CN105568369B - A kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment - Google Patents
A kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment Download PDFInfo
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- CN105568369B CN105568369B CN201610054686.1A CN201610054686A CN105568369B CN 105568369 B CN105568369 B CN 105568369B CN 201610054686 A CN201610054686 A CN 201610054686A CN 105568369 B CN105568369 B CN 105568369B
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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
- C30B15/20—Controlling or regulating
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of lower crystal methods for method of crystal growth by crystal pulling, including step：Crucible is heated, the crystalline material being located in crucible fusing is made；Slowly move down seed crystal；When seed crystal quality changes, continues slow move down and reach lower brilliant depth；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, original heated condition is kept to crucible, 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 moves up, and descends again brilliant.The lower crystal method of the present invention avoids causing thermal shock to seed crystal by the temperature gradient of heat-insulation system during lower crystalline substance, can be by adjusting lower brilliant temperature, again lower crystalline substance operation when seeded growth occurs and overruns with seed crystal melting phenomenon.The present invention also provides a kind of automatic lower brilliant equipment, full-automatic lower crystalline substance is realized in the automatic progress of the control device control crystal growing process of the equipment, so that lower brilliant operation is detached from artificial.
Description
Technical field
The present invention relates to method of crystal growth by crystal pulling field more particularly to a kind of lower crystal methods for method of crystal growth by crystal pulling
With automatic lower brilliant equipment.
Background technology
Lower brilliant operation is that the committed step of quality is determined in crystal growing process.In the prior art, it is used for Czochralski grown
The predominantly artificial hand lower crystal type of the equipment of crystal and automatic lower brilliant function device.Lower brilliant major defect is to be easy manually
Cause the accumulation of seed crystal tip dislocation or even seed crystal cracking.And brilliant equipment is descended automatically, seed crystal completion is uniformly slowly moved down using motor
Lower brilliant operation.But although solving the problems, such as that seed temperature changes too fast in operational process, but still whether can not judge lower crystalline substance
Success.Whether lower crystalline substance succeeds and the judgement of seed crystal faint situation of change in the melt, in industry all using observation
The method of " seed crystal aperture ".The major defect of this method is exactly highly to rely on artificial experience, the observation of the lower brilliant engineer of difference
It is likely to be obtained entirely different judging result.Moreover, in lower melting-point crystal, aperture unobvious even are difficult to find, this
The foundation for judging seed crystal variation is just lost completely.
Also, it after judgement lower brilliant success, begins to enter " necking down stage ", the duration in this stage is shorter
(0.5-2 hours) are also often defined as a part for lower brilliant process.And existing operation, according to the seed crystal observed by human eye
" aperture " situation of change lifts seed crystal, or uses fixed necking method, ignores seed crystal situation of change, it is specified that a set of constant
Necking down flow.This just loses the meaning of necking operation completely, often leads to " shouldering " overlong time, or do not reach completely
Eliminate growth interface dislocation purpose.
Thus, lower brilliant operation in the prior art fully relies on artificial experience, using the method for observation " seed crystal aperture ",
It can not fundamentally solve the problems, such as how to judge lower brilliant success or failure.
Invention content
It is an object of the invention to overcome shortcoming and defect in the prior art, provide a kind of for method of crystal growth by crystal pulling
Lower crystal method.
The present invention is achieved by the following technical solutions：A kind of lower crystal method for method of crystal growth by crystal pulling, including
Following steps：
(1) crucible is heated, makes the crystalline material being located in crucible fusing；
(2) seed crystal is slowly moved down；
(3) when seed crystal quality changes, continue slow move down and reach lower brilliant depth；
(4) 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 (2) is executed, again lower crystalline substance.
Compared with the existing technology, lower crystal method of the invention is avoided lower brilliant in the process by the temperature gradient of heat-insulation system
Thermal shock is caused to seed crystal, when seeded growth occurs and overruns with seed crystal melting phenomenon can by adjusting lower brilliant temperature, again under
Crystalline substance operation；It can be according to the lower brilliant success or failure of speed judgement that seed crystal quality increaseds or decreases.
Further, the lower crystal method further includes step (5), according to the rate of seed crystal mass change, selection heating necking down
Or constant temperature necking down.
Further, 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 heating necking down.
Further, the speed for moving down seed crystal is 100~150mm/h.
Further, the lower brilliant depth is 0.5~1mm.
The present invention also provides a kind of automatic lower brilliant equipment for method of crystal growth by crystal pulling, including furnace body, crucible, seed crystal
Bar, heating device, upper weight sensor and/or lower weight sensor, control device；The crucible is set to the furnace chamber of furnace body
It is interior；The heating device is set in the furnace chamber and is heated to the crucible；The upper weight sensor is set to seed rod
The upper and/or described lower weight sensor is set to crucible bottom；The control device respectively with the seed rod, heating device,
Upper weight sensor and/or the electrical connection of lower weight sensor；The control device monitors seed crystal quality speed of increasing and decrease, and according to seed
Brilliant speed of increasing and decrease controls heating device to the heating of crucible and moving up, move down or rotating for seed rod.
Compared with the existing technology, the automatic lower brilliant equipment for method of crystal growth by crystal pulling of the invention, is filled by controlling
The automatic progress for controlling crystal growing process is set, and can judge to adjust lower brilliant temperature according to practical lower brilliant process, is realized entirely certainly
The lower brilliant process of dynamicization makes lower brilliant operation be detached from artificial, avoids artificial interference.
Further, the control device includes temperature control module, monitoring module and lifting rotation control module；The lifting rotation
Turn control module to be electrically connected with temperature control module and monitoring module respectively；The temperature control module is electrically connected with heating device, the prison
Control module is electrically connected with upper weight sensor and/or lower weight sensor respectively, the lifting rotation control module and seed rod
Electrical connection；The temperature control module measures crucible temperature and controls heating device according to the temperature that crucible measures in real time；The monitoring
Crystal weight in seed weight and/or crucible on module monitors seed rod；The lifting rotates control module according to temperature control module
Crystal weight in seed weight and/or crucible, adjusts seed crystal on the seed rod that the crucible temperature and monitoring module of acquisition obtain
Bar lifts or the speed of rotation.
Further, further include the grating scale of one and seed rod linkage setting.
Further, the control device monitors seed crystal quality speed of increasing and decrease, when seed crystal quality speed of increasing and decrease range is in threshold
In value V, original heated condition is kept to crucible；It is more than threshold value V when seed crystal quality increaseds or decreases velocity interval, is raised and lowered
Then the temperature of crucible moves up seed crystal, again lower crystalline substance.
Further, it is 100~150mm/h that the seed rod, which drives the speed that moves down of seed crystal,.
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
The step of Fig. 1 is lower crystal method of the present invention for method of crystal growth by crystal pulling is schemed.
Fig. 2 is the curve that the mass change of brilliant seed crystal lower in the process under the present invention changes over time.
Fig. 3 is the connection diagram of each module of control device of automatic lower brilliant equipment of the invention.
Specific implementation mode
The lower crystal method for method of crystal growth by crystal pulling of the present invention contains the temperature of the crucible of crystalline material by monitoring
And the state of seed crystal mass change selects lower brilliant opportunity appropriate, referring to Fig. 1, specifically including following steps：
(1) crucible is heated, makes the crystalline material being located in crucible fusing；
(2) seed crystal is slowly moved down；
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.
(3) when seed crystal quality changes, continue slow move down and reach lower brilliant depth；Specifically, when seed crystal contact is molten
When the crystalline material of change, the crystalline material of seed crystal absorption fusing, seed crystal quality increases.In the present embodiment, the lower brilliant depth
For 0.5~1mm.But lower crystalline substance depth is not limited to this.
(4) 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 (2) is executed, again lower crystalline substance.Referring to Fig. 2, it is the mass change of brilliant seed crystal lower in the process under the present invention
The curve changed over time.When seed crystal quality reduction amount or incrementss are less than the mass change in step (3), illustrate lower crystalline substance at
Work(.When quickly the amount of increaseing or decreasing is more than the mass change in step (3) to seed crystal quality, crystalline substance fails under illustrating, again lower crystalline substance.
Specifically, in step (4), when seed crystal quality range of advancing the speed is more than threshold value V, illustrates that lower brilliant temperature is relatively low, melt
The crystalline material of change is quickly in seed crystal surrounding crystalline.The temperature for increasing crucible at this time, melts the crystallization around seed crystal, then again
Carry out lower brilliant operation.Brilliant temperature drift, seed crystal rapid melting under seed crystal quality reduction speed range is more than threshold value V, is illustrated.This
When reduce the temperature of crucible, then re-start lower brilliant operation.
(5) 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 lower crystal method for method of crystal growth by crystal pulling, the present invention provides one kind being used for czochralski method crystal
The automatic lower crystalline substance equipment of growth, including furnace body, crucible, seed rod 10, heating device 20, upper weight sensor 30 and/or lower heavy
Quantity sensor 40, control device 50.The hollow formation furnace chamber of furnace interior.The crucible is set in the furnace chamber of furnace body.Institute
Heating device 20 is stated to be set in the furnace chamber and heat the crucible.The upper weight sensor 30 is set to seed rod 10
The upper and/or described lower weight sensor 40 is set to crucible bottom.The control device 50 respectively with the seed rod 10, heating
Device 20, upper weight sensor 30 and/or lower weight sensor 40 are electrically connected.The upper weight sensor 30 monitors the matter of seed crystal
Amount, for upper weighing system.The lower weight sensor 40 monitors the quality of crystal in crucible, system control device of weighing under.
The control device 50 monitors seed crystal quality speed of increasing and decrease, and controls heating device 20 to crucible according to the speed of increasing and decrease of seed crystal
Heating and seed rod 10 are moved up, move down or are rotated.It is linkedly set with grating scale on the seed rod 10.
The control device 50 includes temperature control module 51, monitoring module 52 and lifting rotation control module 53.Please refer to figure
3, it is the connection diagram of 50 modules of control device of the automatic lower brilliant equipment of the present invention.The lifting rotation control mould
Block 53 is electrically connected with temperature control module 51 and monitoring module 52 respectively.The temperature control module 51 is electrically connected with heating device 20.It is described
Monitoring module 52 is electrically connected with upper weight sensor 30 and/or lower weight sensor 40 respectively.The lifting rotates control module
53 are electrically connected with seed rod 10.The temperature control module 51 measures crucible temperature and controls heating according to the temperature that crucible measures in real time
Device 20.The monitoring module 52 monitors on seed rod 10 crystal weight in seed weight and/or crucible.The lifting rotation control
Seed weight on the seed rod 10 that the crucible temperature and monitoring module 52 that molding block 53 is obtained according to temperature control module 51 obtain
And/or crystal weight in crucible, adjust the speed of the lifting of seed rod 10 or rotation.
The automatic lower brilliant equipment of the present invention is further described with reference to the present embodiment：
According to the property of different crystal material, seed crystal appropriate is selected to move down speed, avoids lower brilliant process long or right
Seed crystal causes to damage.
It monitors whether quality changes by upper weighing system, when quality changes, illustrates that seed crystal enters liquid level.
Control seed crystal persistently moves down the lower brilliant depth of 0.5-1mm at this time, then stops moving down.
Mass change is monitored, when seed crystal quality, which increaseds or decreases velocity interval, is more than threshold value V, judges that lower brilliant temperature is relatively low
Or it is higher, temperature control module 51 controls heating device 20 and increases or decreases lower brilliant temperature, and then lifting rotation control module 53 controls
Seed crystal moves up, and restarts lower brilliant operation.It is within threshold value V when seed crystal quality increaseds or decreases velocity interval, temperature control module
The 51 lower brilliant temperature of control heating device 20 fine tuning, make seed crystal quality maintain variation steady constant or by a small margin.When seed crystal matter
After amount is stablized, 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.
Compared with the existing technology, lower crystal method of the invention is avoided lower brilliant in the process by the temperature gradient of heat-insulation system
Thermal shock is caused to seed crystal, and is added to lower brilliant mechanism for correcting errors, it can when seeded growth occurs and overruns with seed crystal melting phenomenon
By adjusting lower brilliant temperature, again lower brilliant operation.The automatic lower brilliant equipment of the present invention, realizes full-automatic lower brilliant process, under making
Crystalline substance operation is 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 (1)
1. a kind of lower crystal method for method of crystal growth by crystal pulling, it is characterised in that：Include the following steps：
(1) crucible is heated, makes the crystalline material being located in crucible fusing；
(2) seed crystal is slowly moved down；The speed for moving down seed crystal is 100~150mm/h；
(3) when seed crystal quality changes, continue slow move down and reach lower brilliant depth；The lower brilliant depth is 0.5~1mm；
(4) seed crystal quality speed of increasing and decrease is monitored, it is original to crucible holding when seed crystal quality speed of increasing and decrease range be in threshold value V
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 moves up
Seed crystal executes step (2), again lower crystalline substance；
(5) according to the rate of seed crystal mass change, selection heating necking down or constant temperature necking down；Seed crystal quality advances the speed as 0.5~-
2g/h selects constant temperature necking down；Seed crystal quality is advanced the speed more than 0.5g/h, selection heating necking down.
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| CN201610054686.1A CN105568369B (en) | 2016-01-26 | 2016-01-26 | A kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment |
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| CN201610054686.1A CN105568369B (en) | 2016-01-26 | 2016-01-26 | A kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment |
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| CN101701356A (en) * | 2009-11-17 | 2010-05-05 | 中山大学 | Lower weighing method used for equal-diameter growth of photoelectric crystal |
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