CN110359091A - A kind of kyropoulos sapphire crystal production technology - Google Patents
A kind of kyropoulos sapphire crystal production technology Download PDFInfo
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- CN110359091A CN110359091A CN201910768190.4A CN201910768190A CN110359091A CN 110359091 A CN110359091 A CN 110359091A CN 201910768190 A CN201910768190 A CN 201910768190A CN 110359091 A CN110359091 A CN 110359091A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
Abstract
The present invention mainly passes through using a kind of specific " sitting pot " ending and mends the crystal growing technology of Wen Tituo, alleviates bottom centre's steamed bun shape bubble to the greatest extent, even grows the gem-quality crystal of complete bubble-free.Particularly, bottom protrusion is the water-drop-shaped crystal of annulus or circle ring array, and convex portion can effectively reduce crystal and fall the crack probability after crystalline substance, realizes the growth of complete bubble-free crystal.
Description
Technical field
The present invention relates to a kind of new methods and new process suitable for the ending growth of kyropoulos sapphire single-crystal, more particularly to
A kind of sapphire crystal suitable for 160kg grades or more finishes up growing method, is applied particularly to the technology of Sapphire Crystal Growth
Field.
Background technique
Sapphire have fusing point high (2045 DEG C), it is thermally conductive it 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, mirror surface, and is applied to guided missile dome, goes straight up to arbor
Equal military enterprises.There are many methods for sapphire crystal growth, are mainly at present kyropoulos for the method that businessman generallys use.Bubble life
Method abbreviation KY method, principle are that fusing forms melt after first heating the raw material to fusing point, then touches melt with the seed crystal of monocrystalline
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, and seed crystal is with slow
Speed is up promoted, and is formed brilliant neck after seed crystal lifts a period of time upwards, is stablized to melt and the solidification rate at seed crystal interface
Afterwards, seed crystal is not lifting, and only solidifies monocrystalline gradually down from top in a manner of controlling cooling rate to reduce power, finally
Form a complete single-crystal boule.Hereafter, by draw stick in the way of lacked to stick, the crystal of such method growth draw along C
Fall into less, dislocation density it is low, become the mainstream growing method of sapphire crystal industry.It is brilliant with the innovation of kyropoulos technology
Body weight is incrementally increased to current 160kg or more, and crucible diameter increases, and crucible bottom gradient reduces, and interface is also easy to produce
Overturning, forms serious born of the same parents' shape interface, after interface inversion, is also easy to produce constitutional supercooling, solute tail, bubble and melt wrappage
The defects of, especially there are in the case where high pulling rate in crystal ending growth course, sapphire crystal bottom centre bubble is in
Sheet or bottom centre's steamed bun shape, are illustrated in fig. 1 shown below, and due to the presence of crystal bottom steamed bun shape bubble, utilization rate of crystal is tight
Decline again.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention mainly passes through using a kind of specific " sitting pot " ending and mends the long brilliant of Wen Tituo
Technique alleviates bottom centre's steamed bun shape bubble to the greatest extent, even grows the gem-quality crystal of complete bubble-free.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of kyropoulos sapphire crystal production technology, which comprises the steps of:
1), with alcohol and/or non-dust cloth and/or brass wire brush and/or industrial dust collector clearing furnace and insulating layer；
2) it is, that 5N alumina raw material is attached in crucible by purity in toilet, is encapsulated with clean plastic cloth stand-by；
3), the crucible for filling raw material is packed into burner hearth, by A to seed crystal device in seedholder, and is rotatably connected on seed rod, it is complete
At furnace is closed after seed rod centering, vacuumizes and hunt leak；
4) it, according to different thermal field and raw material, determines material technique and heats up；
5) it, after melting sources, is kept for melt constant 3~5 hours under the high temperature conditions；
6), lower by seed crystal, according to flow stream velocity, liquid fluid line thickness, whether there is or not chinampas and chinampa size, seed crystal end whether to have fusing
And electric thermo-couple temperature situation of change judges melt temperature if appropriate for seeding in the brightness of seed crystal end, furnace；
7) seed crystal, is dropped into 20~80mm of liquid level or less after suitable seeding, control seed crystal end is melted by rectangular for arc surface,
Seed crystal is bright, and black deposit is avoided to adhere to；
8), by 10~40mm below bright seed crystal insertion liquid level, weight is reset, constant 10~30min, if seed crystal is in solid-liquid
Thick 3~8mm is slowly grown in interface, assert that temperature is suitable；
If 9), quickly grown in 1~5min, according to thermal field situation increase by 150~500 watts of power, constant 2~3 hours,
Again crystalline substance is washed, step 8 is repeated；
10) it, can not grown in 30min such as or seed crystal fusing, 300~700 watts of power of drop constant 2~3 hours, wash crystalline substance again, weight
Multiple step 8；
11), when judging that long speed is suitable, the pull rate of 0.1~5mm/h is controlled, and with the wink of 5~10min/ times/2~3mm
Shi Tila, until shoulder growth is expanded in incision after brilliant knot diameter reaches 50~80mm；
12), crystal growth carries out expanding shoulder growth according to technique in step 11), expands shoulder length speed≤weight 3%~8%, pulling rate is
0.05~1mm/h, weight turn isodiametric growth after reaching 13~15kg, stop lifting after isodiametric growth, and rate of crystalline growth≤
1.5kg/h；
13), ending growth: after weighing shows weight M=135~155kg, weight distribution curve can be become wave from straight line, characterization
Crystal touches crucible wall surface or crucible bottom, needs continued growth at this time H hours, enters mention the de- stage afterwards；
14) it, proposes de- process: after continued growth H hours, mending 1.5~2kw of temperature, the pulling rate of seed rod is given after waiting 2 hours；
15), cool down: slowly reducing power, crystal is made annealing treatment: temperature fall time 160H-170H, after cooling, from
Air or argon gas are so filled after cooling 48~60H, 15~20H inflation terminates, and blow-on takes crystal.
As previous step preferred embodiment, the calculation method of H in the step 13) are as follows: H=(160-M)/V, V characterization weight reach
When to 135kg, to the average long speed for being pushed forward 24 hours.
As previous step preferred embodiment, the step 14) mentions given pulling rate >=20mm/h of de- process, after starting lifting,
Weighing display numerical value steeply rises, and rear step type, which is fallen after rise to crystal weight signal, maintains 160kg or so, tends to be steady, at this time
It can determine whether that crystal growth terminates and is detached from crucible.
(3) beneficial effect
The present invention provides a kind of kyropoulos sapphire crystal production technology, have it is following the utility model has the advantages that
The present invention mainly passes through using a kind of specific " sitting pot " ending and mends the crystal growing technology of Wen Tituo, alleviates to the greatest extent
Bottom centre's steamed bun shape bubble, even grows the gem-quality crystal of complete bubble-free.Particularly, by forming protrusion in bottom
For annulus or the water-drop-shaped crystal of circle ring array, convex portion can effectively reduce crystal and fall the crack probability after crystalline substance, realized
The growth of whole bubble-free crystal.
Detailed description of the invention
Fig. 1 is that the vertical paper direction of the prior art is C to schematic diagram；
Fig. 2 is schematic structural view of the invention.
1, the water-drop-shaped crystal of annulus or circumference array.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of kyropoulos sapphire crystal production technology, which comprises the steps of:
1), with alcohol and/or non-dust cloth and/or brass wire brush and/or industrial dust collector clearing furnace and insulating layer；
2) it is, that 5N alumina raw material is attached in crucible by purity in toilet, is encapsulated with clean plastic cloth stand-by；
3), the crucible for filling raw material is packed into burner hearth, by A to seed crystal device in seedholder, and is rotatably connected on seed rod, it is complete
At furnace is closed after seed rod centering, vacuumizes and hunt leak；
4) it, according to different thermal field and raw material, determines material technique and heats up；
5) it, after melting sources, is kept for melt constant 3 hours under the high temperature conditions；
6), lower by seed crystal, according to flow stream velocity, liquid fluid line thickness, whether there is or not chinampas and chinampa size, seed crystal end whether to have fusing
And electric thermo-couple temperature situation of change judges melt temperature if appropriate for seeding in the brightness of seed crystal end, furnace；
7) seed crystal, is dropped into liquid level or less 20mm after suitable seeding, control seed crystal end is melted by rectangular for arc surface, seed crystal
It is bright, avoid black deposit from adhering to；
8), by 10mm below bright seed crystal insertion liquid level, weight is reset, constant 10min, if seed crystal is slow at solid liquid interface
Slowly thick 3mm is grown, assert that temperature is suitable；
If 9), quickly grown in 1min, increases by 150 watts of power according to thermal field situation, constant 2 hours, wash crystalline substance again, weight
Multiple step 8；
10) it, can not grown in 30min such as or seed crystal fusing, 300 watts of power of drop constant 2 hours, wash crystalline substance again, repeat step 8；
11), when judging that long speed is suitable, the pull rate of 0.1mm/h is controlled, and with the instantaneous lifting of 5min/ times/2mm, until
Shoulder growth is expanded in incision after crystalline substance knot diameter reaches 50mm；
12), crystal growth carries out expanding shoulder growth according to technique in step 11), expands shoulder length speed≤weight 3%, pulling rate is
0.05mm/h, weight turn isodiametric growth after reaching 13~1kg, stop lifting, rate of crystalline growth≤1.5kg/ after isodiametric growth
h；
13), ending growth: after weighing shows weight M=135kg, weight distribution curve can be become wave from straight line, characterize crystal
Crucible wall surface or crucible bottom are touched, needs continued growth at this time H hours, enters propose de- stage, the calculation method of H are as follows: H afterwards
When=(160-M)/V, V characterization weight reach 135kg, to the average long speed for being pushed forward 24 hours；
14) it, proposes de- process: after continued growth H hours, mending temperature 1.5kw, the pulling rate of seed rod is given after waiting 2 hours；It mentions and taking off
Given pulling rate >=20mm/h of journey, after starting lifting, weighing display numerical value is steeply risen, and rear step type, which is fallen after rise to crystal weight, to be believed
Number 160kg or so is maintained, tends to be steady, can determine whether that crystal growth terminates and is detached from crucible at this time；
15), cool down: slowly reducing power, crystal is made annealing treatment: temperature fall time 160HH is naturally cold after cooling
But air or argon gas are filled after 48H, 15H inflation terminates, and blow-on takes crystal.
Embodiment 2:
A kind of kyropoulos sapphire crystal production technology, which comprises the steps of:
1), with alcohol and/or non-dust cloth and/or brass wire brush and/or industrial dust collector clearing furnace and insulating layer；
2) it is, that 5N alumina raw material is attached in crucible by purity in toilet, is encapsulated with clean plastic cloth stand-by；
3), the crucible for filling raw material is packed into burner hearth, by A to seed crystal device in seedholder, and is rotatably connected on seed rod, it is complete
At furnace is closed after seed rod centering, vacuumizes and hunt leak；
4) it, according to different thermal field and raw material, determines material technique and heats up；
5) it, after melting sources, is kept for melt constant 4 hours under the high temperature conditions；
6), lower by seed crystal, according to flow stream velocity, liquid fluid line thickness, whether there is or not chinampas and chinampa size, seed crystal end whether to have fusing
And electric thermo-couple temperature situation of change judges melt temperature if appropriate for seeding in the brightness of seed crystal end, furnace；
7) seed crystal, is dropped into liquid level or less 50mm after suitable seeding, control seed crystal end is melted by rectangular for arc surface, seed crystal
It is bright, avoid black deposit from adhering to；
8), by 25mm below bright seed crystal insertion liquid level, weight is reset, constant 20min, if seed crystal is slow at solid liquid interface
Slowly thick 5.5mm is grown, assert that temperature is suitable；
If 9), quickly grown in 3.5min, increases by 375 watts of power according to thermal field situation, constant 2.5 hours, wash again
Crystalline substance repeats step 8；
10) it, can not grown in 30min such as or seed crystal fusing, 500 watts of power of drop constant 2.5 hours, wash crystalline substance again, repeat step
8；
11), when the long speed of judgement is suitable, the pull rate of 2.5mm/h is controlled, and with the instantaneous lifting of 7.5min/ times/2.5mm,
Until shoulder growth is expanded in incision after brilliant knot diameter reaches 65mm；
12), crystal growth carries out expanding shoulder growth according to technique in step 11), expands shoulder length speed≤weight 5.5%, pulling rate is
0.5mm/h, weight turn isodiametric growth after reaching 14kg, stop lifting, rate of crystalline growth≤1.5kg/h after isodiametric growth；
13), ending growth: after weighing shows weight M=145kg, weight distribution curve can be become wave from straight line, characterize crystal
Crucible wall surface or crucible bottom are touched, needs continued growth at this time H hours, enters propose de- stage, the calculation method of H are as follows: H afterwards
When=(160-M)/V, V characterization weight reach 135kg, to the average long speed for being pushed forward 24 hours；
14) it, proposes de- process: after continued growth H hours, mending temperature 1.75kw, the pulling rate of seed rod is given after waiting 2 hours；It mentions de-
Given pulling rate >=20mm/h of process, after starting lifting, weighing display numerical value is steeply risen, and rear step type is fallen after rise to crystal weight
Signal maintains 160kg or so, tends to be steady, and can determine whether that crystal growth terminates and is detached from crucible at this time；
15), cool down: slowly reducing power, crystal is made annealing treatment: temperature fall time 165H, after cooling, natural cooling
Air or argon gas are filled after 54H, 17.5H inflation terminates, and blow-on takes crystal.
Embodiment 3:
A kind of kyropoulos sapphire crystal production technology, which comprises the steps of:
1), with alcohol and/or non-dust cloth and/or brass wire brush and/or industrial dust collector clearing furnace and insulating layer；
2) it is, that 5N alumina raw material is attached in crucible by purity in toilet, is encapsulated with clean plastic cloth stand-by；
3), the crucible for filling raw material is packed into burner hearth, by A to seed crystal device in seedholder, and is rotatably connected on seed rod, it is complete
At furnace is closed after seed rod centering, vacuumizes and hunt leak；
4) it, according to different thermal field and raw material, determines material technique and heats up；
5) it, after melting sources, is kept for melt constant 5 hours under the high temperature conditions；
6), lower by seed crystal, according to flow stream velocity, liquid fluid line thickness, whether there is or not chinampas and chinampa size, seed crystal end whether to have fusing
And electric thermo-couple temperature situation of change judges melt temperature if appropriate for seeding in the brightness of seed crystal end, furnace；
7) seed crystal, is dropped into liquid level or less 80mm after suitable seeding, control seed crystal end is melted by rectangular for arc surface, seed crystal
It is bright, avoid black deposit from adhering to；
8), by 40mm below bright seed crystal insertion liquid level, weight is reset, constant 30min, if seed crystal is slow at solid liquid interface
Slowly thick 8mm is grown, assert that temperature is suitable；
If 9), quickly grown in 5min, increases by 500 watts of power according to thermal field situation, constant 3 hours, wash crystalline substance again, weight
Multiple step 8；
10) it, can not grown in 30min such as or seed crystal fusing, 700 watts of power of drop constant 3 hours, wash crystalline substance again, repeat step 8；
11), when judging that long speed is suitable, the pull rate of 5mm/h is controlled, and with the instantaneous lifting of 10min/ times/3mm, until
Shoulder growth is expanded in incision after crystalline substance knot diameter reaches 80mm；
12), crystal growth carries out expanding shoulder growth according to technique in step 11), expands shoulder length speed≤weight 8%, pulling rate 1mm/
H, weight turn isodiametric growth after reaching 15kg, stop lifting, rate of crystalline growth≤1.5kg/h after isodiametric growth；
13), ending growth: after weighing shows weight M=155kg, weight distribution curve can be become wave from straight line, characterize crystal
Crucible wall surface or crucible bottom are touched, needs continued growth at this time H hours, enters propose de- stage, the calculation method of H are as follows: H afterwards
When=(160-M)/V, V characterization weight reach 135kg, to the average long speed for being pushed forward 24 hours；
14) it, proposes de- process: after continued growth H hours, mending temperature 2kw, the pulling rate of seed rod is given after waiting 2 hours；Propose de- process
Given pulling rate >=20mm/h, after starting lifting, weighing display numerical value steeply rise, rear step type is fallen after rise to crystal weight signal
160kg or so is maintained, is tended to be steady, can determine whether that crystal growth terminates and is detached from crucible at this time；
15), cool down: slowly reducing power, crystal is made annealing treatment: temperature fall time 170H, after cooling, natural cooling
Air or argon gas are filled after 60H, 20H inflation terminates, and blow-on takes crystal.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (3)
1. a kind of kyropoulos sapphire crystal production technology, which comprises the steps of:
1), with alcohol and/or non-dust cloth and/or brass wire brush and/or industrial dust collector clearing furnace and insulating layer；
2) it is, that 5N alumina raw material is attached in crucible by purity in toilet, is encapsulated with clean plastic cloth stand-by；
3), the crucible for filling raw material is packed into burner hearth, by A to seed crystal device in seedholder, and is rotatably connected on seed rod, it is complete
At furnace is closed after seed rod centering, vacuumizes and hunt leak；
4) it, according to different thermal field and raw material, determines material technique and heats up；
5) it, after melting sources, is kept for melt constant 3~5 hours under the high temperature conditions；
6), lower by seed crystal, according to flow stream velocity, liquid fluid line thickness, whether there is or not chinampas and chinampa size, seed crystal end whether to have fusing
And electric thermo-couple temperature situation of change judges melt temperature if appropriate for seeding in the brightness of seed crystal end, furnace；
7) seed crystal, is dropped into 20~80mm of liquid level or less after suitable seeding, control seed crystal end is melted by rectangular for arc surface,
Seed crystal is bright, and black deposit is avoided to adhere to；
8), by 10~40mm below bright seed crystal insertion liquid level, weight is reset, constant 10~30min, if seed crystal is in solid-liquid
Thick 3~8mm is slowly grown in interface, assert that temperature is suitable；
If 9), quickly grown in 1~5min, according to thermal field situation increase by 150~500 watts of power, constant 2~3 hours,
Again crystalline substance is washed, step 8 is repeated；
10) it, can not grown in 30min such as or seed crystal fusing, 300~700 watts of power of drop constant 2~3 hours, wash crystalline substance again, weight
Multiple step 8；
11), when judging that long speed is suitable, the pull rate of 0.1~5mm/h is controlled, and with the wink of 5~10min/ times/2~3mm
Shi Tila, until shoulder growth is expanded in incision after brilliant knot diameter reaches 50~80mm；
12), crystal growth carries out expanding shoulder growth according to technique in step 11), expands shoulder length speed≤weight 3%~8%, pulling rate is
0.05~1mm/h, weight turn isodiametric growth after reaching 13~15kg, stop lifting after isodiametric growth, and rate of crystalline growth≤
1.5kg/h；
13), ending growth: after weighing shows weight M=135~155kg, weight distribution curve can be become wave from straight line, characterization
Crystal touches crucible wall surface or crucible bottom, needs continued growth at this time H hours, enters mention the de- stage afterwards；
14) it, proposes de- process: after continued growth H hours, mending 1.5~2kw of temperature, the pulling rate of seed rod is given after waiting 2 hours；
15), cool down: slowly reducing power, crystal is made annealing treatment: temperature fall time 160H-170H, after cooling, from
Air or argon gas are so filled after cooling 48~60H, 15~20H inflation terminates, and blow-on takes crystal.
2. a kind of kyropoulos sapphire crystal production technology according to claim 1, it is characterised in that: the step 13)
The calculation method of middle H are as follows: when H=(160-M)/V, V characterization weight reach 135kg, to the average long speed for being pushed forward 24 hours.
3. a kind of kyropoulos sapphire crystal production technology according to claim 1, it is characterised in that: the step 14)
Given pulling rate >=the 20mm/h for proposing de- process, after starting lifting, weighing display numerical value is steeply risen, and rear step type is fallen after rise to crystal
Weight signal maintains 160kg or so, tends to be steady, and can determine whether that crystal growth terminates and is detached from crucible at this time.
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| CN114280136A (en) * | 2021-12-28 | 2022-04-05 | 江西理工大学 | Preparation method of scheelite main trace element micro-area analysis quantitative correction standard substance |
| CN114875489A (en) * | 2022-07-12 | 2022-08-09 | 太原源瀚科技有限责任公司 | Rapid crystal growth process of large-size sapphire crystal ingot |
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