CN110499532B - Device for rapidly preparing silicon carbide - Google Patents
Device for rapidly preparing silicon carbide Download PDFInfo
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- CN110499532B CN110499532B CN201910918243.6A CN201910918243A CN110499532B CN 110499532 B CN110499532 B CN 110499532B CN 201910918243 A CN201910918243 A CN 201910918243A CN 110499532 B CN110499532 B CN 110499532B
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
The invention discloses a device for rapidly preparing silicon carbide, and relates to the technical field of silicon carbide. According to the device, a silicon carbide block is placed between a first growth chamber and a second growth chamber, seed crystals are located in a porous boron nitride lining of the first growth chamber, and the temperature of the seed crystals is reduced through a ceramic seed crystal rod internally provided with a thermocouple and liquid metal cooling liquid, so that proper growth temperature and temperature gradient are established nearby the seed crystals. The thermocouple is arranged in the porous boron nitride lining through the growth cavity main body, the growth temperature of the growth environment and the temperature gradient in the atmosphere are monitored, and the carrier gas pipeline on the growth cavity main body enables high-temperature carrier gas to carry gas volatilized by the silicon carbide to grow on seed crystals. The temperature gradient and the transportation process of the device are controllable, and the prepared silicon carbide has higher quality.
Description
Technical Field
The invention relates to the technical field of silicon carbide preparation devices, in particular to a device for rapidly preparing silicon carbide.
Background
Silicon carbide is an important wide bandgap semiconductor material, and due to the characteristics of large forbidden band width, high thermal conductivity, high breakdown electric field, high chemical stability and high electron saturation migration rate, the silicon carbide is widely applied to the power electronic fields of high frequency, high efficiency, high voltage resistance, high temperature resistance, radiation resistance and the like, and is also one of basic materials of fifth-generation mobile communication. Since it only has a pressure of up to 1010Pa, when the temperature reaches 3200 ℃, the melt with stoichiometric ratio can be formed, and the direct growth by the melt method is extremely difficult. Therefore, experiments were conducted to lower the saturation vapor pressure of the melt by the co-solvent method and to produce silicon carbide crystals by the melt method. The other method is vapor deposition, in which SiH is reacted in the reaction chamber at 2000-2300 deg.C4By means of a carrier gas (usually H)2) Carrying and combining with C2H4Or C3H8Mixing and then entering a reaction chamber to prepare the silicon carbide, wherein the reaction pressure is about 40 KPa. The method can prepare high-purity silicon carbide and has the characteristic of low crystal defects, but the method is not mature.
The most mature growth method at present is the physical vapor transport method, in which silicon carbide particles are heated to above 2000 ℃ for sublimation, and the sublimation gas grows into silicon carbide single crystals on seed crystals again. However, since the saturation vapor pressure of silicon is higher than that of carbon, a carbon coating is easily formed on the seed crystal in the sublimation gas due to the difference between the saturation vapor pressures of silicon and carbon, and the growth is easily damaged. In addition, the defects of the micropipes during the growth process of the method are difficult to control. According to the current theory, the defects are related to the temperature distribution of a growth interface, the appearance of the growth interface and the like, so that the gas transportation process and the temperature gradient distribution of a growth area in the whole growth process need to be well controlled, and the defects are also key parameters for preparing the silicon carbide crystal. There is therefore a need for a method of producing high quality silicon carbide crystals with controlled temperature gradients and transport processes.
Disclosure of Invention
The invention aims to solve the technical problem of how to provide a device for quickly preparing silicon carbide, which has controllable temperature gradient and transportation process.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the device for rapidly preparing the silicon carbide is characterized in that: the growth chamber comprises a furnace body, a growth chamber main body is arranged in the furnace body, a growth chamber upper cover is arranged on an opening at the upper end of the growth chamber main body, the growth chamber main body and the growth chamber upper cover form a second growth chamber, an upper resistance heater is arranged on the upper side of the second growth chamber, an upper induction coil and a main induction coil are arranged on the periphery of the second growth chamber from top to bottom, a lower induction coil is arranged on the lower side of the second growth chamber, and the second growth chamber is heated through the upper resistance heater, the upper induction coil, the main induction coil and the lower induction coil; a porous boron nitride lining main body is arranged in the second growth cavity, a plurality of lining holes are formed in the lining main body, a boron nitride lining upper cover is arranged at an opening at the upper end of the lining main body, the porous boron nitride lining main body and the boron nitride lining upper cover form a first growth cavity, and a silicon carbide block is arranged in a space between the first growth cavity and the second growth cavity; the lower end of the ceramic seed rod sequentially penetrates through the furnace body, the growth cavity upper cover and the boron nitride lining upper cover from top to bottom and then enters the first growth cavity, a liquid cooling metal cavity is formed in the ceramic seed rod, liquid metal is injected into the cooling metal cavity through a liquid cooling metal injection pipe, a seed crystal clamp is fixedly connected to one end, located in the first growth cavity, of the silicon carbide seed rod, the silicon carbide seed crystal is fixed on the seed crystal clamp, an inflation pipe and an exhaust pipe are arranged on the furnace body, and inert gas is injected into the furnace body through the inflation pipe; the silicon carbide block is heated to sublimate into SimCnAfter the gas is discharged, the gas continuously enters into the first growth chamber through the action of the carrier gas, and SimCnGas is transported to the solid/gas interface of the silicon carbide seed crystal to form the silicon carbide crystal continuouslyGrow up until the desired size is reached, where m =1 or 2 and n =0, 1 or 2.
The further technical scheme is as follows: the upper resistance heaters are respectively positioned at the left side and the right side of the silicon carbide seed crystal rod, the upper side of each upper resistance heater is provided with a flow guide screen, and the flow guide screens are used for guiding gas volatilized from the growth cavity to the positions near the deposition plate.
The further technical scheme is as follows: a deposition plate is arranged on the inner wall of the furnace body at the upper side of each flow guide screen and used for depositing and collecting sublimed Si which does not participate in depositionmCnAnd the deposition plate is internally provided with a water cooling device for reducing the surface temperature of the deposition plate.
The further technical scheme is as follows: the ceramic seed rod comprises a liquid metal flow guide pipe, the lower end of the liquid metal flow guide pipe is provided with a connecting part, the inner diameter of the connecting part is larger than the inner diameter of the flow guide pipe, the flow guide pipe is communicated with a cavity in the connecting part, the periphery of the connecting part is provided with external threads, internal threads are arranged on seed crystal clamping, seed crystal clamping is connected with the connecting part through mutually matched thread fixing, the lower end of the seed crystal clamping is provided with a seed crystal clamping cavity, the upper end of a silicon carbide seed crystal is inserted into the seed crystal clamping cavity, and the seed crystal is fixed through a seed crystal jackscrew positioned on two sides of the clamping cavity.
The further technical scheme is as follows: the liquid cooling metal guide pipe is internally provided with a liquid cooling metal injection pipe, a first thermocouple is arranged in the liquid cooling metal injection pipe, the lower end of the first thermocouple is embedded into the bottom of the connecting part and used for measuring temperature information of the silicon carbide seed crystal, and the liquid cooling metal injection pipe is used for injecting liquid cooling metal into the cavity of the connecting part.
The further technical scheme is as follows: a ceramic stopper is arranged between the ceramic seed rod and the upper cover of the growth cavity, and an internal heating wire is arranged in the upper cover of the boron nitride lining and used for preventing the silicon carbide from being deposited on the connecting part; and a power supply lead of the inner heating wire is led out through a ceramic stopper electrode hole on the ceramic stopper.
The further technical scheme is as follows: the growth chamber comprises a growth chamber body and is characterized in that more than one side wall gas carrying pipe is arranged on the left side wall, the lower side wall and the right side wall of the growth chamber body, the inner side of the side wall gas carrying pipe is communicated with the growth chamber body, the outer side end of the side wall gas carrying pipe extends to the outer side of the furnace body, a lower wall thermocouple cavity is arranged on the lower side wall of the growth chamber body, a right wall thermocouple cavity is arranged on the right side wall of the growth chamber body, and the right wall thermocouple cavity and the lower wall thermocouple cavity are fixed on the growth chamber body in a threaded connection mode. And after the porous boron nitride lining main body is placed into the growth cavity main body, connecting the right-wall thermocouple cavity and the lower-wall thermocouple cavity to the growth cavity main body.
The further technical scheme is as follows: the porous boron nitride lining main body is provided with a lining lower wall thermocouple jack at a position corresponding to the lower wall thermocouple cavity, and the porous boron nitride lining main body is provided with a lining right wall thermocouple jack at a position corresponding to the right wall thermocouple cavity.
The further technical scheme is as follows: the porous boron nitride lining is characterized in that a second thermocouple is arranged in the right-wall thermocouple cavity, a third thermocouple is arranged in the lower-wall thermocouple cavity, the second thermocouple is used for measuring temperature information of the middle of the right side of the porous boron nitride lining main body, the third thermocouple is used for measuring temperature information of the middle of the bottom side of the porous boron nitride lining main body, and water-cooling copper coils are arranged on the peripheries of the second thermocouple and the third thermocouple outside the first growth cavity.
The further technical scheme is as follows: the contact part of the side wall gas carrier pipe and the furnace body is provided with an electroforming metal interface, and the side wall gas carrier pipe is hermetically connected with the furnace body through the electroforming metal interface; and valve bodies are arranged on the side wall gas carrying pipe, the gas inlet pipe and the gas exhaust pipe.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: according to the device, a silicon carbide block is placed between a first growth chamber and a second growth chamber, seed crystals are located in a porous boron nitride lining of the first growth chamber, and the temperature of the seed crystals is reduced through a ceramic seed crystal rod with a thermocouple and liquid metal cooling liquid arranged inside, so that proper growth temperature and temperature gradient are established nearby the seed crystals. The thermocouple is arranged in the porous boron nitride lining through the growth cavity main body, the growth temperature of the growth environment and the temperature gradient in the atmosphere are monitored, and the carrier gas pipeline on the growth cavity main body enables high-temperature carrier gas to carry gas volatilized by the silicon carbide to grow on seed crystals. The device has the advantages that the temperature gradient and the transportation process are controllable, and the prepared silicon carbide has higher quality.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic cross-sectional view of an apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic cross-sectional view of a porous boron nitride liner in an apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic cross-sectional view of a growth chamber body in an apparatus according to an embodiment of the invention;
FIG. 4 is a schematic cross-sectional view of a ceramic stopper in an apparatus according to an embodiment of the present invention;
FIG. 5 is a schematic cross-sectional view of a liquid metal flow conduit and a connecting portion of a seed rod in an apparatus according to an embodiment of the present invention;
FIG. 6 is a schematic cross-sectional view of a seed holder of the apparatus according to the embodiment of the present invention;
FIG. 7 is a schematic diagram of the structure of the boron nitride liner top cap in the apparatus according to an embodiment of the present invention;
wherein: 1: a ceramic seed rod; 1-1, liquid metal guide pipe; 1-2: a connecting portion; 1-3: an external thread; 1-4: liquid cooling metal injection pipe; 2: a liquid metal; 3: a first thermocouple; 4: a ceramic stopper; 4-1: a ceramic stopper electrode hole; 5: a flow guide screen; 6: an upper resistance heater; 7: covering the growth cavity; 8: a growth chamber body; 8-1: a right wall thermocouple cavity; 8-2: a lower wall thermocouple cavity; 9: a side wall carrier gas pipe; 10: silicon carbide seed crystals; 11: water-cooling the copper coil; 12: a second thermocouple; 13: a silicon carbide crystal; 14: a lower induction coil; 15: a third thermocouple; 16: a lower wall carrier gas pipe; 17: an inflation inlet; 18: a porous boron nitride liner; 18-1: a thermocouple jack on the right wall of the lining; 18-2: a thermocouple jack on the lower wall of the lining; 18-3: a lining hole; 19: a main induction coil; 20: an upper induction coil; 21: graphite paper; 22: an inner heating wire; 23: a boron nitride lining upper cover; 23-1: a liner upper cover assembly; 24: an exhaust port; 25: depositing a plate; 26: a power supply lead; 27: a silicon carbide block; 28: seed crystal clamping; 28-1: an internal thread; 28-2: a seed crystal jackscrew; 29: and electroforming a metal interface.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
As shown in fig. 1, the embodiment of the invention discloses a device for rapidly preparing silicon carbide, which comprises a furnace body, wherein a growth cavity main body 8 is arranged inside the furnace body, a growth cavity upper cover 7 is arranged on an upper end opening of the growth cavity main body 8, the growth cavity main body 8 and the growth cavity upper cover 7 form a second growth cavity, an upper resistance heater 6 is arranged on the upper side of the second growth cavity, an upper induction coil 20 and a main induction coil 19 are arranged on the periphery of the second growth cavity from top to bottom, a lower induction coil 14 is arranged on the lower side of the second growth cavity, and the second growth cavity is heated through the upper resistance heater 6, the upper induction coil 20, the main induction coil 19 and the lower induction coil 14; a porous boron nitride lining main body 18 is arranged in the second growth cavity, a plurality of lining holes 18-3 are arranged on the lining main body, and a boron nitride lining is arranged at an opening at the upper end of the lining main bodyThe porous boron nitride lining main body 18 and the boron nitride lining upper cover 23 form a first growth cavity, and a silicon carbide block 27 is arranged in a space between the first growth cavity and the second growth cavity; the lower end of the ceramic seed crystal rod 1 sequentially penetrates through a furnace body, a growth cavity upper cover 7 and a boron nitride lining upper cover 23 from top to bottom and then enters into the first growth cavity, a liquid cooling metal cavity is arranged in the ceramic seed crystal rod 1, liquid metal is injected into the cooling metal cavity through a liquid cooling metal injection pipe 1-4, a seed crystal holder 28 is fixedly connected to one end of the silicon carbide seed crystal rod, which is positioned in the first growth cavity, the silicon carbide seed crystal 10 is fixed on the seed crystal holder 28, an air charging pipe 17 and an air discharging pipe 24 are arranged on the furnace body, and inert gas is injected into the furnace body through the air charging pipe 17; the silicon carbide block 27 is sublimed to Si by heatingmCnAfter the gas is discharged, the gas continuously enters into the first growth chamber through the action of the carrier gas, and SimCnThe gas is transported to the solid/gas interface of the silicon carbide seed crystal 10 to form a silicon carbide crystal and grow continuously (since the temperature at the seed crystal is lowest, where the sublimation gases are in a supersaturated state, the silicon carbide crystal will begin to grow along the seed crystal) until the desired size is reached, where m =1 or 2 and n =0, 1 or 2.
As shown in fig. 1, two upper resistance heaters 6 are arranged and located on the left and right sides of the silicon carbide seed rod 1, and a flow guide screen 5 is arranged on the upper side of each upper resistance heater 6 and used for guiding the gas volatilized from the growth chamber to the vicinity of the deposition plate 25. A deposition plate 25 is arranged on the inner wall of the furnace body at the upper side of each flow guide screen 5 and is used for depositing and collecting sublimed Si which does not participate in depositionmCnA gas. The deposition plate 25 has a water cooling means inside to reduce its surface temperature.
As shown in fig. 5-6, the ceramic seed rod 1 comprises a liquid metal flow guide tube 1-1, the lower end of the liquid metal draft tube 1-1 is provided with a connecting part 1-2, the inner diameter of the connecting part 1-2 is larger than that of the draft tube, the honeycomb duct is communicated with the cavity in the connecting part 1-2, the periphery of the connecting part 1-2 is provided with an external thread 1-3, the seed crystal holder 28 is provided with an internal thread 28-1, the seed crystal holder 28 and the connecting part 1-2 are fixedly connected through mutually matched threads, the lower end of the seed crystal holder 28 is provided with a seed crystal holding cavity, the upper end of the silicon carbide seed crystal 10 is inserted into the seed crystal holding cavity, and is fixed by seed crystal jackscrew screws 28-2 located on both sides of the holding cavity. As shown in fig. 1 and 5, a liquid cooling metal injection pipe 1-4 is arranged in the liquid metal draft tube 1-1, a first thermocouple 3 is arranged in the liquid cooling metal injection pipe 1-4, the lower end of the first thermocouple 3 is embedded into the bottom of the connecting part 1-2 and is used for measuring temperature information at the silicon carbide seed crystal 10, and the liquid cooling metal injection pipe 1-4 is used for injecting liquid cooling metal into the cavity of the connecting part.
As shown in fig. 1, a ceramic stopper 4 is arranged between the ceramic seed rod 1 and the growth cavity upper cover 7; an inner heating wire 22 is arranged in the upper cover 23 of the boron nitride lining and is used for preventing the silicon carbide from being deposited on the connecting part 1-2; as shown in fig. 1 and 4, the power supply lead 26 of the inner heating wire 22 is led out through the ceramic stopper electrode hole 4-1 of the ceramic stopper 4.
As shown in fig. 3, more than one sidewall carrier gas pipe is arranged on the left sidewall, the lower sidewall and the right sidewall of the growth chamber main body 8, the inner side of the sidewall carrier gas pipe is communicated with the growth chamber main body 8, the outer end of the sidewall carrier gas pipe extends to the outer side of the furnace body, a lower wall thermocouple cavity 8-2 is arranged on the lower sidewall of the growth chamber main body 8, a right wall thermocouple cavity 8-1 is arranged on the right sidewall of the growth chamber main body 8, and the right wall thermocouple cavity 8-1 and the lower wall thermocouple cavity 8-2 are fixed on the growth chamber main body 8 in a threaded connection manner. And after the porous boron nitride lining main body 18 is placed into the growth cavity main body 8, connecting the right-wall thermocouple cavity 8-1 and the lower-wall thermocouple cavity 8-2 to the growth cavity main body 8.
As shown in fig. 2, the porous boron nitride lining main body 18 is provided with a lining lower wall thermocouple insertion hole 18-2 at a position corresponding to the lower wall thermocouple cavity 8-2, and the porous boron nitride lining main body 18 is provided with a lining right wall thermocouple insertion hole 18-1 at a position corresponding to the right wall thermocouple cavity 8-1. Further, as shown in fig. 1, a second thermocouple 12 is arranged in the right-wall thermocouple cavity 8-1, a third thermocouple 15 is arranged in the lower-wall thermocouple cavity 8-2, the second thermocouple 12 is used for measuring temperature information of the middle part of the right side of the porous boron nitride lining main body 18, the third thermocouple 15 is used for measuring temperature information of the middle part of the bottom side of the porous boron nitride lining main body 18, and water-cooling copper coils 11 are arranged on the peripheries of the second thermocouple 12 and the third thermocouple 15 outside the first growth cavity.
As shown in fig. 1, an electroformed metal interface 29 is arranged at the contact part of the side wall carrier gas pipe and the furnace body, and the sealing connection with the furnace body is realized through the electroformed metal interface 29; and valve bodies are arranged on the side wall gas carrying pipe, the gas inlet pipe 17 and the gas outlet pipe 24.
Correspondingly, the embodiment of the invention also discloses a method for rapidly preparing silicon carbide, which uses the device for rapidly preparing silicon carbide and comprises the following steps:
assembling a silicon carbide seed crystal 10 on a seed crystal holder 28, screwing a seed crystal jackscrew 28-2, and then mutually matching a connecting part 1-2 with an external thread 1-3 on the seed crystal holder through an internal thread 28-1 to install the connecting part on a ceramic seed crystal rod 1;
assembling a growth cavity main body 8 into a furnace body, assembling a porous boron nitride lining 18 into the growth cavity main body 8, moving a ceramic seed rod 1 to lower a silicon carbide seed crystal 10 into the porous boron nitride lining 18, placing an inner heating wire 22, covering two lining upper cover components 23-1 to an opening at the upper end of the porous boron nitride lining 18 to form a first growth cavity, meanwhile, wrapping the silicon carbide seed crystal 10 and the inner heating wire 22 in the first growth cavity, filling a silicon carbide block 27 between the growth cavity main body 8 and the first growth cavity, placing graphite paper 21 on the upper edge of the growth cavity main body 8, covering a growth cavity upper cover 7 and fixing;
inserting a second thermocouple 12 and a third thermocouple 15 into the growth cavity right side wall thermocouple cavity 8-1 and the growth cavity lower wall thermocouple cavity 8-2 respectively; then the left side wall carrier gas pipe, the right side wall carrier gas pipe 9 and the lower wall carrier gas pipe 16 are sealed with the furnace body through an electroforming metal interface 29 and connected with a carrier gas pipeline outside the furnace body, and the water-cooling copper coil 11 cools the second thermocouple 12 and the third thermocouple 15;
vacuumizing the whole furnace body, then filling inert gas, and keeping the pressure at 133Pa-13300 Pa; heating the growth cavity upper cover 7 and the growth cavity main body 8 through a main induction coil 19, an upper induction coil 20, an upper resistance heater 6 and a lower induction coil 14 which are arranged outside a second growth cavity and formed by the growth cavity main body 8 and the growth cavity upper cover 7, so that the temperatures of a second thermocouple 12 and a third thermocouple 15 reach 2000-2300 ℃; starting the internal heater 22 for preventing silicon carbide from being deposited on the ceramic seed rod 1;
then adjusting the flow and temperature of the liquid metal 2 in the ceramic seed rod 1 (the liquid metal 2 can adjust the temperature, adjust and control the heat transfer condition on the silicon carbide seed crystal 10, and further control the growth of the silicon carbide seed crystal), and cooling the silicon carbide seed crystal 10 at the lower end of the ceramic seed rod 1, so that the first thermocouple 3 in the ceramic seed rod 1 reaches 1700-2100 ℃; then adjusting the power of the upper resistance heater 6, the main induction coil 19, the upper induction coil 20 and the lower induction coil 14 to establish a temperature gradient of 2K/mm to 20K/mm between the first thermocouple 3 and the third thermocouple 15;
injecting inert gas into the second growth cavity through the left side wall carrier gas pipe, the right side wall carrier gas pipe 9 and the lower wall carrier gas pipe 16 to form carrier gas, and heating and sublimating the silicon carbide block 27 into Si through the carrier gasmCnIs continuously brought into the first growth chamber and accelerates the sublimation process of the silicon carbide mass 27, SimCnThe gas is transported to the solid/gas interface of the silicon carbide seed crystal 10 to form a silicon carbide crystal and grows continuously until it grows to a desired size.
According to the device and the method, the silicon carbide block is placed between the first growth chamber and the second growth chamber, the seed crystal is positioned in the porous boron nitride lining of the first growth chamber, and the ceramic seed crystal rod with the thermocouple and the liquid metal cooling liquid arranged inside is used for cooling the seed crystal, so that a proper growth temperature and temperature gradient are established nearby the seed crystal. The thermocouple is arranged in the porous boron nitride lining through the growth cavity main body, the growth temperature of the growth environment and the temperature gradient in the atmosphere are monitored, and the carrier gas pipeline on the growth cavity main body enables high-temperature carrier gas to carry gas volatilized by the silicon carbide to grow on seed crystals. The device and the method have the advantages that the temperature gradient and the transportation process are controllable, and the prepared silicon carbide is high in quality.
Claims (2)
1. The device for rapidly preparing the silicon carbide is characterized in that: the furnace comprises a furnace body, wherein a growth cavity main body (8) is arranged in the furnace body, a growth cavity upper cover (7) is arranged on an upper end opening of the growth cavity main body (8), the growth cavity main body (8) and the growth cavity upper cover (7) form a second growth cavity, an upper resistance heater (6) is arranged on the upper side of the second growth cavity, an upper induction coil (20) and a main induction coil (19) are arranged on the periphery of the second growth cavity from top to bottom, a lower induction coil (14) is arranged on the lower side of the second growth cavity, and the second growth cavity is heated through the upper resistance heater (6), the upper induction coil (20), the main induction coil (19) and the lower induction coil (14); a porous boron nitride lining main body (18) is arranged in the second growth cavity, a plurality of lining holes (18-3) are formed in the lining main body, a boron nitride lining upper cover (23) is arranged at an opening at the upper end of the lining main body, the porous boron nitride lining main body (18) and the boron nitride lining upper cover (23) form a first growth cavity, and a silicon carbide block (27) is arranged in a space between the first growth cavity and the second growth cavity; the lower end of a ceramic seed rod (1) sequentially penetrates through a furnace body, a growth cavity upper cover (7) and a boron nitride lining upper cover (23) from top to bottom and then enters a first growth cavity, a liquid cooling metal cavity is arranged in the ceramic seed rod (1), liquid metal is injected into the liquid cooling metal cavity through a liquid cooling metal injection pipe (1-4), a seed crystal clamp (28) is fixedly connected to one end of the ceramic seed rod, which is positioned in the first growth cavity, a silicon carbide seed crystal (10) is fixed on the seed crystal clamp (28), an inflation pipe (17) and an exhaust pipe (24) are arranged on the furnace body, and inert gas is filled into the furnace body through the inflation pipe (17); the silicon carbide block (27) is sublimed into Si when heatedmCnAfter the gas is discharged, the gas continuously enters the first part by the action of the carrier gasIn the growth chamber, SimCnGas is transported to the solid/gas interface of the silicon carbide seed crystal (10) to form a silicon carbide crystal and grow continuously until the silicon carbide crystal grows to a required size, wherein m =1 or 2, and n =0, 1 or 2;
the two upper resistance heaters (6) are respectively positioned at the left side and the right side of the ceramic seed rod (1), the upper side of each upper resistance heater (6) is provided with a flow guide screen (5), and the flow guide screens are used for guiding gas volatilized from the growth cavity to the vicinity of the deposition plate (25); a deposition plate (25) is arranged on the inner wall of the furnace body at the upper side of each flow guide screen (5), and the deposition plate is used for depositing and collecting sublimed Si which does not participate in depositionmCnThe deposition plate (25) is internally provided with a water cooling device for reducing the surface temperature of the deposition plate;
the ceramic seed crystal rod (1) comprises a liquid metal guide pipe (1-1), the lower end of the liquid metal guide pipe (1-1) is provided with a connecting part (1-2), the inner diameter of the connecting part (1-2) is larger than that of the guide pipe, the honeycomb duct is communicated with the cavity in the connecting part (1-2), the periphery of the connecting part (1-2) is provided with external threads (1-3), the seed crystal holder (28) is provided with internal threads (28-1), the seed crystal holder (28) is fixedly connected with the connecting part (1-2) through mutually matched threads, the lower end of the seed crystal holder (28) is provided with a seed crystal holding cavity, the upper end of the silicon carbide seed crystal (10) is inserted into the seed crystal holding cavity, and is fixed by seed crystal jackscrew screws (28-2) positioned at two sides of the clamping cavity; a liquid cooling metal injection pipe (1-4) is arranged in the liquid metal guide pipe (1-1), a first thermocouple (3) is arranged in the liquid cooling metal injection pipe (1-4), the lower end of the first thermocouple (3) is embedded into the bottom of the connecting part (1-2) and used for measuring temperature information of the silicon carbide seed crystal (10), and the liquid cooling metal injection pipe (1-4) is used for injecting liquid cooling metal into a cavity of the connecting part;
a ceramic stopper (4) is arranged between the ceramic seed rod (1) and the growth cavity upper cover (7), and an inner heating wire (22) is arranged inside the boron nitride lining upper cover (23) and used for preventing the silicon carbide from being deposited on the connecting part (1-2); a power supply lead (26) of the inner heating wire (22) is led out through a ceramic blocking plug electrode hole (4-1) on the ceramic blocking plug (4);
more than one side wall gas carrying pipe is arranged on the left side wall, the lower side wall and the right side wall of the growth cavity main body (8), the inner side of the side wall gas-carrying pipe is communicated with the growth cavity main body (8), the outer side end of the side wall gas-carrying pipe extends to the outer side of the furnace body, a lower wall thermocouple cavity (8-2) is arranged on the lower side wall of the growth cavity main body (8), a right wall thermocouple cavity (8-1) is arranged on the right side wall of the growth cavity main body (8), the right-wall thermocouple cavity (8-1) and the lower-wall thermocouple cavity (8-2) are fixed on the growth cavity main body (8) in a threaded connection mode, and the right-wall thermocouple cavity (8-1) and the lower-wall thermocouple cavity (8-2) are connected to the growth cavity main body (8) after the porous boron nitride lining main body (18) is placed into the growth cavity main body (8); the porous boron nitride lining main body (18) is provided with a lining lower wall thermocouple jack (18-2) at a position corresponding to the lower wall thermocouple cavity (8-2), and the porous boron nitride lining main body (18) is provided with a lining right wall thermocouple jack (18-1) at a position corresponding to the right wall thermocouple cavity (8-1); the porous boron nitride lining is characterized in that a second thermocouple (12) is arranged in the right-wall thermocouple cavity (8-1), a third thermocouple (15) is arranged in the lower-wall thermocouple cavity (8-2), the second thermocouple (12) is used for measuring temperature information of the middle of the right side of the porous boron nitride lining main body (18), the third thermocouple (15) is used for measuring temperature information of the middle of the bottom side of the porous boron nitride lining main body (18), and water-cooling copper coils (11) are arranged on the peripheries of the second thermocouple (12) and the third thermocouple (15) outside the first growth cavity.
2. The apparatus for rapid preparation of silicon carbide according to claim 1, wherein: the contact part of the side wall gas carrier pipe and the furnace body is provided with an electroforming metal interface (29), and the sealing connection with the furnace body is realized through the electroforming metal interface (29); and valve bodies are arranged on the side wall gas carrying pipe, the gas filling pipe (17) and the exhaust pipe (24).
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