CN115650237A - Method and device for preparing silicon carbide raw material by chemical vapor deposition method - Google Patents
Method and device for preparing silicon carbide raw material by chemical vapor deposition method Download PDFInfo
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Abstract
The application relates to a device and a method for preparing a silicon carbide raw material by a chemical vapor deposition method, and the device comprises a furnace body, a graphite piece, a gas supply system, a vacuum pump and a water storage container; graphite spare sets up inside the furnace body for the deposit sample is treated in the fixed heating, and the bottom of furnace body is equipped with the intake pipe, this intake-tube connection gas supply system, and gas supply system is used for carrying the deposit gas source gas in to the furnace body, and the top side of furnace body passes through the pipe connection vacuum pump, wherein is equipped with filter equipment between vacuum pump and the furnace body, vacuum pump connection water container. The method is carried out by adopting a device for preparing the silicon carbide coating by a chemical vapor deposition method, a graphite piece is placed in a vapor deposition furnace, the vacuum pumping is carried out, gas source gas is introduced into the vapor deposition furnace, the vapor deposition furnace is heated, then the temperature is kept, HCl, siC and impurities are generated by decomposition, and the silicon carbide is attached to the graphite piece and collected. The device and the process for producing the silicon carbide have the advantages of low cost, high productivity, large crystal grains and less impurities.
Description
Technical Field
The application relates to the technical field of third-generation semiconductors, in particular to a method and a device for preparing a silicon carbide raw material by a chemical vapor deposition method.
Background
The semiconductor industry has been developed through 3 stages, the first generation of semiconductor materials is represented by silicon; gallium arsenide, a second generation semiconductor material, has also been widely used; and the third generation semiconductor material represented by silicon carbide has obvious performance advantages compared with the first two generations. The silicon carbide is a core material in important fields such as satellite communication, high-voltage power transmission and transformation, rail transit, electric automobiles, communication base stations and the like, and particularly has an irreplaceable effect in the fields such as aerospace and the like. The silicon carbide material has huge demand, the silicon carbide industry is vigorously developed, and two billions of industries of raw materials and equipment can be led and driven. It is particularly important to produce silicon carbide raw material of optimum quality.
The conventional high-temperature synthesis process is mainly used for manufacturing silicon carbide in the industry at present, and the conventional method has the disadvantages of high cost, low yield, small crystal grains and more impurities.
The traditional synthetic silicon carbide is synthesized by heating high-purity metal silicon powder and high-purity carbon powder (graphite powder) in vacuum or protective atmosphere. The silicon carbide is produced by the reaction of elemental silicon and carbon at 1150-1250 ℃ and is synthesized by the following reaction:
Si+C→SiC
however, metal silicon inevitably contains metal impurities such as iron, aluminum, calcium and the like, so that the silicon carbide finished product has more impurities and lower purity.
Disclosure of Invention
In order to overcome the problems in the prior art, the application provides a method and a device for preparing a silicon carbide raw material by a chemical vapor deposition method.
The method and the device for preparing the silicon carbide raw material by the chemical vapor deposition method adopt the following technical scheme:
a device for preparing a silicon carbide raw material by a chemical vapor deposition method comprises a furnace body, a graphite piece, an air supply system, a vacuum pump and a water storage container; graphite spare sets up inside the furnace body for the deposit sample is treated in the fixed heating, and the bottom of furnace body is equipped with the intake pipe, this intake-tube connection gas supply system, and gas supply system is used for carrying the deposit gas source gas in to the furnace body, and the top side of furnace body passes through the pipe connection vacuum pump, wherein is equipped with filter equipment between vacuum pump and the furnace body, vacuum pump connection water container.
By adopting the technical scheme, the silicon carbide coating is prepared on the graphite piece body by a chemical vapor deposition method with a specific device, so that the preparation period of the coating is shortened, and the preparation cost of the material is reduced. The tail gas discharged after the reaction contains HCl generated by the reaction, naCl and water can be discharged by adding NaOH to react, the vacuum pump is used for adjusting the pressure in the furnace body and discharging the tail gas, and the filtering device is arranged between the vacuum pump and the furnace body, so that furnace dust in the furnace body can be effectively collected.
Preferably, a pressure regulating valve is arranged on a connecting pipeline between the furnace body and the vacuum pump, a furnace cover at the top of the furnace body is hermetically connected with the furnace body, and a detachable dust collecting pipe is arranged at the top of the furnace cover.
Through adopting above-mentioned technical scheme, pressure regulating valve can adjust the pressure of furnace body according to the operating condition of furnace body, and the dust collecting pipe that is equipped with on the bell of furnace body sealing connection is after the furnace body work is ended, opens and can collect the ashes in the furnace body between the bell, has reduced the influence that the furnace ash is healthy to operating personnel after the bell is opened.
Preferably, the gas supply system comprises a plurality of methyl trichlorosilane raw material tanks, a mixing tank for mixing chemical gas and a buffer tank for buffering raw materials, wherein the raw material tanks, the mixing tank and the buffer tank are sequentially connected, and the buffer tank is communicated with a gas inlet of the furnace body; the external of the raw material tank is connected with an oil temperature machine, and the mixing tank and the buffer tank are both charged with air through an inflation tube.
Preferably, an inflation switch valve and a flowmeter are arranged on an inflation tube arranged in the air supply system
Through adopting above-mentioned technical scheme, the design of a plurality of feed tanks can switch after methyl trichlorosilane in one of them feed tank runs out, has avoided the influence of shut down operation to carborundum quality. And the gas guide setting from the raw material tank to the mixing tank and then to the buffer tank controls the gas intake from the raw material gas, the carrier gas and the buffer gas through an inflation switch valve and a flowmeter on the inflation pipe, and effectively controls the gas intake rate.
Preferably, valves are arranged on a plurality of trichloromethylsilane (MTS) raw material tanks in the gas supply system, the flow rate of MTS is 20-400g/H, ar or N2 is used as diluent gas in the buffer tank, the flow rate of the diluent gas is 0.02-0.4m3/H, H2 is used as a carrier of trichloromethylsilane in the mixing tank, and the flow rate of H2 is 0.02-0.4m3/H.
By adopting the technical scheme, the silicon carbide coating is prepared by adopting a chemical vapor deposition method, so that the preparation period of the coating is shortened, and the preparation cost of the material is reduced.
Preferably, the heating mechanism is annularly distributed in the furnace body, the discharging plate, the deposition box and the air inlet box are sequentially distributed in the furnace body from top to bottom, the upper heater, the middle heater and the lower heater are distributed on the side walls of the heating mechanism corresponding to the discharging plate, the deposition box and the air inlet box, and the bottom of the air inlet chamber is further provided with the bottom heater.
Through adopting above-mentioned technical scheme, the inlet box in the furnace body can heat the gas that just got into the furnace body, is used for in the control of carborundum deposition in-process temperature in the setting box, and the upper portion heater of stripper side can heat the furnace body top, and the heating mechanism of distributing type can let the more swift even of the interior temperature adjustment of furnace body.
Preferably, the furnace shell of the furnace body is of a double-layer water-cooling jacket structure, the inner wall is made of stainless steel, a furnace lining is installed on the inner wall, the outer wall is made of carbon steel, a groined rib plate is welded outside the inner wall, and a water jacket is welded outside the groined rib plate.
By adopting the technical scheme, the furnace shell is optimally designed because the furnace body is required to have a high-temperature and high-pressure state when reaction is carried out. The design of the internal heating resistance furnace is a double-layer water-cooling jacket structure, the inner wall is made of stainless steel, the outer wall is made of carbon steel, a # -shaped rib plate is welded outside the inner wall, and a water jacket is welded inside a # -shaped frame.
Preferably, the furnace lining adopts a three-layer refractory structure and comprises an aluminum carbonate fiber felt, an aluminum silicate fiber folding block and a vacuum forming module which are laminated from outside to inside, wherein the heating mechanism adopts a heat-resistant steel nail screwed into the vacuum forming module.
By adopting the technical scheme, the electric heating mechanism is screwed into the vacuum forming module by adopting the heat-resistant steel nails and is fixed by the heating vacuum module, the integral structure thickness of the furnace lining is 300mm,20mm aluminum silicate fiber blanket, the capacity is 160g/cm < 3 >, 200mm thick aluminum silicate fiber block, the volume weight is 160g/cm < 3 >, 80mm thick vacuum forming module, the capacity is 420g/cm < 3 >, and the density of the vacuum forming module is relatively higher, so the heat-resistant steel nails adopted by elements for fixing the heating mechanism are very stable and reliable in connection of the heating mechanism.
A method for preparing silicon carbide raw material by chemical vapor deposition method is carried out by adopting a device for preparing silicon carbide coating by electric coupling chemical vapor deposition method, putting a graphite piece into a vapor deposition furnace, vacuumizing, introducing mixed gas of methyltrichlorosilane, dilution gas and buffer gas into the vapor deposition furnace, heating again, then preserving heat, and decomposing to generate HCl, siC and impurities; introducing HCl into a water storage container added with NaOH to react to generate NaCl, discharging the NaCl, crushing SiC, introducing oxygen to anneal, weighing and packaging to obtain a finished product; hydrofluoric acid and isopropanol are added into the impurities for cleaning to generate waste liquid and acid mist waste gas.
Preferably, the silicon carbide is methyl trichlorosilane, the temperature is raised to 400-600 ℃ within 2-4 hours in a vapor deposition furnace, the temperature is kept for 2-3 hours, the temperature is raised to 800-1200 ℃ within 5-8 hours, the temperature is kept for 1-2 hours, and the whole process is carried out under the condition of 30-100torr, and the reaction equation is as follows: siCl3CH3 → SiC +3HCl.
By adopting the technical scheme, through the step-by-step heating program and heat preservation, impurities and moisture in the graphite piece can be fully volatilized after heat preservation is carried out for 2-3 hours at 400-600 ℃, and the product is prevented from being polluted. The temperature distribution in the furnace body can be more uniform by keeping the temperature at 800-1200 ℃ for 1-2 hours, the temperature difference is eliminated, and the phenomenon that the silicon carbide deposition speed is too high due to high local temperature, the particle gap of the silicon carbide is enlarged, and the density is reduced is avoided.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the vapor deposition furnace has the advantages that through the staged temperature rise procedure and heat preservation, the temperature distribution in the furnace body is more uniform, the temperature difference is eliminated, the phenomenon that the deposition speed of silicon carbide is too high due to high local temperature is avoided, and the density of the silicon carbide is improved;
the silicon carbide particles produced by CVD are large, averaging about 50mm3. While the largest competitor in Japan currently in the industry produces particles of a size of only 0.2-8mm3. The larger particle size can increase the crystal growth time, and grow thicker crystal bars, thereby processing more substrates;
3. the company adopts the advanced Chemical Vapor Deposition (CVD) technology, can overcome the defects of high cost, low productivity, small crystal grains and more impurities in the traditional method for manufacturing the silicon carbide, can better meet the market demand and has strong competitiveness.
Drawings
FIG. 1 is a process flow diagram of a chemical vapor deposition method for producing a silicon carbide feedstock;
FIG. 2 is a schematic view showing the overall structure of an apparatus for producing a silicon carbide raw material by a chemical vapor deposition method;
FIG. 3 is a schematic view showing the structure of a furnace shell in an apparatus for producing a silicon carbide raw material by a chemical vapor deposition method;
FIG. 4 is a schematic view showing the connection structure of the lining and the heating structure in an apparatus for producing a silicon carbide raw material by a chemical vapor deposition method
Description of reference numerals: 1. a furnace body; 11. an air inlet pipe; 12. a furnace cover; 13. a dust collecting pipe; 15. A heating mechanism; 151. an upper heater; 152. a middle heater; 153. a lower heater; 154. a bottom heater; 16. a stripper plate; 17. a deposition chamber; 18. an air intake box; 19. A furnace shell; 191. an inner wall; 1911. a groined rib plate; 1912. a water jacket; 192. a furnace lining; 193. An outer wall; 194. an aluminum carbonate fiber mat; 195. an aluminum silicate fiber folding block; 196. a vacuum forming module; 2. a graphite piece; 3. an air supply system; 31. a raw material tank; 311. an oil temperature machine; 312. A valve; 32. a mixing tank; 33. a buffer tank; 34. an inflation tube; 341. an inflation switch valve; 342. a flow meter; 4. a vacuum pump; 41. a filtration device; 42. a pressure regulating valve; 5. A water storage container.
Detailed Description
The present application is described in further detail below with reference to figures 1-4.
The embodiment of the application discloses a device and a method for preparing a silicon carbide raw material by a chemical vapor deposition method.
Referring to fig. 2, 3 and 4, an apparatus for preparing a silicon carbide raw material by a chemical vapor deposition method includes a furnace body 1, a graphite piece 2, a gas supply system 3, a vacuum pump 4 and a water storage container 5; graphite part 2 sets up inside furnace body 1 for the deposit sample is treated in the fixed heating, and the bottom of furnace body 1 is equipped with intake pipe 11, and this intake pipe 11 is connected gas supply system 3, and gas supply system 3 is used for carrying the deposit gas source gas in to furnace body 1, and the top side of furnace body 1 passes through pipe connection vacuum pump 4, wherein is equipped with filter equipment 41 between vacuum pump 4 and the furnace body 1, and water container 5 is connected to vacuum pump 4. Only a special device is used for preparing the silicon carbide coating on the graphite piece 2 body by a chemical vapor deposition method, so that the preparation period of the coating is shortened, and the preparation cost of the material is reduced. The tail gas discharged after the reaction contains HCl generated by the reaction, and can be discharged by adding NaOH to react NaCl and water, the vacuum pump 4 is used for adjusting the pressure in the furnace body 1 and discharging the tail gas, and the filtering device 41 is arranged between the vacuum pump 4 and the furnace body 1, so that the furnace dust in the furnace body 1 can be effectively collected.
Referring to fig. 4, a method for preparing a silicon carbide raw material by a chemical vapor deposition method is carried out by adopting a device for preparing a silicon carbide coating by an electric coupling chemical vapor deposition method, a graphite piece 2 is placed in a vapor deposition furnace, vacuum pumping is carried out, mixed gas of methyl trichlorosilane, dilution gas and buffer gas is introduced into the vapor deposition furnace, the temperature is raised again, and then heat preservation is carried out, and HCl, siC and impurities are generated by decomposition; introducing HCl into a water storage container 5 added with NaOH to react to generate NaCl, discharging the NaCl, crushing SiC, introducing oxygen to anneal, weighing and packaging to obtain a finished product; hydrofluoric acid and isopropanol are added into the impurities for cleaning to generate waste liquid and acid mist waste gas.
Referring to fig. 2, 3 and 4, a pressure regulating valve 42 is arranged on a connecting pipeline between the furnace body 1 and the vacuum pump 4, the furnace cover 12 on the top of the furnace body 1 is hermetically connected with the furnace body 1, and a detachable dust collecting pipe 13 is arranged on the top of the furnace cover 12. The pressure regulating valve 42 can regulate the pressure of the furnace body 1 according to the working state of the furnace body 1, and after the furnace body 1 finishes working, the dust collecting pipe 13 arranged on the furnace cover 12 connected with the furnace body 1 in a sealing way is opened between the furnace covers 12 to collect the furnace dust in the furnace body 1, so that the influence of the furnace dust on the health of operators after the furnace cover 12 is opened is reduced.
Referring to fig. 2, 3 and 4, the gas supply system 3 includes a plurality of methyltrichlorosilane raw material tanks 31, a mixing tank 32 for mixing chemical gas, and a buffer tank 33 for buffering raw material, wherein the raw material tanks 31, the mixing tank 32 and the buffer tank 33 are connected in sequence, and the buffer tank 33 is communicated with the gas inlet of the furnace body 1; an oil temperature machine 311 is connected outside the raw material tank 31, and the mixing tank 32 and the buffer tank 33 are filled with air through an inflation pipe 34.
Referring to fig. 2, 3 and 4, an inflation switch valve 341 and a flow meter 342 are provided on the inflation tube 34 provided in the gas supply system 3. The design of a plurality of raw material tanks 31 can be switched after the methyl trichlorosilane in one raw material tank 31 is used up, so that the influence of shutdown operation on the quality of silicon carbide is avoided. And the gas guiding arrangement from the raw material tank 31 to the mixing tank 32 to the buffer tank 33, the gas intake from the raw material gas, the carrier gas and the buffer gas is controlled by the inflation switch valve 341 and the flow meter 342 on the inflation tube 34, and the gas intake rate is effectively controlled.
Referring to fig. 2, 3 and 4, valves 312 are provided on a plurality of trichloromethylsilane (MTS) feed tanks 31 in the gas supply system 3, the MTS flow rate is 20 to 400g/H, ar or N2 is used as a diluent gas in the buffer tank 33, the diluent gas flow rate is 0.02 to 0.4m3/H, H2 is used as a carrier of trichloromethylsilane in the mixing tank 32, and the H2 flow rate is 0.02 to 0.4m3/H. The silicon carbide coating is prepared by adopting a chemical vapor deposition method, so that the preparation period of the coating is shortened, and the preparation cost of the material is reduced.
Referring to fig. 2, 3 and 4, a heating mechanism is annularly distributed in the furnace body 1, a discharging plate 16, a deposition box 17 and an air inlet box 18 are sequentially distributed in the furnace body 1 from top to bottom, an upper heater 151, a middle heater 152 and a lower heater 153 are distributed on the side wall of the heating mechanism 15 corresponding to the discharging plate 16, the deposition box 17 and the air inlet box 18, and a bottom heater 154 is further arranged at the bottom of the air inlet chamber. The gas inlet box 18 in the furnace body 1 can heat the gas which just enters the furnace body 1, the deposition box 17 is used for controlling the temperature in the silicon carbide deposition process, the upper heater 151 on the side surface of the discharging plate 16 can heat the top of the furnace body 1, and the distributed heating mechanism 15 can enable the temperature in the furnace body 1 to be adjusted more quickly and uniformly.
Referring to fig. 2, 3 and 4, the furnace shell 19 of the furnace body 1 is a double-layer water-cooling jacket structure, the inner wall 191 is made of stainless steel, the furnace lining 192 is installed on the inner wall 191, the outer wall 193 is made of carbon steel, a # -shaped rib plate 1911 is welded outside the inner wall 191, and a water jacket 1912 is welded outside the # -shaped rib plate 1911. Since the inside of the furnace body 1 is required to have a state of high temperature and high pressure at the time of performing the reaction, the furnace shell 19 is optimally designed. The design of the internal heating type resistance furnace is a double-layer water-cooling jacket structure, the inner wall 191 is made of stainless steel, the outer wall 193 is made of carbon steel, a # -shaped rib plate is welded outside the inner wall 191, and a water jacket 1912 is welded in a # -shaped frame.
Referring to fig. 2, 3 and 4, the furnace lining 192 has a three-layer refractory structure, and includes an aluminum carbonate fiber felt 194, an aluminum silicate fiber folded block 195 and a vacuum forming module 196, which are stacked from outside to inside, wherein the heating mechanism 15 is screwed into the vacuum forming module 196 by heat-resistant steel nails. The electric heating mechanism is screwed into the vacuum forming module 196 by adopting heat-resistant steel nails and is fixed by the heating vacuum module, the integral structure thickness of the furnace lining 192 is 300mm,20mm aluminum silicate fiber blanket, the capacity is 160g/cm3,200mm thick aluminum silicate fiber block, the volume weight is 160g/cm3, the capacity of the 80mm thick vacuum forming module 196 is 420g/cm3, and the density of the vacuum forming module 196 is relatively higher in the form, so the heat-resistant steel nails adopted for fixing elements of the heating mechanism 15 are adopted, and the connection of the heating mechanism 15 is very stable and reliable.
The working principle is as follows: hang the graphite spare in the deposit box through the tungsten filament on the stripper in the furnace body to seal the lid dress, then can carry out the evacuation to the furnace body through the vacuum pump, intake through the intake pipe of air supply system follow furnace body bottom after accomplishing the evacuation, and heat in the furnace body through heating mechanism. Among the gas supply system, methyl trichlorosilane in the head tank mixes with H2 through the hybrid tube, and enters into the furnace body along the intake pipe after mixing with rare gas through the buffer tank. The gas entering the furnace body is heated, insulated, heated and insulated in the furnace body, silicon carbide particles are attached to the graphite piece, the generated HCl and impurities enter a water storage container under the action of a vacuum pump, naOH and HCl are heated in the water storage container to react into NaCl, and the residual impurities are cleaned by hydrofluoric acid and isopropanol to generate waste liquid and acid mist waste gas which are collected.
Example 2
Referring to fig. 2, 3 and 4, an apparatus for preparing a silicon carbide raw material by a chemical vapor deposition method includes a furnace body 1, a graphite piece 2, a gas supply system 3, a vacuum pump 4 and a water storage container 5; graphite part 2 sets up inside furnace body 1 for the deposit sample is treated in the fixed heating, and the bottom of furnace body 1 is equipped with intake pipe 11, and this intake pipe 11 is connected gas supply system 3, and gas supply system 3 is used for carrying the deposit gas source gas in to furnace body 1, and the top side of furnace body 1 passes through pipe connection vacuum pump 4, wherein is equipped with filter equipment 41 between vacuum pump 4 and the furnace body 1, and water container 5 is connected to vacuum pump 4. Only a special device is used for preparing the silicon carbide coating on the graphite piece 2 body by a chemical vapor deposition method, so that the preparation period of the coating is shortened, and the preparation cost of the material is reduced. The tail gas discharged after the reaction contains HCl generated by the reaction, and can be discharged by adding NaOH to react with NaCl and water, the vacuum pump 4 is used for adjusting the pressure in the furnace body 1 and discharging the tail gas, and the filtering device 41 is arranged between the vacuum pump 4 and the furnace body 1, so that the furnace dust in the furnace body 1 can be effectively collected.
Referring to fig. 1, a method for preparing a silicon carbide raw material by a chemical vapor deposition method is carried out by adopting a device for preparing a silicon carbide coating by an electric coupling chemical vapor deposition method, a graphite piece 2 is placed in a vapor deposition furnace, vacuum pumping is carried out, mixed gas of methyl trichlorosilane, dilution gas and buffer gas is introduced into the vapor deposition furnace, the temperature is raised again, and then heat preservation is carried out, and HCl, siC and impurities are generated by decomposition; introducing HCl into a water storage container 5 added with NaOH to react to generate NaCl, discharging the NaCl, crushing SiC, introducing oxygen to anneal, weighing and packaging to obtain a finished product; hydrofluoric acid and isopropanol are added into the impurities for cleaning to generate waste liquid and acid mist waste gas.
Referring to fig. 1, the silicon carbide is prepared by heating methyltrichlorosilane to 400-600 ℃ in a vapor deposition furnace for 2-4 hours, preserving heat for 2-3 hours, then heating to 800-1200 ℃ in 5-8 hours, preserving heat for 1-2 hours, and the whole process is carried out under the condition of 30-100torr, and the reaction equation is as follows: siCl3CH3 → SiC +3HCl. Through the staged heating program and heat preservation, impurities and moisture in the graphite piece 2 can be fully volatilized after heat preservation is carried out for 2-3 hours at 400-600 ℃, and the product is prevented from being polluted. The temperature distribution in the furnace body 1 can be more uniform by keeping the temperature at 800-1200 ℃ for 1-2 hours, the temperature difference is eliminated, and the phenomenon that the silicon carbide deposition speed is too high due to high local temperature, the particle gap of the silicon carbide is enlarged, and the density is reduced is avoided.
The silicon carbide particles produced by the CVD process are large in size, averaging about 50mm3. While the largest competitor in Japan currently in the industry produces particles of a size of only 0.2-8mm3. Larger grain sizes may allow for increased nucleation times, resulting in thicker boules and thus more substrates to be processed.
The following table compares the CVD process with the conventional high temperature synthesis process
The following table compares the impurity levels of the CVD process and the high temperature synthesis process of the Japanese competitor
The raw material generated by adopting the high-temperature synthesis method has small granularity and short crystal growth time, and the thickness of a crystal bar is generally not more than 2cm. The thickness of the crystal bar grown by adopting the CVD method raw material is generally 3-5cm.
The preparation of silicon carbide has been a global problem, and the crystal growth process with high stability is the most core technology, and the core technology has the advantages of low cost, high yield, large crystal grain and little impurity. The silicon carbide produced by the Chemical Vapor Deposition (CVD) method completely meets the market demand, not only can make up for the domestic vacancy, but also can lead a brand-new era.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A device for preparing silicon carbide raw material by chemical vapor deposition method is characterized in that: comprises a furnace body (1), a graphite piece (2), an air supply system (3), a vacuum pump (4) and a water storage container (5); graphite spare (2) set up inside furnace body (1) for the sample is waited to deposit in the fixed heating, the bottom of furnace body (1) is equipped with intake pipe (11), and air supply system (3) are connected in this intake pipe (11), air supply system (3) are used for carrying the gas source gas for the deposit in to furnace body (1), the top side of furnace body (1) passes through pipe connection vacuum pump (4), and wherein be equipped with filter equipment (41) between vacuum pump (4) and furnace body (1), and water storage container (5) is connected in vacuum pump (4).
2. An apparatus for preparing silicon carbide feedstock by chemical vapor deposition as claimed in claim 1, wherein: the furnace is characterized in that a pressure regulating valve (42) is arranged on a connecting pipeline between the furnace body (1) and the vacuum pump (4), the furnace cover (12) at the top of the furnace body (1) is hermetically connected with the furnace body (1), and a detachable dust collecting pipe (13) is arranged at the top of the furnace cover (12).
3. An apparatus for preparing silicon carbide feedstock by chemical vapor deposition as claimed in claim 1, wherein: the gas supply system (3) comprises a plurality of methyltrichlorosilane raw material tanks (31), a mixing tank (32) for mixing chemical gas and a buffer tank (33) for buffering raw materials, wherein the raw material tanks (31), the mixing tank (32) and the buffer tank (33) are sequentially connected, and the buffer tank (33) is communicated with a gas inlet of the furnace body (1); the oil temperature machine (311) is connected outside the raw material tank (31), and the mixing tank (32) and the buffer tank (33) are filled with air through the inflation pipe (34).
4. An apparatus for preparing silicon carbide feedstock by chemical vapor deposition as claimed in claim 3, wherein: an inflation switch valve (341) and a flowmeter (342) are arranged on an inflation tube (34) arranged in the gas supply system (3).
5. An apparatus for preparing silicon carbide feedstock by chemical vapor deposition as claimed in claim 4, wherein: valves (312) are arranged on a plurality of trichloromethyl silane (MTS) raw material tanks (31) in the gas supply system (3), the flow rate of MTS is 20-400g/H, ar or N2 is used as diluent gas in a buffer tank (33), the flow rate of the diluent gas is 0.02-0.4m3/H, H2 is used as a carrier of trichloromethyl silane in a mixing tank (32), and the flow rate of H2 is 0.02-0.4m3/H.
6. An apparatus for preparing silicon carbide feedstock by chemical vapor deposition as claimed in claim 1, wherein: the annular distribution has heating mechanism (15) in furnace body (1), and furnace body (1) is interior from top to bottom distributes in proper order has stripper (16), deposit case (17) and inlet box (18), heating mechanism (15) distribute on the lateral wall that stripper (16), deposit case (17) and inlet box (18) correspond and have upper portion heater (151), middle part heater (152) and lower part heater (153), and the bottom of inlet chamber still is equipped with bottom heater (154).
7. An apparatus for preparing silicon carbide feedstock by chemical vapor deposition according to claim 6 wherein: the furnace shell (19) of the furnace body (1) is of a double-layer water-cooling jacket structure, the inner wall (191) is made of stainless steel, the furnace lining (192) is installed on the inner wall (191), the outer wall (193) is made of carbon steel, a groined rib plate (1911) is welded outside the inner wall (191), and a water jacket (1912) is welded outside the groined rib plate (1911).
8. An apparatus for producing silicon carbide feedstock by chemical vapor deposition as claimed in claim 7, wherein: the furnace lining (192) adopts a three-layer refractory structure and comprises an aluminum carbonate fiber felt (194), an aluminum silicate fiber folding block (195) and a vacuum forming module (196), which are laminated from outside to inside, wherein the heating mechanism (15) adopts heat-resistant steel nails to screw into the vacuum forming module (196).
9. A method for preparing silicon carbide raw material by chemical vapor deposition is characterized in that: the method is carried out by adopting a device for preparing the silicon carbide coating by adopting an electric coupling chemical vapor deposition method, a graphite piece (2) is placed in a vapor deposition furnace, the vacuum pumping is carried out, mixed gas of methyl trichlorosilane, dilution gas and buffer gas is introduced into the vapor deposition furnace, the temperature is raised again, and then the heat is preserved, and HCl, siC and impurities are generated by decomposition; introducing HCl into a water storage container (5) added with NaOH to react to generate NaCl, discharging the NaCl, crushing SiC, introducing oxygen to anneal, weighing and packaging to obtain a finished product; hydrofluoric acid and isopropanol are added into the impurities for cleaning to generate waste liquid and acid mist waste gas.
10. A chemical vapor deposition process for preparing a silicon carbide feedstock as recited in claim 9, wherein: the silicon carbide is prepared by heating methyltrichlorosilane to 400-600 ℃ within 2-4 hours in a vapor deposition furnace, preserving heat for 2-3 hours, then heating to 800-1200 ℃ within 5-8 hours, preserving heat for 1-2 hours, and keeping the whole process at 30-100torr, wherein the reaction equation is as follows: siCl3CH3 → SiC +3HCl.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116815318A (en) * | 2023-06-07 | 2023-09-29 | 山西烁科晶体有限公司 | Device and method for preparing high-purity SiC polycrystalline rod |
| CN117248275A (en) * | 2023-11-20 | 2023-12-19 | 希科半导体科技(苏州)有限公司 | Silicon carbide chemical vapor deposition epitaxial method and silicon carbide epitaxial wafer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977795A (en) * | 2017-05-31 | 2018-12-11 | 中国科学院金属研究所 | A kind of device and method for being electrically coupled chemical vapour deposition technique and preparing coat of silicon carbide |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108977795A (en) * | 2017-05-31 | 2018-12-11 | 中国科学院金属研究所 | A kind of device and method for being electrically coupled chemical vapour deposition technique and preparing coat of silicon carbide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116815318A (en) * | 2023-06-07 | 2023-09-29 | 山西烁科晶体有限公司 | Device and method for preparing high-purity SiC polycrystalline rod |
| CN117248275A (en) * | 2023-11-20 | 2023-12-19 | 希科半导体科技(苏州)有限公司 | Silicon carbide chemical vapor deposition epitaxial method and silicon carbide epitaxial wafer |
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