CN105648521B - A kind of growing method and equipment - Google Patents
A kind of growing method and equipment Download PDFInfo
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- CN105648521B CN105648521B CN201610056010.6A CN201610056010A CN105648521B CN 105648521 B CN105648521 B CN 105648521B CN 201610056010 A CN201610056010 A CN 201610056010A CN 105648521 B CN105648521 B CN 105648521B
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- temperature
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- seed crystal
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/08—Downward pulling
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/203—Controlling or regulating the relationship of pull rate (v) to axial thermal gradient (G)
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/30—Mechanisms for rotating or moving either the melt or the crystal
Abstract
The invention discloses a kind of growing methods, including S1：The lower brilliant temperature of capture；S2：Crucible temperature is set to reach lower crystalline substance temperature in step S1；S3：Lower brilliant operation is carried out according to crucible temperature and seed crystal mass change；Specifically, being heated to the crucible for holding crystalline material, make it with certain heating rate constant heating rates sintering to target temperature；Crucible temperature in acquisition temperature-rise period, which changes over time, is formed by curve, and the corresponding temperature of point for choosing maximum slope in curve is lower brilliant temperature；Crucible temperature is set to reach lower brilliant temperature；Slowly move down seed crystal；When seed crystal quality changes, continues slow move down and reach lower brilliant depth；Crucible temperature is finely tuned according to seed crystal mass change.The growing method of the present invention changes over time curve acquisition crystal accurately lower brilliant temperature using temperature in temperature-rise period；And it avoids causing thermal shock to seed crystal by the temperature gradient of heat-insulation system during lower crystalline substance, adjusts suitable temperature at any time according to seed crystal mass change.
Description
Technical field
The present invention relates to field of crystal growth more particularly to a kind of growing method and equipment.
Background technology
Lower brilliant operation is that the committed step of crystal quality is determined in crystal growing process.And wherein, the selection of lower crystalline substance temperature
It is a most important step during method of crystal growth by crystal pulling.Lower crystalline substance temperature is excessively high, can directly result in growth interface by compared with heat-flash
The problem of impact, necking down overlong time or even seed crystal directly fusing etc. seriously affect crystal production.On the other hand, lower brilliant temperature
It is too low, rapid crystallization at crystal growth interface can be led to, while generating a large amount of dislocations.This must just melt the part grown, carry
Relative superiority or inferiority crystalline substance temperature, regrow crystal.Therefore, accurate lower brilliant temperature is the guarantee of crystal smooth growth.
In the prior art, " brilliant temperature under judging " this key technology still fully relies on artificial experience.Although crystal is given birth to
The degree of automation of long equipment has reached higher level, or even there are so-called " automatic lower crystalline substance " designs, but is all based on artificial
It is operated on the basis of pre-set lower brilliant temperature.And the automatic decision of lower brilliant temperature this key problem, still without
To solution.
In general, during method of crystal growth by crystal pulling, lower crystalline substance temperature can be adjusted to the fusion temperature of slightly above crystal.According to crystalline substance
Volume property is different, adjustment amplitude slightly difference.It is determined by crystalline material property, each crystal all has specific fusing point.
Therefore, theoretically, the lower brilliant temperature that crystal is suitble to also should be a smaller temperature range.But actually growing crystal
In the process, there is also very big differences for the lower brilliant temperature of crystal even of the same race.Only by taking lithium columbate crystal as an example, even if same heat preservation
System building personnel execute in strict accordance with operation standard, and artificial caused inevitable difference may still make the lower crystalline substance of crystal
Nearly 100 DEG C of temperature difference.This phenomenon is mainly caused by the fine difference of heat-insulation system.Therefore, the lower brilliant temperature of crystal growth
It is different.The problem of due to heat-insulation system difference, can not avoid completely, the judgement of following brilliant temperature extremely difficult break away from manual intervention.
Under setting after brilliant temperature, start lower brilliant operation.Mainly there is artificial hand lower brilliant equipment and automatic in the prior art
Lower crystalline substance function device.Lower brilliant major defect is to be easy to cause the dislocation accumulation of seed crystal tip or even seed crystal cracking manually.And from
Dynamic lower brilliant equipment is uniformly slowly moved down seed crystal using motor and completes lower brilliant operation.But although solves seed crystal in operational process
The too fast problem of temperature change, but still can not judge whether lower crystalline substance succeeds.Whether lower crystalline substance succeeds and seed crystal is faint in the melt
Situation of change judgement, in industry all using observation " seed crystal aperture " method.The major defect of this method is exactly,
Height relies on artificial experience, the observation of the lower brilliant engineer of difference to be likely to be obtained entirely different judging result.Moreover, fusing point compared with
In low crystal, aperture unobvious even are difficult to find, this just loses the foundation for judging seed crystal variation completely.
In addition, entire crystal growing process, due to the particularity of environment of crystal growth, system long-term work is in high temperature, height
In pressure, strong-electromagnetic field environment.Conventional intervention monitoring means, such as mechanical arm, air-flow feedback, the devices such as radio frequency signal without
Method runs well in environment of crystal growth.Moreover, usually crystal growth temperature is very high (1000 DEG C or more), necessary heat preservation
System is also at higher temperature.It therefore, just completely can not be to being sealed in furnace chamber once crystal growth system starts normal operation
Insulation cover make any adjustment.Particularly with the large-size crystals of growth cycle length, single crystal growth cycles nearly 1,000 are small
When.Even if period finds if temperature gradient is not suitable for without any adjustment means.Therefore, under working condition, in furnace chamber in real time
Adjustment thermal field is of great significance to crystal growth.
Invention content
It is an object of the invention to overcome shortcoming and defect in the prior art, provide brilliant temperature under a kind of accurate judgement,
Adjust the growing method of temperature in real time according to seed crystal mass change speed.
The present invention is achieved by the following technical solutions：A kind of growing method, includes the following steps：
S1：The lower brilliant temperature of capture；
S2：Crucible temperature is set to reach the lower brilliant temperature described in step S1；
S3：Lower brilliant operation is carried out according to crucible temperature and seed crystal mass change；
Wherein, step S1 includes the following steps：
S11：Crucible to holding crystalline material heats, and makes it with certain heating rate constant heating rates sintering to target temperature
Degree, the target temperature are higher than the fusing point of crystalline material；
S12：Crucible temperature in acquisition temperature-rise period, which changes over time, is formed by curve, chooses maximum slope in curve
The corresponding temperature of point be lower brilliant temperature；
Step S3 includes the following steps：
S31：Slowly move down seed crystal；
S32：When seed crystal quality changes, continues slow move down and reach lower brilliant depth；
S33：Seed crystal quality speed of increasing and decrease is monitored, when seed crystal quality speed of increasing and decrease range be in threshold value V, to crucible holding
Original heated condition；It is more than threshold value V when seed crystal quality increaseds or decreases velocity interval, the temperature of crucible is raised and lowered, then
Seed crystal is moved up, step S31 is executed, again lower crystalline substance.
Compared with the existing technology, growing method of the invention only passes through simple warming temperature, you can utilizes heating
Temperature changes over time curve acquisition crystal accurately lower brilliant temperature in the process；In lower brilliant operating process, avoid in lower brilliant process
Temperature gradient in middle furnace shell causes thermal shock to seed crystal, adjusts crucible temperature at any time according to seed crystal mass change, and add
Lower brilliant mechanism for correcting errors, can be by adjusting lower brilliant temperature when seeded growth occurs and overruns with seed crystal melting phenomenon, lower crystalline substance again
Operation.
Further, step S1 further includes step S13, and when crucible temperature reaches target temperature, crucible is constant at target temperature
Degree makes crystalline material bath component be uniformly mixed.
Further, step S3 further includes step S34, according to the rate of seed crystal mass change, selection heating necking down or constant temperature
Necking down.
Further, in step S34, when seed crystal quality is advanced the speed as 0.5~-2g/h, selection constant temperature necking down；When seed crystal matter
Amount is advanced the speed more than 0.5g/h, selection heating necking down.
Further, the heating rate in the step S11 is 3-7 DEG C/min.
Further, the speed that seed crystal is moved down in the step S31 is 100~150mm/h.
Further, the lower brilliant depth in the step S32 is 0.5~1mm.
The present invention also provides a kind of crystal growth equipments, including furnace shell, attemperator, crucible, seed rod, heating dress
It sets, upper weight sensor and/or lower weight sensor, control device；The furnace shell is hollow housing, the attemperator setting
In in furnace shell, the heating device and crucible are set in attemperator, and the heating device heats the crucible, the control
Device processed is electrically connected with the seed rod, heating device, upper weight sensor and/or lower weight sensor respectively；The control
Device obtains the heated in real-time temperature of heating device, and draws the temperature curve that temperature changes over time, and chooses in temperature curve
The corresponding temperature of point of maximum slope is lower brilliant temperature；And the control device detection seed crystal quality speed of increasing and decrease, and according to
The speed of increasing and decrease of seed crystal controls heating device to the heating of crucible and moving up, move down or rotating for seed rod.
Compared with the existing technology, crystal growth equipment of the invention changes over time choosing by the utilization temperature of control device
Take crystal accurately lower brilliant temperature, exclude influence of the artificial experience to lower brilliant operation, solve influenced by thermal field, thermocouple temperature measurement
Lower crystalline substance temperature judges inaccurate problem caused by the problems such as difference, can be with the lower brilliant temperature of accurate judgement novel crystal.And
And lower brilliant equipment of the invention, it realizes full-automatic lower brilliant process, lower brilliant operation is made to be detached from manual operation.
Further, the control device includes temperature control module, temperature curve drafting module, lower brilliant temperature selection module, prison
Control module and lifting rotation control module；The temperature control module chooses module and lifting rotation control module with lower brilliant temperature respectively
Electrical connection；The temperature curve drafting module is chosen module with lower brilliant temperature and is electrically connected, the monitoring module and lifting rotation control
Molding block is electrically connected；The temperature control module and the difference heating device electrical connection of temperature curve drafting module, the lifting rotation control
Molding block is electrically connected with seed rod, and the monitoring module is electrically connected with upper weight sensor and/or lower weight sensor respectively；Institute
Temperature control module is stated to measure crucible temperature in real time and control heating device according to the temperature that crucible measures；The temperature curve draws mould
The real time temperature that root tuber is obtained according to temperature control module draws heating device temperature and changes over time curve；The lower brilliant temperature chooses mould
Root tuber changes over time curve according to the temperature that temperature curve drafting module obtains, and it is corresponding to choose maximum slope point in change curve
Temperature is lower brilliant temperature；Crystal weight in seed weight and/or crucible on monitoring module monitoring seed rod；The lifting rotation
Turn on the crucible temperature that control module is obtained according to temperature control module and the seed rod that monitoring module obtains seed weight and/or
Crystal weight in crucible adjusts the speed of seed rod lifting or rotation.
Further, the equipment further includes a controlling convection, and the controlling convection includes convection control device, wind
Machine, gas distribution channel and pressure regulator；Convection control device center is engraved structure, is provided with convection control device axis centre
Symmetrical first air inlet and the second air inlet；The wind turbine by gas distribution channel respectively with the first air inlet and the second air inlet
Connection；The pressure regulator is electrically connected with wind turbine；The convection control device of the controlling convection is set to the heat preservation inside furnace shell
The top of device, the seed rod are each passed through the top of convection control device and attemperator.The controlling convection can
Free convection in the attemperator of adjusting device, and then adjust the thermal field in attemperator.It can be real in crystal growing process
When adjust thermal field, optimum environment of crystal growth is provided.
In order to better understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Description of the drawings
Fig. 1 is the step flow chart of growing method of the present invention.
Fig. 2 is the curve that temperature-rise period temperature and power change over time in step S1 of the present invention.
Fig. 3 is the curve that the mass change of seed crystal in step S3 of the present invention changes over time.
Fig. 4 is the structural schematic diagram of crystal growth equipment of the present invention.
Fig. 5 is the structure top view of crystal growth equipment of the present invention.
Fig. 6 is the main view sectional view of the convection control device of crystal growth equipment of the present invention.
Fig. 7 is the vertical view of the convection control device of crystal growth equipment of the present invention.
Fig. 8 is the connection diagram of each module of control device of crystal growth equipment of the present invention.
Specific implementation mode
The lower brilliant temperature of crystal growth is higher than the fusing point of crystalline material, but due to thermal field difference, each crystal growth experiment
Result it is inconsistent.But applicant it is discovered by experiment that the solid-liquid phase-change process of crystalline material temperature variation curve extremely one
It causes.And the state of temperature and seed crystal mass change that the crucible of crystalline material can be contained by monitoring is appropriate to select
Lower crystalline substance opportunity.Based on this, applicant proposed a kind of growing methods.
The growing method of the present invention, referring to Fig. 1, including the following steps：
S1：The lower brilliant temperature of capture；
S2：Crucible temperature is set to reach the lower brilliant temperature described in step S1；
S3：Lower brilliant operation is carried out according to crucible temperature and seed crystal mass change.
The step S1 of the lower brilliant temperature of capture includes the following steps：
S11：Crucible to holding crystalline material heats, and makes it with certain heating rate constant heating rates sintering to target temperature
Degree, the target temperature are higher than the fusing point of crystalline material.
Specifically, target temperature is selected primarily based upon crystalline material fusing point.Target temperature is higher than the fusing point of crystalline material.
For new material, usual target temperature can be set above 20 DEG C of fusing point.The objectives temperature of traditional material can be according to ripe
It is selected to practice technique.The main root of fusing point of material it is documented that process experiences it is selected.For example, pure congruent lithium niobate material
The fusing point of material is 1240 DEG C, and according to process experiences, setting target temperature is the fusing point of the material.And for doped lithium columbate
Crystal, since accurate fusing point is unknown, usually setting is target temperature higher than 20 DEG C of fusing point is prejudged.Heating rate is needed according to difference
The property of crystalline material is selected, and 3-7 DEG C/min is usually arranged as.When heating rate is excessively high, by heating power supply power institute
Limit, is not readily accomplished heating, and " overshoot " effect of temperature control is apparent；When heating rate is too low, temperature curve at solid-liquid phase change
Change unobvious.Therefore the main principle of selection heating rate is the temperature curve made in temperature-rise period corresponding to solid-liquid phase change
It maximizes, it will be apparent that curve can improve the accuracy chosen to lower brilliant temperature, while cannot be because of under " overshoot " phenomena impair
The selection of brilliant temperature.Record the temperature T of crucible in real time in temperature-rise period, and the variation for drawing crucible temperature T t at any time is bent
Line.In the present embodiment, the heating power that crucible is heated in detection changes with time, to control crucible heating rate.
S12：Crucible temperature in drafting temperature-rise period, which changes over time, is formed by curve, chooses maximum slope in curve
The corresponding temperature of point be lower brilliant temperature.
S13：When crucible temperature reaches target temperature, crucible is constant at target temperature, keeps crystalline material bath component mixed
It closes uniform.In the present embodiment, when crucible temperature reaches target temperature, crucible is made to be constant at target temperature 1 hour.
Specifically, referring to Fig. 2, it is the song that temperature and power change over time in step S1 temperature-rise periods of the present invention
Line.Due to crucible constant heating rates sintering to target temperature, when crystalline substance material is initially located in solid-liquid, crystal melting process can absorb largely
Heat.In order to maintain constant heating rate, heating power to be significantly increased, even if reach rated power be also unable to maintain that it is original
Heating rate.Thus, when polycrystal material starts fusing in solid-liquid state, the crucible temperature slope that changes with time is apparent
Reduce, heating rate reduces, but heating power numerical value is very high (being close to or up to rated power).When crystal is completely melt,
Solid-liquid phase change terminates, melt just no longer a large amount of heat absorptions of crystalline material, but heating power will not adjust back rapidly previous level.
Excessively high power can cause crucible temperature drastically to increase, and temperature is far above target temperature and heating rate sharply increases.It is rising
Acquisition crucible temperature, which changes over time, during temperature is formed by curve, and the point that wherein temperature starts to surge is that brilliant material is completely melt
Temperature spot, and the corresponding temperature of point for choosing maximum slope in curve is lower brilliant temperature.In the present embodiment, the heating speed
Rate is 3-7 DEG C/min.
After capture lower brilliant temperature, the operation of step S2 is carried out, so that crucible temperature is reduced to lower brilliant temperature, and be constant at down
Brilliant temperature, the lower brilliant operation of pending step S3.
The step S3 that lower brilliant operation is carried out according to crucible temperature and seed crystal mass change, includes the following steps：
S31：Slowly move down seed crystal.
Specifically, the speed for moving down seed crystal selects as needed.When move down seed crystal it is excessively slow when can influence working efficiency；And work as
Move down seed crystal it is too fast then can to seed crystal generate thermal shock, seed crystal is caused to damage.In the present embodiment, the speed for moving down seed crystal
Degree is 100~150mm/h.But seed crystal to move down speed not limited to this.
S32：When seed crystal quality changes, continues slow move down and reach lower brilliant depth.
Specifically, when the crystalline material of seed crystal contact melting, the crystalline material of seed crystal absorption fusing, seed crystal quality increases
Add.In the present embodiment, the lower brilliant depth is 0.5~1mm.But lower crystalline substance depth is not limited to this.
S33：Seed crystal quality speed of increasing and decrease is monitored, when seed crystal quality speed of increasing and decrease range be in threshold value V, to crucible holding
Original heated condition；It is more than threshold value V when seed crystal quality increaseds or decreases velocity interval, the temperature of crucible is raised and lowered, then
Seed crystal is moved up, step S31 is executed, again lower crystalline substance.
Referring to Fig. 3, it is the curve that the mass change of seed crystal in step S3 of the present invention changes over time.When seed crystal quality
When reduction amount or incrementss are less than the mass change in step S32, illustrate lower brilliant success.When seed crystal quality quickly increaseds or decreases
Amount is more than the mass change in step S32, illustrates lower brilliant failure, again lower crystalline substance.Specifically, in step S33, when seed crystal quality increases
Rate of acceleration range is more than threshold value V, illustrates that lower brilliant temperature is relatively low, the crystalline material of fusing is quickly in seed crystal surrounding crystalline.It rises at this time
The temperature of high crucible melts the crystallization around seed crystal, then re-starts lower brilliant operation.When seed crystal quality reduction speed range is super
Threshold value V is crossed, illustrates lower brilliant temperature drift, seed crystal rapid melting.Then the temperature for reducing crucible at this time re-starts lower brilliant behaviour
Make.
S34：According to the rate of seed crystal mass change, selection heating necking down or constant temperature necking down.Specifically, when seed crystal quality increases
When deceleration range is in threshold value V, illustrate lower brilliant success, at this time according to the rate of seed crystal mass change, selection heating necking down
Or constant temperature necking down, that is, accelerate to move up the rate of seed crystal, and rotate seed crystal simultaneously, to eliminate prolonging for original dislocation in seed crystal as possible
It stretches.After seed weight is stablized, there are three types of the mass changes of seed crystal：Gently, slowly reduce or be slowly increased.Necking operation can be with
Reduce it is lower brilliant during in seed crystal face as caused by thermal shock dislocation.Compared to the fixation necking down set pattern generally used, this hair
It is bright to select suitable necking down mode according to the quality change situation during lower crystalline substance.Necking operation can be classified as slowly
Seed crystal fusion process, by while lifting seed crystal heat up or constant temperature make the contact surface of seed crystal and melt reduce.Specifically,
When seed crystal quality is advanced the speed as 0.5~-2g/h, selection constant temperature necking down.When seed crystal quality is advanced the speed more than 0.5g/h, selection
Heat up necking down.Specific heating rate and rate of mass change existence function relationship.
Based on above growing method, the present invention provides a kind of crystal growth equipments.Fig. 4 and Fig. 5 please be participate in,
It is the structural schematic diagram and vertical view of the crystal growth equipment respectively.The crystal growth equipment includes furnace shell 10, heat preservation dress
Set 20, crucible, seed rod 30, heating device 40, upper weight sensor 50 and/or lower weight sensor 60,70 and of control device
Controlling convection 80.The furnace shell 10 is hollow housing.The attemperator 20 is set in furnace shell 10.The crucible setting
In in attemperator 20.The heating device 40 is set in attemperator 20 and is heated to the crucible.The seed rod 30
For lifting and rotating crystal, the top of attemperator 20 is passed through, is moved up and down in attemperator 20, and its lower end can
Contact the crystalline material in crucible.The upper weight sensor 50 is set on seed rod 30 and/or the lower weight sensor
60 are set to crucible bottom.In the present embodiment, the seed rod 30 is set on the axis of attemperator 20.It is described to flow control
Device 80 processed is set to the top of attemperator 20.The attemperator 20 includes furnace body and the heat preservation for being set to furnace interior
Cover.A cavity is formed between the furnace body and insulation cover.
The controlling convection 80 includes convection control device 81, wind turbine 82, gas distribution channel 83, pressure regulator 84, gas mistake
Filter unit and semiconductor chilling plate.The convection control device 81 is set to the top of the insulation cover inside furnace shell 10.The convection current
The bottom surface of controller 81 is bonded with the top planes of the insulation cover, and convection control device 81 and the axis of both insulation covers are mutual
It overlaps.The wind turbine 82 is set in furnace shell 10, and is connect with convection control device 81 by gas distribution channel 83.The pressure regulator 84
It is set to outside furnace shell 10.The pressure regulator 84 is real by the vacuum aircraft plug 11 being set on furnace shell 10 with the wind turbine 82
It is now electrically connected, the input voltage by controlling pressure regulator 84 controls the power of 82 outlet air of wind turbine.The filtering unit setting
In the air inlet of wind turbine 82, and then purify the gas by wind turbine 82.The semiconductor chilling plate is set to the air inlet of wind turbine 82
Mouthful, the cooling effect of convection control device 81 can be enhanced.In the present embodiment, the seed rod 30 passes through 81 He of convection control device
The top of attemperator 20.
It is the main view sectional view and vertical view of the convection control device respectively please refer to Fig. 6 and Fig. 7.It is described right
81 center of stream controller is engraved structure, and there are two air inlets, respectively the first air inlet 812 and the second air inlet for setting
814.First air inlet, 812 and second air inlet 814 is symmetrical with the axis centre of convection control device 81.The convection control
Device 81 is made of refractory material.In the present embodiment, the convection control device 81 is made of zirconia material.
The wind turbine 82 by the gas distribution channel 83 respectively with the first air inlet 812 and second of convection control device 81 into
Gas port 814 connects.The gas distribution channel 83 is flexible refractory material.In the present embodiment, the gas distribution channel 83 is silicone tube.
The control device 70 respectively with the seed rod 30, heating device 40, upper weight sensor 50 and/or lower weight
Sensor 60 is electrically connected.The upper weight sensor 50 monitors the quality of seed crystal, for upper weighing system.The lower weight sensor
The quality of crystal, system control device of weighing under in 60 monitoring crucibles.The control device 70 obtains the reality of heating device 40
Shi Wendu, and the temperature curve that temperature changes over time is drawn, the corresponding temperature of point for choosing maximum slope in curve is lower crystalline substance
Temperature；The control device 70 monitors seed crystal quality speed of increasing and decrease, and right according to the speed of increasing and decrease of seed crystal control heating device 40
The heating of crucible and moving up, move down or rotating for seed rod 30.It is linkedly set with grating scale on the seed rod 30.
The control device 70 includes temperature control module 71, temperature curve drafting module 72, lower brilliant temperature selection module 73, work(
Rate monitoring modular 74, monitoring module 75, lifting rotation control module 76.Referring to Fig. 8, it is that the control device 70 of the present invention is each
The connection diagram of a module.The temperature control module 71 chooses module 73, power monitoring module 74, lifting with lower brilliant temperature respectively
Control module 76 is rotated to be electrically connected.The temperature curve drafting module 72 is chosen module 73 with lower brilliant temperature and is electrically connected.The prison
Control module 75 is electrically connected with lifting rotation control module 76.The temperature control module 71, temperature curve drafting module 72, power monitoring
Module 74 is electrically connected with heating device 40 respectively.The lifting rotation control module 76 is electrically connected with seed rod 30.The monitoring
Module 75 is electrically connected with upper weight sensor 50 and/or lower weight sensor 60 respectively.Under capture when brilliant temperature, the temperature control
Module 71 obtains 40 real-time temperature of heating device and controls the heating device 40 according to the Current Temperatures with certain heating speed
Rate constant heating rates sintering is to target temperature.The temperature curve drafting module 72 is drawn according to the real time temperature that temperature control module 71 obtains to be added
40 temperature of thermal changes over time curve.The lower brilliant temperature chooses what module 73 was obtained according to temperature curve drafting module 72
Real time temperature drafting 40 temperature of heating device changes over time the corresponding temperature of maximum slope point in curve selection change curve
Lower crystalline substance temperature.The power monitoring module 74 monitors 40 heating power P of heating device according to crucible temperature in real time, so as to better
Crucible is controlled with certain heating rate constant heating rates sintering to target temperature.After capture lower brilliant temperature, lower crystalline substance temperature chooses module
The lower brilliant temperature of selection is sent to temperature control module 71 by 73, and temperature control module 71 controls 40 temperature of heating device and reaches lower brilliant temperature,
Start lower brilliant operation.In lower crystalline substance operating process, the temperature control module 71 measures crucible temperature and in real time according to the temperature of crucible measurement
Degree control heating device 40.The monitoring module 75 monitors on seed rod 30 crystal weight in seed weight and/or crucible.It is described
On the seed rod 30 that the crucible temperature and monitoring module 75 that lifting rotation control module 76 is obtained according to temperature control module 71 obtain
Crystal weight in seed weight and/or crucible adjusts the speed of the lifting of seed rod 30 or rotation.
Equipment of the present invention is further described with reference to the present embodiment：
Root it is documented that or process experiences determine the fusing point of crystalline material.Target temperature is set above 20 DEG C of fusing point
Or suitable target temperature is selected according to technique.Temperature control module 71 controls heating device 40 and is warming up to target temperature.
Suitable heating rate is then selected according to the property of crystalline material, to meet the temperature made corresponding to solid-liquid phase change
Curve maximizes, and the principle of the handling result of lower brilliant temperature cannot be captured because of " overshoot " phenomena impair.It is selected suitable
After heating rate, temperature control module 71 controls heating device 40 with selected heating rate, makes crucible constant speed liter residing for crystalline material
Temperature.When real time temperature reaches the fusing point of crystalline material, crystalline material starts to melt.
When the real time temperature T of crucible reaches the target temperature of setting, temperature control module 71, which controls heating device 40, to be stopped rising
Temperature, and it is constant at target temperature for a period of time, so that the bath component of crystalline material is uniformly mixed.
The temperature curve drafting module 72 draws 40 temperature of heating device according to the real time temperature that temperature control module 71 obtains
Curve is changed over time, the lower brilliant temperature chooses module 73 and changes over time slope in curve selection change curve according to temperature
The corresponding temperature of maximum point is lower brilliant temperature.
Then, lower brilliant temperature chooses module 73 and the lower brilliant temperature of selection is sent to temperature control module 71, and temperature control module 71 is controlled
40 temperature of refrigerating/heating apparatus reaches lower brilliant temperature, starts lower brilliant operation.
Lifting rotation control module 76 controls seed crystal and moves down.According to the property of different crystal material, seed crystal appropriate is selected
Speed is moved down, avoid lower brilliant process long or seed crystal is caused to damage.
It monitors whether quality changes by upper weighing system, when quality changes, illustrates that seed crystal enters liquid level.
The control module 76 of lifting rotation at this time controls the lower brilliant depth that seed crystal persistently moves down 0.5-1mm, then stops moving down.
Monitoring module 75 monitors mass change, when seed crystal quality, which increaseds or decreases velocity interval, is more than threshold value V, under judgement
Brilliant temperature is relatively low or higher, and temperature control module 71 controls heating device 40 and increases or decreases lower brilliant temperature, then lifting rotation control
Module 76 controls seed crystal and moves up, and restarts lower brilliant operation.When seed crystal quality increased or decrease velocity interval be in threshold value V it
Interior, temperature control module 71 controls the lower brilliant temperature of the fine tuning of heating device 40, and seed crystal quality is made to maintain change steady constant or by a small margin
Change.After seed crystal stable quality, steady temperature.Finally, the rate increasedd or decreased according to seed crystal judges and selects heating necking down
Or constant temperature necking down.
Since the quality of melt in seed crystal quality and crucible is shifting relationship, thus carried out by lower weighing system
The step of operation with mentioned by upper weighing system can reach same control effect.
Instantly in brilliant operating process, when stove body temperature is not suitable for, start wind turbine 82, and wind turbine is adjusted by pressure regulator 84
82 input voltage adjusts the current rate of the wind screen formed inside convection control device 81, up in the furnace body for reaching suitable
Temperature.Then normal crystal growth operations are carried out.In crystal growing process, since thermal insulation material deformation or monocrystalline are constantly long
Go out, the thermal field in attemperator 20 can be caused to change, thermal field can be adjusted by finely tuning the input voltage of wind turbine 82.
In addition, in the existing crystal growth equipment course of work, often there is the damage of insulation cover, lead to attemperator
Convection current inside and outside 20 changes, and adjusts the wind screen power in convection control device 81 by controlling convection 80 at this time, in turn
The thermal field inside attemperator 20 is adjusted, to maintain the original growing environment of crystal.
Compared with the existing technology, growing method of the invention only passes through simple warming temperature, you can utilizes heating
Temperature changes over time curve acquisition crystal accurately lower brilliant temperature in the process；In lower brilliant operating process, avoid in lower brilliant process
Temperature gradient in middle furnace shell causes thermal shock to seed crystal, adjusts crucible temperature at any time according to seed crystal mass change, and add
Lower brilliant mechanism for correcting errors, can be by adjusting lower brilliant temperature when seeded growth occurs and overruns with seed crystal melting phenomenon, lower crystalline substance again
Operation.The crystal growth equipment of the present invention chooses module by the lower brilliant temperature of control device and changes over time selection using temperature
The accurate lower brilliant temperature of crystal, excludes influence of the artificial experience to lower brilliant operation, solve influenced by thermal field, thermocouple temperature measurement it is poor
Lower crystalline substance temperature judges inaccurate problem caused by the problems such as different, can be with the lower brilliant temperature of accurate judgement novel crystal.Also,
The lower brilliant equipment of the present invention realizes full-automatic lower brilliant process, lower brilliant operation is made to be detached from manual operation.
The invention is not limited in the above embodiments, if the various changes or deformation to the present invention do not depart from the present invention
Spirit and scope, if these changes and deformation belong within the scope of the claim and equivalent technologies of the present invention, then this hair
It is bright to be also intended to comprising these changes and deformation.
Claims (2)
1. a kind of crystal growth equipment, it is characterised in that：Including furnace shell, attemperator, crucible, seed rod, heating device, upper heavy
Quantity sensor and/or lower weight sensor, control device；The furnace shell is hollow housing, and the attemperator is set to furnace shell
Interior, the heating device and crucible are set in attemperator, and the heating device heats the crucible, the control device
It is electrically connected respectively with the seed rod, heating device, upper weight sensor and/or lower weight sensor；The control device obtains
Heating device heated in real-time temperature, and draw the temperature curve that temperature changes over time, choose in temperature curve slope most
The big corresponding temperature of point is lower brilliant temperature；And the control device detects seed crystal quality speed of increasing and decrease, and according to seed crystal
Speed of increasing and decrease controls heating device to the heating of crucible and moving up, move down or rotating for seed rod；The crystal growth equipment
Further include a controlling convection, the controlling convection includes convection control device, wind turbine, gas distribution channel and pressure regulator；Institute
It is engraved structure to state convection control device center, is provided with symmetrical first air inlet of convection control device axis centre and second
Air inlet；The wind turbine is connect with the first air inlet and the second air inlet respectively by gas distribution channel；The pressure regulator and wind turbine
Electrical connection；The convection control device of the controlling convection is set to the top of the attemperator inside furnace shell, the seed rod
It is each passed through the top of convection control device and attemperator.
2. crystal growth equipment according to claim 1, it is characterised in that：The control device includes temperature control module, temperature
Line drafting module, the lower brilliant temperature of writing music choose module, monitoring module and lifting rotation control module；The temperature control module respectively with
Lower crystalline substance temperature chooses module and lifting rotation control module electrical connection, and the temperature curve drafting module chooses mould with lower brilliant temperature
Block is electrically connected, and the monitoring module is electrically connected with lifting rotation control module；The temperature control module and temperature curve drafting module
Heating device electrical connection respectively, the lifting rotate control module and are electrically connected with seed rod, the monitoring module respectively with it is upper heavy
Quantity sensor and/or the electrical connection of lower weight sensor；The temperature control module measures crucible temperature and is measured according to crucible in real time
Temperature controls heating device；The temperature curve drafting module draws heating device temperature according to the real time temperature that temperature control module obtains
Degree changes over time curve；The lower brilliant temperature is chosen module and is changed over time according to the temperature that temperature curve drafting module obtains
Curve, it is lower brilliant temperature to choose the corresponding temperature of maximum slope point in change curve；Seed on the monitoring module monitoring seed rod
Crystal weight in brilliant weight and/or crucible；Crucible temperature that the lifting rotation control module is obtained according to temperature control module and
Crystal weight in seed weight and/or crucible on the seed rod that monitoring module obtains, adjusts the speed of seed rod lifting or rotation.
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| CN109576780A (en) * | 2018-12-28 | 2019-04-05 | 宁夏隆基硅材料有限公司 | A kind of seed crystal welding process and equipment |
| CN114775057B (en) * | 2022-06-23 | 2022-09-23 | 天通控股股份有限公司 | Method for growing 6-inch lithium tantalate crystal |
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