CN114679832A - Sliding arc discharge plasma device and preparation method of nano powder - Google Patents
Sliding arc discharge plasma device and preparation method of nano powder Download PDFInfo
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- CN114679832A CN114679832A CN202210362740.4A CN202210362740A CN114679832A CN 114679832 A CN114679832 A CN 114679832A CN 202210362740 A CN202210362740 A CN 202210362740A CN 114679832 A CN114679832 A CN 114679832A
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- H05H1/00—Generating plasma; Handling plasma
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- H05H1/482—Arrangements to provide gliding arc discharges
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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; adjusting the proportion of carrier gas, precursor gas and etching gas, and introducing into a closed sliding arc plasma reactor; starting a power supply, an induced draft fan or a vacuum pump, adjusting the reaction pressure of the plasma region, and maintaining the sliding arc to perform discharge reaction in a stable state; the plasma cracks the precursor and etching gas and nucleates, the gas flow velocity is increased in a Venturi tube with a specific proportion, the nano powder material further grows in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector. The method can be used for directly preparing the nano powder material in a gas phase environment, has the characteristics of few arcing limiting factors, simple operation, quick and continuous production and the like, and can be used for various front-edge fields, and the obtained nano powder has various types, small size and high quality.
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, plasma has exhibited its specific advantages in the fields of nanomaterial science and technology. Shenhua group Limited liability company discloses a preparation method of carbon black (patent grant publication No. CN 106543777B), which comprises cracking carbonaceous material at 1400-1800 ℃ by high-temperature plasma to obtain acetylene-rich product, and continuously decomposing the obtained product to obtain carbon black. The method can simplify the acetylene purification step, shorten the production flow of the carbon black and reduce the production cost.
The lithium battery is used as a new energy source to provide a power source for most portable electronic equipment and even electric automobiles, and lithium ions are easier to insert and remove due to the special layered and stacked structure of the graphene powder, so that the graphene is a good choice as a conductive material of the lithium ion battery. Courage et al of electronics technology university disclose a graphene preparation method (patent grant publication No.: CN 108190864B). The method adopts liquid metal tin as a carrier, sugar as a solid carbon source, and dissolves carbon atoms at high temperature. And after cooling, generating graphene on the surface of the metal tin, and then obtaining the graphene through cleaning and separation. Compared with the mechanical stripping, liquid phase stripping and vapor deposition methods of graphene, the method has certain advantages, but a substrate and other operations such as separation, drying and the like are required in the preparation process. In addition, compared with graphite materials, the silicon-carbon composite material has many advantages and is one of the most potential lithium ion battery cathode materials at present. The doped graphene or doped carbon has wide application prospects in the application fields of electrochemistry and electrocatalysts. The preparation method of the nitrogen-doped graphene material is disclosed by Kwangnac university Ganmai and the like, and comprises the following steps: and adding a micromolecular aliphatic amine aqueous solution into the ultrasonically dispersed graphite oxide aqueous solution for hydrothermal reaction for 36-72 h, and separating, washing and drying to obtain the nitrogen-doped graphene material (the patent authorization publication number is CN 103691471B). The material prepared by the method shows good catalytic activity in Michael addition reaction and ester exchange reaction, but the whole preparation needs 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 nonequilibrium of the thermal plasma and the low-temperature plasma on the plasma chemical process, and most of input electric energy can greatly improve the chemical reaction efficiency, so that the low-temperature plasma has high energy utilization rate. In addition, the sliding arc device has simple structure, low cost and convenient operation, and can not be limited by pressure change. Therefore, sliding arc discharge is widely used and studied in methane gas reforming, pollutant degradation, nanomaterial preparation, modification and other fields. Zhangshun et al, Asian silicon industries (Qinghai) GmbH, disclose a method for obtaining hydrogenated silicon tetrachloride material 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 No. CN 108439413B). However, there are few researches and patents on the method for directly preparing nano-powder in a gas phase environment by using a plasma process of sliding arc discharge.
Disclosure of Invention
The invention aims to solve the problem of how to rapidly, simply, continuously, effectively, controllably, low-cost and low-energy-consumption production of a nano powder material in a preparation process, and provides a sliding arc discharge plasma device and a preparation method of the nano powder.
In order to achieve the 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 tangent to the cylindrical electrode; the insulating base plate 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 insulating base plate is separated from the conical electrode through a ceramic wafer, and a gap generated by connecting the other surface of the insulating base plate with the conical electrode is sealed through silicon rubber capable of being cured at room temperature; the venturi tube with the preset proportion is a pipeline with large outlet areas at two ends and small section in the middle, 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 plate and the insulating chassis are connected through an electrode height adjusting hole in the center of the insulating chassis and the height of the insulating chassis is adjusted, and a gap generated between the conical electrode and the insulating chassis is filled through silicon rubber capable of being cured at room temperature; the insulation base plate is a polytetrafluoroethylene disc which is easy to process, can prevent a high-voltage end and a low-voltage end from being short-circuited when being electrified, and is 1/4-1/3 thick; the potsherd is a concentric ring potsherd, can alleviate because the burning phenomenon that a small amount of powder materials lead to is piled up in the electrode zone causes the damage to the reactor chassis, and does not need extra coolant and device to cool down electrode and chassis, and the interior circle is the toper electrode regulation hole, and the excircle diameter slightly is less than tube-shape electrode diameter, remains 1~2 mm between the end circle face of potsherd and toper electrode.
In an embodiment of the invention, the air inlet is positioned below the cylindrical electrode and at the same height with 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 plate.
In an embodiment of the present invention, the ratio of the inlet pipe to the throat pipe of the venturi tube with the predetermined ratio is 5:1 to 20:1, preferably 10:1, so that the conversion rate of the raw material can be 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 less 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 flow meter, 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 the plasma region, and maintaining the sliding arc to perform discharge reaction in a stable state;
(3) the plasma cracks the precursor and the etching gas and nucleates, the gas flow velocity is increased in a Venturi tube with a preset proportion, the nano powder material further grows 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 step (1) is a mixed gas of 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), and nitrogen precursor gas, such as: silicon precursor and carbon precursor, carbon precursor and nitrogen precursor (ammonia or nitrogen gas); the etching gas is a mixed gas of one or more of hydrogen, carbon dioxide and water vapor; the temperature of the gas introduced into the gas inlet can range from room temperature to 300 ℃, and the heated gas can enhance the plasma cracking effect.
In an embodiment of the present invention, when the pressure of the sealed plasma reactor in 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 is in the range of 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 an embodiment of the invention, the plasma reaction under atmospheric pressure in the step (2) adopts an induced draft fan to drive airflow, and the plasma reaction under reduced pressure adopts a vacuum pump to regulate and control pressure so as to reduce the flow of used carrier gas and achieve the purpose of reducing the production cost of the nano powder material. .
In an embodiment of the present invention, the power range of the power source in step (2) is 1 to 50 kW, preferably 20 kW, so that the plasma generator can work for a long time without ablation of the electrode; the range of the no-load voltage is 20 kV-50 kV, preferably 30 kV, the polyatomic gas can be promoted to generate plasma, arc breaking is avoided, and abnormal conditions of electric leakage are avoided.
In an embodiment of the present invention, the final nanopowder obtained in step (3) is a silicon-carbon composite material, graphene, doped nanocarbon or other composite nanopowder materials.
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 materials have great application potential in a plurality of leading-edge fields.
(2) The method can be free from pressure limitation, the reduced plasma reaction pressure is provided by the vacuum pump, the use of carrier gas flow and power consumption is greatly reduced, and the aim of reducing the production cost of the nano powder material is fulfilled.
(3) The method of the invention prevents the damage of the chassis of the reactor caused by abnormal arc combustion phenomenon generated by accumulation of a small amount of nano powder materials on the electrode by adding the ceramic plates, and also prevents the abnormal discharge caused by the falling of the nano powder materials in a plasma region to reduce the yield by increasing a device similar to a Venturi tube 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-an air inlet; 3-silicon rubber; 4-an insulating chassis; 5-ceramic plate; 6-a tapered electrode; 7-a flange; 8-a venturi tube; 9-fluidized bed.
FIG. 2 is an SEM photograph of example 2;
FIG. 3 is an SEM photograph of example 3.
Detailed Description
The technical scheme of the invention is specifically explained 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 is 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 tangent to the cylindrical electrode; the insulating base plate 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 insulating base plate is separated from the conical electrode through a ceramic wafer, and a gap generated by connecting the other surface of the insulating base plate with the conical electrode is sealed through silicon rubber capable of being cured at room temperature; the venturi tube with the preset proportion is a pipeline with large outlet areas at two ends and small section in the middle, 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 flow meter, 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 the plasma region, and maintaining the sliding arc to perform discharge reaction in a stable state;
(3) the plasma cracks the precursor and the etching gas and nucleates, the gas flow velocity is increased in a Venturi tube with a preset proportion, the nano powder material further grows in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector.
The following are specific embodiments of the present invention.
Example 1
As shown in fig. 1, a sliding arc discharge plasma device is used for preparing a nano split material, and the device comprises a cylindrical electrode 1, a tapered electrode 6, an air inlet 2, an insulating base plate (polytetrafluoroethylene base plate) 4, a ceramic plate 5, silicon rubber (high temperature resistant silicon rubber cured 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 ceramic wafer of the concentric ring and the polytetrafluoroethylene chassis are connected through an electrode height adjusting hole in the center of the disk and the height of the polytetrafluoroethylene chassis is adjusted, and a gap generated between the conical electrode and the chassis is filled through room-temperature cured silicon rubber; the bottom of the cylindrical electrode is mechanically connected with a polytetrafluoroethylene chassis through a welding flange; the top of the cylindrical electrode is mechanically connected with the inlet of the Venturi tube with a specific proportion through a welding flange; the inlet of the fluidized bed is mechanically connected with the outlet of the Venturi tube with a specific proportion.
Step 2: injecting gas into the gas inlet, and turning on a power switch; selecting a draught fan or a vacuum pump device according to the pressure required in the reaction process and adjusting the pressure;
and step 3: after the reaction is finished, collecting final powder products in a cyclone separator connected with the fluidized bed and a bag-type dust collector connected with the cyclone separator.
Example 2
A preparation method of graphene powder applying the method of embodiment 1 comprises the following specific steps: the flow rates of argon, methane and carbon dioxide are respectively adjusted to be 14 slm, 2 slm and 1 slm by a mass flow meter, and all gases are mixed and preheated and then tangentially enter from an air inlet of the plasma generator. The power supply is turned on, the power is 20 kw, and the reaction time is 10 min. And opening the induced draft fan to ensure that the reaction pressure of the plasma region is under 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 the folding of each other and the edge curling in the prepared graphene nanoplatelets.
Example 3
A preparation method of a silicon-carbon composite material applying the method of the embodiment 1 comprises the following specific steps: the flow rates of argon, methane and hydrogen are respectively adjusted to 10 slm, 1 slm and 0.5 slm by a mass flow meter, and the mixed gas of argon, methane and hydrogen is tangentially fed from the gas inlet of the plasma generator. After the sliding arc was stabilized, the silane flow was adjusted to 1 slm with a mass flow meter and silane was fed in from the gas inlet. The power supply is turned on, the power is 20 kw, and the reaction time is 10 min. And opening a vacuum pump to enable the reaction pressure of the plasma region to be 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 sheet-shaped.
The above are preferred embodiments of the present invention, and all changes made according to the technical scheme of the present invention that produce functional effects do not exceed the scope of the technical scheme of the present invention belong to the protection scope of the present invention.
Claims (10)
1. A sliding arc discharge plasma device is characterized by comprising 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 tangent to the cylindrical electrode; the insulating base plate 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 insulating base plate is separated from the conical electrode through a ceramic wafer, and a gap generated by connecting the other surface of the insulating base plate with the conical electrode is sealed through silicon rubber capable of being cured at room temperature; the venturi tube with the preset proportion is a pipeline with large outlet areas at two ends and small section in the middle, 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.
2. The sliding arc discharge plasma device according to claim 1, wherein the conical electrode, the ceramic plate and the insulating base plate are connected through an electrode height adjusting hole in the center of the insulating base plate, the height of the insulating base plate is adjusted, and a gap generated between the conical electrode and the insulating base plate is filled by silicon rubber capable of being cured at room temperature; the insulating base plate is a polytetrafluoroethylene disc, and the thickness of the insulating base plate is 1/4-1/3 of the diameter of the disc; the ceramic wafer is a concentric ring ceramic wafer, 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 bottom circular surfaces of the ceramic wafer and the conical electrode.
3. The sliding arc discharge plasma device according to 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.
4. The sliding arc discharge plasma device according to claim 1, wherein the ratio of the inlet pipe to the throat pipe of the venturi tube with the predetermined ratio is 5:1 to 20: 1; the proportion of the length of the Venturi tube to the inlet tube is 5: 1-15: 1.
5. The method for preparing nano powder by using the device as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
(1) the proportion of the carrier gas, the precursor gas and the etching gas is adjusted by a mass flow meter, 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 the plasma region, and maintaining the sliding arc to perform discharge reaction in a stable state;
(3) the plasma cracks the precursor and the etching gas and nucleates, the gas flow velocity is increased in a Venturi tube with a preset proportion, the nano powder material further grows in a fluidized bed, and finally the nano powder material is collected through a cyclone separator and a bag-type dust collector.
6. The method for preparing nano-powder according to claim 5, wherein the plasma reaction under atmospheric pressure in the step (2) adopts a draught fan to drive airflow, and the plasma reaction under reduced pressure adopts a vacuum pump to regulate and control pressure.
7. The method for preparing nano powder according to claim 5, 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 a mixed gas of one or more of hydrogen, carbon dioxide and water vapor; the temperature of the gas introduced into the gas inlet may range from room temperature to 300 deg.c.
8. The method for preparing the nano powder according to claim 5, wherein 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: 1-16: 1, and the mass flow ratio of the precursor gas to the etching gas is 1: 1-10: 1; when the pressure is in the range of 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.
9. The method for preparing nano powder according to claim 5, wherein the power range of the power supply in the step (2) is 1-50 kW; the range of the no-load voltage is 20 kV-50 kV.
10. The method for preparing nano powder according to claim 5, wherein the final nano powder in the step (3) is a silicon-carbon composite material, graphene, doped nano carbon or other composite nano powder materials.
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