CN210366998U - Device for macro preparation of carbon-silicon nano material - Google Patents
Device for macro preparation of carbon-silicon nano material Download PDFInfo
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- CN210366998U CN210366998U CN201921052496.1U CN201921052496U CN210366998U CN 210366998 U CN210366998 U CN 210366998U CN 201921052496 U CN201921052496 U CN 201921052496U CN 210366998 U CN210366998 U CN 210366998U
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Abstract
The utility model belongs to the technical field of the nano-material, a macro preparation carbon silicon nanomaterial device is related to, including plasma power control's plasma rifle, the inner chamber of plasma rifle is connected with hydrocarbon gas and the gaseous storage tank of silicon-containing, and the lower extreme of plasma rifle is provided with cooling container, is provided with the gaseous gas cooling ring of release cooling gas among the cooling container. The utility model discloses a control hydrocarbon gas, the gaseous minute chamber of silicon containing admit air or admit air with the chamber, prepare nanometer carbon silicon mixture material and high-purity nanometer carborundum precursor material respectively. The utility model provides a macro preparation carbon silicon nanomaterial device has realized carbon silicon nanomaterial's industrial preparation, has reduced material manufacturing cost by a wide margin.
Description
Technical Field
The utility model belongs to the technical field of the nano-material, a device of macro preparation carbon silicon nano-material is related to.
Background
Silicon carbide single crystals are one of the ideal third-generation semiconductors because of their unique characteristics of large forbidden bandwidth, high breakdown electric field, large thermal conductivity, high electron saturation drift velocity, small dielectric constant, strong radiation resistance, good chemical stability, etc. At present, the most effective method for growing silicon carbide crystals is a Physical Vapor Transport (PVT) method, silicon carbide powder is a main raw material for growing semiconductor silicon carbide single crystals by the PVT method, and the purity of the raw material is a key factor directly influencing the crystal quality and the electrical properties of the grown single crystals. When the nano silicon carbide is applied to a nano composite coating on the surface of a high-temperature alloy and an aviation high-performance structural ceramic, single-crystal nano silicon carbide is needed. The high-purity nano silicon carbide can also be used for preparing a nano composite coating on the surface of a high-temperature alloy, high-performance structural ceramics of an aeroengine, a wave-absorbing coating, electronic and optoelectronic devices of high-frequency, high-power, low-energy consumption, high-temperature-resistant and anti-radiation devices and the like.
Chinese utility model patent application CN108557823A discloses an ultrapure nanometer silicon carbide and a preparation method thereof, comprising the following steps: preparing a gas reaction precursor: mixing carbon-containing gas and silicon-containing gas according to the molar ratio of Si to C of 1: 1.0-1: 1.06 to obtain a gas reaction precursor; preparing ultrapure nano silicon carbide: introducing the gas reaction precursor into the preheated ceramic reactor, and directly synthesizing the nano silicon carbide with the granularity of 50-500nm in a high-temperature region in the ceramic reactor by using the gas reaction precursor. A preparation method of ultrapure nanometer silicon carbide comprises the following steps: respectively introducing carbon-containing gas and silicon-containing gas into the preheated ceramic reactor, and mixing the carbon-containing gas and the silicon-containing gas entering the ceramic reactor according to the Si-C molar ratio of 1: 1.0-1: 1.06; the high temperature area in the ceramic reactor for carbon-containing gas and silicon-containing gas can directly synthesize nano silicon carbide with grain size of 50-500 nm. The silicon carbide produced by the patent has insufficient productivity and purity.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a device of macro preparation carbon silicon nano-material has realized carbon silicon nano-material's industrial preparation, has reduced material manufacturing cost by a wide margin.
The purpose of the utility model is realized through following technical means:
a device for preparing carbon-silicon nano materials in a macroscopic scale comprises a plasma gun controlled by a plasma power supply, wherein an inner cavity of the plasma gun is connected with a hydrocarbon gas and silicon-containing gas storage tank, the lower end of the plasma gun is provided with a cooling container, and a gas cooling ring for releasing cooling gas is arranged in the cooling container.
The cooling gas may be a circulating gas or a disposable gas which is evacuated after use.
The cooling container is connected with the gas-solid separator and is provided with an air suction device, a gas outlet of the gas-solid separator is sequentially connected with the heat exchanger and the mixed gas storage tank, and the mixed gas storage tank is connected with the gas cooling ring to output cooled mixed gas.
When the nano carbon-silicon mixture material is prepared, two plasma guns are respectively connected with a hydrocarbon gas storage tank and a silicon-containing gas storage tank.
When the high-purity nanometer silicon carbide precursor material is prepared, one plasma gun is synchronously connected with a hydrocarbon gas storage tank and a silicon-containing gas storage tank or directly connected with the hydrocarbon gas and the silicon-containing gas.
The air suction device is a blower or a vacuum pump, the blower or the vacuum pump is used for gas replacement and sucking out the separated mixed gas, the lower end of the gas-solid separator is provided with a solid collecting part, the solid collecting part is connected with a vacuum suction storage barrel, and the vacuum suction storage barrel is connected with the vacuum pump.
The power of the blower or the vacuum pump is 10-100 kw/h, and 35000g of carbon-silicon nano material is produced in each hour.
The plasma gun is a non-transferred arc plasma gun with a direct current power supply, a gas input pipeline and an electrode electrically connected with the plasma power supply are arranged in the cavity, and an inner nozzle and an outer nozzle are arranged below the electrode.
When the plasma gun is a DC power supply non-transferred arc plasma gun, the cavity sleeve is made of a circular air inlet cavity sleeve made of a metal conductive material, such as copper alloy, carbon steel material and stainless steel material. When the plasma gun is a high-frequency induction plasma gun, the cavity sleeve is made of quartz or alumina material.
The gas-solid separator is structurally a gas-solid separator with a cooling water jacket, and a transverse partition plate is arranged in the gas-solid separator and divides the gas-solid separator into an upper cavity and a lower cavity. The lower cavity is internally provided with metal filter pipes or/and cloth bag filter pipes at intervals, the lower ends of the filter pipes are closed, the upper ends of the filter pipes are connected through threads, and the upper cavities are opened after penetrating through the diaphragm plates. Each connecting pipe in the upper cavity is provided with an electromagnetic valve for back blowing, the connecting pipe between the electromagnetic valve and the partition plate is connected with an air supply pipe communicated with an air storage tank through a Y-pipe, a connecting pipeline of the cooling container is connected with a lower cavity of the gas-solid separator, an air outlet of the gas-solid separator is arranged in the upper cavity of the gas-solid separator, and a material collecting part is arranged at the lower part of the lower cavity of the gas-solid separator.
A growth controller can be arranged between the plasma gun and the cooling container to better control the appearance characteristics of the carbon-silicon nano material. The growth controller comprises a cylindrical high-temperature resistant pipe, a high-temperature heater is arranged outside the high-temperature resistant pipe, a heat insulation layer such as a heat insulation carbon felt layer or an asbestos layer is arranged outside the heater, a stainless steel water cooling protective shell is arranged outside the heat insulation layer, the water cooling protective shell is provided with two layers, and a cooling medium is arranged in the middle of the water cooling protective shell. The mixed gas storage tank is connected with the growth controller through a pipeline, and a gas flow controller is arranged on the pipeline.
The method for massively preparing the silicon nano material by using the device comprises the following steps:
(1) inputting hydrocarbon gas and silicon-containing gas into a plasma gun, and ionizing and thermally decomposing carbon ions, silicon ions and hydrogen ions in the plasma gun;
(2) the decomposed ions or/and silicon carbide generated by the reaction enter a cooling container, and the cooling gas released by the cooling gas ring is rapidly cooled and stably formed to generate the carbon-silicon nano material.
(3) The generated carbon-silicon nano material, the cooling gas and the hydrogen generated by recombination enter a gas-solid separator for gas-solid separation, the carbon-silicon nano material is retained at the bottom of the gas-solid separator, and the gas enters a pipeline and enters circulation after being rapidly cooled by a heat exchanger.
Firstly, nano carbon-silicon mixture material:
when preparing the nano carbon-silicon mixture material, the two plasma guns are respectively used for inputting hydrocarbon gas and silicon-containing gas, and carbon ions, silicon ions and hydrogen ions which are decomposed enter a cooling container and are mixed to form the carbon-silicon nano material.
The silicon-containing gas is selected from one or more of monosilane, trichlorosilane, dichlorosilane, silicon tetrachloride and chlorotrifluoro silane, preferably monosilane, and the hydrocarbon gas is selected from one or more of methane, ethane, ethylene, acetylene, styrene, benzene and toluene, preferably methane.
The molar ratio of carbon element to silicon element in the hydrocarbon gas and the silicon-containing gas is 10 to 90%: 90 to 10 percent.
The application of the nano carbon-silicon mixture material is as follows: through liquid phase dispersion, adding into solution containing organic matter, further dispersing, and spray drying or oven drying. And (3) entering a closed heating furnace, and coating the carbon-silicon nano mixture material with outer surface layer carbon in a temperature field of 600-1000 ℃ under the protection of inert gas to obtain the lithium ion battery silicon-carbon cathode material.
Secondly, preparing a high-purity nano silicon carbide precursor material:
when the high-purity nano silicon carbide precursor material is prepared, one plasma gun is used, high-purity methane and high-purity silicane are synchronously input or are input after premixing, silicon carbide generated by reaction in the plasma gun and carbon ions, silicon ions and hydrogen ions which are not completely reacted enter a cooling container, and the silicon carbide and the carbon ions, the silicon ions and the hydrogen ions are mixed to form the silicon carbide nano material. The high-purity methane refers to methane gas with the purity of 99.9% -99.999%, the high-purity monosilane refers to monosilane gas with the purity of more than 99.9999%, and the purity of the high-purity nano silicon carbide precursor material is 99.995% -99.9999%.
The molar ratio of the methane to the monosilane is 1: 1-1.1.
The application of the high-purity nano silicon carbide precursor material is as follows: the high-purity nano silicon carbide precursor material is placed in a vacuum heating furnace to carry out further high-temperature carbonization reaction on the precursor material, the reaction temperature is 1200-1600 ℃, and the reaction time is 2-6 hours. Obtaining the crystal growth material applied to the third generation semiconductor single crystal silicon carbide.
The utility model discloses as follows for prior art's beneficial effect:
1. the utility model discloses in inputing into the plasma rifle with hydrocarbon gas and silicon-containing gas, at first the ionization goes out carbon ion in the plasma chamber, silicon ion and hydrogen ion, it is regional to have hydrocarbon gas and the silicon-containing gas that do not have the ionization chemical bond simultaneously and continue to get into the plasma rifle of high frequency induction plasma or the not transfer special high temperature (6000) of DC power supply arc plasma rifle production and become 18000 ℃) plasma arc, hydrocarbon gas and silicon-containing gas high temperature thermal decomposition generate carbon ion, silicon ion and hydrogen ion, thereby make hydrocarbon gas and the more thorough dissociation of silicon-containing gas, improve hydrocarbon gas and silicon-containing gas's effective air input by a wide margin, reach the purpose of macro preparation.
2. The utility model discloses a control hydrocarbon gas, the gaseous minute chamber of silicon containing admit air or admit air with the chamber, both can prepare nanometer carbon silicon mixture material, can prepare high-purity nanometer carborundum precursor material again.
3. The nano carbon-silicon mixed material is an excellent lithium ion battery cathode material: silicon is a semiconductor material, has poor conductivity, is not easy to enter and remove lithium ions, has poor rate capability, and carbon is a good conductor material. The carbon-silicon nano material is mixed, silicon exists in the carbon, and carbon exists in the silicon, so that the entering and the removing of lithium ions are greatly improved, the rate capability is improved, and the lithium ion battery silicon-carbon nano material is a creative precursor material of a lithium ion battery silicon-carbon negative electrode material.
4. After a large amount of cooling gas is cooled by the heat exchanger, a continuous circulating cooling system is formed, so that high-temperature mixed gas generated after ionization and the gas cost required by cooling a large amount of cooling gas for materials are greatly saved, and the material manufacturing cost is greatly reduced.
5. The utility model discloses a plasma rifle, gas-solid separator, heat exchanger, heater, air-blower, vacuum pump etc. be conventional equipment, purchase and equipment convenience, low cost.
6. The device provided by the utility model can realize the macro preparation of carbon silicon nano-material, and its preparation speed can reach 35000g/h at most.
Drawings
FIG. 1 is a connection diagram of an apparatus for preparing a nano carbon-silicon mixture material according to the present invention;
FIG. 2 is a connection diagram of the apparatus for preparing high-purity nano-SiC precursor material according to the present invention;
FIG. 3 is a block diagram of the plasma apparatus of the present invention;
description of the drawings: 1. a plasma power supply; 2. a plasma gun; 3. a hydrocarbon gas storage tank; 4. a silicon source storage tank; 5. cooling the container; 6. a gas cooling ring; 7. a gas-solid separator; 8. a suction device; 9. a heat exchanger; 10. a mixed gas storage tank; 11. a vacuum material sucking and storing barrel; 12. a vacuum pump; 13. an input pipe; 14. An electrode; 15. an inner nozzle; 16. an outer nozzle; 17. a partition plate; 18. an upper chamber; 19. the lower cavity.
Detailed Description
The invention will now be further described with reference to the accompanying drawings, in which reference is made to figures 1-3, showing specific embodiments.
A device for preparing carbon-silicon nano materials in a macroscopic quantity comprises a plasma gun 2 controlled by a plasma power supply 1, wherein an inner cavity of the plasma gun 2 is connected with a hydrocarbon gas and silicon-containing gas storage tank, the lower end of the plasma gun 2 is provided with a cooling container 5, a gas cooling ring 6 is arranged in the cooling container 5, the cooling container 5 is connected with a gas-solid separator 7 and is provided with an air suction device 8, a gas outlet of the gas-solid separator 7 is sequentially connected with a heat exchanger 9 and a mixed gas storage tank 10, and the mixed gas storage tank 10 is connected with the gas cooling ring 6 to output cooled mixed gas.
Referring to the attached figure 1, the number of the plasma guns 2 is two, the two plasma guns are respectively connected with a hydrocarbon gas storage tank 3 and a silicon-containing gas storage tank 4, and the device is used for preparing the nano carbon-silicon mixed material.
Referring to fig. 2, the plasma gun 2 is one, and is connected with a hydrocarbon gas storage tank 3 and a silicon-containing gas storage tank 4 synchronously, the device is used for preparing high-purity nanometer silicon carbide precursor material, and the hydrocarbon gas storage tank 3 and the silicon-containing gas storage tank 4 can also be replaced by a premixed storage tank of hydrocarbon gas and silicon-containing gas.
The air suction device 8 is an air blower or a vacuum pump, the lower end of the gas-solid separator 7 is provided with a solid collecting part, the solid collecting part is connected with a vacuum material suction storage barrel 11, and the vacuum material suction storage barrel 11 is connected with a vacuum pump 12.
Referring to fig. 3, the plasma gun 2 is a dc power non-transferred arc plasma gun, a gas input pipe 13 and an electrode 14 electrically connected to the plasma power are respectively disposed in the chamber, and an inner nozzle 15 and an outer nozzle 16 are disposed below the electrode 14. The DC power supply non-transferred arc plasma gun can be replaced by a high-frequency induction plasma gun.
The gas-solid separator 7 is a gas-solid separator 7 with a cooling water jacket, and a transverse partition plate 17 is arranged in the gas-solid separator 7 to divide the gas-solid separator 7 into an upper chamber 18 and a lower chamber 19. Metal filter pipes or/and cloth bag filter pipes are arranged in the lower cavity 19 at intervals, the lower ends of the filter pipes are closed, the upper ends of the filter pipes are connected through threads, and the upper cavities 18 are opened after penetrating through the diaphragm 17. Each connecting pipe in the upper cavity 18 is provided with an electromagnetic valve for back blowing, a connecting pipe between the electromagnetic valve and the partition plate 17 is connected with an air supply pipe communicated with an air storage tank through a Y-pipe, a connecting pipeline of the cooling container 7 is connected with a lower cavity 19 of the gas-solid separator 9, an air outlet of the gas-solid separator 7 is arranged on the upper cavity 18 of the gas-solid separator 7, and a material collecting part is arranged at the lower part of the lower cavity 19 of the gas-solid separator 7.
The device is provided with various control air valves, water valves, various instruments, meters, gas flow meters and safety anti-aeration valves at corresponding parts so as to control the smooth operation of the device.
The utility model discloses a method of above-mentioned device preparation nanometer carbon silicon mixture material is:
and starting the plasma power supply 1 to respectively input the silicon-containing gas such as monosilane in the silicon source storage tank 4 and the hydrocarbon gas such as methane in the hydrocarbon gas storage tank 3 into the inner cavities of the two plasma guns 2 through the gas flow controllers.
The hydrocarbon gas and the silicon-containing gas are input into the cavities of the plasma guns 2 respectively to ionize and thermally decompose at millisecond-level speed to open chemical bonds combined by carbon ions and hydrogen ions or chemical bonds combined by silicon ions and hydrogen ions, the carbon ions, the hydrogen ions, the silicon ions and the hydrogen ions which are opened through ionization and thermal decomposition respectively enter the cooling container 5, the mixed cooling gas released in large amount through the cooling gas ring 6 efficiently and quickly cools and stably forms the nano carbon-silicon mixture material, the hydrogen formed by recombining the nano carbon-silicon material and the ionized hydrogen ions in the cooling container 5 and the mixed gas released in large amount through the cooling ring enter the gas-solid separator 7 through the connecting pipeline by suction of the suction device 8, and the nano carbon-silicon mixture material and the mixed gas are subjected to gas-solid separation.
Through separation, the nano carbon-silicon mixture material is reserved at the bottom of an inner cavity of a gas-solid separator 7, the separated mixed gas enters a heat exchanger 9 through an air suction device 8 for heat exchange, the hot mixed gas is rapidly cooled to be below 90 ℃, the hot mixed gas is sent into a mixed gas storage tank 10 through a pipeline, and the cooled mixed gas is formed into a circulating reciprocating mode through a connecting pipeline and a gas flow controller and then sent into a gas cooling ring 6.
After the nano carbon-silicon mixture material is rapidly cooled and stably formed, the nano carbon-silicon mixture material is gathered at a solid collecting position at the lower end of the gas-solid separator 7, a vacuum pump 12 is started to vacuumize the vacuum material suction storage barrel 11 to 50-80 kpa, a valve at the bottom of the gas-solid separator 7 is opened to vacuum and suck the material in the gas-solid separator 7 into the vacuum material suction storage barrel 11, and continuous production without stopping is formed.
The utility model discloses a method of above-mentioned device preparation high-purity nanometer carborundum precursor material is:
and starting the plasma power supply 1 to simultaneously input the high-purity monosilane in the silicon source storage tank 4 and the methane in the hydrocarbon gas storage tank 3 into the inner cavity of the same plasma gun 2 through the gas flow controller.
The hydrocarbon gas and the silicon-containing gas are input into a cavity of a plasma gun 2, chemical bonds combined by carbon ions and hydrogen ions and chemical bonds combined by silicon ions and hydrogen ions are opened by ionization and thermal decomposition at a millisecond-level speed, the carbon ions and the silicon ions after the opening of the ionization and thermal decomposition react to produce silicon carbide, then the silicon carbide enters a cooling container 5, the silicon carbide is efficiently and quickly cooled and stably formed into a high-purity nano silicon carbide precursor material by a large amount of mixed cooling gas released by a cooling gas ring 6, the hydrogen formed by recombining the high-purity nano silicon carbide precursor material and ionized hydrogen ions in the cooling container 5 and a large amount of mixed gas released by the cooling ring enter a gas-solid separator 7 through a connecting pipeline by suction of a suction device 8, and the high-purity nano silicon carbide precursor material and the mixed gas are subjected to gas-solid separation.
Through separation, high-purity nano silicon carbide precursor materials are reserved at the bottom of an inner cavity of a gas-solid separator 7, the separated mixed gas enters a heat exchanger 9 through a gas suction device 8 for heat exchange, the hot mixed gas is rapidly cooled to be below 90 ℃, the hot mixed gas is sent into a mixed gas storage tank 10 through a pipeline, and the cooled mixed gas is formed into circulation through a connecting pipeline and a gas flow controller and is sent into a gas cooling ring 6 in a reciprocating mode.
After the high-purity nano silicon carbide precursor material is rapidly cooled and stably formed, the high-purity nano silicon carbide precursor material is gathered at a solid collecting position at the lower end of the gas-solid separator 7, a vacuum pump 12 is started to vacuumize the vacuum material suction storage barrel 11 to 50-80 kpa, a valve at the bottom of the gas-solid separator 7 is opened to vacuum and suck the material in the gas-solid separator 7 into the vacuum material suction storage barrel 11, and continuous production without stopping is formed.
The above-mentioned embodiment is only the preferred embodiment of the present invention, and does not limit the protection scope of the present invention according to this, so: all equivalent changes made according to the structure, shape and principle of the utility model are covered within the protection scope of the utility model.
Claims (9)
1. The device for preparing the carbon-silicon nano material in a macroscopic quantity is characterized by comprising a plasma gun controlled by a plasma power supply, wherein a hydrocarbon gas and silicon-containing gas storage tank is connected to the inner cavity of the plasma gun, a cooling container is arranged at the lower end of the plasma gun, and a gas cooling ring for releasing cooling gas is arranged in the cooling container.
2. The apparatus for macro preparation of carbon silicon nano-material according to claim 1, wherein the cooling container is connected with a gas-solid separator and provided with a gas suction device, a gas outlet of the gas-solid separator is sequentially connected with a heat exchanger and a mixed gas storage tank, and the mixed gas storage tank is connected with a gas cooling ring to output cooled mixed gas.
3. The apparatus for macro preparation of carbon-silicon nanomaterial according to claim 1, wherein there are two plasma guns connected to the hydrocarbon gas storage tank and the silicon-containing gas storage tank, respectively.
4. The apparatus of claim 1, wherein the plasma gun is a single gun that is connected to the hydrocarbon gas tank and the silicon-containing gas tank simultaneously or directly to the hydrocarbon gas and the silicon-containing gas in a pre-mixing tank.
5. The apparatus of claim 1, wherein the plasma gun is a high frequency induction plasma gun or a dc power source non-transferred arc plasma gun.
6. The apparatus for macro preparation of carbon silicon nanometer material according to claim 5, wherein the plasma gun is a DC power supply non-transferred arc plasma gun, a gas input pipe is arranged in the cavity, and an electrode electrically connected with the plasma power supply, and an inner nozzle and an outer nozzle are arranged below the electrode.
7. The apparatus for macro production of carbon silicon nano-materials according to claim 2, wherein the getter device is a blower or a vacuum pump.
8. The apparatus for macro production of carbon-silicon nanomaterial according to claim 2, wherein a transverse partition is provided in the gas-solid separator to divide the gas-solid separator into an upper chamber and a lower chamber, the connecting pipe of the cooling vessel is connected to the lower chamber of the gas-solid separator, and the gas outlet of the gas-solid separator is provided in the upper chamber of the gas-solid separator.
9. The device for macro preparation of carbon-silicon nanomaterial as claimed in claim 2, wherein the lower end of the gas-solid separator is provided with a solid collection part, the solid collection part is connected with a vacuum material suction storage barrel, and the vacuum material suction storage barrel is connected with a vacuum pump.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110255532A (en) * | 2019-07-06 | 2019-09-20 | 金雪莉 | A kind of magnanimity prepares the method and device of carbon silicon nano material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255532A (en) * | 2019-07-06 | 2019-09-20 | 金雪莉 | A kind of magnanimity prepares the method and device of carbon silicon nano material |
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