous production and the like.
Drawings
FIG. 1 is a schematic diagram of a sliding arc discharge plasma reaction of example 1; wherein, 1-a cylindrical electrode; 2-air inlet; 3-silicone rubber; 4-an insulating chassis; 5-ceramic plates; 6-a conical electrode; 7-a flange; 8-a venturi; 9-fluidized bed.
FIG. 2 is an SEM image of example 2;
fig. 3 is an SEM image of example 3.
Detailed Description
The technical scheme of the invention is specifically described below with reference to the accompanying drawings.
The invention relates to a sliding arc discharge plasma device, which comprises a sliding arc plasma generator, a venturi tube and a fluidized bed, wherein the venturi tube and the fluidized bed are in a preset proportion; the sliding arc plasma generator comprises an insulating chassis, a cylindrical electrode and a conical electrode; the cylindrical electrode and the conical electrode are connected with a power supply, and the air inlet is tangential to the cylindrical electrode; the insulation chassis is connected with the bottom of the cylindrical electrode and the conical electrode, wherein the conical electrode is positioned in the cylindrical electrode, one surface of the insulation chassis is separated from the conical electrode through a ceramic plate, and a gap generated by connecting the other surface of the insulation chassis with the conical electrode is sealed through silicon rubber which can be solidified at room temperature; the venturi tube with the preset proportion is a pipeline with large outlet areas at two ends and small middle section, the outlet end of the venturi tube with the preset proportion is connected with the inlet of the fluidized bed, and the inlet end of the venturi tube with the preset proportion is connected with the top of the cylindrical electrode.
The invention also provides a preparation method of the nano powder by adopting the device, which comprises the following steps:
(1) The proportion of the carrier gas, the precursor gas and the etching gas is adjusted by a mass flowmeter, and the carrier gas, the precursor gas and the etching gas are introduced into a closed sliding arc plasma generator;
(2) Starting a power supply, an induced draft fan or a vacuum pump, adjusting the reaction pressure of a plasma region, and maintaining a sliding arc to perform discharge reaction in a stable state;
(3) The plasma cracks the precursor and etching gas and nucleates, the gas flow rate is increased in a venturi tube with a preset proportion, the precursor and etching gas further grow in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector.
The following is a specific embodiment of the present invention.
Example 1
As shown in fig. 1, a sliding arc discharge plasma device is used for preparing nano split materials, and comprises a cylindrical electrode 1, a conical electrode 6, an air inlet 2, an insulating base plate (polytetrafluoroethylene base plate) 4, a ceramic plate 5, silicone rubber (high temperature resistant silicone rubber solidified at room temperature) 3, a venturi tube 8 with a specific proportion, a flange 7 for connection and a fluidized bed 9.
The device comprises the following specific operation steps:
step 1: the conical electrode, the concentric ring ceramic sheet and the polytetrafluoroethylene chassis are connected through an electrode height adjusting hole in the center of the disk, the height is adjusted, and a gap generated between the conical electrode and the chassis is filled by room-temperature cured silicon rubber; the bottom of the cylindrical electrode is mechanically connected with the polytetrafluoroethylene chassis through a welding flange; the top of the cylindrical electrode is mechanically connected with the venturi tube inlet with a specific proportion through a welding flange; the fluidized bed inlet is mechanically connected with the venturi outlet with a specific proportion.
Step 2: injecting gas into the gas inlet, and opening a power switch; selecting an induced draft fan or a vacuum pump device according to the pressure required in the reaction process and adjusting the pressure;
step 3: after the reaction is finished, collecting a final powder product in a cyclone separator connected with the fluidized bed and a bag-type dust collector connected with the cyclone separator.
Example 2
The preparation method of the graphene powder by applying the method of the embodiment 1 comprises the following specific steps: and regulating the flow rates of argon, methane and carbon dioxide to be 14 slm, 2 slm and 1 slm respectively by using a mass flowmeter, and tangentially feeding all gases from an air inlet of the plasma generator after mixing and preheating. The power was turned on at 20 kw and the reaction time was 10 min. And opening the induced draft fan to enable the reaction pressure of the plasma region to be under the atmospheric pressure, and collecting graphene powder in the cyclone separator and the bag-type dust collector after the reaction is finished. Fig. 2 is an SEM image of example 1, which clearly shows that the graphene nanoplatelets are folded and edge curled with each other as prepared.
Example 3
The preparation method of the silicon-carbon composite material applying the method of the embodiment 1 comprises the following specific steps: and regulating the flow rates of argon, methane and hydrogen to be 10 slm, 1 slm and 0.5 slm respectively by using a mass flowmeter, and tangentially feeding the mixed gas of the argon, the methane and the hydrogen from an air inlet of the plasma generator. After the sliding arc is stable, the flow rate of silane is adjusted to be 1 slm by a mass flowmeter, and silane is introduced from an air inlet. The power was turned on at 20 kw and the reaction time was 10 min. And (3) turning on a vacuum pump to enable the reaction pressure of the plasma region to be under 90 kPa, and collecting the silicon-carbon composite powder material in a cyclone separator and a bag-type dust collector after the reaction is finished. Fig. 3 is an SEM image of example 3, from which it can be seen that the silicon material is mainly spherical and the pure carbon material is entirely in a sheet shape.
The above is a preferred embodiment of the present invention, and all changes made according to the technical solution of the present invention belong to the protection scope of the present invention when the generated functional effects do not exceed the scope of the technical solution of the present invention.
Claims (9)
1. The sliding arc discharge plasma device is characterized by comprising a sliding arc plasma generator, a venturi tube and a fluidized bed in a preset proportion; the sliding arc plasma generator comprises an insulating chassis, a cylindrical electrode and a conical electrode; the cylindrical electrode and the conical electrode are connected with a power supply, and the air inlet is tangential to the cylindrical electrode; the insulation chassis is connected with the bottom of the cylindrical electrode and the conical electrode, wherein the conical electrode is positioned in the cylindrical electrode, one surface of the insulation chassis is separated from the conical electrode through a ceramic plate, and a gap generated by connecting the other surface of the insulation chassis with the conical electrode is sealed through silicon rubber which can be solidified at room temperature; the venturi tube with the preset proportion is a pipeline with large outlet areas at two ends and small middle section, the outlet end of the venturi tube with the preset proportion is connected with the inlet of the fluidized bed, and the inlet end of the venturi tube with the preset proportion is connected with the top of the cylindrical electrode; the conical electrode, the ceramic sheet and the insulating chassis are connected through an electrode height adjusting hole in the center of the insulating chassis, the height is adjusted, and gaps generated by the conical electrode and the insulating chassis are filled by silicon rubber which can be solidified at room temperature; the insulation chassis is a polytetrafluoroethylene disc, and the thickness of the insulation chassis is 1/4-1/3 of the diameter of the disc; the ceramic plate is a concentric ring ceramic plate, the inner circle is a conical electrode adjusting hole, the diameter of the outer circle is slightly smaller than that of the cylindrical electrode, and 1-2 mm is reserved between the ceramic plate and the bottom circular surface of the conical electrode.
2. The sliding arc discharge plasma apparatus of claim 1 wherein the gas inlet is located below the cylindrical electrode at the same height as the bottom circular surface of the conical electrode.
3. The sliding arc discharge plasma apparatus of claim 1 wherein the ratio of the inlet pipe to the throat of the venturi tube is 5:1 to 20:1; the ratio of the length of the venturi tube to the inlet tube is 5:1-15:1.
4. A method for preparing nano-powder using the device according to any one of claims 1 to 3, comprising the steps of:
(1) The proportion of the carrier gas, the precursor gas and the etching gas is adjusted by a mass flowmeter, and the carrier gas, the precursor gas and the etching gas are introduced into a closed sliding arc plasma generator;
(2) Starting a power supply, an induced draft fan or a vacuum pump, adjusting the reaction pressure of a plasma region, and maintaining a sliding arc to perform discharge reaction in a stable state;
(3) The plasma cracks the precursor and etching gas and nucleates, the gas flow rate is increased in a venturi tube with a preset proportion, the precursor and etching gas further grow in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector.
5. The method of claim 4, wherein the plasma reaction under the atmospheric pressure in the step (2) uses an induced draft fan to drive the air flow, and the plasma reaction under the reduced pressure uses a vacuum pump to regulate the pressure.
6. The method of preparing nano-powder according to claim 4, wherein the carrier gas in the step (1) is a mixed gas of one or more of air, argon, neon, helium and nitrogen; the precursor gas is a mixed gas of one or more of carbon precursor gas, silicon precursor gas and nitrogen precursor gas; the etching gas is one or a mixture of more of hydrogen, carbon dioxide and water vapor; the gas temperature introduced into the inlet ranges from room temperature to 300 ℃.
7. The method of preparing nano-powder according to claim 4, wherein when the pressure of the sealed plasma reactor in the step (1) is atmospheric pressure, the mass flow ratio of carrier gas to precursor gas is 6:1 to 16:1, and the mass flow ratio of precursor gas to etching gas is 1:1 to 10:1; when the pressure range is 20-90 kPa, the mass flow ratio of the carrier gas to the precursor gas is 0:1-10:1, and the mass flow ratio of the precursor gas to the etching gas is 2:1-5:1.
8. The method for preparing nano-powder according to claim 4, wherein the power of the power source in the step (2) ranges from 1 to 50 to kW; the range of no-load voltage is 20 kV-50 kV.
9. The method of claim 4, wherein the final nanopowder in step (3) is a silicon carbon composite material, graphene, doped nanocarbon or other composite nanopowder material.
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