CN107142520A - One kind control silicon carbide monocrystal growth device - Google Patents
One kind control silicon carbide monocrystal growth device Download PDFInfo
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- CN107142520A CN107142520A CN201710346415.8A CN201710346415A CN107142520A CN 107142520 A CN107142520 A CN 107142520A CN 201710346415 A CN201710346415 A CN 201710346415A CN 107142520 A CN107142520 A CN 107142520A
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- crucible
- induction coil
- crystal
- shaft
- raw material
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Classifications
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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
-
- 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
- C30B23/002—Controlling or regulating
Abstract
One kind control silicon carbide monocrystal growth device, its induction coil (1), crucible (2), air-channel system and lifting rotation control system are respectively positioned in vacuum chamber.Crucible (2) is located between the top tray (8) of lifting rotation control system and lower tray (10), is placed on the middle position in induction coil (1).Crucible (2) is coated with heat-insulation layer (4).Induction coil (1) is located at vacuum chamber center, to heating crucible (2).Crucible (2) is built with sic powder and seed crystal, for growing silicon carbice crystals.Air-channel system is connected on the wall of vacuum chamber side.By the movement of upper and lower pallet, the relative position of control crucible and coil；Rotary speed and the direction of crucible bottom and crucible pot cover are adjusted, the distance in raw material area and crystal growth area during control growing silicon carbice crystals；By raw material area and crystal growth offset from control, realize the accurate control of crystal growth temperature.
Description
Technical field
It is used to control silicon carbide monocrystal growth device the present invention relates to one kind.
Background technology
Carborundum is as third generation semiconductor material with wide forbidden band, compared with traditional semi-conducting material such as silicon and GaAs,
The features such as with broad-band gap, high heat conductance, high critical breakdown electric field and high carrier saturation drift velocity, its superior performance can
To meet modern electronic technology to high temperature, high frequency, high-power, photoelectron and radiation-resistant new demand, it is considered to be semiconductor
One of most promising material in Material Field.
Method prepared by single-crystal silicon carbide is mainly physical vapor transport.This conventional method is：Crystal growing process
In, inside crucible, sic raw material is in crucible bottom relatively-high temperature area (2200-2300 DEG C), and seed crystal is bonded in crucible pot
Cover as relatively low warm area (2100-2200 DEG C), crucible is integrally that closing is placed in the middle of heating coil, crucible bottom and pot
There is a certain distance in the middle of lid, the sic raw material distillation of high-temperature region, because raw material area and seed crystal have temperature difference, raw material is with gas
The form of state is sublimate into seed crystal face, and gas phase composition mainly has Si, Si2C and SiC2, gas phase crystallizes on seed crystal and forms carborundum
The temperature difference that crystal, raw material area and seed crystal face are present is the driving force source of silicon carbide monocrystal growth, such as United States Patent (USP)
US6261363B1 and Chinese patent CN1247831C.In Chinese patent CN1261622C, said structure is improved, earthenware
Crucible lid can be moved up and down, control crystal growth area temperature, but in crystal growth, raw material can be consumed constantly so that raw material area
Temperature can constantly change, so that thermograde can be influenceed, cause growing silicon carbice crystals quality to be difficult to control to.
In growth course, because raw material can be consumed constantly, the position of raw material surface relative induction coil can also become
Change, cause raw material area temperature to be continually changing change.Meanwhile, crystal constantly grows at seed crystal, can be gradually thickening, and plane of crystal is continuous
Moved to high-temperature region, surface temperature also can more and more higher, gas phase zone is shorter and shorter, causes the driving force of silicon carbide monocrystal growth to drop
It is low.The change of thermograde caused by the change of raw material sublimation temperature and plane of crystal temperature, can change thermal field inside crucible, shadow
The chemical composition of gaseous component is rung, in single crystal growth process, early stage temperature conditionss and the generation of latter temperature condition are very big
Change, is unfavorable for the stable growth of crystal.
The content of the invention
The purpose of the present invention is to overcome the problem of prior art is present, and proposes a kind of control silicon carbide monocrystal growth device.
The present invention can realize the accurate control of the raw material area that single-crystal silicon carbide is prepared to physical vapor transport and crystal growth area temperature
System, keeping temperature gradient uniformity is stable, single-crystal silicon carbide is grown in a stably and controllable environment, improves monocrystalline life
Long quality.
Silicon carbide monocrystal growth device of the present invention includes vacuum chamber, induction coil, crucible, air-channel system and lifting rotation
Control system.Induction coil, crucible, air-channel system and lifting rotation control system are respectively positioned in vacuum chamber, wherein the line of induction
Circle is located at vacuum chamber center, to heating crucible.Crucible is heater, and inside is equipped with sic powder and seed crystal, is used
In growing silicon carbice crystals.Crucible is located between the top tray of lifting rotation control system and lower tray, is placed on induction coil
Heat-insulation layer is coated with outside inside, crucible.Air-channel system is connected on the wall of vacuum chamber side, for providing growing silicon carbice crystals
When required atmosphere.
Described lifting rotation control system includes top tray, lower tray, upper rotary shaft and Shaft.Described pop-up
Disk and lower tray are separately fixed in rotary shaft and Shaft.Upper rotary shaft and Shaft are located at the center of pallet, lead to
Crossing servo-controlled motor controls upper and lower rotary shaft to move up and down and circular motion, drive top tray and lower tray lifting and
Circumference rotates.Raw material thing sic powder is positioned over the inner bottom part of crucible, and seed crystal is bonded in crucible crucible and covered.The bottom of crucible is consolidated
It is scheduled in lower tray, crucible crucible lid is fixed on the lower surface of top tray, crucible and crucible crucible cover split-type can also be fastened.Button
Crucible and crucible cover after conjunction can integrally vertically mobile and along the circumferential direction 360 ° of rotations of level.The crucible and earthenware of split
Crucible lid each 360 ° of independence can also rotate and move up and down.Crucible and crucible crucible lid are able to follow top tray and lower tray
Lifting or circular-rotation.Crucible, top tray, lower tray and induction coil and upper rotary shaft, Shaft are coaxial.Axial direction
On, top tray and lower tray are outside induction coil, in the radial direction, and top tray and lower tray are inside induction coil.
The upright projection of pallet is located at induction coil upright projection center.Vacuum chamber and induction coil are respectively arranged with cooling water dress
Put, there is a cooling water intake and delivery port to carry out water circulation respectively, recirculated water keeps constant temperature using external refrigeration machine
Degree.Induction coil, crucible, heat-insulation layer, air-channel system, top tray, lower tray, upper rotary shaft and Shaft are in vacuum chamber
It is interior.Vacuum chamber is provided with gas circuit import and export, gas is passed through, to adjust air inflow and gaseous species.
Crucible crucible lid is bonded with seed crystal, and seed crystal face is crystal growth area, grows single-crystal silicon carbide；Raw material area is located at crucible
Interior bottom.
During crystal growth, raw material zone position and crystal in crucible can be made by adjusting the motion of crucible and crucible pot cover
Vitellarium surface location relative induction coil position is constant, so as to ensure temperature and thermograde in whole crystal growing process
It is consistent.
Apparatus of the present invention are during silicon carbide monocrystal growth, and induction coil is fixed, by controlling top tray with
The rotating speed of pallet and the speed of oscilaltion movement, realize that raw material area and crystal growth area temperature are accurately controlled.Due to crucible with
Top tray and lower tray are moved up and down, and by the lifting of crucible, the medium position in control crucible inner bottom part raw material area is located all the time
Peak in induction coil center, namely heating-up temperature.By the lifting of crucible pot cover, the height of gas phase zone in crucible is set to begin
Keep eventually constant.
The rotating speed of lifting rotation control system is controllable in 0.05-30rpm, and lifting speed is divided into two grades of speed, and shelves rise at a slow speed
Drop scope is 0.06-20mm/h, and quick shelves range is 0.1-60mm/min；
Induction coil heating uses heating in medium frequency mode, by controlling power output, makes induction coil middle portion temperature highest
Point range is 2200-2300 DEG C, and the region between seed crystal and growth raw material surface is referred to as gas phase zone, and gas phase zone altitude range can
It is set to 5-60mm；Rotary shaft drives top tray and lower tray to rotate and move up and down, and control crucible and crucible pot cover are mutually transported
It is dynamic, growth raw material area temperature is kept constant, while the thermograde on growth raw material area to crystal growth area surface keeps constant,
So the height of gas phase zone also keeps constant, realizes the accurate control of growth temperature and thermograde.
The present invention can accurately control the temperature in growth raw material area and crystal growth area, make growth raw material area all the time in most
Good temperature, while keeping growth raw material area and plane of crystal apart from constant, so, is used as the temperature in crystal growth driving force source
Gradient and the chemical composition of gaseous component keep constant, therefore, are grown in the environment that crystal is being stablized always, greatly improve
Crystal growth quality and efficiency.
Growth raw material is carborundum powder, and purity is more than 99.999%, and particle diameter is between 0.05-1 scope.
Brief description of the drawings
Fig. 1 is section of structure of the invention；1 induction coil；2 crucibles；3 crucible pot covers；4 heat-insulation layers；5 raw material areas；6 seeds
It is brilliant；Rotary shaft on 7；8 top trays；9 Shafts；10 lower trays；11 fix bars；12 vacuum chambers；
Fig. 2 is structure top view of the invention.
Embodiment
The present invention is further illustrated with reference to the accompanying drawings and detailed description.
As shown in figure 1, crystal growing apparatus of the present invention include vacuum chamber 12, induction coil 1, crucible 2, air-channel system and
Lifting rotation control system, induction coil 1, crucible 2, air-channel system and lifting rotation control system are respectively positioned in vacuum chamber.
Crucible 2 is located between the top tray 8 of lifting rotation control system and lower tray 10, is placed on the middle position in induction coil 1.
Crucible 2 is coated with heat-insulation layer 4.Induction coil 1 is located at vacuum chamber center, to heating crucible 2.Crucible 2 is heating
Body, built with sic powder and seed crystal, for growing silicon carbice crystals.Air-channel system is connected on the wall of vacuum chamber side, is used
Required atmosphere when growing silicon carbice crystals are provided.
Described lifting rotation control system includes top tray 8, lower tray 10, upper rotary shaft 7 and Shaft 9.Pop-up
Disk 8, lower tray 10 are separately fixed in rotary shaft 7 and Shaft 9.Upper rotary shaft 7 and Shaft 9 are located in pallet
The heart, moving up and down and circular motion for upper and lower rotary shaft is controlled by servo-controlled motor, to drive top tray 8 and lower tray
10 lifting and circumference rotation.Crucible 2 is placed between top tray 8 and lower tray 10, and the bottom of crucible 2 is fixed on lower tray 10
On, crucible crucible lid 3 is fixed on the lower surface of top tray 8.Crucible 2 and the split of crucible crucible lid 3, can also be fastened.After fastening
Crucible and crucible cover can integrally vertically mobile and along the circumferential direction 360 ° of rotations of level.The crucible and crucible cover of split
Can it is independent 360 ° rotation and move up and down.Crucible 2 and crucible crucible lid 3 can follow top tray 8 and lower tray 10 to lift respectively
Or circumferentially horizontally rotate.Crucible 2 is placed in induction coil 1, positioned at the center of induction coil 1.The outside of crucible 2 is coated with guarantor
Warm layer 4.Crucible 2, top tray 8, lower tray 10 and induction coil 1 and upper rotary shaft 7, Shaft 9 are coaxial, on axial direction,
Upper rotary shaft 7 and Shaft 9 are in the outside of induction coil 1, and in the radial direction, upper rotary shaft 7 and Shaft 9 are in the line of induction
Inside circle 1.Upper and lower pallet, crucible 2, the upright projection of heat-insulation layer 4 and induction coil 1 are as shown in Fig. 2 upper and lower pallet, earthenware
Crucible 2 and heat-insulation layer 4 are coaxial, positioned at induction coil upright projection center.
Crucible crucible lid 3 is bonded with seed crystal 6, and the surface of seed crystal 6 is crystal growth area, grows single-crystal silicon carbide.Raw material area 5 is located at
The inner bottom part of crucible 2.
The embodiment 1 of present invention growth crystal
Particle diameter>0.5mm carborundum powder is placed in crucible 2, is placed in the bottom of crucible 2, and seed crystal 6 is bonded in crucible pot
On lid 3.Crucible 2 is fixed in lower tray 10, and crucible pot cover 3 is fixed in top tray 8.Lifting rotation control system controls crucible
2 and crucible pot cover 3 move, the medium position in growth raw material area 5 in crucible 2 is in the central heating-up temperature of induction coil 1 most
High point.Induction coil 1 uses heating in medium frequency mode, when growing single-crystal silicon carbide using physical vapor transport, and raw material heating rises
China, crystallization forms single-crystal silicon carbide on seed crystal.In order to mitigate the influence of radial symmetry gradient, deposited when raw material gas phase is distilled
It is more uniform, in crystal growing process, pass through the upper rotary shaft 7 of regulation and Shaft 9, drive top tray 8 and lower tray
10 rotate according to same rotating speed is consistent with direction.In crystal growing process, because carborundum particle diameter is larger, raw material accumulation pine
Dissipate, distillation passage is unobstructed, consumption of raw materials ratio is very fast, and crystal growth is slow, and the general speed proportional for consuming and growing is 2:1,
With the increase of growth time, the distance of charge level and plane of crystal is increasing, and thermograde can change.Charge level and crystal
The change of surface location, residing warm area can also change, therefore in crystal growth, and crucible 2 is according to the distillation amount of raw material
Slow motion, keeps charge level to be constantly in highest warm area upwards.Crucible pot cover 3 is also moved up with slower speed simultaneously, is protected
Charge level and plane of crystal are held apart from constant, namely the length of whole gas phase zone is constant, it is ensured that while residing warm area is constant, seed crystal
Thermograde between 6 surfaces and the surface of raw material area 5 is also constant.
The embodiment 2 of present invention growth crystal
Particle diameter<0.1mm carborundum powder is placed in crucible 2, is placed in the inner bottom part of crucible 2, and seed crystal 6 is bonded in crucible
On pot cover 3, wherein crucible 2 is fixed in lower tray 10, and crucible pot cover 3 is fixed in top tray 8.Lifting rotation control system control
Crucible 2 and crucible pot cover 3 processed are moved, and the medium position in raw material area 5 in crucible 2 is in the central heating-up temperature of induction coil most
High point.Induction coil 1 uses heating in medium frequency mode, when growing single-crystal silicon carbide using physical vapor transport, and raw material heating rises
China, crystallization forms single-crystal silicon carbide on seed crystal 6.In order to mitigate the influence of radial symmetry gradient, make raw material gas phase heavy when distilling
Long-pending is more uniform, in crystal growing process, by the upper rotary shaft 7 of regulation and Shaft 9, drives top tray 8 and subiculum
Disk 10 rotates according to same rotating speed is consistent with direction.In crystal growing process, because carborundum particle diameter is smaller, raw material accumulation is caused
Close, in this case, carborundum powder is in sublimation process, and distillation passage is easily blocked, and distils slow, and element silicon is consumed
Ratio it is very fast, easily form graphitization on raw material surface, raw material face is not reduced, and crystal slowly grows, during with growth
Between increase, the distance of charge level and plane of crystal is less and less, and thermograde can change.Therefore in crystal growth, earthenware
Crucible lid 3 can move to raw material area direction with slow speed, and holding charge level and plane of crystal are apart from constant, that is, whole gas phase
The distance in area is constant, it is ensured that while residing warm area is constant, and the thermograde between seed crystal face and growth raw material area is also permanent
Fixed.
The embodiment 3 of present invention growth crystal
0.1mm<Particle diameter<0.5mm carborundum powder is placed in crucible 2, is placed in the inner bottom part of crucible 2, and seed crystal 6 is bonded
On crucible pot cover 3, wherein crucible 2 is fixed in lower tray 10, and crucible pot cover 3 is fixed in top tray 8.Lifting rotation is controlled
System controls crucible 2 and crucible pot cover 3 to move, and the medium position in raw material area 5 in crucible 2 is in induction coil center heating temperature
The peak of degree.Induction coil 1 uses heating in medium frequency mode, when growing single-crystal silicon carbide using physical vapor transport, raw material
Heating sublimation, crystallization forms single-crystal silicon carbide on seed crystal 6.In order to mitigate the influence of radial symmetry gradient, make raw material gas phase liter
What is deposited when magnificent is more uniform, in crystal growing process, by the upper rotary shaft 7 of regulation and Shaft 9, drives top tray 8
Rotated with lower tray 10 according to same rotating speed is consistent with direction.In crystal growing process, crucible 2 and crucible pot cover 3 are buckled completely
It is combined, due to carborundum moderate in grain size, in this case, carborundum powder is in sublimation process, and carborundum powder distillation makes material
The speed of face reduction is identical with the speed of crystal growth, with the increase of growth time, and charge level and plane of crystal distance do not become
Change, that is, the distance of whole gas phase zone is constant, and the height opposed coil middle position of charge level can decline, therefore in crystal life
When long, crucible 2 and crucible pot cover 3 are moved up with same speed, keep charge level to be constantly in highest warm area, seed crystal face and
Thermograde between growth raw material area is also constant.
The device of the present invention can according to concrete condition in crystal growing process, adjust charge level and crystal growth area away from
From making the length of whole gas phase zone constant, it is ensured that raw material area and crystal growth area surface temperature do not change, and maintain
Thermograde is stable, therefore, it is possible to realize the accurate control to growing silicon carbice crystals temperature and thermograde, improves carborundum
Crystal growth quality and efficiency.
Claims (5)
1. one kind is based on silicon carbide monocrystal growth device, including vacuum chamber (12), induction coil (1), crucible (2) and gas circuit system
System, it is characterised in that：Described single-crystal growing apparatus also includes lifting rotation control system；Described induction coil (1), crucible
(2), air-channel system and lifting rotation control system are respectively positioned in vacuum chamber (12)；Crucible (2) is located at lifting rotation and controls system
Between the top tray (8) and lower tray (10) of system, the middle position in induction coil (1) is placed on；Crucible (2) is coated with guarantor
Warm layer (4)；Induction coil (1) is located at vacuum chamber (12) center, to heating crucible (2)；Crucible (2) is heater,
Built with sic powder and seed crystal, for growing silicon carbice crystals；Air-channel system is connected on the wall of vacuum chamber (12) side, is used
Required atmosphere when growing silicon carbice crystals are provided.
2. according to described in claim 1 based on silicon carbide monocrystal growth device, it is characterised in that：Described lifting rotation control
System includes top tray (8), lower tray (10), upper rotary shaft (7) and Shaft (9)；Top tray (8) and lower tray (10) point
It is not fixed in rotary shaft (7) and Shaft (9)；Upper rotary shaft (7) and Shaft (9) are located at the center of pallet, lead to
Cross servo-controlled motor control upper rotary shaft, Shaft to move up and down and circular motion, to drive top tray (8) and subiculum
The lifting of disk (10) and circumference rotation.
3. according to described in claim 1 based on silicon carbide monocrystal growth device, it is characterised in that：The bottom of described crucible (2)
Portion is fixed in lower tray (10), and crucible crucible lid (3) is fixed on the lower surface of top tray (8)；Crucible (2) and crucible crucible lid (3)
Split can integrally vertically mobile and along the circumferential direction 360 ° of rotations of level, can also follow respectively top tray (8) and under
Pallet (10) is lifted or circumferentially horizontally rotated.
4. according to described in Claims 2 or 3 based on silicon carbide monocrystal growth device, it is characterised in that：Described crucible (2),
Top tray (8), lower tray (10), induction coil (1) and upper rotary shaft (7), Shaft (9) coaxially, on axial direction, upper rotation
The outside of rotating shaft (7) and Shaft (9) in induction coil (1)；In the radial direction, upper rotary shaft (7) and Shaft (9) exist
Induction coil (1) is internal；Upper and lower pallet, crucible (2) and heat-insulation layer (4) coaxially, positioned at induction coil upright projection centre bit
Put.
5. according to described in claim 1 based on silicon carbide monocrystal growth device, it is characterised in that：Crucible crucible lid (3) is bonded with
Seed crystal, seed crystal face is crystal growth area, grows single-crystal silicon carbide；Raw material area is located at the bottom in crucible (2)；In carborundum list
During crystals growth, described induction coil (1) is fixed, by control top tray (8) and lower tray (10) rotating speed and
The speed of oscilaltion movement, control follows the crucible (2) and crucible pot cover that top tray (8) and lower tray (10) are moved up and down
(3) mutual motion, makes the medium position in crucible (2) inner bottom part raw material area be in the center of induction coil (1), Ye Jijia all the time
The peak of hot temperature；By the lifting of crucible pot cover (3), the height of crucible (2) interior gas phase zone is set to remain constant, simultaneously
The thermograde on raw material area to crystal growth area surface keeps constant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710346415.8A CN107142520A (en) | 2017-05-17 | 2017-05-17 | One kind control silicon carbide monocrystal growth device |
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| CN201710346415.8A CN107142520A (en) | 2017-05-17 | 2017-05-17 | One kind control silicon carbide monocrystal growth device |
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| CN115198366A (en) * | 2022-09-14 | 2022-10-18 | 青禾晶元(天津)半导体材料有限公司 | Growth device and growth method of large-size silicon carbide crystals |
| CN115287760A (en) * | 2022-08-04 | 2022-11-04 | 顾赢速科技(合肥)有限公司 | Method and device for growing silicon carbide crystal by high-temperature chemical vapor deposition method |
| CN115369479A (en) * | 2022-07-19 | 2022-11-22 | 连城凯克斯科技有限公司 | Temperature automated inspection regulates and control equipment during carborundum production |
| CN115679449A (en) * | 2022-12-30 | 2023-02-03 | 浙江晶越半导体有限公司 | Composite crucible for growing silicon carbide crystals by sublimation method |
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