CN106702481B - A kind of improved multiple-piece EFG technique synthetic sapphire preparation process - Google Patents
A kind of improved multiple-piece EFG technique synthetic sapphire preparation process Download PDFInfo
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- CN106702481B CN106702481B CN201710166226.2A CN201710166226A CN106702481B CN 106702481 B CN106702481 B CN 106702481B CN 201710166226 A CN201710166226 A CN 201710166226A CN 106702481 B CN106702481 B CN 106702481B
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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
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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 present invention relates to a kind of improved multiple-piece EFG technique synthetic sapphire preparation processes.The present invention relates to sapphire processing technology fields, and in particular to a kind of guided mode processing method of flaky sapphire mainly includes step are as follows: (1) feedstock processing;(2) it clears up die-filling;(3) furnace body vacuumizes;(4) heat temperature raising;(5) seeding necking down;(6) expand shoulder;(7) isodiametric growth;(8) processes such as annealing cooling, are on the one hand effectively ensured the purity of growth flat crystal;It is protected by vacuumize process and argon gas, additionally it is possible to prevent other impurity in air from reacting with crucible or mold;On the other hand, so that technique of the invention is can be realized the production of multi-disc sapphire sheet body, improve the production efficiency of flaky sapphire;It is cracked in another aspect, can be avoided flat crystal, improves crystal quality;Temperature change caused by the heat dissipation of crucible can be effectively avoided to be distorted by the setting of graphite insulating layer, so that the accurate detection of crucible internal temperature is improved, so that convenient be precisely controlled melt temperature.
Description
Technical field
The present invention relates to sapphire processing technology fields, and in particular to a kind of improved multiple-piece EFG technique synthetic sapphire
Preparation process.
Background technique
Sapphire English name is Sapphire, is derived from Latin Spphins, means blue;Belong to corundum race mineral,
Trigonal system.Assorted Gem Grade corundum except ruby is referred to as sapphire by jewel circle.Sapphire and ruby, emerald
Jinsui River bodhi tourmaline, smooth Sang Shi etc. belong to colored gemstone category.
Because containing the microelements such as iron (Fe) and titanium (Ti) in corundum, and the colors such as blue, sky blue, pale blue are presented, wherein with
Bright-coloured sky blue person is best.Sapphire mineral name is corundum, belongs to corundum race mineral.Jewel actually in nature
For grade corundum in addition to red title ruby, remaining various colors is such as blue, light blue, green, yellow, grey, colourless, claims
For sapphire.Sapphire chemical component (Al2O3), mainly with Fe, Ti, coloring.
Sapphire ingredient is aluminium oxide, because of (the Ti containing Trace Element Titanium4+) or iron (Fe2+) and it is blue.Belong to three prismatic crystals
System.Crystal habit is often cylindrical in shape, short cylinder, plate etc., and solid is mostly granular or compact massive.It is clear to translucent, glass
Gloss.Index of refraction 1.76~1.77, birefringence 0.008, dichroism is strong.Heterogeneous body.Sometimes there is special optical effect-
Asterism.Hardness is 9,3.95~4.1 grams/cc of density.It is cut in cabochon, inside is rich in parallel with bottom surface and fixed
To arrangement three groups of backpack bodies when, when can produce beautiful six-pointed star, referred to as " starlight sapphire ".
Existing synthetic sapphire crystal guided mode processing technology is in specific production process, and there are the following problems: on the one hand, by
In feedstock processing is not clean enough and furnace body is cleared up not thorough enough, causes crystal guided mode processing quality to be affected, make crystals
There are impurity, reduce flat crystal purity;On the other hand, due to the influence of mold design, cause each guided mode pulling growth
Sapphire sheet body quantity is restricted, and existing EFG technique can only generally produce a piece of sapphire every time, and production efficiency is lower;Further
Aspect causes crystal production quality to decline, occurs being cracked or crystal dislocation is tight since the controlling of production process of flat crystal is improper
The deficiencies of weight;Simultaneously as the heat exchange of crucible influences, causes the crucible inner melt temperature error of detection larger, be unfavorable for
The temperature of sapphire crystal controls.
Therefore, based on above-mentioned, the present invention provides a kind of improved multiple-piece EFG technique synthetic sapphire preparation process, with solution
Certainly deficiency and defect that EFG technique of the existing technology production flat crystal limited amount, technique are difficult to control accurately.
Summary of the invention
The object of the invention is that: for presently, there are the above problem, a kind of improved multiple-piece EFG technique is provided
Synthetic sapphire preparation process, to solve, EFG technique of the existing technology produces flat crystal limited amount, technique is difficult to essence
The deficiency and defect really controlled.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of improved multiple-piece EFG technique synthetic sapphire preparation process, includes the following steps:
(1) feedstock processing: the alumina raw material of powdery is cleaned, and is placed in 1200 DEG C~1500 DEG C of crucible
3h is kept the temperature, and is cooled to room temperature under air environment, alumina raw material complete oxidation is made;
(2) it clears up die-filling: after furnace body impurity is cleaned out, the crucible for being loaded with powdery aluminum being placed in furnace body
Entreat position;Seed crystal column is mounted on lifting rod by tungsten wire winding, connecting rod then is set in seed crystal column lower part, in connecting rod
Both ends several seed rods are respectively set, seed rod lower end be arranged seed body, seed body lower end be arranged wedge structure wedge
Shape end;The length direction of tapered end and the length direction of moulding cavity are perpendicular;Before containing powdery aluminum raw material, in earthenware
Crucible bottom is provided with several partitions, and crucible bottom is separated out to the mounting groove to match with mold bottom;The mold is by several
The molybdenum sheet of sheet is composed, and mold is fixed by the way that molybdenum sheet insertion to be mounted in mounting groove;The crucible includes internal layer
Graphite insulating layer with being arranged in outside internal layer, can effectively improve the insulating efficiency of crucible, conducive to the accurate control of melt temperature
System and adjustment;
(3) furnace body vacuumizes: shutting vent valve and fire door, opens vacuum pump and vacuumize to furnace body inner cavity, make furnace interior
Air pressure be evacuated to -0.5~-0.1Pa, be then shut off vacuum pump, open argon gas valve, argon gas is full of to furnace chamber inside, until furnace
It until intracavitary portion's atmospheric pressure is restored to standard atmospheric pressure, and so on vacuumizes-applying argon gas circulation 2~3 times;
(4) heat temperature raising: heat temperature raising is carried out to furnace body, is warming up to temperature in furnace according to the speed of 10 DEG C/min
1500 DEG C, then the heating rate according still further to 25 DEG C/min rises to 2080 DEG C;
(5) seeding necking down: the intermediate frequency power supply of furnace body being switched and is opened, and carries out furnace body heating heating;It is completely melt to raw material
Later, seed crystal is mounted on lifting rod, is moved down at a slow speed, the bottom end for making seed crystal and mould upper surface are at a distance of 5mm~6mm;
Seed crystal is carried out preheating 2~3 times, makes the sheet-like melt and the abundant welding of seed crystal positioned at die surface, forms an entirety;Then
Crystal is lifted up at a slow speed, when crystal range of lift mould upper surface 20mm~30mm, increase heating power, to chip into
Row necking down;The effect of necking down is: the genetic defect in seed crystal can be reduced, by necking down process, crystal it is any non axial
Dislocation can be by successive elimination;The temperature of necking process is excessively high, the easy rapid melting of seed crystal;Necking down temperature is too low, then can lead
Cause necking down effect unobvious;
(6) expand shoulder: after necking down, the upward pull rate of seed crystal being reduced, makes crystal along seed crystal between moulding cavity
Slowly growth upwards;
(7) isodiametric growth: after expansion shoulder terminates, improving pull rate, keeps temperature length constant, carries out to crystal
Isodiametric growth;During isodiametric growth, if pull rate is too fast, blister interface is easily formed, the half-cooked gas at trough is caused
Body causes to generate bubble in the wafer;
(8) annealing cooling: after isodiametric growth is completed, crystal is separated with crucible;Cooled down stage by stage;It is complete to crystal
After total detachment mold, stops lifting, turn off heating power supply, furnace body temperature is made to continue cool to room temperature;Finally by cooling crystalline substance
Body takes out.
On the one hand the technical solution of the application passes through the cleaning process of raw material and furnace body, can be avoided crystal growing process
In occur polluting or be mingled with, so that the purity of growth flat crystal be effectively ensured;It is protected by vacuumize process and argon gas, moreover it is possible to
Enough prevent other impurity in air from reacting with crucible or mold.
On the other hand, by the whole design to mold, user is handled by the raising and lowering lifting of lifting rod, can be with
Seed body is moved upwardly or downwardly by seed crystal column, connecting rod and seed rod;It is designed by the structure of multiple seed crystals body, makes this
The technique of invention can be realized the production of multi-disc sapphire sheet body, improve the production efficiency of flaky sapphire.
In another aspect, the technical solution of the application can be avoided flat crystal and tortoise occur by reasonably adjusting for technique
It splits, improves crystal quality;By the setting of graphite insulating layer, effectively kept the temperature conducive to the melt to crucible and its inside, from
And temperature change caused by the heat dissipation of crucible is effectively avoided to be distorted, so that the accurate detection of crucible internal temperature is improved, thus side
Just melt temperature is precisely controlled.
Preferably, the mold outer surface be smooth surface, be divided between forming between the adjacent molybdenum sheet of mold 0.3mm~
1mm, the thickness of molybdenum sheet and the width dimensions of mounting groove match, and install between molybdenum sheet and mounting groove for transition fit.
Preferably, the inner surface of the crucible is smooth surface, and the width dimensions and length dimension of crucible are respectively greater than institute
State the length and width size of mold;Crucible is prepared using molybdenum or iridium material, and crucible bottom surface is plane.
Preferably, the graphite insulating layer with a thickness of 2mm~3mm, be fixed between graphite insulating layer and the crucible
Paste connection.
Preferably, the shape of the seed crystal column is square column or circular columns;To be fixedly connected between seed crystal column and connecting rod,
Connecting rod and seed rod are connected as an overall structure.
Preferably, the seed body and the tapered end are connected as an entirety, and the wedge angle bottom end angle of tapered end is 20 °
~30 °.
By adopting the above-described technical solution, the beneficial effects of the present invention are:
1, on the one hand the technical solution of the application passes through the cleaning process of raw material and furnace body, can be avoided crystal growth mistake
Occur polluting or being mingled in journey, so that the purity of growth flat crystal be effectively ensured;It is protected by vacuumize process and argon gas, also
It can prevent other impurity in air from reacting with crucible or mold.
2, on the other hand, by the whole design to mold, user is handled by the raising and lowering lifting of lifting rod, can
Be moved upwardly or downwardly seed body by seed crystal column, connecting rod and seed rod;It is designed, is made by the structure of multiple seed crystals body
Technique of the invention can be realized the production of multi-disc sapphire sheet body, improve the production efficiency of flaky sapphire.
3, in another aspect, the technical solution of the application can be avoided flat crystal and tortoise occurs by reasonably adjusting for technique
It splits, improves crystal quality;By the setting of graphite insulating layer, effectively kept the temperature conducive to the melt to crucible and its inside, from
And temperature change caused by the heat dissipation of crucible is effectively avoided to be distorted, so that the accurate detection of crucible internal temperature is improved, thus side
Just melt temperature is precisely controlled.
Detailed description of the invention
Fig. 1 is process flow chart of the invention;
Fig. 2 is mold and long crucible structure schematic diagram of the invention;
Fig. 3 is crucible cross-sectional view of the invention;
Fig. 4 is crucible top view of the invention.
In figure: 1, crucible;2, mold;3, seed body;4, tapered end;5, seed rod;6, connecting rod;7, seed crystal column;8, stone
Black insulating layer;9, crucible;10, mounting groove;11, partition.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments, based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
Embodiment 1, as shown in Figs 1-4:
A kind of improved multiple-piece EFG technique synthetic sapphire preparation process, includes the following steps:
(1) feedstock processing: the alumina raw material of powdery is cleaned, and is placed on 1200 DEG C~1500 DEG C of crucible 1
Middle heat preservation 3h, and be cooled to room temperature under air environment, make alumina raw material complete oxidation;
(2) it clears up die-filling: after furnace body impurity is cleaned out, the crucible 1 for being loaded with powdery aluminum being placed in furnace body
Central location;Seed crystal column 7 is mounted on lifting rod by tungsten wire winding, connecting rod 6 then is set in 7 lower part of seed crystal column,
Several seed rods 5 are respectively set in the both ends of connecting rod 6, seed body 3 are arranged in the lower end of seed rod 5, wedge is arranged in 3 lower end of seed body
The tapered end 4 of shape structure;The length direction of tapered end 4 and the length direction in 2 gap of mold are perpendicular;Containing powdery aluminum
Before raw material, 1 bottom of crucible is provided with several partitions 11,1 bottom of crucible is separated out to the installation to match with 2 bottom of mold
Slot 10;The mold 2 is composed of the molybdenum sheet of several sheets, mold 2 by by molybdenum sheet insertion be mounted in mounting groove 10 into
Row is fixed;The crucible 1 includes internal layer 99 and the graphite insulating layer 8 being arranged in outside internal layer 99, can effectively improve crucible 1
Insulating efficiency, being precisely controlled and adjusting conducive to melt temperature;
(3) furnace body vacuumizes: shutting vent valve and fire door, opens vacuum pump and vacuumize to furnace body inner cavity, make furnace interior
Air pressure be evacuated to -0.5~-0.1Pa, be then shut off vacuum pump, open argon gas valve, argon gas is full of to furnace chamber inside, until furnace
It until intracavitary portion's atmospheric pressure is restored to standard atmospheric pressure, and so on vacuumizes-applying argon gas circulation 2~3 times;
(4) heat temperature raising: heat temperature raising is carried out to furnace body, is warming up to temperature in furnace according to the speed of 10 DEG C/min
1500 DEG C, then the heating rate according still further to 25 DEG C/min rises to 2080 DEG C;
(5) seeding necking down: the intermediate frequency power supply of furnace body being switched and is opened, and carries out furnace body heating heating;It is completely melt to raw material
Later, seed crystal is mounted on lifting rod, is moved down at a slow speed, the bottom end and 2 upper surface of mold for making seed crystal are at a distance of 5mm~6mm;
Seed crystal is carried out preheating 2~3 times, makes the sheet-like melt and the abundant welding of seed crystal positioned at 2 surface of mold, forms an entirety;So
Crystal is lifted up at a slow speed afterwards, when crystal range of lift 2 upper surface 20mm~30mm of mold, heating power is increased, to crystalline substance
Piece carries out necking down;The effect of necking down is: the genetic defect in seed crystal can be reduced, by necking down process, crystal it is any non-
Axial dislocation can be by successive elimination;The temperature of necking process is excessively high, the easy rapid melting of seed crystal;Necking down temperature is too low, then
It is unobvious to will lead to necking down effect;
(6) expand shoulder: after necking down, the upward pull rate of seed crystal being reduced, makes crystal along seed crystal between 2 gap of mold
Slowly growth upwards;
(7) isodiametric growth: after expansion shoulder terminates, improving pull rate, keeps temperature length constant, carries out to crystal
Isodiametric growth;During isodiametric growth, if pull rate is too fast, blister interface is easily formed, the half-cooked gas at trough is caused
Body causes to generate bubble in the wafer;
(8) annealing cooling: after isodiametric growth is completed, crystal is separated with crucible 1;Cooled down stage by stage;To crystal
After completely disengaging mold 2, stops lifting, turn off heating power supply, furnace body temperature is made to continue cool to room temperature;It finally will be cooling
Crystal takes out.
On the one hand the technical solution of the application passes through the cleaning process of raw material and furnace body, can be avoided crystal growing process
In occur polluting or be mingled with, so that the purity of growth flat crystal be effectively ensured;It is protected by vacuumize process and argon gas, moreover it is possible to
Enough prevent other impurity and crucible 1 or mold 2 in air from reacting.
On the other hand, by the whole design to mold 2, user is handled by the raising and lowering lifting of lifting rod, can
Be moved upwardly or downwardly seed body 3 by seed crystal column 7, connecting rod 6 and seed rod 5;It is set by the structure of multiple seed crystals body 3
Meter, makes technique of the invention can be realized the production of multi-disc sapphire sheet body, improves the production efficiency of flaky sapphire.
In another aspect, the technical solution of the application can be avoided flat crystal and tortoise occur by reasonably adjusting for technique
It splits, improves crystal quality;By the setting of graphite insulating layer 8, effectively kept the temperature conducive to the melt to crucible 1 and its inside,
To effectively avoid temperature change caused by the heat dissipation of crucible 1 from being distorted, so that the accurate detection of 1 internal temperature of crucible is improved, from
And conveniently melt temperature is precisely controlled.
As the preferred embodiment of the present embodiment, 2 outer surface of mold is smooth surface, forms the adjacent molybdenum sheet of mold 2
Between between be divided into 0.3mm~1mm, the width dimensions of the thickness and mounting groove 10 of molybdenum sheet match, molybdenum sheet and mounting groove
It is installed between 10 for transition fit.
As the preferred embodiment of the present embodiment, the inner surface of the crucible 1 is smooth surface, the width dimensions of crucible 1 and
Length dimension is respectively greater than the length and width size of the mold 2;Crucible 1 is prepared using molybdenum or iridium material, 1 bottom of crucible
Face is plane.
As the preferred embodiment of the present embodiment, the graphite insulating layer 8 with a thickness of 2mm~3mm, graphite insulating layer 8 with
It is that fixed paste connects between the crucible 1.
As the preferred embodiment of the present embodiment, the shape of the seed crystal column 7 is square column or circular columns;Seed crystal column 7 and company
To be fixedly connected between extension bar 6, connecting rod 6 and seed rod 5 are connected as an overall structure.
As the preferred embodiment of the present embodiment, the seed body 3 is connected as an entirety, tapered end 4 with the tapered end 4
Wedge angle bottom end angle be 20 °~30 °.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art within the technical scope of the present disclosure, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be subject to the protection scope in claims.
Claims (1)
1. a kind of improved multiple-piece EFG technique synthetic sapphire preparation process, characterized by the following steps:
(1) feedstock processing: the alumina raw material of powdery is cleaned, and is placed in 1200 DEG C~1500 DEG C of crucible and is kept the temperature
3h, and be cooled to room temperature under air environment, make alumina raw material complete oxidation;
(2) it clears up die-filling: after furnace body impurity is cleaned out, the crucible for being loaded with powdery aluminum being placed in furnace body center position
It sets;Seed crystal column is mounted on lifting rod by tungsten wire winding, connecting rod then is set in seed crystal column lower part, the two of connecting rod
Several seed rods are respectively set in end, seed body are arranged in the lower end of seed rod, the tapered end of wedge structure is arranged in seed body lower end;
The length direction of tapered end and the length direction of moulding cavity are perpendicular;Before containing powdery aluminum raw material, at crucible bottom
Portion is provided with several partitions, and crucible bottom is separated out to the mounting groove to match with mold bottom;The mold is by several sheets
Molybdenum sheet be composed, mold is by the way that molybdenum sheet insertion to be mounted in mounting groove and is fixed;The crucible include internal layer and
Graphite insulating layer outside internal layer is set, can be realized the raising of crucible heat insulation efficiency, conducive to being precisely controlled for melt temperature
And adjustment;
(3) furnace body vacuumizes: shutting vent valve and fire door, opens vacuum pump and vacuumize to furnace body inner cavity, make the gas of furnace interior
Pressure is evacuated to -0.5~-0.1Pa, is then shut off vacuum pump, opens argon gas valve, is full of argon gas to furnace chamber inside, until in furnace chamber
It until portion's atmospheric pressure is restored to standard atmospheric pressure, and so on vacuumizes-applying argon gas circulation 2~3 times;
(4) heat temperature raising: heat temperature raising is carried out to furnace body, temperature in furnace is made to be warming up to 1500 according to the speed of 10 DEG C/min
DEG C, then the heating rate according still further to 25 DEG C/min rises to 2080 DEG C;
(5) seeding necking down: the intermediate frequency power supply of furnace body being switched and is opened, and carries out furnace body heating heating;After being completely melt to raw material,
Seed crystal is mounted on lifting rod, is moved down at a slow speed, the bottom end for making seed crystal and mould upper surface are at a distance of 5mm~6mm;To seed crystal
It carries out preheating 2~3 times, makes the sheet-like melt and the abundant welding of seed crystal positioned at die surface, form an entirety;Then by crystal
It is lifted up at a slow speed, when crystal range of lift mould upper surface 20mm~30mm, increases heating power, contract to chip
Neck;The effect of necking down is: the genetic defect in seed crystal can be reduced, by necking down process, and any non axial position of crystal
Mistake can be by successive elimination;The temperature of necking process is excessively high, the easy rapid melting of seed crystal;Necking down temperature is too low, then will lead to contracting
Neck effect is unobvious;
(6) expand shoulder: after necking down, the upward pull rate of seed crystal being reduced, make crystal along seed crystal between moulding cavity upwards
Slowly growth;
(7) isodiametric growth: after expansion shoulder terminates, improving pull rate, keeps temperature-resistant, carries out isometrical life to crystal
It is long;During isodiametric growth, if pull rate is too fast, blister interface is easily formed, leads to the half-cooked gas at trough, causes
Bubble is generated in the wafer;
(8) annealing cooling: after isodiametric growth is completed, crystal is separated with crucible;Cooled down stage by stage;It is completely de- to crystal
After mold, stops lifting, turn off heating power supply, furnace body temperature is made to continue cool to room temperature;Finally cooling crystal is taken
Out;
The mold outer surface is smooth surface, and 0.3mm~1mm is divided between forming between the adjacent molybdenum sheet of mold, molybdenum sheet
The width dimensions of thickness and mounting groove match, and install between molybdenum sheet and mounting groove for transition fit;The crucible it is interior
Surface is smooth surface, and the width dimensions and length dimension of crucible are respectively greater than the length and width size of the mold;Crucible
It is prepared using molybdenum or iridium material, crucible bottom surface is plane;The graphite insulating layer with a thickness of 2mm~3mm, graphite heat preservation
It is that fixed paste connects between layer and the crucible;The shape of the seed crystal column is square column or circular columns;Seed crystal column with connect
To be fixedly connected between bar, connecting rod and seed rod are connected as an overall structure;The seed body is connect with the tapered end
For an entirety, the wedge angle bottom end angle of tapered end is 20 °~30 °.
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CN109989106A (en) * | 2017-12-31 | 2019-07-09 | 江苏拜尔特光电设备有限公司 | Dual rotary pulling apparatus and its switching method |
CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
CN109811411B (en) * | 2019-03-26 | 2021-10-08 | 四川联合晶体新材料有限公司 | System and method for simultaneously growing two large-size sapphire single crystal plates |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102333909A (en) * | 2008-12-30 | 2012-01-25 | Memc新加坡私人有限公司 | Methods and pulling assemblies for pulling a multicrystalline silicon ingot from a silicon melt |
CN102560630A (en) * | 2012-01-12 | 2012-07-11 | 徐州协鑫光电科技有限公司 | Thermal field capable of allowing synchronous growth of a plurality of crystals with edge-defined film-fed crystal growth technique and method thereof |
CN103060901A (en) * | 2013-02-05 | 2013-04-24 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
CN103696004A (en) * | 2014-01-07 | 2014-04-02 | 镇江和和蓝晶科技有限公司 | Mold for simultaneously growing multiple thin platy sapphires by edge-defined film-fed growth technique |
CN103849928A (en) * | 2014-03-19 | 2014-06-11 | 江苏苏博瑞光电设备科技有限公司 | Multiple-piece guided mode method growth technology for sapphire wafer |
-
2017
- 2017-03-20 CN CN201710166226.2A patent/CN106702481B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102333909A (en) * | 2008-12-30 | 2012-01-25 | Memc新加坡私人有限公司 | Methods and pulling assemblies for pulling a multicrystalline silicon ingot from a silicon melt |
CN102560630A (en) * | 2012-01-12 | 2012-07-11 | 徐州协鑫光电科技有限公司 | Thermal field capable of allowing synchronous growth of a plurality of crystals with edge-defined film-fed crystal growth technique and method thereof |
CN103060901A (en) * | 2013-02-05 | 2013-04-24 | 元亮科技有限公司 | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method |
CN103696004A (en) * | 2014-01-07 | 2014-04-02 | 镇江和和蓝晶科技有限公司 | Mold for simultaneously growing multiple thin platy sapphires by edge-defined film-fed growth technique |
CN103849928A (en) * | 2014-03-19 | 2014-06-11 | 江苏苏博瑞光电设备科技有限公司 | Multiple-piece guided mode method growth technology for sapphire wafer |
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