CN109234796A - A kind of system and method for EFG technique growing large-size sapphire single-crystal plate - Google Patents
A kind of system and method for EFG technique growing large-size sapphire single-crystal plate Download PDFInfo
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- CN109234796A CN109234796A CN201811314343.XA CN201811314343A CN109234796A CN 109234796 A CN109234796 A CN 109234796A CN 201811314343 A CN201811314343 A CN 201811314343A CN 109234796 A CN109234796 A CN 109234796A
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- crucible
- raw material
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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
- C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
-
- 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
- C30B15/005—Simultaneous pulling of more than one crystal
-
- 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
- C30B15/36—Single-crystal growth by pulling from a melt, e.g. Czochralski method characterised by the seed, e.g. its crystallographic orientation
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of system and methods of EFG technique growing large-size sapphire single-crystal plate, by heater, thermal insulation material, mold, crucible, ejection channel, seed crystal elevating mechanism and raw material ejection mechanism composition, the mold is provided with multiple, the crucible center offers hole, the central location in the hole is placed with the trunk portion of ejection channel, the raw material ejection mechanism is located at the bottom of crucible, for that feed particulate material will be launched to higher than edge on crucible, it is provided at the top of the ejection channel for rebounding granular feedstock to the raw material rebounding device inside crucible crucible, kinetic energy absorption material is placed in the crucible；Also disclose a kind of method of EFG technique growing large-size sapphire single-crystal plate；The case where the beneficial effects of the present invention are: not destroying the temperature configuration of crystal growth needs and the temperature gradient of solid liquid interface position, realizing and feed to crucible, while conveying channel blockage caused by particulate material softens is not present, reliable performance.
Description
Technical field
The invention belongs to crystal fabrication technology fields, and in particular to a kind of EFG technique growing large-size sapphire single-crystal plate
System and EFG technique growing large-size sapphire single-crystal plate method.
Background technique
When sapphire single-crystal Al2O3 is as optical window material, with transmission region is wide, medium-wave infrared light transmission is good, bending resistance
The advantages that intensity height, heat resistant and wear resistant；In certain specific use environments, need to use large-sized sapphire single-crystal plate
Material, and it is processed into large-sized optical window, the crystal growing technology of EFG technique is long relative to the sapphire of the mainstreams such as kyropoulos at present
Crystal technique has stock utilization height, the big advantage of size.
EFG technique is a kind of growing method of sapphire crystal material, and principle is passed through using the capillary gap on mold
Alumina raw material after melting in crucible is promoted to die tip by capillary phenomenon, and forms liquid film in die top, seed crystal with
It after liquid film contact, lifts upwards, under the control of temperature gradient appropriate, is grown into out width close to die width, height
The identical monocrystalline plate with seed crystal lifting height.
When die tip is more than critical value away from melt liquid level distance, die tip will be unable to form liquid film, big in growth
When size sapphire single-crystal plate, by temperature uniformity, capillary seam melt delivery rate, crucible inner melt liquid level falling head
One mold, is usually only placed in crucible by limitation, to ensure that monocrystalline plate can be grown enough to big, as crystal is raw
Long, liquid level will be gradually reduced in crucible, be caused the driving force of die tip feedstock transportation to weaken, be influenced crystallization process, make crystal
It is unable to continued propagation or plate deforms.
The system of double molds or multi-mould design so that it is original just as the speed of melt liquid level decline faster, sapphire is brilliant
The growth of body will be interrupted because crucible inner melt amount declines the reason of in advance.
In order to research and develop a kind of charging system, melt is persistently supplemented, so that crucible inner melt is highly stable during long brilliant
It is held in position in, gets rid of the limitation risen under melt liquid level, according to the principle of temperature symmetry, while growing two pieces of rulers
Very little biggish sapphire crystal plate；Thus it is proposed that a kind of system of EFG technique growing large-size sapphire single-crystal plate and
Method.
Summary of the invention
The purpose of the present invention is to provide a kind of system and method for EFG technique growing large-size sapphire single-crystal plate, with
Solve die tip mentioned above in the background art away from melt liquid level distance be more than critical value when, die tip will be unable to be formed
Liquid film is stitched melt delivery rate, crucible inner melt by temperature uniformity, capillary in growing large-size sapphire single-crystal plate
The limitation of liquid level falling head, with crystal growth, liquid level will be gradually reduced in crucible, cause the drive of die tip feedstock transportation
Power weakens, the problem of influencing crystallization process, crystal is prevented to deform from continued propagation or plate.
To achieve the above object, the invention provides the following technical scheme: a kind of EFG technique growing large-size sapphire single-crystal
The system of plate, by heater, thermal insulation material, mold, crucible, ejection channel, seed crystal elevating mechanism and raw material ejection mechanism group
It is provided at, the mold multiple, the crucible center offers hole, and the central location in the hole is placed with the trunk of ejection channel
Part, the raw material ejection mechanism are located at the bottom of crucible, for will by feed particulate material launch to be higher than crucible on edge, it is described
Be provided at the top of ejection channel for by granular feedstock rebound to the raw material rebounding device inside crucible crucible, in the crucible
It is placed with kinetic energy absorption material.
As a preferred technical solution of the invention, the mold and crucible are process by tungsten or molybdenum material.
As a preferred technical solution of the invention, hollow knot that the ejection channel is processed by graphite, tungsten or molybdenum
Component and the thermal insulation material being wrapped in outside hollow structural members form.
As a preferred technical solution of the invention, the thermal insulation material is the hard felt of graphite or graphite soft felt.
As a preferred technical solution of the invention, the raw material rebounding device is the cone of graphite, tungsten or molybdenum processing
Shape or wedge structural member.
As a preferred technical solution of the invention, the kinetic energy absorption material is the tungsten wire or molybdenum filament of reticular structure
Composition.
The invention also discloses a kind of methods of EFG technique growing large-size sapphire single-crystal plate, include the following steps:
Step 1: being heated by heater and crucible heat up, and by internal melting sources；
Step 2: decline seed crystal elevating mechanism, make two seed crystals on seed crystal elevating mechanism respectively with two die surfaces
It is in contact；
Step 3: after seed portion fusing, seed crystal is lifted by seed crystal elevating mechanism upwards, while appropriate cooling makes mold
The liquid film on surface crystallizes into monocrystalline in seed crystal face；Melt in crucible rises to die surface by mould inside capillary channel
Supplement the liquid film being solidified；
Step 4: according to the speed of crystallization, the alumina granules of corresponding weight is launched upwards by raw material ejection mechanism
Raw material, the raw material launched are rebounded by the raw material rebounding device at the top of ejection channel to inside crucible；
Step 5: the particulate material into crucible drops on kinetic energy absorption material, and crucible is fusing into after being heated, supplement
The oxidation aluminum melt being consumed makes melt liquid level keep stablizing；
Step 6: the lasting lifting of seed crystal elevating mechanism, since lasting ejection feeds, this process will not be by under melt liquid level
It drops and interrupts, until growing large-scale sapphire single-crystal plate.
Compared with prior art, the beneficial effects of the present invention are:
The temperature configuration of crystal growth needs and the temperature gradient of solid liquid interface position are not destroyed, are realized and are added to crucible
The case where expecting, while conveying channel blockage caused by particulate material softens is not present, reliable performance.
Detailed description of the invention
Fig. 1 is that system structure diagram of the invention (is just being shown in the big face of plate, the A-A section of embodiment 1 and implementation
The B-B section of example 1)；
Fig. 2 be general growing large-size sapphire single-crystal plate of the invention system structure diagram (side view is in plate
The big face of material, embodiment 1)；
Fig. 3 be growing large-size sapphire single-crystal plate of the invention system structure diagram (side view is in the big of plate
Face, embodiment 2)；
Fig. 4 is the long crucible structure schematic diagram of growing large-size sapphire single-crystal plate system of the invention；
Fig. 5 is the ejection channel structure 3D fragmentary sectional view of growing large-size sapphire single-crystal plate system of the invention；
In figure: 1, heater；2, thermal insulation material；3, mold；4, crucible；5, seed crystal elevating mechanism；6, crystal；7, melt；
8, ejection channel；9, raw material ejection mechanism；10, conveying mechanism；11, raw material cabin；12, kinetic energy absorption material；21, upper reflection cone；
22, lower reflection cone；23, main channel insulating layer；24, main channel；26, support column.
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
Fig. 1 and Fig. 2 are please referred to, the present invention provides a kind of technical solution: a kind of EFG technique growing large-size sapphire single-crystal
The system and method for plate, by heater 1, thermal insulation material 2, mold 3, crucible 4, ejection channel 8, seed crystal elevating mechanism 5 and original
Expect that ejection mechanism 9 forms, mold 3 is provided with multiple, and 4 center of crucible offers hole, and it is logical that the central location in the hole is placed with ejection
The trunk portion in road 8, raw material ejection mechanism 9 are located at the bottom of crucible 4, for that will launch feed particulate material to higher than crucible 4
Upper edge, the top of ejection channel 8 are provided with for rebounding granular feedstock to the raw material rebounding device inside crucible crucible 4, earthenware
Kinetic energy absorption material is placed in crucible 4.
In the present embodiment, it is preferred that mold 3 and crucible 4 are process by tungsten or molybdenum material, help to increase mold 3
With the stability of crucible 4.
In the present embodiment, it is preferred that the hollow structural members and be wrapped in hollow that ejection channel 8 is processed by graphite, tungsten or molybdenum
Thermal insulation material composition outside structural member, facilitates the heat preservation of ejection channel 8.
In the present embodiment, it is preferred that thermal insulation material is the hard felt of graphite or graphite soft felt, facilitates thermal insulation material operation.
In the present embodiment, it is preferred that raw material rebounding device is the taper or wedge structural member of graphite, tungsten or molybdenum processing, is had
Help improve the performance of raw material rebounding device.
In the present embodiment, it is preferred that kinetic energy absorption material is the tungsten wire or molybdenum filament composition of reticular structure, facilitates kinetic energy suction
Receive the operation of material.
When crystal 6 is grown, 3 lower part of mold point is immersed in melt 7, the liquid of the decline of seed crystal elevating mechanism 5 and 3 top of mold
Film is in contact, while seed portion being melted, and later, cools down and changes the temperature gradient around mold 3, while promoting seed crystal liter
Descending mechanism 5, crystal 6 will gradually be grown since seed crystal up to forming crystal 6 as shown in Figure 1, as long as the melt 7 of mold 3 is defeated
Send that there is no problem, with the upward lifting of seed crystal elevating mechanism 5, crystal 6 will grow tall always, last because 7 liquid level of melt declines
The problem of, it conveys the melt 7 of mold 3 and disruption occurs, the growth of crystal 6 terminates.
Embodiment 2
Please refer to Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5, the present invention provides a kind of technical solution: a kind of EFG technique grows big ruler
The system and method for very little sapphire single-crystal plate, by heater 1, thermal insulation material 2, mold 3, crucible 4, ejection channel 8, seed crystal liter
Descending mechanism 5 and raw material ejection mechanism 9 form, and mold 3 is provided with multiple, and raw material ejection mechanism 9 and raw material cabin 11 pass through conveyer
Structure 10 is connected, and granular high purity aluminium oxide raw material is placed in raw material cabin 11, and conveying mechanism 10 uses the principle of vibrating transportation,
The rate that the raw material of raw material cabin 11 clicks is transported in raw material ejection mechanism 9, there is a spring-in raw material ejection mechanism 9
Cam ejection mechanism, the alumina raw material that can will be delivered to ejection mechanism launch upwards in time, and there is hole in 4 center of crucible, by molybdenum
Material is process, and cylindrical structure can usually be processed using economic rotary pressing processing mode, and ejection channel 8 is placed in hole center
Trunk portion, there is at the top of ejection channel 8 raw material rebounding device, have granular feedstock rebound to the ability inside crucible 4,
Ejection channel 8 includes main channel 24, main channel insulating layer 23, lower reflection cone 22, upper reflection cone 21 and support column 26, wherein main logical
The material in road 24 is molybdenum, and the material of main channel insulating layer 23 is the hard felt of graphite, lower reflection cone 22, support column 26 and upper reflection cone 21
Material be tungsten, kinetic energy absorption material 12 is also placed with inside crucible 4, kinetic energy absorption material passes through three-dimensional by molybdenum filament and tungsten wire
It weaves, the diameter of molybdenum filament and tungsten wire is 0.2-2mm, and when temperature is raised to 1800 degree or more, molybdenum filament will soften, and lose bullet
Property, and the gap between molybdenum filament and molybdenum filament can be still in kinetic energy absorption material after the multiple rebound when alumina raw material falls
On material, the overall stability of kinetic energy absorption material at high temperature is can be improved in the addition of tungsten wire.
In the present embodiment, it is preferred that mold 3 and crucible 4 are process by tungsten or molybdenum material, help to increase mold 3
With the stability of crucible 4.
In the present embodiment, it is preferred that the hollow structural members and be wrapped in hollow that ejection channel 8 is processed by graphite, tungsten or molybdenum
Thermal insulation material composition outside structural member, facilitates the heat preservation of ejection channel 8.
In the present embodiment, it is preferred that thermal insulation material is the hard felt of graphite or graphite soft felt, facilitates thermal insulation material operation.
In the present embodiment, it is preferred that raw material rebounding device is the taper or wedge structural member of graphite, tungsten or molybdenum processing, is had
Help improve the performance of raw material rebounding device.
In the present embodiment, it is preferred that kinetic energy absorption material is the tungsten wire or molybdenum filament composition of reticular structure, facilitates kinetic energy suction
Receive the operation of material.
A kind of method of EFG technique growing large-size sapphire single-crystal plate, includes the following steps:
Step 1: being heated by heater 1 and crucible 4 heat up, and by internal melting sources；
Step 2: decline seed crystal elevating mechanism 5, make two seed crystals on seed crystal elevating mechanism 5 respectively with two 3 tables of mold
Face is in contact；
Step 3: after seed portion fusing, seed crystal is lifted by seed crystal elevating mechanism 5 upwards, while appropriate cooling makes mould
The liquid film for having 3 surfaces crystallizes into monocrystalline in seed crystal face；Melt 7 in crucible 4 rises to mould by 3 internal capillary pathway of mold
Have 3 surfaces and supplements the liquid film being solidified；
Step 4: according to the speed of crystallization, the alumina granules of corresponding weight is launched upwards by raw material ejection mechanism 9
Raw material, the raw material launched are rebounded by the raw material rebounding device at 8 top of ejection channel to inside crucible 4；
Step 5: the particulate material into crucible 4 drops on kinetic energy absorption material 12, and crucible 4 is fusing into after being heated,
The oxidation aluminum melt being consumed is supplemented, 7 liquid level of melt is made to keep stablizing；
Step 6: the lasting lifting of seed crystal elevating mechanism 5, since lasting ejection feeds, this process will not be by 7 liquid level of melt
Decline and interrupt, until growing large-scale sapphire single-crystal plate.
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 (7)
1. a kind of system of EFG technique growing large-size sapphire single-crystal plate, which is characterized in that by heater (1), thermal insulating material
Expect (2), mold (3), crucible (4), ejection channel (8), seed crystal elevating mechanism (5) and raw material ejection mechanism (9) composition, the mould
Tool (3) is provided with multiple, and crucible (4) center offers hole, and the central location in the hole is placed with the trunk of ejection channel (8)
Part, the raw material ejection mechanism (9) are located at the bottom of crucible (4), for that will launch feed particulate material to higher than crucible (4)
Upper edge is provided at the top of the ejection channel (8) for granular feedstock rebound to rebound to the internal raw material of crucible crucible (4)
Device, the crucible (4) is interior to be placed with kinetic energy absorption material.
2. a kind of system of EFG technique growing large-size sapphire single-crystal plate according to claim 1, it is characterised in that:
The mold (3) and crucible (4) are process by tungsten or molybdenum material.
3. a kind of system of EFG technique growing large-size sapphire single-crystal plate according to claim 1, it is characterised in that:
Ejection channel (8) hollow structural members processed by graphite, tungsten or molybdenum and the thermal insulation material being wrapped in outside hollow structural members
Composition.
4. a kind of system of EFG technique growing large-size sapphire single-crystal plate according to claim 3, it is characterised in that:
The thermal insulation material is the hard felt of graphite or graphite soft felt.
5. a kind of system of EFG technique growing large-size sapphire single-crystal plate according to claim 1, it is characterised in that:
The raw material rebounding device is the taper or wedge structural member of graphite, tungsten or molybdenum processing.
6. a kind of system of EFG technique growing large-size sapphire single-crystal plate according to claim 1, it is characterised in that:
The kinetic energy absorption material is the tungsten wire or molybdenum filament composition of reticular structure.
7. a kind of method of EFG technique growing large-size sapphire single-crystal plate according to claim 1-6,
It is characterized in that, includes the following steps:
Step 1: being heated up crucible (4) by heater (1) heating, and by internal melting sources；
Step 2: decline seed crystal elevating mechanism (5), make two seed crystals on seed crystal elevating mechanism (5) respectively with two molds (3)
Surface is in contact；
Step 3: after seed portion fusing, seed crystal is lifted by seed crystal elevating mechanism (5) upwards, while appropriate cooling makes mold
(3) liquid film on surface crystallizes into monocrystalline in seed crystal face；Melt (7) in crucible (4) passes through on mold (3) internal capillary pathway
It is raised to mold (3) surface and supplements the liquid film being solidified；
Step 4: according to the speed of crystallization, the alumina granules for launching corresponding weight upwards by raw material ejection mechanism (9) is former
Material, the raw material launched are internal to crucible (4) by the raw material rebounding device rebound at the top of ejection channel (8)；
Step 5: the particulate material for entering crucible (4) drops on kinetic energy absorption material (12), is fusing into crucible after being heated
(4), the oxidation aluminum melt being consumed is supplemented, melt (7) liquid level is made to keep stablizing；
Step 6: the lasting lifting of seed crystal elevating mechanism (5), since lasting ejection feeds, this process will not be by melt (7) liquid level
Decline and interrupt, until growing large-scale sapphire single-crystal plate.
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| CN201811314343.XA CN109234796A (en) | 2018-11-06 | 2018-11-06 | A kind of system and method for EFG technique growing large-size sapphire single-crystal plate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109811411A (en) * | 2019-03-26 | 2019-05-28 | 四川联合晶体新材料有限公司 | System and method that is a kind of while growing two blocks of large-size sapphire single-crystal plate |
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| CN203976973U (en) * | 2014-06-27 | 2014-12-03 | 江西豪安能源科技有限公司 | On a kind of quartz crucible stove, take out tubular type feeder |
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| CN108275867A (en) * | 2018-04-09 | 2018-07-13 | 江苏奥赛斯现代农业科技有限公司 | A kind of production of quartz tubes continuous smelting furnace feeder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109811411A (en) * | 2019-03-26 | 2019-05-28 | 四川联合晶体新材料有限公司 | System and method that is a kind of while growing two blocks of large-size sapphire single-crystal plate |
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Application publication date: 20190118 |