CN110499532A - Quickly prepare the device of silicon carbide - Google Patents
Quickly prepare the device of silicon carbide Download PDFInfo
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- CN110499532A CN110499532A CN201910918243.6A CN201910918243A CN110499532A CN 110499532 A CN110499532 A CN 110499532A CN 201910918243 A CN201910918243 A CN 201910918243A CN 110499532 A CN110499532 A CN 110499532A
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- C—CHEMISTRY; METALLURGY
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- C—CHEMISTRY; METALLURGY
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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Abstract
The invention discloses a kind of devices for quickly preparing silicon carbide, are related to silicon carbide technology field.Silicon carbide bulk is placed between the first growth chamber and the second growth chamber by described device, seed crystal is located in the porous boron nitride liner of the first growth chamber, cooled down by built-in thermocouple and the ceramic seed rod of liquid metal coolant liquid to seed crystal, it is made nearby to set up suitable growth temperature and temperature gradient.Entered in porous boron nitride liner by growth cavity main body and arranges thermocouple, temperature gradient in the growth temperature and atmosphere of monitoring growth environment grows and grows on the gas to seed crystal that the carrier gas channel on cavity main body will make high temperature carrier gas carrying silicon carbide volatilize.The temperature gradient and transport process of described device are controllable, and the silicon carbide quality of preparation is higher.
Description
Technical field
The present invention relates to silicon carbide preparation facilities technical fields, more particularly to a kind of device for quickly preparing silicon carbide.
Background technique
Silicon carbide is a kind of important semiconductor material with wide forbidden band, since its forbidden bandwidth is big, high heat conductance, high breakdown
Electric field, high chemical stability, high electronics saturation migration rate the characteristics of, make its be widely used in high frequency, it is efficient, high pressure resistant,
The field of power electronics such as high temperature resistant, anti-radiation are also one of the basic material of the 5th third-generation mobile communication.Since it only has pressure
Reach 1010Pa could form the melt of stoichiometric ratio when temperature reaches 3200 DEG C, directly be grown extremely by melt method
It is difficult.Therefore people start to test through flux method the saturated vapor pressure for reducing melt, and prepare carbon by melt method
SiClx crystal.Another method be vapour deposition process, 2000-2300 DEG C of reaction chamber at a temperature of, SiH4(usually by carrier gas
For H2) carry and and C2H4Or C3H8It is mixed into reaction chamber and prepares silicon carbide, reaction pressure is 40KPa or so.This method can
To prepare high-purity silicon carbide and the low feature of crystal defect, but this method is still immature.
Presently the most mature growing method is physical carbon burdening, by silicon-carbide particle be heated to 2000 DEG C with
Upper distillation, sublimation gases are grown to single-crystal silicon carbide on seed crystal again.But since the saturated vapor pressure of silicon is higher than carbon member
Element, therefore be easy in sublimation gases because the saturated vapor pressure difference of silicon and carbon is easy to the formation carbon coating on seed crystal and shows
As destroying growth.In addition the micropipe defects in this method growth course are also difficult to control.According to current theory, these are lacked
It falls into all related with the pattern etc. of the Temperature Distribution of growth interface, growth interface, it is therefore desirable to control entire growth course well
Transport process and growth district temperature gradient distribution, this is also the key parameter for preparing carborundum crystals.Therefore it needs
A kind of temperature gradient and the controllable method of transport process are wanted to prepare the carborundum crystals of high quality.
Summary of the invention
The technical problem to be solved by the present invention is to how provide a kind of temperature gradient and the controllable quick system of transport process
The device of standby silicon carbide.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of device for quickly preparing silicon carbide,
It is characterized by comprising furnace body, the furnace body is internally provided with growth cavity main body, in the upper end opening of the growth cavity main body
Be provided with growth chamber upper cover, the growth cavity main body and growth chamber upper cover constitute the second growth chamber, second growth chamber it is upper
Side is provided with resistance heater, and the periphery of second growth chamber is provided with induction coil and main induction line from top to bottom
It encloses, is provided with lower induction coil on the downside of second growth chamber, passes through the upper resistance heater, upper induction coil, main sense
Coil and lower induction coil is answered to heat second growth chamber；It is provided in porous boron nitride in second growth chamber
Main body is served as a contrast, several liner holes is provided in the liner main body, is provided with boron nitride at the upper end opening of the liner main body
Liner upper cover, the porous boron nitride liner main body and the boron nitride liner upper cover constitute the first growth chamber, and described first is raw
Silicon carbide bulk is provided in space between long chamber and the second growth chamber；It successively wears from top to bottom the lower end of the ceramics seed rod
It is entered in first growth chamber after crossing furnace body, growth chamber upper cover, boron nitride liner upper cover, setting in the ceramics seed rod
There is liquid cooled wire chamber, it is described that liquid metal, the carbonization are injected to cooling wire chamber by liquid cooled metal injection pipe
Seed crystal clamping is fixedly connected on one end that silicon seed bar is located in the first growth chamber, the silicon carbide seed is fixed on the seed
In crystalline substance clamping, it is provided with gas tube and exhaust pipe on the furnace body, indifferent gas is poured into the furnace body by the gas tube
Body；The silicon carbide bulk is being Si by heat sublimationmCnAfter gas, the first growth is endlessly entered by the effect of carrier gas
It is intracavitary, SimCnCarborundum crystals are formed on gas transport to the solid/gas interface of silicon carbide seed and are constantly grown up, until growing to
Required size, wherein m=1 or 2, n=0,1 or 2.
A further technical solution lies in: there are two the upper resistance heater settings, is located at the silicon carbide seed
The left and right sides of crystalline style is provided with a flow guiding screen on the upside of each upper resistance heater, and the flow guiding screen will be for that will give birth to
Near the long intracavitary gas flow guiding to deposition plate volatilized.
A further technical solution lies in: a deposition plate is provided on the inboard wall of furnace body on the upside of each flow guiding screen,
The deposition plate is used to deposit the Si for collecting the distillation for having neither part nor lot in depositionmCnGas has water cooling plant inside the deposition plate, uses
In its surface temperature of reduction.
A further technical solution lies in: the ceramics seed rod includes liquid metal diversion pipe, and the liquid metal is led
The lower end of flow tube is provided with interconnecting piece, and the internal diameter of the interconnecting piece is greater than the internal diameter of the diversion pipe, and the diversion pipe and institute
The cavity stated in interconnecting piece is connected, and the periphery of the interconnecting piece is provided with external screw thread, is provided with internal screw thread, seed in seed crystal clamping
By the mutually matched connection that is screwed between crystalline substance clamping and the interconnecting piece, the lower end of the seed crystal clamping is provided with seed crystal
Holding chamber, it is intracavitary that the upper end of silicon carbide seed is inserted into the seed crystal clamping, and passes through the seed crystal positioned at the holding chamber two sides
Jackscrew screw rod is fixed.
A further technical solution lies in: liquid cooled metal injection pipe, institute are provided in the liquid metal diversion pipe
It states and is provided with the first thermocouple in liquid cooled metal injection pipe, the bottom of the lower end insertion interconnecting piece of first thermocouple,
For measuring the temperature information at silicon carbide seed, the liquid cooled metal injection pipe is used for into the cavity of the interconnecting piece
Inject liquid cooled metal.
A further technical solution lies in: ceramic gear is provided between the ceramics seed rod and the growth chamber upper cover
Plug, interior heater strip is arranged in the boron nitride liner upper cover inside, for preventing interconnecting piece depositing silicon silicon；The interior heater strip
Current supply line is drawn by the ceramic stopper electrode hole in ceramic stopper.
A further technical solution lies in: one is provided on the left side wall for growing cavity main body, lower wall and right side wall
Side wall carrier gas pipe more than root, the inside of the side wall carrier gas pipe are connected with the growth cavity main body, the side wall carrier gas pipe
Outboard end extend to the outside of the furnace body, be provided with lower wall thermocouple cavity, institute in the lower wall of the growth cavity main body
It states and is provided with right wall thermocouple cavity on the right side wall of growth cavity main body, the right wall thermocouple cavity and lower wall thermocouple cavity pass through spiral shell
The mode of line connection is fixed on growth cavity main body.Again by right wall after porous boron nitride liner main body is placed into growth cavity main body
Thermocouple cavity and lower wall thermocouple cavity are connected on growth cavity main body.
A further technical solution lies in: the porous boron nitride liner main body is corresponding with the lower wall thermocouple cavity
Position be provided with liner lower wall thermocouple jack, the porous boron nitride liner main body is opposite with the right wall thermocouple cavity
The position answered is provided with liner right wall thermocouple jack.
A further technical solution lies in: the second thermocouple, the lower wall thermoelectricity are provided in the right wall thermocouple cavity
Occasionally intracavitary to be provided with third thermocouple, second thermocouple is for measuring the porous boron nitride liner main body right side central
Temperature information, the third thermocouple are used to measure the temperature information in the middle part of the porous boron nitride liner main body bottom side, be located at
Water cooling copper coil is arranged in the periphery of second thermocouple and third thermocouple outside first growth chamber.
A further technical solution lies in: the contact portion of the side wall carrier gas pipe and the furnace body is provided with electroforming metal and connects
Mouthful, the sealed connection with furnace body is realized by the electroforming metal interface；On the side wall carrier gas pipe, air inlet pipe and exhaust pipe
It is provided with valve body.
The beneficial effects of adopting the technical scheme are that silicon carbide bulk is placed in the first life by described device system
Between long chamber and the second growth chamber, seed crystal is located in the porous boron nitride liner of the first growth chamber, passes through built-in thermocouple and liquid
The ceramic seed rod of metal coolant liquid cools down to seed crystal, it is made nearby to set up suitable growth temperature and temperature gradient.Pass through
Growth cavity main body, which enters in porous boron nitride liner, arranges thermocouple, the temperature in the growth temperature and atmosphere of monitoring growth environment
Gradient grows and gives birth on the gas to seed crystal that the carrier gas channel on cavity main body will make high temperature carrier gas carrying silicon carbide volatilize
It is long.The temperature gradient and transport process of herein described device are controllable, and the silicon carbide quality of preparation is higher.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the schematic cross-sectional view of device described in the embodiment of the present invention；
Fig. 2 is the schematic cross-sectional view of porous boron nitride liner in described device of the embodiment of the present invention；
Fig. 3 is the schematic cross-sectional view that cavity main body is grown in described device of the embodiment of the present invention；
Fig. 4 is the schematic cross-sectional view of ceramic stopper in described device of the embodiment of the present invention；
Fig. 5 is that the sectional structure of liquid metal diversion pipe and interconnecting piece is illustrated in seed rod in described device of the embodiment of the present invention
Figure；
Fig. 6 is the schematic cross-sectional view that seed crystal clamps in described device of the embodiment of the present invention；
Fig. 7 is the structural schematic diagram of boron nitride liner upper cover in described device of the embodiment of the present invention；
Wherein: 1: ceramic seed rod；1-1: liquid metal diversion pipe；1-2: interconnecting piece；1-3: external screw thread；1-4: liquid cooled gold
Belong to injection pipe；2: liquid metal；3: the first thermocouples；4: ceramic stopper；4-1: ceramic stopper electrode hole；5: flow guiding screen；6: on
Resistance heater；7: growth chamber upper cover；8: growth cavity main body；8-1: right wall thermocouple cavity；8-2: lower wall thermocouple cavity；9: side wall
Carrier gas pipe；10: silicon carbide seed；11: water cooling copper coil；12: the second thermocouples；13: carborundum crystals；14: lower induction coil；
15: third thermocouple；16: lower wall carrier gas pipe；17: inflating port；18: porous boron nitride liner；18-1: liner right wall thermocouple is inserted
Hole；18-2: liner lower wall thermocouple jack；18-3: liner hole；19: main induction coil；20: upper induction coil；21: graphite paper；
22: interior heater strip；23: boron nitride liner upper cover；23-1: liner cover assembly；24: exhaust outlet；25: deposition plate；26: for conductance
Line；27: silicon carbide bulk；28: seed crystal clamping；28-1: internal screw thread；28-2: seed crystal jackscrew screw rod；29: electroforming metal interface.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
As shown in Figure 1, the embodiment of the invention discloses a kind of device for quickly preparing silicon carbide, including furnace body, the furnace
Body is internally provided with growth cavity main body 8, is provided with growth chamber upper cover 7, the life in the upper end opening of the growth cavity main body 8
Long cavity main body 8 constitutes the second growth chamber with growth chamber upper cover 7, is provided with resistance heater 6 on the upside of second growth chamber,
The periphery of second growth chamber is provided with induction coil 20 and main induction coil 19 from top to bottom, second growth chamber
Downside is provided with lower induction coil 14, passes through the upper resistance heater 6, upper induction coil 20, main induction coil 19 and lower sense
Coil 14 is answered to heat second growth chamber；Porous boron nitride liner main body 18 is provided in second growth chamber,
It is provided with several liner holes 18-3 in the liner main body, is provided with boron nitride liner at the upper end opening of the liner main body
Upper cover 23, the porous boron nitride liner main body 18 and the boron nitride liner upper cover 23 the first growth chamber of composition, described first
Silicon carbide bulk 27 is provided in space between growth chamber and the second growth chamber；The lower end of the ceramics seed rod 1 is from top to bottom
It is entered in first growth chamber after sequentially passing through furnace body, growth chamber upper cover 7, boron nitride liner upper cover 23, the ceramics seed
Liquid cooled wire chamber is provided in crystalline style 1, it is described that liquid is injected to cooling wire chamber by liquid cooled metal injection pipe 1-4
Metal is fixedly connected with seed crystal clamping 28, the silicon carbide on one end that the silicon carbide seed bar is located in the first growth chamber
Seed crystal 10 is fixed in the seed crystal clamping 28, and gas tube 17 and exhaust pipe 24 are provided on the furnace body, passes through the inflation
Pipe 17 pours inert gas into the furnace body；The silicon carbide bulk 27 is being Si by heat sublimationmCnAfter gas, pass through carrier gas
Effect endlessly enters in the first growth chamber, SimCnIt is formed on gas transport to the solid/gas interface of silicon carbide seed 10
Carborundum crystals and constantly grow up (since temperature is minimum at seed crystal, sublimation gases this everywhere in hypersaturated state, silicon carbide whisker
Body will start to grow along seed crystal), until growing to required size, wherein m=1 or 2, n=0,1 or 2.
As shown in Figure 1, being located at the left and right of the silicon carbide seed bar 1 there are two the settings of upper resistance heater 6
Two sides, the upside of each upper resistance heater 6 are provided with a flow guiding screen 5, and the flow guiding screen in growth chamber for will wave
Near the gas flow guiding of sending to deposition plate 25.A deposition plate is provided on the inboard wall of furnace body of each 5 upside of the flow guiding screen
25, the deposition plate is used to deposit the Si for collecting the distillation for having neither part nor lot in depositionmCnGas.There is water cooling dress inside the deposition plate 25
It sets, to reduce its surface temperature.
As shown in Fig. 5-Fig. 6, the ceramics seed rod 1 includes liquid metal diversion pipe 1-1, the liquid metal diversion pipe
The lower end of 1-1 is provided with interconnecting piece 1-2, and the internal diameter of the interconnecting piece 1-2 is greater than the internal diameter of the diversion pipe, and the diversion pipe
It is connected with the cavity in the interconnecting piece 1-2, the periphery of the interconnecting piece 1-2 is provided with external screw thread 1-3, and seed crystal clamps on 28
It is provided with internal screw thread 28-1, seed crystal is clamped by the mutually matched connection that is screwed between the 28 and interconnecting piece 1-2, described
The lower end of seed crystal clamping 28 is provided with seed crystal holding chamber, and it is intracavitary that the upper end of silicon carbide seed 10 is inserted into the seed crystal clamping, and
Seed crystal jackscrew screw rod 28-2 by being located at the holding chamber two sides is fixed.As shown in Figure 1 and Figure 5, the liquid metal
It is provided with liquid cooled metal injection pipe 1-4 in diversion pipe 1-1, is provided with first in the liquid cooled metal injection pipe 1-4
Thermocouple 3, the bottom of the lower end insertion interconnecting piece 1-2 of first thermocouple 3, for measuring the temperature at silicon carbide seed 10
Information, the liquid cooled metal injection pipe 1-4 are used to inject liquid cooled metal into the cavity of the interconnecting piece.
As shown in Figure 1, being provided with ceramic stopper 4 between the ceramics seed rod 1 and the growth chamber upper cover 7；The nitrogen
Change heater strip 22 in being arranged inside boron liner upper cover 23, for preventing interconnecting piece 1-2 depositing silicon silicon；As shown in Figure 1 and Figure 4,
The current supply line 26 of the interior heater strip 22 is drawn by the ceramic stopper electrode hole 4-1 in ceramic stopper 4.
As shown in figure 3, being provided with one or more side on the left side wall of the growth cavity main body 8, lower wall and right side wall
Wall carrier gas pipe, the inside of the side wall carrier gas pipe are connected with the growth cavity main body 8, the outboard end of the side wall carrier gas pipe
The outside of the furnace body is extended to, is provided with lower wall thermocouple cavity 8-2, the growth in the lower wall of the growth cavity main body 8
It is logical that right wall thermocouple cavity 8-1, the right wall thermocouple cavity 8-1 and lower wall thermocouple cavity 8-2 are provided on the right side wall of cavity main body 8
The mode being threadedly coupled is crossed to be fixed on growth cavity main body 8.After porous boron nitride liner main body 18 is placed into growth cavity main body 8
Right wall thermocouple cavity 8-1 and lower wall thermocouple cavity 8-2 are connected on growth cavity main body 8 again.
As shown in Fig. 2, the porous boron nitride liner main body 18 is in position corresponding with the lower wall thermocouple cavity 8-2
Be provided with liner lower wall thermocouple jack 18-2, the porous boron nitride liner main body 18 with the right wall thermocouple cavity 8-1
Corresponding position is provided with liner right wall thermocouple jack 18-1.Further, as shown in Figure 1, the right wall thermocouple cavity
It is provided with the second thermocouple 12 in 8-1, third thermocouple 15, second thermoelectricity are provided in the lower wall thermocouple cavity 8-2
Even 12 for measuring the temperature information of 18 right side central of porous boron nitride liner main body, and the third thermocouple 15 is for surveying
The temperature information in the middle part of 18 bottom side of porous boron nitride liner main body is measured, second heat outside first growth chamber
Water cooling copper coil 11 is arranged in the periphery of galvanic couple 12 and third thermocouple 15.
As shown in Figure 1, the contact portion of the side wall carrier gas pipe and the furnace body is provided with electroforming metal interface 29, pass through institute
State the sealed connection of electroforming metal interface 29 realization and furnace body；It is set on the side wall carrier gas pipe, air inlet pipe 17 and exhaust pipe 24
It is equipped with valve body.
Correspondingly, the embodiment of the invention also discloses a kind of method for quickly preparing silicon carbide, described in the method use
The device for quickly preparing silicon carbide, includes the following steps:
By the assembly of silicon carbide seed 10 in seed crystal clamping 28, seed crystal jackscrew screw rod 28-2 is tightened, then passes through interconnecting piece 1-2
External screw thread 1-3 mutual cooperation on internal screw thread 28-1 and seed crystal clamping is installed on ceramic seed rod 1；
Growth cavity main body 8 is assembled in furnace body, and porous boron nitride liner 18 is assembled to inside growth cavity main body 8, it is mobile
Silicon carbide seed 10 is down to inside porous boron nitride liner 18 by ceramic seed rod 1, is placed in interior heater strip 22, then will be in two pieces
Lining cap assemblies 23-1 is covered to the upper end opening of porous boron nitride liner 18, forms the first growth chamber, while by silicon carbide seed
Crystalline substance 10 and interior heater strip 22 are wrapped in the first growth chamber, and silicon carbide bulk 27 is filled in growth cavity main body 8 and the first growth chamber
Between, along upper placement graphite paper 21 on growth cavity main body 8, then covers growth chamber upper cover 7 and fix；
The second thermocouple 12 and third thermocouple 15 are inserted into growth chamber right side wall thermocouple cavity 8-1 and growth chamber lower wall respectively
In thermocouple cavity 8-2；Then left side wall carrier gas pipe, right side wall carrier gas pipe 9 and lower wall carrier gas pipe 16 are passed through into electroforming metal interface
29 and furnace sealing, and be connected with the carrier gas channel outside furnace body, water cooling copper coil 11 gives the second thermocouple 12 and third thermoelectricity
Even 15 cool down；
It is vacuumized to entire furnace body, is then charged with inert gas, keep pressure 133Pa-13300Pa；By growth cavity main body 8 with
Main induction coil 19, upper induction coil 20, upper resistance heater 6, lower sense on the outside of second growth chamber of the composition of growth chamber upper cover 7
Coil 14 is answered to heat to growth chamber upper cover 7 and growth cavity main body 8, so that the temperature of the second thermocouple 12 and third thermocouple 15 reaches
To 2000 DEG C -2300 DEG C；Start internal heater 22, for preventing depositing silicon silicon on ceramic seed rod 1；
Then the flow of liquid metal 2 and temperature (the adjustable temperature of liquid metal 2, regulation carbonization in ceramic seed rod 1 are adjusted
Heat transfer situation on silicon seed 10, and then control the growth of silicon carbide seed), to the silicon carbide seed of ceramic 1 lower end of seed rod
10 coolings, so that the first thermocouple 3 in ceramic seed rod 1 reaches 1700-2100 DEG C；Then upper resistance heater 6, master are adjusted
The power of induction coil 19, upper induction coil 20 and lower induction coil 14 makes between the first thermocouple 3 and third thermocouple 15
Set up the temperature gradient of 2K/mm to 20K/mm；
It is injected inert gas by left side wall carrier gas pipe, right side wall carrier gas pipe 9 and lower wall carrier gas pipe 16 into the second growth chamber
Formed carrier gas, by carrier gas by silicon carbide bulk 27 by heat sublimation be SimCnGas continually bring into the first growth chamber and add
The sublimation process of fast silicon carbide bulk 27, SimCnCarborundum crystals are formed on gas transport to the solid/gas interface of silicon carbide seed 10
And constantly grow up, until growing to required size.
Silicon carbide bulk is placed between the first growth chamber and the second growth chamber by described device and method system, and seed crystal is located at the
In the porous boron nitride liner of one growth chamber, dropped by built-in thermocouple and the ceramic seed rod of liquid metal coolant liquid to seed crystal
Temperature makes it nearby set up suitable growth temperature and temperature gradient.Entered in porous boron nitride liner by growing cavity main body
Arrange thermocouple, the temperature gradient in the growth temperature and atmosphere of monitoring growth environment, the carrier gas channel grown on cavity main body will
It is grown on the gas to seed crystal that silicon carbide volatilizes so that high temperature carrier gas carries.The temperature of herein described device and method
Gradient and transport process are controllable, and the silicon carbide quality of preparation is higher.
Claims (10)
1. a kind of device for quickly preparing silicon carbide, it is characterised in that: including furnace body, the furnace body is internally provided with growth chamber
Main body (8), it is described growth cavity main body (8) upper end opening on be provided with growth chamber upper cover (7), the growth cavity main body (8) and
Growth chamber upper cover (7) constitutes the second growth chamber, is provided with resistance heater (6) on the upside of second growth chamber, and described the
The periphery of two growth chambers is provided with induction coil (20) and main induction coil (19) from top to bottom, under second growth chamber
Side is provided with lower induction coil (14), passes through the upper resistance heater (6), upper induction coil (20), main induction coil (19)
Second growth chamber is heated with lower induction coil (14)；Porous boron nitride liner is provided in second growth chamber
Main body (18) is provided with several liner holes (18-3) in the liner main body, is arranged at the upper end opening of the liner main body
There is a boron nitride liner upper cover (23), the porous boron nitride liner main body (18) and the boron nitride liner upper cover (23) constitute the
One growth chamber is provided with silicon carbide bulk (27) in the space between first growth chamber and the second growth chamber；The ceramics seed
The lower end of crystalline style (1) enters institute after sequentially passing through furnace body, growth chamber upper cover (7), boron nitride liner upper cover (23) from top to bottom
It states in the first growth chamber, is provided with liquid cooled wire chamber in the ceramics seed rod (1), is infused by the liquid cooled metal
Enter pipe (1-4) to cooling wire chamber injection liquid metal, the silicon carbide seed bar is located on one end in the first growth chamber solid
Surely it is connected with seed crystal clamping (28), the silicon carbide seed (10) is fixed on the seed crystal clamping (28), sets on the furnace body
It is equipped with gas tube (17) and exhaust pipe (24), by pouring inert gas in the gas tube (17) Xiang Suoshu furnace body；The carbon
SiClx block (27) is being Si by heat sublimationmCnAfter gas, endlessly entered in the first growth chamber by the effect of carrier gas,
SimCnCarborundum crystals are formed on gas transport to the solid/gas interface of silicon carbide seed (10) and are constantly grown up, until growing to
Required size, wherein m=1 or 2, n=0,1 or 2.
2. quickly preparing the device of silicon carbide as described in claim 1, it is characterised in that: the upper resistance heater (6) sets
There are two setting, it is located at the left and right sides of the silicon carbide seed bar (1), the upside of each upper resistance heater (6)
A flow guiding screen (5) is provided with, near gas flow guiding to deposition plate (25) of the flow guiding screen for that will volatilize in growth chamber.
3. quickly preparing the device of silicon carbide as claimed in claim 2, it is characterised in that: on the upside of each flow guiding screen (5)
Inboard wall of furnace body on be provided with a deposition plate (25), the deposition plate is used to deposit the Si for the distillation that collection has neither part nor lot in depositionmCn
Gas, the deposition plate (25) is internal water cooling plant, for reducing its surface temperature.
4. quickly preparing the device of silicon carbide as described in claim 1, it is characterised in that: the ceramics seed rod (1) includes
The lower end of liquid metal diversion pipe (1-1), the liquid metal diversion pipe (1-1) is provided with interconnecting piece (1-2), the interconnecting piece
The internal diameter of (1-2) is greater than the internal diameter of the diversion pipe, and the diversion pipe is connected with the cavity in the interconnecting piece (1-2),
The periphery of the interconnecting piece (1-2) is provided with external screw thread (1-3), is provided with internal screw thread (28-1), seed crystal in seed crystal clamping (28)
It is connect between clamping (28) and the interconnecting piece (1-2) by mutually matched be screwed, under the seed crystal clamping (28)
End is provided with seed crystal holding chamber, and it is intracavitary and described by being located at that the upper end of silicon carbide seed (10) is inserted into the seed crystal clamping
The seed crystal jackscrew screw rod (28-2) of holding chamber two sides is fixed.
5. quickly preparing the device of silicon carbide as claimed in claim 4, it is characterised in that: the liquid metal diversion pipe (1-
1) it is provided with liquid cooled metal injection pipe (1-4) in, is provided with the first thermoelectricity in the liquid cooled metal injection pipe (1-4)
Even (3), the bottom of lower end insertion interconnecting piece (1-2) of first thermocouple (3), for measuring at silicon carbide seed (10)
Temperature information, the liquid cooled metal injection pipe (1-4) are used to inject liquid cooled metal into the cavity of the interconnecting piece.
6. quickly preparing the device of silicon carbide as described in claim 1, it is characterised in that: the ceramics seed rod (1) and institute
It states and is provided between growth chamber upper cover (7) ceramic stopper (4), interior heater strip is set inside the boron nitride liner upper cover (23)
(22), for preventing interconnecting piece (1-2) depositing silicon silicon；The current supply line (26) of the interior heater strip (22) is by ceramic stopper
(4) the ceramic stopper electrode hole (4-1) on is drawn.
7. quickly preparing the device of silicon carbide as described in claim 1, it is characterised in that: a left side for growth cavity main body (8)
One or more side wall carrier gas pipe, the inside of the side wall carrier gas pipe and the life are provided on side wall, lower wall and right side wall
Long cavity main body (8) is connected, and the outboard end of the side wall carrier gas pipe extends to the outside of the furnace body, the growth cavity main body
(8) it is provided in lower wall lower wall thermocouple cavity (8-2), right wall heat is provided on the right side wall of growth cavity main body (8)
The mode that galvanic couple chamber (8-1), the right wall thermocouple cavity (8-1) and lower wall thermocouple cavity (8-2) are connected through a screw thread is fixed on
It grows on cavity main body (8), again by right wall thermocouple cavity after porous boron nitride liner main body (18) is placed into growth cavity main body (8)
(8-1) and lower wall thermocouple cavity (8-2) are connected in growth cavity main body (8).
8. quickly preparing the device of silicon carbide as claimed in claim 7, it is characterised in that: the porous boron nitride liner main body
(18) position corresponding with lower wall thermocouple cavity (8-2) is provided with liner lower wall thermocouple jack (18-2), it is described
Porous boron nitride liner main body (18) is provided with liner right wall thermoelectricity in position corresponding with right wall thermocouple cavity (8-1)
Double jacks (18-1).
9. quickly preparing the device of silicon carbide as claimed in claim 8, it is characterised in that: the right wall thermocouple cavity (8-1)
It is inside provided with the second thermocouple (12), is provided with third thermocouple (15) in the lower wall thermocouple cavity (8-2), second heat
Galvanic couple (12) is used to measure the temperature information of porous boron nitride liner main body (18) right side central, the third thermocouple
(15) for measuring the temperature information in the middle part of porous boron nitride liner main body (18) bottom side, it is located at outside first growth chamber
Second thermocouple (12) and third thermocouple (15) periphery be arranged water cooling copper coil (11).
10. quickly preparing the device of silicon carbide as described in claim 1, it is characterised in that: the side wall carrier gas pipe with it is described
The contact portion of furnace body is provided with electroforming metal interface (29), realizes that the sealing with furnace body connects by the electroforming metal interface (29)
It connects；Valve body is provided on the side wall carrier gas pipe, air inlet pipe (17) and exhaust pipe (24).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112064110A (en) * | 2020-10-16 | 2020-12-11 | 璨隆科技发展有限公司 | Temperature control device for growth of silicon carbide crystal |
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