阅读说明：本技术 快速制备碳化硅的方法 (The method for quickly preparing silicon carbide ) 是由 李超 于 2019-09-26 设计创作，主要内容包括：本发明公开了一种快速制备碳化硅的方法,涉及碳化硅技术领域。所述方法将碳化硅块放置于第一生长腔与第二生长腔之间,籽晶位于第一生长腔的多孔氮化硼内衬中,通过内置热偶及液态金属冷却液的陶瓷籽晶杆给籽晶降温,使其附近建立起合适的生长温度和温度梯度。通过生长腔主体进入多孔氮化硼内衬中布置热电偶,监控生长环境的生长温度和气氛中的温度梯度,生长腔主体上的载气管道将使得高温载气携带碳化硅挥发出的气体至籽晶上进行生长。所述方法的温度梯度及输运过程可控,制备的碳化硅质量较高。(The invention discloses a kind of methods 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 the method, 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 the method are controllable, and the silicon carbide quality of preparation is higher.)

1. a kind of method for quickly preparing silicon carbide, the method use the device for quickly preparing silicon carbide, it is characterised in that packet Include following steps:

Silicon carbide seed (10) is assemblied in seed crystal clamping (28), seed crystal jackscrew screw rod (28-2) is tightened, then by interconnecting piece (1-2) is installed on ceramic seed rod (1) by external screw thread (1-3) mutual cooperation on internal screw thread (28-1) and seed crystal clamping；

Growth cavity main body (8) is assembled in furnace body, and porous boron nitride liner (18) is assembled in growth cavity main body (8) Silicon carbide seed (10) is down to porous boron nitride liner (18) inside by portion, mobile ceramics seed rod (1), is placed in interior heater strip (22), first then is formed by two pieces of liner cover assembly (23-1) lids to the upper end opening of porous boron nitride liner (18) Growth chamber, while silicon carbide seed (10) and interior heater strip (22) being wrapped in the first growth chamber, silicon carbide bulk (27) is filled out It fills between growth cavity main body (8) and the first growth chamber, along upper placement graphite paper (21) in growth cavity main body (8), then covers Upper growth chamber upper cover (7) is simultaneously fixed；

The second thermocouple (12) and third thermocouple (15) are inserted into growth chamber right side wall thermocouple cavity (8-1) and growth respectively In chamber lower wall 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 Electroforming metal interface (29) and furnace sealing, and be connected with the carrier gas channel outside furnace body, water cooling copper coil (11) is to the second warm Galvanic couple (12) and third thermocouple (15) cooling；

It is vacuumized to entire furnace body, is then charged with inert gas, keep pressure 133Pa-13300Pa；By growing cavity main body (8) The main induction coil (19) on the outside of the second growth chamber, the upper induction coil (20), upper resistance heating constituted with growth chamber upper cover (7) Device (6), lower induction coil (14) are to growth chamber upper cover (7) and growth cavity main body (8) heating, so that the second thermocouple (12) and the The temperature of three thermocouple (15) reaches 2000 DEG C -2300 DEG C；Start internal heater (22), for preventing ceramic seed rod (1) Depositing silicon silicon；

Then the flow and temperature for adjusting ceramic seed rod (1) interior liquid metal (2), to the carbonization of ceramic seed rod (1) lower end Silicon seed (10) cooling, so that the first thermocouple (3) in ceramic seed rod (1) reaches 1700-2100 DEG C；Then it adjusts and powers on The power for hindering heater (6), main induction coil (19), upper induction coil (20) and lower induction coil (14) makes the first thermocouple (3) temperature gradient of 2K/mm to 20K/mm is set up between third thermocouple (15)；

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) to the second growth Carrier gas is formed in chamber, by carrier gas by silicon carbide bulk (27) by heat sublimation be Si_mC_nGas continually bring the first growth chamber into In and accelerated carbonation silico briquette (27) sublimation process, Si_mC_nIt is formed on gas transport to the solid/gas interface of silicon carbide seed (10) Carborundum crystals are simultaneously constantly grown up, until growing to required size, wherein m=1 or 2, n=0,1 or 2.

2. the method for quickly preparing silicon carbide as described in claim 1, it is characterised in that: the Si_mC_nGas is Si, Si₂C、 SiC₂, SiC mixed gas.

3. the method for quickly preparing silicon carbide as described in claim 1, it is characterised in that: the dress for quickly preparing silicon carbide It sets including furnace body, the furnace body is internally provided with growth cavity main body (8), sets in the upper end opening of growth cavity main body (8) It is equipped with growth chamber upper cover (7), the growth cavity main body (8) and growth chamber upper cover (7) constitute the second growth chamber, second growth It is provided on the upside of chamber resistance heater (6), the periphery of second growth chamber is provided with induction coil from top to bottom (20) and main induction coil (19) lower induction coil (14), are provided on the downside of second growth chamber, pass through the upper resistance Heater (6), upper induction coil (20), main induction coil (19) and lower induction coil (14) add second growth chamber Heat；It is provided with porous boron nitride liner main body (18) in second growth chamber, is provided in several in the liner main body It serves as a contrast hole (18-3), is provided with boron nitride liner upper cover (23) at the upper end opening of the liner main body, in the porous boron nitride Serve as a contrast main body (18) and the boron nitride liner upper cover (23) and constitute the first growth chamber, first growth chamber and the second growth chamber it Between space in be provided with silicon carbide bulk (27)；The lower end of the ceramics seed rod (1) sequentially passes through furnace body, growth from top to bottom It is entered in first growth chamber after chamber upper cover (7), boron nitride liner upper cover (23), setting in the ceramics seed rod (1) There is liquid cooled wire chamber, liquid metal is injected to cooling wire chamber by the liquid cooled metal injection pipe (1-4), it is described Seed crystal clamping (28), the silicon carbide seed (10) are fixedly connected on one end that silicon carbide seed bar is located in the first growth chamber It is fixed on the seed crystal clamping (28), gas tube (17) and exhaust pipe (24) is provided on the furnace body, passes through the inflation Inert gas is poured in pipe (17) Xiang Suoshu furnace body；The silicon carbide bulk (27) is being Si by heat sublimation_mC_nAfter gas, pass through load The effect of gas endlessly enters in the first growth chamber, Si_mC_nSolid/gas interface of the gas transport to silicon carbide seed (10) Upper formation carborundum crystals are simultaneously constantly grown up, until growing to required size, wherein m=1 or 2, n=0,1 or 2.

4. the method for quickly preparing silicon carbide as claimed in claim 3, 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； A deposition plate (25) is provided on inboard wall of furnace body on the upside of each flow guiding screen (5), the deposition plate is collected for depositing Have neither part nor lot in the Si of the distillation of deposition_mC_nGas, the deposition plate (25) is internal water cooling plant, for reducing its surface temperature.

5. as claimed in claim 3 quickly prepare silicon carbide method, it is characterised in that: it is described ceramics seed rod (1) include 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.

6. the method for quickly preparing silicon carbide as claimed in claim 5, 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； It is provided with ceramic stopper (4) between the ceramics seed rod (1) and the growth chamber upper cover (7), the boron nitride liner upper cover (23) internal that interior heater strip (22) is set, for preventing interconnecting piece (1-2) depositing silicon silicon；The power supply of the interior heater strip (22) Conducting wire (26) is drawn by the ceramic stopper electrode hole (4-1) on ceramic stopper (4).

7. the method for quickly preparing silicon carbide as claimed in claim 3, 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. the method for quickly preparing 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. the method for quickly preparing 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. as claimed in claim 3 quickly prepare silicon carbide method, 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).

Technical field

The present invention relates to carbonization silicon preparation method technical fields, more particularly to a kind of method 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 method of standby silicon carbide.

In order to solve the above technical problems, the technical solution used in the present invention is: a kind of method for quickly preparing silicon carbide, The method uses the device for quickly preparing silicon carbide, it is characterised in that includes the following steps:

By silicon carbide seed assembly in seed crystal clamping, seed crystal jackscrew screw rod is tightened, interconnecting piece is then passed through into internal screw thread and seed External screw thread mutual cooperation in crystalline substance clamping is installed on ceramic seed rod；

Growth cavity main body is assembled in furnace body, and porous boron nitride liner is assembled to growth chamber body interior, mobile ceramics Silicon carbide seed is down to porous boron nitride liner by seed rod, interior heater strip is placed in, then by two pieces of liner cover assemblies At lid to the upper end opening of porous boron nitride liner, the first growth chamber is formed, while silicon carbide seed and interior heater strip being wrapped up In the first growth chamber, silicon carbide bulk is filled between growth cavity main body and the first growth chamber, along upper on growth cavity main body Graphite paper is placed, growth chamber upper cover and fixation are then covered；

The second thermocouple and third thermocouple are inserted into growth chamber right side wall thermocouple cavity and growth chamber lower wall thermocouple respectively In chamber；Then by left side wall carrier gas pipe, right side wall carrier gas pipe and lower wall carrier gas pipe by electroforming metal interface and furnace sealing, and It is connected with the carrier gas channel outside furnace body, water cooling copper coil cools down to the second thermocouple and third thermocouple；

It is vacuumized to entire furnace body, is then charged with inert gas, keep pressure 133Pa-13300Pa；By growth cavity main body with Main induction coil, upper induction coil, upper resistance heater, lower induction coil on the outside of second growth chamber of growth chamber upper cover composition To growth chamber upper cover and growth cavity main body heating, so that the temperature of the second thermocouple and third thermocouple reaches 2000 DEG C -2300 ℃；Start internal heater, for preventing depositing silicon silicon on ceramic seed rod；

Then the flow and temperature for adjusting liquid metal in ceramic seed rod are dropped to the silicon carbide seed of ceramic seed rod lower end Temperature, so that the first thermocouple in ceramic seed rod reaches 1700-2100 DEG C；Then upper resistance heater, main induction line are adjusted The power of circle, upper induction coil and lower induction coil to set up 2K/mm extremely between the first thermocouple and third thermocouple The temperature gradient of 20K/mm；

It injects inert gas into the second growth chamber and is formed by left side wall carrier gas pipe, right side wall carrier gas pipe and lower wall carrier gas pipe Carrier gas, by carrier gas by silicon carbide bulk by heat sublimation be Si_mC_nGas continually bring into the first growth chamber and accelerated carbonation The sublimation process of silico briquette, Si_mC_nCarborundum 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: the Si_mC_nGas is Si, Si₂C、SiC₂, SiC mixed gas.

A further technical solution lies in: described quickly to prepare the device of silicon carbide include furnace body, the inside of the furnace body Be provided with growth cavity main body, be provided with growth chamber upper cover in the upper end opening of the growth cavity main body, the growth cavity main body and Growth chamber upper cover constitutes the second growth chamber, and resistance heater, second growth are provided on the upside of second growth chamber The periphery of chamber is provided with induction coil and main induction coil from top to bottom, is provided with lower induction on the downside of second growth chamber Coil, by the upper resistance heater, upper induction coil, main induction coil and lower induction coil to second growth chamber into Row heating；It is provided with porous boron nitride liner main body in second growth chamber, is provided in several in the liner main body Hole is served as a contrast, is provided with boron nitride liner upper cover, the porous boron nitride liner main body and institute at the upper end opening of the liner main body It states boron nitride liner upper cover and constitutes the first growth chamber, be provided with carbon in the space between first growth chamber and the second growth chamber SiClx block；It is laggard that the lower end of the ceramics seed rod sequentially passes through furnace body, growth chamber upper cover, boron nitride liner upper cover from top to bottom Enter into first growth chamber, liquid cooled wire chamber is provided in the ceramics seed rod, it is described to pass through liquid cooled gold Belong to injection pipe and inject liquid metal to cooling wire chamber, the silicon carbide seed bar is located on one end in the first growth chamber fixed It is connected with seed crystal clamping, the silicon carbide seed is fixed in the seed crystal clamping, is provided with gas tube and row on the furnace body Tracheae pours inert gas into the furnace body by the gas tube；The silicon carbide bulk is being Si by heat sublimation_mC_nGas Afterwards, it is endlessly entered in the first growth chamber by the effect of carrier gas, Si_mC_nGas transport is to the solid/gas of silicon carbide seed Carborundum crystals are formed on interface 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 deposition_mC_nGas 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 the method 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 method 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 sublimation_mC_nAfter gas, pass through carrier gas Effect endlessly enters in the first growth chamber, Si_mC_nIt 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 deposition_mC_nGas.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 Si_mC_nGas continually bring into the first growth chamber and add The sublimation process of fast silicon carbide bulk 27, Si_mC_nCarborundum 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.