CN109371461A - A kind of electric-resistivity method growth carborundum crystals device and method - Google Patents
A kind of electric-resistivity method growth carborundum crystals device and method Download PDFInfo
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- CN109371461A CN109371461A CN201811419785.0A CN201811419785A CN109371461A CN 109371461 A CN109371461 A CN 109371461A CN 201811419785 A CN201811419785 A CN 201811419785A CN 109371461 A CN109371461 A CN 109371461A
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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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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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
Abstract
A kind of electric-resistivity method growth carborundum crystals device, device includes growth furnace body, there is pedestal below furnace interior, it is connect above pedestal with crucible tray, has seed rod above crucible, seed slot is arranged at bottom, it is with temperature thermocouple outside, there is insulation cover between furnace body and crucible, furnace body is equipped with air inlet pipe and an air outlet pipe, volume control device, thermometer and barometer are equipped on escape pipe.Electric-resistivity method growth carborundum crystals method includes: heating test run step, cooling dummy run phase, adjustment and the practical growth preparation process of amendment step, crystal.
Description
Technical field
The present invention relates to carborundum crystals correlative technology field, specially a kind of electric-resistivity method growth silicon-carbide crystal and
Method.
Background technique
Carborundum crystals as a kind of important technology crystal, be widely used in science and technology, national defence with it is civilian
Industrial, electronic technology many fields.Such as infra-red transmitting window gate material, the substrate base of microelectronic field, laser host, optics
Element and other purposes etc..Kyropoulos are one kind of melt method.Silicon carbide is grown using kyropoulos, first has to utilize crystal growth
System constructs one in the temperature field for longitudinally and radially possessing suitable gradient including calandria, tungsten crucible and tungsten radiation shield etc.；
Then by heating, melt high purity aluminium oxide raw material in crucible；Using journeys such as seeding, shouldering, isometrical, ending and annealing
Sequence finally obtains single-crystal silicon carbide.The growing large-size single-crystal silicon carbide advantage incomparable there are many other techniques, but its is right
Process and temperature field requirement are high, and any subtle procedure operation is improper or thermal field design is unreasonable all to cause experiment to be lost
It loses.
Current various growth of silicon carbide all pay close attention tos one problem, exactly slow and evenly cool down as far as possible, to avoid as far as possible
Undesirable variation occurs for crystals in temperature-fall period, influences the quality of crystal, but all over seeing the prior art, there is no for
How the effective embodiment that at the uniform velocity cools down is implemented, therefore due to the complexity of temperature-fall period, only straight line is downgraded in proportion,
It can not be achieved and at the uniform velocity cool down, because being protected in low-temperature zone as the temperature difference inside and outside device constantly changes
Temperature acts on more obvious, but any crystal growing apparatus can be kept the temperature again, then simply implementing at the uniform velocity cooling is nothing
What method was realized, only straight line downgrades heating power in proportion, and actually or speed change cools down, and the variation of rate can not be pre-
Estimate.
Summary of the invention
The purpose of the present invention is to provide a kind of kyropoulos electric-resistivity method growth silicon-carbide crystal and methods, existing to solve
There is technology to cannot achieve the problem of really at the uniform velocity cooling down, and proposes a kind of realization side at the uniform velocity to cool down that really can be implemented
Method.
To achieve the above object, the invention provides the following technical scheme: a kind of kyropoulos electric-resistivity method grows carborundum crystals
Device, the device include: growth furnace body, insulation cover, crucible, electronic pulling apparatus, axle sleeve, seed rod, heating device, flow
Control device, escape pipe, barometer, pedestal, crucible tray, seed slot, vacuum system, temperature thermocouple, thermometer and air inlet pipe.
It is characterized by: being welded with pedestal below the growth furnace furnace interior, it is connected above the pedestal with crucible tray, and crucible
Support top is chimeric crucible, seed rod is mounted with above the crucible, and pass through axle sleeve and electronic pulling apparatus at the top of seed rod
It is connected, the crucible bottom is provided with seed slot, and crucible periphery is mounted at least two groups heating device, the crucible periphery
It is mounted at least two groups posture temperature thermocouple group, and at least two groups posture temperature thermocouple group adds at least two groups
Thermal is alternately installed in the z-axis direction, insulation cover is equipped between growth furnace body and the crucible, and grow under furnace body
Side left side is equipped with the vacuum system that can be evacuated outward, on the left of the growth furnace body top and lower right-hand side be separately installed with into
Tracheae and escape pipe, and from extroversion growth furnace body direction, to be sequentially installed with volume control device, thermometer gentle in air inlet pipe
Pressure is counted, and is sequentially installed with volume control device, thermometer and barometer from extroversion growth furnace body direction on the escape pipe.Institute
State air inlet pipe entrance gas from outer suction port be sent into, and be sent into air inlet pipe before by insertion growth the left outside wall of furnace body it
Interior heat exchanging part is to be heated to the temperature roughly the same in device.Each group of heating device all connects identical heating power supply,
The voltage peak of the heating power supply can make each group of heating device promote temperature to 2000 DEG C, and each group of heating device is right with its
Automatically controlled slide rheostat is provided between the heating power supply answered, the automatically controlled slide rheostat is with Serial regulation load voltage
Mode adjusts the actual output temperature of each group of heating device.
Further, pairs of convective tank is provided on the insulation cover, and insulation cover is set as the cylinder of open-ended
Body structure；Heating device described in every group is circular heating tube, and is provided with and is parallel to each other two-by-two and height different at least two,
And downward projection position is overlapped；The circular heating tube is two semicircles heating ring in parallel, is passing through opposite 180 ° in the center of circle
Opposite location is respectively connected to positive and negative load；The volume control device is to automatically control the anti-corrosion perpendicular to escape pipe or air inlet pipe
The mode of the opening and closing of baffle is to realize flow control；The crucible tray material is set as high temperature resistant and the stronger ceramics of toughness, institute
The material for stating crucible and seed slot is set as ceramics resistant to high temperature；The thermometer is inductive thermal dipole thermometer, the temperature
The connected thermocouple of degree meter is directly protruding into the gas circuit in air inlet pipe and an air outlet pipe to be contacted with gas；The seed slot upper surface
To lower recess, the seed crystal inside groove to lower recess equipped with the square or rectangular for setting seed crystal in 1 is to place seed crystal；The frame
Formula temperature thermocouple group is to be provided with two groups on the frame of annular, and there are four heat for the setting of posture temperature thermocouple group described in every group
Posture temperature thermocouple, the evenly dispersed setting on the frame of annular of four posture temperature thermocouples；The pedestal is closed by high temperature resistant
Gold is made；The vacuum system can be opened and closed to connect with space within insulation cover, and have air exhauster；The axle sleeve and seed rod
The central axis insertion hit exactly from the top of the growth furnace body and insulation cover.The heat exchanging part is the disk for coiling 50 groups or more
Pipe group.More coiled structure just can guarantee that the gas temperature to be passed through in heat exchanging part is effectively promoted, with in device
Temperature is identical to be advisable.
A kind of method of kyropoulos electric-resistivity method growth carborundum crystals, it is raw according to a kind of foregoing kyropoulos electric-resistivity method
Long silicon-carbide crystal has been carried out, which is characterized in that includes the following steps.
1) test run step is heated: device is closed, it is evacuated to 0.9-0.95 atmospheric pressure with vacuum system, heats the heating
Device to device internal temperature reaches 1900 DEG C, restores internal pressure to standard atmospheric pressure, passes through the linear tune of slide rheostat
Drop is downgraded the heating power of the heating device by the speed that straight line declines, and at the same time with 0.2-0.4m3The speed of/min is same
When from escape pipe outlet and from outer suction port air inlet, device internal temperature is down to 50 DEG C or more, monitoring is each in the process
In the normal range whether component working order, temperature decline situation and the closed situation of device, problematic, is overhauled, is supervised
Optionally normally then enter step (2).
2) cool down the dummy run phase: on the basis of being cooled to 50 DEG C from 1900 DEG C of constant speed, designing the heating device and pass through cunning
Move it is rheostatic linearly downgrade, by straight line decline speed downgrade the heating device heating power power curve, and
The flow changing curve for designing vacuum degree and escape pipe and air inlet pipe is evacuated to 0.1-0.03 atmosphere with device is closed
Between pressure, heats the heating device to device internal temperature and reach 1900 DEG C, it is flat by the Detection & Controling installed in PC machine
Platform issues real-time command to the heating device and volume control device, starts to simulate temperature-fall period, from escape pipe outlet and from
Outer suction port air inlet, and internal temperature lowering curve is measured by the posture temperature thermocouple group, by each posture thermometric heat
The average value of galvanic couple is as actual inside temperature.
3) the posture temperature thermocouple adjustment and amendment step: is received by the Detection & Controling platform installed in PC machine
Group measures internal temperature lowering curve data, observes whether it is constant speed temperature lowering curve, if being cooled to 50 DEG C from 1900 DEG C of constant speed
Isokinetic conditions are all satisfied, the flow changing curve for recording determining power curve and determining enters step (4)；If not full
Sufficient isokinetic conditions then return to step (2), re-start setting adjustment.
4) the practical growth preparation process of crystal: the powdery sic raw material of predetermined weight is taken, is put among crucible, by device
It is closed, it is evacuated between 0.1-0.03 atmospheric pressure, is warming up to 1900 DEG C, constant temperature 2 hours or more, guarantees that raw material is all molten
Change；In heat preservation, seed rod is dropped into predetermined seeding position with extremely slow speed, is lifted upwards with the speed of 0.5-5mm/h
Seeding, and constantly fill raw material and pass through aforementioned Detection & Controling at the same time from escape pipe outlet and from outer suction port air inlet
Platform carries out control heating power and outlet charge flow rate according to determining power curve and the flow changing curve determined, with etc.
While prompt drop temperature, crystal growth is controlled；It lifts to seed rod to predetermined position, when crystal reaches predetermined altitude, does not refill
Raw material simultaneously upwards with pole jogging speed be pulled away from seeding bar, by slide rheostat linearly downgrade, with speed identical with front end after
Continuous to execute constant speed cooling, temperature is to 50 DEG C hereinafter, pressure to 1 atmospheric pressure, device for opening takes in raising device in reduction device
Crystal out.
Further, the above method can be corrected are as follows: in the step (1), be evacuated to vacuum system 0.9-0.95 big
Air pressure, and at the same time with 0.2-0.4m3The speed of/min is simultaneously from escape pipe outlet and from air inlet pipe air inlet；The step (4)
In, A DEG C of temperature when predetermined altitude is reached by actual observation record crystal, it will be described from 1900 DEG C of constant speed in abovementioned steps (2)
It is divided into slope different two sections of constant speed temperature-fall period high temperature section B and low-temperature zone C on the basis of being cooled to 50 DEG C, and low-temperature zone C's is oblique
Rate is more precipitous than high temperature section B, simulates temperature-fall period in two stages, and obtains adapting to high temperature section B and low-temperature zone C in step (3)
Two stage determination power curve and the flow changing curve that determines, and in step (4), with what is be consistent with low-temperature zone C
The cooling of cooling rate constant speed.
Compared with prior art, although the invention has the following advantages: 1) the ring heater heating of at least two circles
Area is few, but can satisfy requirement, the device and cost of saving；2) at least in being arranged symmetrically between ring heater
Thermocouple measuring temperature, can obtain most true most proper temperature value, it is remote super arbitrarily to place thermometric dress in the prior art
The method for sensing set；3) many people think, it is the best mode for preventing crystal from ging wrong that cooling is at the uniform velocity carried out for crystal, but
It is how to carry out tuning at the uniform velocity to meet the requirements, the prior art there are no similar scheme or enlightenment.If only with this field skill
Art personnel's universal experience is difficult to infer application scheme, and application scheme is had breakthrough by careful consideration.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
In figure: 1, grow furnace body, 2, insulation cover, 3, crucible, 4, electronic pulling apparatus, 5, axle sleeve, 6, seed rod, 7, plus
Thermal, 8, volume control device, 9, escape pipe, 10, barometer, 11, pedestal, 12, crucible tray, 13, seed slot, 14, vacuum
System, 15, temperature thermocouple, 16, thermometer, 17, air inlet pipe, 18, outer suction port, 19, heat exchanging part.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are 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.
Embodiment 1
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of kyropoulos electric-resistivity method growth silicon-carbide crystal,
The device includes: growth furnace body 1, insulation cover 2, crucible 3, electronic pulling apparatus 4, axle sleeve 5, seed rod 6, heating device 7, stream
Amount control device 8, escape pipe 9, barometer 10, pedestal 11, crucible tray 12, seed slot 13, vacuum system 14, temperature thermocouple
15, thermometer 16 and air inlet pipe 17.It is characterized by: 1 lower inside of growth furnace body is welded with pedestal 11, the pedestal
11 tops are connected with crucible tray 12, and it is chimeric above crucible tray 12 have crucible 3, be mounted with seed rod 6 above the crucible 3,
And be connected by axle sleeve 5 with electronic pulling apparatus 4 at the top of seed rod 6,3 bottom of crucible is provided with seed slot 13, and earthenware
3 periphery of crucible is mounted at least two groups heating device 7, and 3 periphery of crucible is mounted at least two groups posture temperature thermocouple group 15,
And at least two groups posture temperature thermocouple group 15 replaces installation, institute at least two groups heating device 7 in the z-axis direction
It states insulation cover 2 is installed between growth furnace body 1 and crucible 3, and grow 1 lower left of furnace body and be equipped with and can be evacuated outward
Vacuum system 14,1 left side top of the growth furnace body and lower right-hand side are separately installed with air inlet pipe 18 and escape pipe 9, and into
It is sequentially installed with volume control device 8, thermometer 16 and barometer 10 from extroversion growth 1 direction of furnace body on tracheae 18, it is described
Volume control device 8, thermometer 16 and barometer 10 are sequentially installed with from extroversion growth 1 direction of furnace body on escape pipe 9.This
In, although the ring heater heating surface (area) (HS of at least two circles is few, it can satisfy requirement, the device and cost of saving；With extremely
The thermocouple measuring temperature being arranged symmetrically between ring heater less can obtain most true most proper temperature number
Value, the remote super method for sensing for arbitrarily placing temperature measuring equipment in the prior art.Flow control dress is respectively provided in air inlet pipe and an air outlet pipe
It sets, and a part of core scheme of the present invention, provides condition for the following realization at the uniform velocity to cool down.What the air inlet pipe entered
Gas is sent into from outer suction port, and is sent into before air inlet pipe by the heat exchanging part within the insertion growth left outside wall of furnace body to add
The heat extremely temperature roughly the same in device.Each group of heating device 7 all connects identical heating power supply, the heating power supply
Voltage peak can make each group of heating device 7 promote temperature to 2000 DEG C, each group of heating device 7 heating power supply corresponding with its
Between be provided with automatically controlled slide rheostat, which is adjusted each in a manner of Serial regulation load voltage
The actual output temperature of group heating device 7.
Further, it is provided with pairs of convective tank on the insulation cover 2, and insulation cover 2 is set as the circle of open-ended
Column structure；Heating device 7 described in every group is circular heating tube, and is provided with and is parallel to each other two-by-two and height different at least two
It is a, and downward projection position is overlapped；The circular heating tube is two semicircles heating ring in parallel, opposite by the center of circle
180 ° of opposite locations are respectively connected to positive and negative load；The volume control device 8 is to automatically control perpendicular to escape pipe or air inlet pipe
Anti-corrosion baffle opening and closing mode to realize flow control；12 material of crucible tray is set as high temperature resistant and toughness is stronger
The material of ceramics, the crucible 3 and seed slot 13 is set as ceramics resistant to high temperature；The thermometer 16 is inductive thermal galvanic couple temperature
Degree is counted, and is contacted in the gas circuit that the thermocouple that the thermometer 16 is connected is directly protruding into air inlet pipe 17 and escape pipe 9 with gas；
13 upper surface of seed slot is to lower recess, in the seed crystal to lower recess equipped with the square or rectangular for setting seed crystal in 1
Slot is to place seed crystal；The posture temperature thermocouple group 15 is two groups to be provided on the frame of annular, and posture described in every group is surveyed
The setting of galvanic couple group 15 is warmed there are four hot posture temperature thermocouple, four posture temperature thermocouples are evenly dispersed on the frame of annular
Setting；The pedestal 11 is made of high-temperature alloy；The vacuum system 14 can be opened and closed to connect with space within insulation cover 2,
And has air exhauster；The central axis that the axle sleeve 5 and seed rod 6 are hit exactly from the top of the growth furnace body 1 and insulation cover 2
Insertion.The heat exchanging part is the coil pipe group for coiling 50 groups or more.More coiled structure, just can guarantee in heat exchanging part wait be passed through
Gas temperature is effectively promoted, and is advisable with identical as temperature in device.
Embodiment 2
A kind of method of kyropoulos electric-resistivity method growth carborundum crystals, according to a kind of kyropoulos electric-resistivity method growth carbon above-mentioned
SiClx crystal unit has been carried out, which is characterized in that includes the following steps.
1) test run step is heated: device is closed, it is evacuated to 0.9-0.95 atmospheric pressure with vacuum system 14, heating is described to be added
Thermal 7 to device internal temperature reaches 1900 DEG C, restores internal pressure to standard atmospheric pressure, passes through the linear of slide rheostat
It downgrades, the heating power of the heating device is downgraded by the speed that straight line declines, and at the same time with 0.2-0.4m3The speed of/min
Simultaneously from escape pipe outlet and from outer suction port air inlet, device internal temperature is down to 50 DEG C or more, is monitored in the process
In the normal range whether each component working order, temperature decline situation and the closed situation of device, problematic, is overhauled,
Monitoring situation normally then enters step (2).
2) cool down the dummy run phase: on the basis of being cooled to 50 DEG C from 1900 DEG C of constant speed, designing the heating device 7 and pass through cunning
Move it is rheostatic linearly downgrade, by straight line decline speed downgrade the heating device heating power power curve, and
The flow changing curve for designing vacuum degree and escape pipe and air inlet pipe is evacuated to 0.1-0.03 atmosphere with device is closed
Between pressure, heats the heating device 7 to device internal temperature and reach 1900 DEG C, it is flat by the Detection & Controling installed in PC machine
Platform issues real-time command to the heating device 7 and volume control device 8, starts to simulate temperature-fall period, from escape pipe outlet and
From outer suction port air inlet, and internal temperature lowering curve is measured by the posture temperature thermocouple group 15, each posture is surveyed
The average value of galvanic couple is warmed as actual inside temperature.
3) the posture temperature thermocouple adjustment and amendment step: is received by the Detection & Controling platform installed in PC machine
Group 15 measures internal temperature lowering curve data, observes whether it is constant speed temperature lowering curve, if being cooled to 50 from 1900 DEG C of constant speed
DEG C isokinetic conditions are all satisfied, the flow changing curve for recording determining power curve and determining enters step (4)；If no
Meet isokinetic conditions, then return to step (2), re-starts setting adjustment.Here step (2) and (3) are core ideas, here only
If only downgrading heating power in proportion, since inside and outside temperature difference is not that constant and device is kept the temperature when temperature is lower
Effect is better, and when actually temperature is low, cooling target is difficult to realize, and needs to increase the flow of outlet in practice, together
When in order to guarantee internal pressure, feed rate here is needed according to throughput and the internal pressure to be kept is gone out, and both is considered
Under the premise of adjust and obtain.
4) the practical growth preparation process of crystal: the powdery sic raw material of predetermined weight is taken, is put among crucible, by device
It is closed, it is evacuated between 0.1-0.03 atmospheric pressure, is warming up to 1900 DEG C, constant temperature 2 hours or more, guarantees that raw material is all molten
Change；In heat preservation, seed rod (6) is dropped into predetermined seeding position with extremely slow speed, is mentioned upwards with the speed of 0.5-5mm/h
Pull is brilliant, and constantly fills raw material, from escape pipe outlet and from outer suction port air inlet, passes through aforementioned detection and control at the same time
Platform processed carries out control heating power and air inlet outgassing rate according to determining power curve and the flow changing curve determined, with
While constant speed cools down, crystal growth is controlled；It lifts to seed rod to predetermined position, when crystal reaches predetermined altitude, no longer fills out
It fills raw material and seeding bar is pulled away from pole jogging speed upwards, by linearly downgrading for slide rheostat, with speed identical with front end
Constant speed cooling is continued to execute, reduces in device temperature to 50 DEG C hereinafter, pressure is to 1 atmospheric pressure in raising device, device for opening,
Take out crystal.
Embodiment 3
Alternatively, it such as the method for embodiment 2, in the step (1), is evacuated to vacuum system (14) 0.9-0.95 big
Air pressure, and at the same time with the speed of 0.2-0.4m3/min simultaneously from escape pipe outlet and from air inlet pipe air inlet；The step (4)
In, A DEG C of temperature when predetermined altitude is reached by actual observation record crystal, it will be described from 1900 DEG C of constant speed in abovementioned steps (2)
It is divided into slope different two sections of constant speed temperature-fall period high temperature section B and low-temperature zone C on the basis of being cooled to 50 DEG C, and low-temperature zone C's is oblique
Rate is more precipitous than high temperature section B, simulates temperature-fall period in two stages, and obtains adapting to high temperature section B and low-temperature zone C in step (3)
Two stage determination power curve and the flow changing curve that determines, and in step (4), with what is be consistent with low-temperature zone C
The cooling of cooling rate constant speed.Here it is mainly in view of such problems, i.e., at a lower temperature, a possibility that defect occurs in crystal
It substantially reduces, in order to shorten overall time, here lower than after some temperature, rate of temperature fall can be adjusted to more precipitous
Cool down straight line, cools down at faster speed, to meet production requirement.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection scope of invention.
Claims (4)
1. a kind of electric-resistivity method grows carborundum crystals device, which includes: growth furnace body (1), insulation cover (2), crucible
(3), electronic pulling apparatus (4), axle sleeve (5), seed rod (6), heating device (7), volume control device (8), escape pipe (9),
Barometer (10), pedestal (11), crucible tray (12), seed slot (13), vacuum system (14), temperature thermocouple (15), thermometer
(16) and air inlet pipe (17), outer suction port (18), heat exchanging part (19), it is characterised in that:
Growth furnace body (1) lower inside is welded with pedestal (11), is connected above the pedestal (11) with crucible tray (12)
Connect, and it is chimeric above crucible tray (12) have crucible (3), be mounted with seed rod (6) above the crucible (3), and seed rod (6) pushes up
Portion is connected by axle sleeve (5) with electronic pulling apparatus (4), and crucible (3) bottom is provided with seed slot (13), and crucible
(3) periphery is mounted at least two groups heating device (7), and crucible (3) periphery is mounted at least two groups posture temperature thermocouple
Group (15), and at least two groups posture temperature thermocouple group (15) and at least two groups heating device (7) are in the z-axis direction
It alternately installs, is equipped with insulation cover (2) between the growth furnace body (1) and crucible (3), and grow left below furnace body (1)
Side is equipped with the vacuum system (14) that can be evacuated outward, and top and lower right-hand side are installed respectively on the left of the growth furnace body (1)
There are air inlet pipe (18) and escape pipe (9), and is sequentially installed with flow control from extroversion growth furnace body (1) direction in air inlet pipe (18)
Device (8), thermometer (16) and barometer (10) processed are successively pacified from extroversion growth furnace body (1) direction on the escape pipe (9)
Equipped with volume control device (8), thermometer (16) and barometer (10)；
The gas that the air inlet pipe (17) enters is sent into (18) from outer suction port, and is sent into before air inlet pipe (17) by insertion
The heat exchanging part (19) within furnace body (1) left outside wall is grown to be heated to the temperature roughly the same in device；
Each group of heating device (7) all connects identical heating power supply, and the voltage peak of the heating power supply can make each group to add
Thermal (7) promotes temperature to 2000 DEG C, is provided between each group of heating device (7) and its corresponding heating power supply automatically controlled
Slide rheostat, the automatically controlled slide rheostat adjust each group of heating device (7) in a manner of Serial regulation load voltage
Actual output temperature.
2. a kind of electric-resistivity method according to claim 1 grows carborundum crystals device, it is characterised in that:
Pairs of convective tank is provided on the insulation cover (2), and insulation cover (2) is set as the cylindrical structure of open-ended；
Heating device described in every group (7) is circular heating tube, and is provided with and is parallel to each other two-by-two and height different at least two,
And downward projection position is overlapped；The circular heating tube is two semicircles heating ring in parallel, is passing through opposite 180 ° in the center of circle
Opposite location is respectively connected to positive and negative load；
The volume control device (8) by automatically control perpendicular to the opening and closing of escape pipe or the anti-corrosion baffle of air inlet pipe in a manner of with
Realize flow control；
Crucible tray (12) material is set as high temperature resistant and the stronger ceramics of toughness, the crucible (3) and seed slot (13)
Material is set as ceramics resistant to high temperature；
The thermometer (16) is inductive thermal dipole thermometer, the thermocouple that the thermometer (16) is connected be directly protruding into
It is contacted in gas circuit in tracheae (17) and escape pipe (9) with gas；
Seed slot (13) upper surface to lower recess, equipped with the square or rectangular for setting seed crystal in 1 to lower recess
Seed crystal inside groove is to place seed crystal；
The posture temperature thermocouple group (15) is to be provided with two groups, and posture temperature thermocouple described in every group on the frame of annular
There are four hot posture temperature thermocouple, the evenly dispersed settings on the frame of annular of four posture temperature thermocouples for group (15) setting；
The pedestal (11) is made of high-temperature alloy；
The vacuum system (14) can be opened and closed to connect with space within insulation cover (2), and have air exhauster；
The central axis that the axle sleeve (5) and seed rod (6) are hit exactly from the top of growth furnace body (1) and insulation cover (2)
Insertion；
The heat exchanging part is the coil pipe group for coiling 50 groups or more.
3. a kind of electric-resistivity method grows carborundum crystals method, a kind of electric-resistivity method growth silicon carbide according to claim 2
Crystal device is to implement, which comprises the following steps:
1) test run step is heated: device is closed, it is evacuated to 0.9-0.95 atmospheric pressure with vacuum system (14), heats the heating
Device (7) to device internal temperature reaches 1900 DEG C, restores internal pressure to standard atmospheric pressure, passes through the linear of slide rheostat
It downgrades, the heating power of the heating device is downgraded by the speed that straight line declines, and at the same time with the speed of 0.2-0.4m3/min
Simultaneously from escape pipe outlet and from outer suction port air inlet, device internal temperature is down to 50 DEG C or more, is monitored in the process
In the normal range whether each component working order, temperature decline situation and the closed situation of device, problematic, is overhauled,
Monitoring situation normally then enters step (2)；
2) cool down the dummy run phase: on the basis of being cooled to 50 DEG C from 1900 DEG C of constant speed, designing the heating device (7) and pass through sliding
It is rheostatic linearly to downgrade, the power curve of the heating power of the heating device, Yi Jishe are downgraded by the speed that straight line declines
The flow changing curve for counting vacuum degree and escape pipe and air inlet pipe is evacuated to 0.1-0.03 atmospheric pressure with device is closed
Between, it heats the heating device (7) to device internal temperature and reaches 1900 DEG C, it is flat by the Detection & Controling installed in PC machine
Platform issues real-time command to the heating device (7) and volume control device (8), starts simulation temperature-fall period, and from escape pipe
Outlet and from outer suction port air inlet, and internal temperature lowering curve is measured by the posture temperature thermocouple group (15), it will be each
The average value of a posture temperature thermocouple is as actual inside temperature；
3) the posture temperature thermocouple group adjustment and amendment step: is received by the Detection & Controling platform installed in PC machine
(15) internal temperature lowering curve data are measured, observe whether it is constant speed temperature lowering curve, if being cooled to 50 from 1900 DEG C of constant speed
DEG C isokinetic conditions are all satisfied, the flow changing curve for recording determining power curve and determining enters step (4)；If no
Meet isokinetic conditions, then return to step (2), re-starts setting adjustment；
4) the practical growth preparation process of crystal: taking the powdery sic raw material of predetermined weight, be put among crucible, and device is close
It closes, is evacuated between 0.1-0.03 atmospheric pressure, be warming up to 1900 DEG C, constant temperature 2 hours or more, guarantee that raw material all melts；
In heat preservation, seed rod (6) is dropped into predetermined seeding position with extremely slow speed, it is upward with the speed of 0.5-5mm/h
Lift seeding, and constantly fill raw material, from escape pipe outlet and from outer suction port air inlet, at the same time by it is aforementioned detection with
Control platform carries out control heating power and air inlet outgassing rate according to determining power curve and the flow changing curve determined,
While cooling with constant speed, crystal growth is controlled；
It lifts to seed rod to predetermined position, when crystal reaches predetermined altitude, does not refill raw material and upwards with the drawing of pole jogging speed
From seeding bar, by linearly downgrading for slide rheostat, constant speed cooling is continued to execute with speed identical with front end, reduces device
Interior temperature is to 50 DEG C hereinafter, pressure to 1 atmospheric pressure, device for opening takes out crystal in raising device.
4. a kind of method of kyropoulos electric-resistivity method growth carborundum crystals as claimed in claim 3, it is characterised in that:
In the step (1), it is evacuated to 0.9-0.95 atmospheric pressure with vacuum system (14), and at the same time with 0.2-0.4m3/min
Speed simultaneously from escape pipe outlet and from air inlet pipe air inlet；
In the step (4), A DEG C of temperature when predetermined altitude is reached by actual observation record crystal, by institute in abovementioned steps (2)
It states to be cooled to from 1900 DEG C of constant speed and is divided into slope different two sections of constant speed temperature-fall period high temperature section B and low-temperature zone C on the basis of 50 DEG C,
And the slope ratio high temperature section B of low-temperature zone C is precipitous, simulates temperature-fall period in two stages, and obtains adapting to high temperature in step (3)
The power curve of the two stage determination of section B and low-temperature zone C and the flow changing curve determined, and in step (4), with it is low
The cooling rate constant speed cooling that temperature section C is consistent.
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