CN106854773A - A kind of crystal growing crucible, device and its growing method - Google Patents
A kind of crystal growing crucible, device and its growing method Download PDFInfo
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- CN106854773A CN106854773A CN201611243558.8A CN201611243558A CN106854773A CN 106854773 A CN106854773 A CN 106854773A CN 201611243558 A CN201611243558 A CN 201611243558A CN 106854773 A CN106854773 A CN 106854773A
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- crystal
- crucible
- heat exchanger
- heater
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/002—Crucibles or containers for supporting the melt
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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
- C30B15/10—Crucibles or containers for supporting the melt
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to technical field of crystal growth, specially a kind of crystal growing crucible, device and its growing method.A kind of crystal growing crucible, including crucible body, also including heat exchanger.Crucible body includes side wall, bottom wall and crucible cover, and side wall, bottom wall and crucible cover surround the crucible chamber that place is provided for crystal growth.Heat exchanger is arranged in crucible cover and stretches to crucible chamber, and one end that heat exchanger is stretched in crucible is provided with seed crystal.Heater is equipped with outside crucible body.Be combined for heat-exchanging method, kyropoulos and czochralski method and there is provided a kind of growing method of optimization by the present invention, and it can reduce matter crystal internal defect, reduces crystal cleavage probability and increase crystal yield.
Description
Technical field
The invention belongs to technical field of crystal growth, specially a kind of crystal growing crucible, device and its growing method.
Background technology
The growing method of crystal includes heat-exchanging method (HEM), kyropoulos (KY) and czochralski method (CZ).Heat-exchanging method principle
It is to take away heat using heat exchanger so that crystal growth forms the longitudinal temperature gradient of a cold lower part and hot upper part, while again by controlling
The size of gas flow and change the height of power and control thermograde in heat exchanger, thus reach crucible inner melt by
The crystal method a kind of long that crucible bottom seed crystal up grows.Its advantage is：The crystalline substance incipient stage long can seeding automatically, it is automated
Degree is high, is easily able to process consistency, while reducing the labour intensity and cost of seeding；And in crystal growing stage without physics
It is mobile, solid liquid interface stabilization.
Kyropoulos raw materials melt first, then the seed crystal and melt contacts that one is caught a cold, if the temperature at interface is less than solidifying
Solid point, then seed crystal start growth.In order that crystal is constantly grown up, it is necessary to gradually reduce the temperature of melt, while rotating crystal,
To improve the Temperature Distribution of melt.Lentamente (or by stages) crystal can also be above carried, to expand radiating surface.Crystal is in growth
During or growth at the end of do not contacted with sidewall of crucible, this greatly reduces the stress of crystal.Its advantage is：Crystal and crucible
Noncontact, final plane of crystal is Free Surface, and its interior pressure is small, not easy to crack；And crystal prevents earthenware with crucible noncontact
Core is given birth on crucible surface, is reduced crucible impurity and is introduced and matter crystal internal defect.
Czochralski method is that crystal raw material is positioned in crucible after side heater heats fusing, by what is clamped by seed rod
Seed crystal insertion bath surface is melted, while rotating seed crystal reversion crucible, seed crystal is slowly lifted up, by seeding, amplification,
The processes such as necking down, shouldering, isodiametric growth, ending finally give crystal.
But have the shortcomings that its is corresponding in traditional heat-exchanging method, kyropoulos and czochralski method, wherein heat-exchanging method is most
Big shortcoming just because crystal in fusion process with place crystal crucible contact, final plane of crystal be constrained surface,
Its interior pressure is big, easy to crack；And because crystal is contacted with crucible increases the probability that crucible surface life core impurity is introduced, increase brilliant
Body internal flaw.
The shortcoming of kyropoulos is to need seeding in the crystalline substance incipient stage long, and it is higher to the requirement of seeding qualification, and difficulty is accomplished
Process consistency；And crystal growing stage has physics to move, and solid liquid interface is easily disturbed, and solid liquid interface is unstable.
The shortcoming brilliant incipient stage long of czochralski method needs seeding, and it is higher to the requirement of seeding qualification, and difficulty accomplishes technique
Uniformity；Length brilliant each stage has mobile and rotates, and solid liquid interface is easily by disturbance without stabilization.
The content of the invention
It is an object of the invention to provide a kind of crystal growing crucible, for realizing the growth of crystal, and heat is may be implemented in
Czochralski method necking down is combined on the basis of exchange process, achievable matter crystal internal defect is few, crystal technique effect not easy to crack, and crucible
Can repeatedly be utilized.
What the present invention was realized in：
A kind of crystal growing crucible, including crucible body.Crystal growing crucible also includes the heat exchanger of fixed seed crystal.Earthenware
Crucible body includes side wall, bottom wall and crucible cover, and side wall, bottom wall and crucible cover surround the crucible chamber that place is provided for crystal growth.
The part for being provided with the heat exchanger of seed crystal stretches to crucible chamber through crucible cover, and heat exchanger alternatively away from or
Near the place motion of bottom wall.Be equipped with heater outside crucible body, heater include being located on the primary heater of side wall and
It is arranged on the secondary heater outside bottom wall.
Further, heat exchanger includes heat exchange unit and is provided with the fluid supply list of fluid flow control unit
Unit.One end of heat exchange unit is connected with fluid feeding unit, and the other end of heat exchange unit runs through crucible cover and stretches into crucible
It is indoor.
Further, heat exchange unit includes outer tube body and interior tube body, and interior tube body is arranged in outer tube body, outer tube body with it is interior
Heat exchanger channels are formed between body.Interior tube body offers the heat exchanging holes connected with heat exchanger channels.Interior tube body is arranged in outer tube body
Crucible cover simultaneously gos deep into crucible chamber.
Present invention also offers a kind of crystal growing apparatus based on above-mentioned crystal growing crucible.
A kind of crystal growing apparatus, including growth furnace and above-mentioned crystal growing crucible.Growth furnace includes body of heater and chamber,
Crucible is arranged in the chamber.Heat-insulation layer is provided between crucible and body of heater, heat exchanger is arranged in body of heater and insulation successively
Layer.
Further, heat exchanger passes through magnetic seal with body of heater.
Present invention also offers a kind of growing method of the crystal based on above-mentioned crystal growing apparatus, this method combines crystalline substance
The heat-exchanging method and czochralski method of body growth, solve the problems, such as crystal defect, realize the multiple utilization of crucible, and crystal is not easy to crack
Technique effect, the following is concrete technical scheme：
A kind of growing method based on above-mentioned crystal growing apparatus, comprises the following steps：
Fusing is placed in the crystal raw material in crucible chamber；
Seed crystal is contacted with the crystal raw material in molten state with preset direction, and make heat exchanger according to default rule
Being passed through cooling gas carries out heat exchange so that the crystal raw material solidification growth in molten state.And when crystal growth extremely
During preset value, necking down treatment, demoulding treatment are carried out to crystal successively.
Further, the method for fusing crystal raw material includes：
The crystal raw material in crucible chamber is heated by primary heater and secondary heater simultaneously.
Further, by seed crystal, contiguously method includes with the crystal raw material in molten state：
Seed crystal is arranged on the end that heat exchanger stretches into crucible chamber, mobile heat exchanger makes the crystalline substance of seed crystal and molten state
Body raw material surface contacts, and keeps the heating-up temperature of primary heater, secondary heater constant.
Further, it is passed through in cooling gas step according to default rule in heat exchanger, default rule is：
The intake of cooling gas increases with the increase of time.
Further, the method that crystal carries out demoulding treatment is included：
Keep the heating-up temperature of primary heater constant, while increase the heating-up temperature of secondary heater, and by heat exchange
Device is moved along default direction in the way of away from crucible, and the crystal and crucible for making growth are realized departing from.
The beneficial effect of such scheme：
It is the combination of crystal growth heat-exchanging method, kyropoulos and czochralski method the invention provides a kind of crystal growing crucible
Place is provided.The end of heat exchanger is provided with seed by the crucible by being arranged on the heat exchanger of crucible body upper end
Crystalline substance realizes the effect that heat exchanger is replaced with lifting rod, and heat exchanger is had lifting crystal growth and provide cooling
The effect of medium, realizes being combined for heat exchange hair and czochralski method.And by the heat heating being arranged on outside crucible body
Device makes crystal easily realize that demoulding is processed between crucible body bottom wall in growth course, and because crystal and crucible wall bottom
Portion is contactless, realizes and grows the technique effect that grain boundary defects are significantly reduced by crucible downside wall and bottom.Simultaneously final crystalline substance
Body is not easily susceptible to cracking.
Present invention also offers a kind of crystal growing apparatus, the device is based on crystal growing crucible, and outside crucible body
Portion is provided with heat-insulation layer, makes the temperature in crucible body not easy to lose, realizes the technique effect of the stabilization of crystal growing process.
Present invention also offers a kind of growing method, the method is based on crystal growing apparatus, by heat-exchanging method, bubble life
Method and czochralski method are combined and there is provided a kind of growing method of optimization, and it can reduce matter crystal internal defect, reduce brilliant
Body cracking probability and increase crystal yield.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be attached to what is used needed for embodiment
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, thus be not construed as it is right
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is crystal growing apparatus structural representation of the present invention；
Fig. 2 is crystal growing crucible structural representation of the present invention；
Knot after the sapphire crystal condensation that Fig. 3 is produced for the crystal growing apparatus and its method that are provided using the present invention
Structure schematic diagram；
Fig. 4 is structural representation after crystal condensation in the prior art；
The isollaothermic chart of the growing method that Fig. 5 is provided for the present invention.
Icon：100- crystal growing apparatus；200- crystal growing crucibles；300- Shaped crystals；300a- Shaped crystals；
400- seed crystals；500- thermoisopleths；110- growth furnaces；120- heat-insulation layers；130- control centres；210- crucible bodies；220- heat is handed over
Parallel operation；230- heating units；111- bodies of heater；112- chambers；131- display devices；211- crucible covers；212- crucible chambers；213- sides
Wall；214- bottom walls；221- fluid feeding units；222- fluid flow control units；223- heat exchange units；224- outer tube bodies；
225- interior tube bodies；226- heat exchanger channels；231- primary heaters；232- secondary heaters.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the present invention, rather than whole embodiments.Present invention implementation generally described and illustrated in accompanying drawing herein
The component of example can be arranged and designed with a variety of configurations.Therefore, reality of the invention below to providing in the accompanying drawings
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
It should be noted that：Similar label and letter represents similar terms in following accompanying drawing, therefore, once a certain Xiang Yi
It is defined in individual accompanying drawing, then it need not be further defined and explained in subsequent accompanying drawing.
In the description of the invention, it is necessary to explanation, term " " center ", " on ", D score, "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " interior ", " outward " be based on orientation shown in the drawings or position relationship, or should
Orientation or position relationship that invention product is usually put when using, are for only for ease of the description present invention and simplify description, without
Be indicate or imply meaning device or element must have specific orientation, with specific azimuth configuration and operation, therefore not
It is understood that to be limitation of the present invention.Additionally, term " first ", " second ", " the 3rd " etc. are only used for distinguishing description, and can not manage
Solve to indicate or implying relative importance.
In the description of the invention, in addition it is also necessary to explanation, unless otherwise clearly defined and limited, term " setting ",
" installation ", " connected ", " connection " should be interpreted broadly, for example, it may be fixedly connected, or be detachably connected, or one
The connection of body ground；Can mechanically connect, or electrically connect；Can be joined directly together, it is also possible to indirect by intermediary
It is connected, can is two connections of element internal.For the ordinary skill in the art, can be with concrete condition understanding
State term concrete meaning in the present invention.
Refering to Fig. 1, a kind of crystal growing apparatus 100 is present embodiments provided, the growth for realizing sapphire crystal.Bag
Include：Crystal growing crucible 200, growth furnace 110 and control centre 130.Set between crystal growing crucible 200 and growth furnace 110
It is equipped with heat-insulation layer 120.
Growth furnace 110 includes body of heater 111 and the chamber 112 being arranged in body of heater 111, and heat-insulation layer 120 is arranged on chamber
In 112.
Crystal growing crucible 200 includes the crucible body 210 being arranged in chamber 112, and crucible body 210 is built with crystal
Raw material.It is equipped with to be additionally provided with heating unit 230, crucible body 210 outside crucible body 210 and wears crucible body 210
Heat exchanger 220.In the present embodiment, heat exchanger 220 is also arranged in heat-insulation layer 120 and body of heater 111.
Connected by magnetic seal between heat exchanger 220 and body of heater 111, heat exchanger 220 is realized vertically moving.
Control centre 130 is connected with heat exchanger 220, heating unit 230, and display is additionally provided with control centre 130
Device 131, for parameter to be visualized.
The material of heat-insulation layer 120 can be refractory material.
Refering to Fig. 1, body of heater 111 is closed body of heater 111 in the present embodiment, spatially shape structure, in the present embodiment stove
Body 111 is ellipsoid, but body of heater 111 can also be other any three-dimensional knots such as square, cuboid in other embodiments
Structure.
Chamber 112 is the hollow-core construction that body of heater 111 is surrounded, and its shape facility is identical with body of heater 111, when body of heater 111 is ellipse
During circle, chamber 112 is similarly ellipsoid.When body of heater 111 is other stereochemical structures, such as when body of heater 111 is cuboid,
Chamber 112 is similarly cuboid.
Refering to Fig. 2, the upper end of crucible body 210 can open and be provided with crucible cover 211, and crucible also includes the He of side wall 213
The crucible chamber 212 that bottom wall 214 and side wall 213 are surrounded with bottom wall 214.Crucible chamber 212 is used to place crystal raw material, is crystal life
Place long, and heat exchanger 220 wears crucible body 210 and carries out longitudinal movement in the crucible chamber 212.Crucible chamber 212
It is the cavity structure of various stereochemical structures, can be with the identical stereochemical structure of chamber 112 of crystal growing apparatus 100, or
The stereochemical structure different from the chamber 112 of crystal growing apparatus 100.In the present embodiment, the structure of crucible chamber 212 is cylinder
Structure.
Heating unit 230 includes primary heater 231 and secondary heater 232, and the wherein ring of primary heater 231 is located at earthenware
Outside the side wall 213 of crucible body 210, secondary heater 232 is arranged on outside the bottom wall 214 of crucible body 210.Wherein primary heater
231 upper end exceedes the top of crucible cover 211, and the length of secondary heater 232 can be less than the diameter of bottom wall 214, also may be used
With the diameter more than bottom wall 214, can also be equal to bottom wall 214 diameter.In the present embodiment, the length of secondary heater 232
More than the diameter of bottom wall 214.
Referring to Fig. 2, heat exchanger 220 includes fluid feeding unit 221, the stream of connection fluid feeding unit 221
Body flow controlling unit 222, and connect flow control unit and be arranged in the heat exchange unit 223 of crucible chamber 212.
Heat exchange unit 223 includes interior tube body 225 and outer tube body 224, and interior tube body 225 is arranged in outer tube body 224, and interior
Cavity structure is formed between body 225 and outer tube body 224, cavity structure is heat exchanger channels 226.Interior tube body 225 is uniformly set
There are heat exchanging holes (not marked in figure), heat exchanging holes are connected with heat exchanger channels 226.Wherein one end of interior tube body 225 and fluid flow control
Unit processed 222 is connected, and the other end of outer tube body 224 and interior tube body 225 is all in crucible chamber 212, and outer tube body 224 is located in
One end in crucible chamber 212 is provided with seed crystal 400.In the present embodiment, interior tube body 225 and outer tube body 224 are along crucible chamber 212
Center line is configured.
Heat exchanger 220 can realize longitudinal movement, specially be capable of achieving interior tube body 225 and outer tube body 224 in crucible chamber
Longitudinal direction reciprocates in 212.
The fixation of seed crystal 400 and outer tube body 224 includes being fixedly connected and being detachably connected, be detachably connected including clamping,
The means such as the bonding of chemical means, are in the present embodiment being detachably connected for plug-in between seed crystal 400 and outer tube body 224.
Seed crystal 400 is completely attached to outer tube body 224 including seed crystal 400 with the contact relation of outer tube body 224, non-fully contacts and excessively connect
Touch, the cross-sectional area and the surface area phase of outer tube body 224 of the seed crystal 400 that the meaning of full contact is and the junction of outer tube body 224
Together；The meaning for non-fully contacting is that seed crystal 400 is less than the surface face of outer tube body 224 with the cross-sectional area of the junction of outer tube body 224
Product；The meaning of excessive contact is that seed crystal 400 is more than the surface area of outer tube body 224 with the cross-sectional area of the contact surface of outer tube body 224.
In the present embodiment, the contact relation between seed crystal 400 and outer tube body 224 is full contact.
The length of outer tube body 224 may be less than or equal to the length of interior tube body 225, and in the present embodiment, outer tube body 224 is less than
Interior tube body 225 it is identical.Heat exchanger channels 226 are used to be exchanged heat, and cooling gas are introduced into interior tube body 225, then by interior
The heat exchanging holes set on body 225 enter to heat exchanger channels 226 carries out heat exchange, is then exhausted from heat exchange unit 223.
A kind of crystal growing apparatus 100 that the present embodiment is provided, realizes the growth of crystal.Crucible chamber 212 is given birth to for crystal
Long to provide place, heating unit 230 is melted crystal raw material and is promoted the growth of crystal for providing high temperature.Heat exchanger
220 realize crystalloid solution of the seed crystal 400 with fusing in the state of crystal raw material is completely melt is in contact, and transmits heat exchange
Medium carries out the growth that cooling promotes crystal to the crystalloid solution for melting.Heat exchange medium can be various crystal growths of being not involved in
Gas, including various inert gases, in the present embodiment, heat exchange medium is helium.Heat exchanger 220 can also realize for
The lifting of crystal, makes crystal be grown upwards and perpendicular to the direction of thermoisopleth 500 to seed crystal 400.By control centre
130 for heat exchanger 220 and the precise control of heating unit 230, realize do not contacted between crystal and crucible body 210 from
And realize reducing the effect for being vigilant internal flaw, the reduction of necking process time is still realized, it has been finally reached crystal and has been difficult
The effect of cracking.
Referring to Fig. 1, crystal growing apparatus 100 can also be arranged as required to supporting control centre 130.Example
Such as, the control centre 130 of display device 131. is provided with control centre 130 to connect respectively with heating unit 230 and heat exchanger 220
Connect, for example, can make to be connected by communication cable by data, or be attached by Wireless Telecom Equipment.In the present embodiment
In, temperature sensor can be set in the inside of crucible chamber 212, wherein temperature sensor is connected with control centre 130.Temperature is passed
Sensor is used to realize the monitor in real time of temperature in crucible chamber 212.
The control terminal of the multiple equipment in crystal growing apparatus 100 is concentrated on into control centre 130, so that it is whole to improve its
The integrated level of body, while improving the convenience that control is made, is easy to be adjusted according to vigilant specific growing state, so as to improve crystalline substance
The quality of body.
A kind of crystal growing apparatus 100 that the present embodiment is provided, realizes the growth of high-quality crystal.Accomplished crystal with
Crystal growing crucible 200 is contacted so as to reduce the effect of matter crystal internal defect less.
All of unlatching and closed action are realized by being arranged on the control centre 130 of outside in the present embodiment
, control centre 130 is connected with each part, including primary heater 231, secondary heater 232.And in the present embodiment,
Since the difference of the position relationship between primary heater 231 and secondary heater 232, and effect has difference.Then first adds
Hot device 231 and the control mode of secondary heater 232 are because of the Bu Tong also different of position relationship.It is molten when heating is carried out in crystal raw material
During change, primary heater 231 is co- controlling with secondary heater 232.After fusing is heated in crystal growing process,
Primary heater 231 can need to be adjusted with secondary heater 232 according to temperature, and the mode of regulation controls first to add for independent
Hot device 231 and secondary heater 232, and make the power increase of secondary heater 232 more than the power of primary heater 231
Increase degree.
Present invention also offers a kind of growing method based on above-mentioned crystal growing apparatus 100, first by crystal raw material
Be placed on the center position in crucible chamber 212, specially crystal raw material mode at the medial center position of bottom wall 214, then
Seed crystal 400 is placed on the center position of one end that interior tube body 225 is not connected with other devices.Then crucible chamber 212 is entered
Row preheating, uses crystal raw material for raw material that purity is 99.99% in the present embodiment.
Preheating makes crystal raw material melt completely after terminating by strengthening the power of primary heater 231 and secondary heater 232
The power for changing and increasing primary heater 231 and secondary heater 232 keeps molten state.In the present embodiment, crucible chamber 212
Interior temperature is 2300 DEG C~2500 DEG C.
After being completely melt, one end that heat exchange unit 223 is provided with seed crystal 400 is longitudinally from top to bottom moved to crystal molten
The surface location of liquid, and turn-on flow rate feeding unit and fluid flow control unit 222 are passed through heat-exchange gas helium.In this reality
Apply in example, the intake of helium now is 34L/min.
The intake of helium is kept to keep constant, until by the diameter melt back of seed crystal 400 to 57~63mm.
Keep the power of primary heater 231 and secondary heater 232 constant, change helium gas flow.The change of helium gas flow
Turn to and increase to 50L/min to increase the speed of 1L/min per hour, then increased to increasing the speed of 2L/min per hour
80L/min.Refering to figure, at this moment crystal will realize seeding process along seed crystal 400 down and perpendicular to the growth of the direction of thermoisopleth 500.
When between crystal growth to 50%~60%, keep the power of secondary heater 232 constant and increase by first adds
The power of hot device 231, artificial necking down is carried out to crystal.
Then the intake for increasing helium makes crystal continue to grow up until crystal bottom touches bottom wall soon to 100L/min
Surveyed in 214.
Holding helium intake is constant, and when the 93%~97% of crystalline solidification ad pond om, heat exchanger 220 is with a constant speed
Degree is lifted up, while improving the power of secondary heater 232, keeps the power of primary heater 231 constant, makes whole crystal
With the inner side demoulding of 212 bottom wall of crucible chamber 214, final crystal growth terminate after enter annealing cool down, obtain full-grown crystal.
In the present embodiment, after success seeding, by controlling the internal cooling gas flow of heat exchanger 220, heat exchanger
220 rates of climb, melt temperature realize necking down jointly, reduce the internal flaw of seed crystal 400 and breed extension to crystals.Long brilliant
When mid-term, i.e. crystal growth are to 50%~60%, crystal and the relative position of crucible body 210 are kept, keep or reduce side heating
Device power, the raising internal cooling gas flow of heat exchanger 220 realize the isometrical stabilization growth of crystal.In the crystalline substance later stage long by control
The power of the rate of climb of heat exchanger 220 and bottom heater realizes the demoulding of bottom wall 214 of crystal and crucible body 210 jointly,
It is final to realize crystal and the Entirely contactless of crucible body 210.
The crystal that this method grows is contactless with the bottom of crucible wall 213, is grown by crucible wall 213 and bottom wall 214
Grain boundary defects are significantly reduced, and the defect of of seed crystal 400 itself is reduced due to the process of the necking down of the crystal method, while final crystalline substance
Body is completely attached to crucible wall 213, and it is easy to crack for crystal.
Below by way of the growing method that growth explanation the present embodiment of sapphire crystal is provided,
Sapphire crystal growth method specific embodiment of the present invention is as follows successively：
(1) center in 70kg high-purity mangesium oxide aluminum feedstocks are put into vacuum environment crucible chamber 212 as requested
Place；
(2) primary heater 231 and secondary heater 232 are constituted with tungsten metal；
(3) open primary heater 231 and secondary heater 232 is heated to crucible, through 24h or so, crucible chamber 212
Interior temperature reaches more than 2050 DEG C, and high-purity mangesium oxide aluminum feedstock is molten into pyrosol, and continues liter high-temperature to 2090 DEG C,
Keeping temperature is constant；
(4) heat exchanger 220 is gradually goed deep into chamber 112, and by outer tube body 224 and interior tube body 225 deeply to earthenware
One end that outer tube body 224 is provided with seed crystal 400 is contacted with high temperature crystal solution surface in crucible room 212, and open heat exchanger
The intake of 220 holding helium is 34L/min, by the diameter melt back of seed crystal 400 to 60mm；
(5) keep the power of primary heater 231 and secondary heater 232 constant, gradually increase helium intake, first with
The speed for increasing 1L/min per hour increases to 50L/min, then increases to 80L/min to increase the speed of 2L/min per hour,
Crystal is set down and perpendicular to the direction of thermoisopleth 500 to be grown along seed crystal 400；
(6) when crystal growth is to 50%~60%, keep the power of secondary heater 232 constant and increase primary heater
231 power, make crystal carry out artificial necking down；
(7) flow for increasing helium makes crystal continue to grow up until crystal bottom touches crucible bottom soon to 100L/min
Portion；
(8) holding helium intake is constant, and when the 95% of crystalline solidification ad pond om, heat exchanger 220 is with certain speed
It is lifted up, while improving the power of secondary heater 232, makes whole crystal and the crucible bottom demoulding；
(9) annealing cooling is carried out after crystal growth terminates and obtains final Shaped crystal 300.
Understood refering to Fig. 3 and Fig. 4, the side wall 213 in Shaped crystal 300 and crucible chamber 212 produced by the present invention
Do not contacted with bottom wall 214, minimize the defect of crystals.And the final shaping crystalline substance produced by traditional czochralski method
Body 300a is then in contact with side wall 213 and bottom wall 214 in crucible chamber 212, and this contact can cause the life of matter crystal internal defect
It is long, crystal is easily ftractureed.
Crystal growing apparatus 100, crystal growing crucible 200 and the growing method that the present embodiment is provided can be used to give birth to
The crystal of sizes long and type.For example, can be used to the larger sapphire crystal of growth size.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of crystal growing crucible, including crucible body, it is characterised in that the crystal growing crucible also includes fixed seed crystal
Heat exchanger；The crucible body includes side wall, bottom wall and crucible cover；The side wall, the bottom wall and the crucible cover enclose
The crucible chamber in place is provided as crystal growth；A part for the heat exchanger for the seed crystal is provided with through the earthenware
Crucible lid stretches to the crucible chamber, and the heat exchanger is alternatively moved in the place away from or near the bottom wall；It is described
Heater is equipped with outside crucible body, the heater includes being located on the primary heater of the side wall and is arranged on the bottom
Secondary heater outside wall.
2. crystal growing crucible according to claim 1, it is characterised in that the heat exchanger include heat exchange unit and
It is provided with the fluid feeding unit of fluid flow control unit；One end of the heat exchange unit connects with the fluid feeding unit
Connect, the other end of the heat exchange unit runs through the crucible cover and stretches into the crucible chamber.
3. crystal growing crucible according to claim 2, it is characterised in that the heat exchange unit includes outer tube body and inner tube
Body, said inner tube body is arranged in the outer tube body, and heat exchanger channels are formed between the outer tube body and said inner tube body；In described
Body offers the heat exchanging holes connected with the heat exchanger channels；Said inner tube body is arranged in the crucible cover simultaneously with the outer tube body
Deeply to the crucible chamber.
4. a kind of crystal growing apparatus, it is characterised in that given birth to crystal described in claims 1 to 3 any one including growth furnace
Crucible long；The growth furnace includes body of heater and chamber；The crucible is arranged in the chamber, the crucible and the body of heater it
Between be provided with heat-insulation layer, the heat exchanger is arranged in the body of heater and the heat-insulation layer successively.
5. crystal growing apparatus according to claim 4, it is characterised in that the heat exchanger passes through magnetic with the body of heater
Sealing.
6. a kind of growing method of the crystal growing apparatus based on described in claim 5, it is characterised in that including following step
Suddenly：
Fusing is placed in the crystal raw material in the crucible chamber；
The seed crystal is contacted with the crystal raw material of molten state with preset direction, and make the heat exchanger according to
Default rule is passed through cooling gas and is exchanged heat so that the crystal raw material solidification growth in molten state；And work as crystal
When growing to preset value, necking down treatment, demoulding treatment are carried out to crystal successively.
7. growing method according to claim 6, it is characterised in that the method for the fusing crystal raw material includes：
The crystal raw material in the crucible chamber is entered by the primary heater and the secondary heater simultaneously
Row heating.
8. growing method according to claim 6, it is characterised in that by the seed crystal and the institute in molten state
Contiguously method includes to state crystal raw material：
The seed crystal is arranged on the end that the heat exchanger stretches into the crucible chamber, the movement heat exchanger makes the seed
Crystalline substance is contacted with the crystal raw material surface of molten state, and keeps the primary heater, the heating of the secondary heater
Temperature is constant.
9. growing method according to claim 6, it is characterised in that logical according to default rule in the heat exchanger
Enter in cooling gas step, the default rule is：
The intake of the cooling gas increases with the increase of time.
10. growing method according to claim 7, it is characterised in that
The method that the crystal carries out demoulding treatment is included：
Keep the heating-up temperature of the primary heater constant, while increase the heating-up temperature of the secondary heater, and by institute
State heat exchanger to be moved in the way of away from the crucible along the default direction, make the crystal of growth and the crucible
Realize departing from.
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Address after: Figure 028000 Town Industrial Park Tongliao city the Inner Mongolia Autonomous Region Muli Horqin district Patentee after: Tongliao Seiko Sapphire Co., Ltd. Address before: Figure 028000 Town Industrial Park Tongliao city the Inner Mongolia Autonomous Region Muli Horqin district Patentee before: Bourne smile sapphire Co., Ltd. |
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