CN108315812A - A kind of method of kyropoulos growing sapphire crystal - Google Patents
A kind of method of kyropoulos growing sapphire crystal Download PDFInfo
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- CN108315812A CN108315812A CN201810442373.2A CN201810442373A CN108315812A CN 108315812 A CN108315812 A CN 108315812A CN 201810442373 A CN201810442373 A CN 201810442373A CN 108315812 A CN108315812 A CN 108315812A
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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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- 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
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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Abstract
The application provides a kind of method of kyropoulos growing sapphire crystal, including feeds, heat material, seeding, expand shoulder growth, isodiametric growth, ending growth, carry the de- and cooling down stage.In expanding shoulder growth course, expanding shoulder length speed is no more than crystal weight 5%~10%, pulling rate is 0.1~1mm/h, when crystal weight is 500g~1000g, instantaneous lifting 2mm upwards, when crystal weight is 1200g~1800g, instantaneous lifting 2mm upwards.In ending growth phase, after crystal weight reaches the 70%~80% of target weight, when crystal weight curve becomes wave, after continued growth H hours, enters back into and carry the de- stage.It uses the expansion shoulder growth technique instantaneously lifted and ending growth technique that bottom does not lift, effectively alleviates the formation and increase of crystal shoulder taper and bottom steamed bun shape bubble, be suitable for large-size sapphire and grow, improve sapphire crystal growth quality.In addition the expansion shoulder technique instantaneously lifted contributes to the round growth of crystal, while having cut off plane of crystal crystal boundary line, is conducive to improve crystal quality.
Description
Technical field
The present invention relates to technical field of crystal growth more particularly to a kind of methods of kyropoulos growing sapphire crystal.
Background technology
Sapphire has that fusing point high (2045 DEG C), heat conduction is good, hardness is high, electrical insulating property is good, strong alkali-acid resistance burn into light transmission
The features such as wide waveband, is widely used in the civil equipments such as mobile phone screen, minute surface, and is applied to guided missile dome, goes straight up to arbor
Equal military enterprises.There are many methods for sapphire crystal growth, and the method generally to use in the industry is mainly kyropoulos at present, such
Method growth crystal defect is few, dislocation density is low, become the mainstream growing method of sapphire crystal industry.
Common kyropoulos with A to based on long crystalline substance, technique include mainly charging, heat temperature raising, constant temperature material, seeding,
The growth of expansion shoulder, isodiametric growth, ending carry the stages such as de-, cooling down.Such as a kind of common 85kg sapphire preparation methods, carry out
Charging heats material and after the seeding stage, isodiametric growth stage, isodiametric growth pulling rate is transferred to after crystal weight reaches 8kg
For 0.1~0.5mm/h.When display weight of weighing is more than 90kg, into the lifting stage of finishing up, by the pulling rate of seed rod from 0.3
~0.5mm/h is improved to 2~5mm/h, until crystal weight signal steadily maintains 85kg, can determine whether that crystal growth terminates at this time
And it is detached from crucible.Heating power is slowly reduced, crystal is made annealing treatment, cooling terminates and after natural cooling, you can blow-on
Take out crystal.
As military-civil equipment increases sharply to sapphire material demand, size and weight to sapphire crystal just by
The increase in year, crystal weight is to incrementally increase to current 100kg or more.And it is blue precious to use existing kyropoulos to carry out large scale
When stone crystal growth, since size is larger and temperature difference gradient and rate fluctuation are larger, as shown in Fig. 1, easily make crystal head
The following taper bubble in portion and shouldering face and crystal bottom steamed bun shape bubble significantly increase, and reduce the quality of sapphire crystal,
Limit the popularization and application of large-size sapphire.Therefore, to further increase large-size sapphire growth quality, one kind is provided
The sapphire growth method that crystal shoulder taper and bottom steamed bun shape bubble can be effectively relieved is particularly important.
Invention content
This application provides a kind of methods of kyropoulos growing sapphire crystal, big for growing to solve existing kyropoulos
When size sapphire crystal, easily increase the following taper bubble in crystal head and shouldering face and crystal bottom steamed bun shape bubble,
The problem of reducing sapphire crystal quality.
A kind of method of kyropoulos growing sapphire crystal, the method includes feeding, heat material, seeding, expand shoulder life
Length, ending growth, carries the de- and cooling down stage at isodiametric growth；
Wherein, in the expansion shoulder growth course, expand shoulder length speed is no more than crystal weight 5%~10%, pulling rate 0.1
~1mm/h, when crystal weight is 500g~1000g, instantaneous lifting 2mm upwards, when crystal weight is 1200g~1800g, wink
When lift 2mm upwards；
In the ending growth phase, after crystal weight reaches the 70%~80% of target weight, crystal weight curve becomes
For wave when, after continued growth H hours, enter back into and carry the de- stage.
Optionally, it can be calculated by the following formula for described H hours：
H=(M-M1)/V
Wherein, M1For crystal weight, M is target weight, when V is that crystal weight reaches the 70% of target weight, to being pushed forward
Average long speed in 15 hours.
Optionally, into it is described put forward de- process after, lift seed rod after mending 5~10 DEG C, 2 hours of temperature, pulling rate is 0.2~
0.5mm/h, until crystal weight steadily maintains the 110%~115% of target weight.
Optionally, when crystal weight reach target weight 8%~10% after be transferred to the isodiametric growth stage, after isodiametric growth
Stop lifting, rate of crystalline growth is no more than 1.2kg/h.
Optionally, in the ending segment of the seeding, when judging that crystal length speed is suitable, seed rod is lifted, pulling rate is 0.3~
3mm/h, and every 5~15min, instantaneously lifting is primary, lifts 2mm every time, until after brilliant knot diameter reaches 50~70mm, incision
The expansion shoulder growth phase.
Optionally, in the cool down, the time totally to cool down is 100h~145h.
Optionally, in the cool down, air or argon gas, inflationtime 15h are filled with after cooling 48h~60h
~20h.
Optionally, the method can grow the sapphire crystal that target weight is more than or equal to 100kg.
Technical solution provided by the present application includes following advantageous effects：
The application provides a kind of method of kyropoulos growing sapphire crystal, with existing kyropoulos sapphire growth technique
It compares, in expanding shoulder growth course, respectively when crystal weight is 500g~1000g and when 1200g~1800g, uses wink
The growth of crystal shoulder bubble can be effectively relieved in the expansion shoulder technique of Shi Tila, cut off plane of crystal crystal boundary line, effectively improve crystal
Quality；The round growth for also contributing to crystal simultaneously, avoids special-shaped growth.And in the growth course that finishes up, work as crystal weight
When curve becomes curve from straight line, the continued growth without lifting, the tailing-in technique not lifted using bottom can effectively avoid
Due to lifting the vibration effect caused by large-size crystals, alleviate the formation and growth of crystal bottom steamed bun shape bubble.There is provided one
Kind is applicable to large-size sapphire growth, and crystal shoulder taper and bottom steamed bun shape bubble is effectively relieved, and it is blue to improve large scale
The kyropoulos sapphire growth technique of gem crystal quality.
Description of the drawings
In order to illustrate more clearly of the technical solution of the application, letter will be made to attached drawing needed in the embodiment below
Singly introduce, it should be apparent that, for those of ordinary skills, without having to pay creative labor,
Other drawings may also be obtained based on these drawings.
Fig. 1 is a kind of bubble distribution schematic diagram of the 100kg sapphire crystals of existing kyropoulos growth provided by the present application；
Fig. 2 is using a kind of bubble distribution of the 100kg sapphire crystals of kyropoulos growth provided by the embodiments of the present application
Schematic diagram.
Specific implementation mode
The drawings herein are incorporated into the specification and forms part of this specification, and shows the implementation for meeting the application
Example, and the principle together with specification for explaining the application.
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, for those of ordinary skill in the art
Speech, without having to pay creative labor, other drawings may also be obtained based on these drawings.
Kyropoulos abbreviation KY methods, principle is that fusing forms melt after first heating the raw material to fusing point, then with the seed of monocrystalline
Crystalline substance touches bath surface, starts the monocrystalline of growth and the identical monoclinic crystal structure of seed crystal in solid liquid interface of the seed crystal with melt.
Seed crystal is up promoted with slow speed, is formed brilliant neck after seed crystal lifts a period of time upwards, is waited for melt and seed crystal interface
After solidification rate is stablized, seed crystal is not lifting, and makes monocrystalline gradual from top in a manner of only controlling cooling rate to reduce power
It solidifies down, eventually forms a complete single-crystal boule.Hereafter, by draw stick in the way of along C to carrying out drawing stick.
The application provides a kind of method of kyropoulos growing sapphire crystal, and the sapphire for being suitable for growing large-size is brilliant
Body, this method include charging, heating material, seeding, expand shoulder growth, isodiametric growth, ending growth, carry and taking off and cooling down is several
A stage.Pure raw material is fitted into crucible first, equipped with rotatable and lifting lifting rod above crucible, the lower end of bar has
One seed holder is equipped with the sapphire seed crystal of orientation on it.Then crucible is heated, reduces lifting rod, seed crystal is made to be inserted into
In melt, the temperature of melt is controlled, liquid level temperature is made to be slightly above fusing point.Seed rod is pulled, pulling rate is controlled and rotating speed, seed crystal is gradual
It grows up.Heating power is adjusted, liquid level temperature is made to be equal to fusing point, realizes necking down-expansion shoulder-isodiametric growth-receipts of gem crystal growth
Tail overall process.Finally make crystal be detached from crucible after, slowly reduce power, to crystal carry out cooling down processing, after blow-on
Take out crystal.
Wherein, in expanding shoulder growth course, expand shoulder length speed be no more than crystal weight 5%~10%, pulling rate be 0.1~
1mm/h, when crystal weight is 500g~1000g, instantaneous lifting 2mm upwards, when crystal weight is 1200g~1800g, instantaneously
Lifting 2mm upwards.It should be noted that crystal weight refers to real-time weight of the crystal in growth course in the embodiment of the present application
Amount, target weight refer to the target weight of the sapphire crystal grown using this method.
During expanding shoulder growth, using the expansion shoulder technique instantaneously lifted, since large-sized sapphire crystal is in life
The temperature gradient at each position and vibration differ greatly in growth process, and the increase of bubble is easily caused in drawing process.Using
The instantaneous time is quickly lifted, and can be slowed down the influence of pulling rate during lifting and be led to bubble in large-size crystals growth
Lead to the problem of and increase, to effectively alleviate crystal head to shouldering face taper bubble below formation and increase.
In the expansion shoulder growth phase of crystal, when crystal weight reach 500g~1000g and crystal weight reach 1200g~
When 1800g, abnormity growth easily occurs for crystal, gives seed rod instantaneous upward lifting at this time, can effectively avoid the different of crystal
Shape is grown, and contributes to the round development of crystal；Plane of crystal crystal boundary line can be cut off in the instantaneous lifting carried out simultaneously in the above-mentioned stage,
Crystal quality can be improved, help to improve the quality of production of large size sapphire crystal.
In ending growth phase, after crystal weight reaches the 70%~80% of target weight, crystal weight curve becomes wave
When unrestrained line, after continued growth H hours, enters back into and carry the de- stage.Reach the 70% of target weight in the weight for display crystal of weighing
After~80%, the weight distribution curve of crystal can become wave from original straight line, show at this time crystal touch crucible wall surface or
The bottom of crucible continues to growth H hours at this time, until crystal weight close to after target weight, enters back into and carries the de- stage.Specifically
H can by actually grow into close to the target weight time carry out judge enter carry the de- stage, can also be calculated by formula,
Setting control enters after H hours carries the de- stage.
In existing kyropoulos technique, seed rod carry de- after carrying the de- stage into ending, keep crystal not adherent
Growth, however lifting at this time can cause the vibration of crystal, even the pulling rate of very little, but for large-sized crystal,
The vibration at each position differs greatly, and the vibration that the slight vibration in top easily causes bottom more serious easily generates bubble, to increase
The big bubble of crystal bottom.And in kyropoulos provided by the present application, it continues to give birth to behind crystal touching crucible wall surface or bottom
Long, de- without carrying out carrying at once, that is, the tailing-in technique for using bottom not lift can effectively avoid pulling rate from generating crystal bubble
Influence, to alleviate the generation and increase of crystal bottom steamed bun shape bubble.
The application provides a kind of method of kyropoulos growing sapphire crystal, it is main use the expansion shoulder technique that instantaneously lifts with
And it is brilliant to improve large-size sapphire to alleviate crystal shoulder taper and bottom steamed bun shape bubble for the tailing-in technique that bottom does not lift
Weight.Expanding in shoulder growth course at it, expands shoulder length speed is no more than crystal weight 5%~10%, pulling rate is 0.1~1mm/h,
When crystal weight is 500g~1000g, instantaneous lifting 2mm upwards is instantaneously carried upwards when crystal weight is 1200g~1800g
Draw 2mm.And in its growth phase that finishes up, after crystal weight reaches the 70%~80% of target weight, crystal weight curve becomes
When wave, after continued growth H hours, enters back into and carry the de- stage.
Attached drawing 2 is referred to, the figure shows use a kind of 100kg of kyropoulos growth provided by the embodiments of the present application blue precious
The bubble distribution schematic diagram of stone crystal, compared to Figure 1, the shoulder and bottom bubble of crystal significantly reduce.It follows that the application
The method for the kyropoulos growing sapphire crystal that embodiment provides, the receipts not lifted using the expansion shoulder technique instantaneously lifted and bottom
Tail technique can alleviate crystal shoulder taper and bottom steamed bun shape bubble to the greatest extent, improve crystal quality, and it is big to be suitable for growth
Size sapphire crystal.Currently, kyropoulos provided by the embodiments of the present application are applicable to growth 260kg sapphire crystals.
Optionally, it can be calculated by the following formula within H hours：
H=(M-M1)/V
Wherein, M1For crystal weight, M is target weight, when V is that crystal weight reaches the 70% of target weight, to being pushed forward
Average long speed in 15 hours.
Optionally, into after putting forward de- process, seed rod is lifted after benefit is 5~10 DEG C, 2 hours warm, pulling rate is 0.2~0.5mm/
H, until crystal weight steadily maintains the 110%~115% of target weight.After continued growth H hours, into carrying the de- stage,
It is carried out after mending temperature by improving heating power, waits for lift seed rod again within 2 hours, until crystal weight steadily maintains target weight
The 110%~115% of amount, may determine that crystal growth terminates and is detached from crucible at this time.2 hours after benefit temperature, the temperature liter of crucible
Height, crystal temperature effect increase, and the bottom surface fusing that crystal is bonded with crucible can effectively help crystal to be detached from crucible.
Optionally, the isodiametric growth stage is transferred to after the 8%-10% that crystal weight reaches target weight, after isodiametric growth
Stop lifting, rate of crystalline growth is no more than 1.2kg/h.
Optionally, in the ending segment of seeding, when judging that crystal length speed is suitable, seed rod is lifted, pulling rate is 0.3~3mm/
H, and every 5~15min, instantaneously lifting is primary, lifts 0.5~2mm every time, until after brilliant knot diameter reaches 50~70mm, incision
Expand shoulder growth phase.After crystal enters growth, its pulling rate is controlled between 0.3mm/h-0.5mm/h, it is mellow and full to be conducive to habit,
Circle is grown into, instantaneous more than 1mm lifts stepped of making a living, and crystal growth can be prevented too fast, while being conducive to cut-out table
Face crystal boundary line.
Optionally, in cool down, the time totally to cool down is 100h~145h.
Optionally, air or argon gas are filled in cool down, after cooling 48h~60h, inflationtime be 15h~
20h。
Optionally, this method can grow the sapphire crystal that target weight is more than or equal to 100kg.
In order to illustrate more clearly of the technical solution of the embodiment of the present application, below using grow 100kg sapphire crystals as
Embodiment is briefly described.
Embodiment 1
The application provides a kind of method of kyropoulos growing sapphire crystal, and this method includes charging, heating material, draws
Brilliant, expansion shoulder growth, ending growth, carries de-, cooling down several stages at isodiametric growth, and specific embodiment includes following walks
Suddenly：
S101：It, will in special cleansing room with the clearing furnaces such as alcohol, non-dust cloth, brass wire brush, industrial dust collector and insulating layer
Purity is that the alumina raw material of 5N is attached in crucible, is encapsulated with clean plastic cloth alternative.
S102：The crucible for filling raw material is packed into burner hearth, by A to seed crystal device in seedholder, and is rotatably connected in seed crystal
On bar, stove is closed after completing seed rod centering, vacuumizes and hunts leak.
S103：It according to different thermal field and raw material, determines material technique and heats up, after melting sources, keep melt
Constant 3~5 hours under the high temperature conditions.
S104：Decline seed crystal, according to flow stream velocity, liquid fluid line thickness, whether there is or not chinampa and chinampa size, seed crystal end whether
There is electric thermo-couple temperature situation of change etc. in fusing and the brightness of seed crystal end, stove to judge melt temperature if appropriate for seeding.By seed
Crystalline substance drops to 50~80mm of liquid level or less, it is ensured that seed crystal end is melted by rectangular for arc surface, and seed crystal is bright, and no black deposit is attached
It.
S105：Bright seed crystal is inserted into 5~40mm of liquid level or less, weight is reset, constant 10~30min, if seed crystal
Thick 3~6mm is slowly grown at solid liquid interface, can assert that temperature is suitable.
If quickly grown in 1~5min, 200~500 watts of power is increased according to thermal field situation, constant 2~3 is small
When, crystalline substance is washed again, repeats step S105.
If can not grown in 30min or seed crystal fusing, 300~500 watts of power of reduction constant 2~3 hours, washed again
Crystalline substance repeats step S105.
S106：When judging that long speed is suitable, the pull rate of 0.1~3mm/h is set, and with 5~15min/ times/2mm's
Instantaneous lifting, until shoulder growth is expanded in incision after brilliant knot diameter reaches 50~70mm.Expand shoulder length speed be no more than weight 5%~
10%, pulling rate is 0.1~1mm/h, when wherein weight is 800g, instantaneous lifting 2mm upwards.It is instantaneous upward when weight is 1500g
Lift 2mm.
S107：Crystal weight turns isodiametric growth after reaching 10kg, stops lifting after isodiametric growth, rate of crystalline growth does not surpass
Cross 1.2kg/h.
S108：After display crystal weight of weighing is 75~85kg, weight distribution curve can become wave from straight line, show crystalline substance
Body touches crucible wall surface or crucible bottom, needs continued growth at this time H hours, enters carry the de- stage afterwards.
S109：After continued growth H hours, 1~2kw of heating power is turned up, mends 5~10 DEG C of temperature, to seed crystal after waiting for 2 hours
The pulling rate of 0.2~0.5mm/h of bar tends to be steady until crystal weight signal maintains 100kg or so, can determine whether crystal at this time
Growth terminates and is detached from crucible.
S110：Power is slowly reduced, annealing cooling processing is carried out to crystal, overall temperature fall time is 135h, and cooling terminates
Afterwards, air or argon gas are filled after 48~60h of natural cooling, inflates and terminates after 15~20h, and crystal is taken out in blow-on.
The application provides a kind of method of kyropoulos growing sapphire crystal, with existing kyropoulos sapphire growth technique
It compares, in expanding shoulder growth course, respectively when crystal weight is 500g~1000g and when 1200g~1800g, uses wink
The growth of crystal shoulder bubble can be effectively relieved in the expansion shoulder technique of Shi Tila, cut off plane of crystal crystal boundary line, effectively improve crystal
Quality；The round growth for also contributing to crystal simultaneously, avoids special-shaped growth.And in the growth course that finishes up, work as crystal weight
When curve becomes curve from straight line, the continued growth without lifting, the tailing-in technique not lifted using bottom can effectively avoid
Due to lifting the vibration effect caused by large-size crystals, alleviate the formation and growth of crystal bottom steamed bun shape bubble.There is provided one
Kind is applicable to large-size sapphire growth, and crystal shoulder taper and bottom steamed bun shape bubble is effectively relieved, and it is blue to improve large scale
The kyropoulos sapphire growth technique of gem crystal quality.
It should be noted that such as the terms "include", "comprise" or its any other variant are intended to nonexcludability
Include but also include not bright so that article or equipment including a series of elements include not only those elements
The other element really listed, or further include for elements inherent to such a process, method, article, or device.Do not having
In the case of more limitations, the element that is limited by sentence "including a ...", it is not excluded that including the element process,
There is also other identical elements in method, article or equipment.
The above is only the specific implementation mode of the application, is made skilled artisans appreciate that or realizing this Shen
Please.Various modifications to these embodiments will be apparent to one skilled in the art, as defined herein
General Principle can in other embodiments be realized in the case where not departing from spirit herein or range.Therefore, the application
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
It should be understood that the application is not limited to the content for being described above and being shown in the accompanying drawings, and can
To carry out various modifications and change without departing from the scope.Scope of the present application is only limited by the accompanying claims.
Claims (8)
1. a kind of method of kyropoulos growing sapphire crystal, which is characterized in that the method includes feeding, heat material, draw
Brilliant, expansion shoulder growth, ending growth, carries the de- and cooling down stage at isodiametric growth；
Wherein, in the expansion shoulder growth course, expand shoulder length speed be no more than crystal weight 5%~10%, pulling rate be 0.1~
1mm/h, when crystal weight is 500g~1000g, instantaneous lifting 2mm upwards, when crystal weight is 1200g~1800g, instantaneously
Lifting 2mm upwards；
In the ending growth phase, after crystal weight reaches the 70%~80% of target weight, crystal weight curve becomes wave
When unrestrained line, after continued growth H hours, enters back into and carry the de- stage.
2. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that described H hours can lead to
Following formula is crossed to be calculated：
H=(M-M1)/V
Wherein, M1For crystal weight, M is target weight, when V is that crystal weight reaches the 70% of target weight, to being pushed forward 15 hours
Interior average long speed.
3. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that carry and taking off described in entrance
Cheng Hou lifts seed rod after benefit is 5~10 DEG C, 2 hours warm, pulling rate is 0.2~0.5mm/h, until crystal weight steadily maintains
The 110%~115% of target weight.
4. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that when crystal weight reaches
It is transferred to the isodiametric growth stage after the 8%~10% of target weight, stops lifting after isodiametric growth, rate of crystalline growth is no more than
1.2kg/h。
5. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that in the knot of the seeding
When beam section, when judging that crystal length speed is suitable, seed rod is lifted, pulling rate is 0.3~3mm/h, and is instantaneously lifted every 5~15min
Once, 2mm is lifted every time, until after brilliant knot diameter reaches 50~70mm, cuts the expansion shoulder growth phase.
6. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that the cooling down mistake
Cheng Zhong, the time totally to cool down are 100h~145h.
7. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that the cooling down mistake
Air or argon gas are filled with after Cheng Zhong, cooling 48h~60h, inflationtime is 15h~20h.
8. the method for kyropoulos growing sapphire crystal according to claim 1, which is characterized in that the method can be grown
Target weight is more than or equal to the sapphire crystal of 100kg.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112631A (en) * | 2018-10-29 | 2019-01-01 | 浙江昀丰新材料科技股份有限公司 | A kind of sapphire C is to long crystal method |
| CN110359091A (en) * | 2019-08-20 | 2019-10-22 | 宿迁学院 | A kind of kyropoulos sapphire crystal production technology |
| CN114836821A (en) * | 2021-02-01 | 2022-08-02 | 浙江大学杭州国际科创中心 | Growth method of low dislocation density gallium oxide bulk single crystal |
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| CN102140675A (en) * | 2011-03-24 | 2011-08-03 | 哈尔滨奥瑞德光电技术股份有限公司 | Kyropoulos method for quickly growing large-size sapphire single crystal |
| CN103966661A (en) * | 2014-04-08 | 2014-08-06 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing sapphire single crystal with Kyropoulos method |
| JP2016117606A (en) * | 2014-12-19 | 2016-06-30 | 株式会社タムラ製作所 | RAISING METHOD OF Ga2O3-BASED SINGLE CRYSTAL, AND CRUCIBLE |
| CN105671630A (en) * | 2015-12-17 | 2016-06-15 | 南京晶升能源设备有限公司 | Ending method for growth of sapphire crystal through kyropoulos method and growth method |
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| CN109112631A (en) * | 2018-10-29 | 2019-01-01 | 浙江昀丰新材料科技股份有限公司 | A kind of sapphire C is to long crystal method |
| CN110359091A (en) * | 2019-08-20 | 2019-10-22 | 宿迁学院 | A kind of kyropoulos sapphire crystal production technology |
| CN114836821A (en) * | 2021-02-01 | 2022-08-02 | 浙江大学杭州国际科创中心 | Growth method of low dislocation density gallium oxide bulk single crystal |
| CN114836821B (en) * | 2021-02-01 | 2023-08-29 | 杭州镓仁半导体有限公司 | Growth method of low dislocation density gallium oxide bulk single crystal |
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