CN106854773B - 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
- Publication number
- CN106854773B CN106854773B CN201611243558.8A CN201611243558A CN106854773B CN 106854773 B CN106854773 B CN 106854773B CN 201611243558 A CN201611243558 A CN 201611243558A CN 106854773 B CN106854773 B CN 106854773B
- Authority
- CN
- China
- Prior art keywords
- crystal
- crucible
- heat exchanger
- growing
- tube body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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 further include heat exchanger.Crucible body includes side wall, bottom wall and crucible cover, and side wall, bottom wall and crucible cover, which surround, provides the crucible chamber in place for crystal growth.Heat exchanger is arranged in crucible cover and stretches to crucible chamber, and one end that heat exchanger stretches in crucible is provided with seed crystal.Heater is equipped with outside crucible body.Heat-exchanging method, kyropoulos and czochralski method are combined and are provided a kind of growing method of optimization by the present invention, be can be reduced matter crystal internal defect, reduce crystal cleavage probability and are increased 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 technique
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 in heat exchanger and control temperature gradient, thus reach crucible inner melt by
A kind of long crystal method that crucible bottom seed crystal is up grown.Its advantage are as follows: the long crystalline substance incipient stage can automatic seeding, automation
Degree is high, is easily able to process consistency, while reducing the labor intensity and cost of seeding；And in crystal growing stage without physics
Mobile, solid liquid interface is stablized.
Kyropoulos raw material first melts, then seed crystal and melt contacts that one is cooled, if the temperature at interface is lower than solidifying
Solid point, then seed crystal starts to grow.In order to make crystal constantly grow up, it is necessary to the temperature of melt, while rotating crystal are gradually decreased,
To improve the Temperature Distribution of melt.Crystal above slowly (or by stages) can also be mentioned, to expand radiating surface.Crystal is being grown
It is not contacted in the process or at the end of growth with sidewall of crucible, this greatly reduces the stress of crystal.Its advantage are as follows: crystal and crucible
Non-contact, final plane of crystal is Free Surface, and interior pressure is small, not easy to crack；And crystal with crucible is non-contact prevents earthenware
Core is given birth on crucible surface, reduces the introducing of crucible impurity and matter crystal internal defect.
Czochralski method be crystal raw material is placed in crucible by side heater heating fusing after, by what is clamped by seed rod
Seed crystal insertion bath surface is melted, while rotating seed crystal reversion crucible, and seed crystal is slowly lifted up, by seeding, amplification,
The processes such as necking down, shouldering, isodiametric growth, ending finally obtain crystal.
But have its corresponding disadvantage in traditional heat-exchanging method, kyropoulos and czochralski method, wherein heat-exchanging method is most
Big disadvantage is exactly because crystal contacts in fusion process with placement crystal crucible, and final plane of crystal is constrained surface,
Its interior pressure is big, easy to crack；And because crystal is contacted with crucible increases the probability that the raw core impurity of crucible surface introduces, increase brilliant
Body internal flaw.
The shortcomings that kyropoulos is to need seeding in the long brilliant incipient stage, and more demanding to seeding qualification, difficulty is accomplished
Process consistency；And crystal growing stage has physics mobile, and for solid liquid interface vulnerable to disturbance, solid liquid interface is unstable.
The shortcomings that czochralski method long brilliant incipient stage needs seeding, and more demanding to seeding qualification, difficulty accomplishes technique
Consistency；Long brilliant each stage has mobile and rotation, solid liquid interface unstable vulnerable to disturbance.
Summary of the invention
The purpose of the present invention is to provide a kind of crystal growing crucibles, for realizing the growth of crystal, and may be implemented in heat
Combine czochralski method necking down, it can be achieved that matter crystal internal defect is few on the basis of exchange process, crystal technical effect not easy to crack, and crucible
It can repeatedly be utilized.
The present invention is implemented as follows:
A kind of crystal growing crucible, including crucible body.Crystal growing crucible further includes the heat exchanger of fixed seed crystal.Earthenware
Crucible ontology includes side wall, bottom wall and crucible cover, and side wall, bottom wall and crucible cover, which surround, provides the crucible chamber in place for crystal growth.
Heat exchanger includes heat exchange unit and the fluid supply unit for being provided with fluid flow control unit；One end of heat exchange unit
It is connect with fluid supply unit, the other end of heat exchange unit through crucible cover and protrudes into crucible chamber, and heat exchanger is optional
Ground is in the place movement far from or close to bottom wall.It is equipped with heater outside crucible body, heater includes be located on side wall the
One heater and the secondary heater being arranged in outside bottom wall.
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 tube body.Interior tube body offers the heat exchanging holes being connected to heat exchanger channels.Interior tube body is arranged in outer tube body
Crucible cover simultaneously gos deep into crucible chamber.
The present invention also provides 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 furnace body and chamber,
Crucible is set in the chamber.Insulating layer is provided between crucible and furnace body, heat exchanger is successively arranged in furnace body and heat preservation
Layer.
Further, heat exchanger and furnace body pass through magnetic seal.
The present invention also provides a kind of growing method of crystal based on above-mentioned crystal growing crucible, 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, crystal is not easy to crack
Technical effect, be specific technical solution below:
A kind of growing method based on above-mentioned crystal growing crucible, comprising the following steps:
Fusing is placed in the indoor crystal raw material of crucible；
It contacts seed crystal with the crystal raw material in molten state with preset direction, and makes heat exchanger according to default rule
It is passed through cooling gas and carries out heat exchange so that the crystal raw material solidification growth in molten state.And work as crystal growth extremely
When preset value, necking down processing successively is carried out to crystal, demoulding is handled.
Further, the method for melting crystal raw material includes:
It is heated simultaneously by primary heater and secondary heater in the indoor crystal raw material of crucible.
Further, by seed crystal, contiguously method includes: with the crystal raw material in molten state
The end that heat exchanger protrudes into crucible chamber is arranged in seed crystal, mobile heat exchanger makes the crystalline substance of seed crystal and molten state
Body stock chart face contact, and keep primary heater, the heating temperature of secondary heater constant.
Further, it is passed through in cooling gas step in heat exchanger according to default rule, presets rule are as follows:
The increase at any time of the intake of cooling gas and increase.
Further, to crystal carry out demoulding processing method include:
It keeps the heating temperature of primary heater constant, while increasing the heating temperature of secondary heater, and by heat exchange
Device moves in a manner of far from crucible along preset direction, realizes the crystal of growth and crucible and is detached from.
Above scheme the utility model has the advantages that
The present invention provides a kind of crystal growing crucibles, are the combination of crystal growth heat-exchanging method, kyropoulos and czochralski method
Place is provided.The crucible passes through the heat exchanger that crucible body upper end is arranged in, and the end of heat exchanger is provided with seed
Crystalline substance realizes the effect that heat exchanger is replaced with to lifting rod, and so that heat exchanger is had lifting crystal growth and provide cooling
The effect of medium realizes combining for heat exchange hair and czochralski method.And by the way that the heat heating outside crucible body is arranged in
Device makes the crystal demoulding processing easy to accomplish between crucible body bottom wall during the growth process, and because crystal and crucible wall bottom
Portion is contactless, realizes and grows the technical effect that grain boundary defects significantly reduce by crucible downside wall and bottom.Crystalline substance final simultaneously
Body is not easily susceptible to cracking.
The present invention also provides a kind of crystal growing apparatus, which is based on crystal growing crucible, and outside crucible body
Portion is provided with insulating layer, keeps the temperature in crucible body not easy to lose, realizes the stable technical effect of crystal growing process.
The present invention also provides a kind of growing method, this method is based on crystal growing apparatus, and heat-exchanging method, bubble are given birth to
Method and czochralski method are combined and provide a kind of growing method of optimization, can be reduced matter crystal internal defect, reduce crystalline substance
Body cracking probability and increase crystal yield.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is crystal growing apparatus structural schematic diagram of the present invention；
Fig. 2 is crystal growing crucible structural schematic diagram of the present invention；
Fig. 3 is the knot after the sapphire crystal condensation produced using crystal growing apparatus provided by the invention and its method
Structure schematic diagram；
Fig. 4 is structural schematic diagram after crystal condensation in the prior art；
Fig. 5 is the isollaothermic chart of growing method provided by the invention.
Icon: 100- crystal growing apparatus；200- crystal growing crucible；300- Shaped crystal；300a- Shaped crystal；
400- seed crystal；500- thermoisopleth；110- growth furnace；120- insulating layer；130- control centre；210- crucible body；220- heat is handed over
Parallel operation；230- heating unit；111- furnace body；112- chamber；131- display device；211- crucible cover；212- crucible chamber；The side 213-
Wall；214- bottom wall；221- fluid supply unit；222- fluid flow control unit；223- heat exchange unit；224- outer tube body；
225- interior tube body；226- heat exchanger channels；231- primary heater；232- secondary heater.
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.The present invention being usually described and illustrated herein in the accompanying drawings is implemented
The component of example can be arranged and be designed with a variety of different configurations.Therefore, below to the reality of the invention provided in the accompanying drawings
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, 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.
It should also be noted that similar label and letter indicate similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined in a attached drawing, does not then need that it is further defined and explained in subsequent attached drawing.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, or be somebody's turn to do
Invention product using when the orientation or positional relationship usually put, be merely for convenience of description of the present invention and simplification of the description, without
It is that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore not
It can be interpreted as limitation of the present invention.In addition, term " first ", " second ", " third " etc. are only used for distinguishing description, and cannot manage
Solution is indication or suggestion relative importance.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, term " setting ",
" installation ", " connected ", " connection " shall be understood in a broad sense, for example, it may be fixedly connected, may be a detachable connection or one
Connect to body；It can be mechanical connection, be also possible to be electrically connected；It can be directly connected, it can also be indirect by intermediary
It is connected, can be the connection inside two elements.For the ordinary skill in the art, on being understood with concrete condition
State the concrete meaning of term in the present invention.
Refering to fig. 1, a kind of crystal growing apparatus 100 is present embodiments provided, for realizing the growth of sapphire crystal.Packet
It includes: crystal growing crucible 200, growth furnace 110 and control centre 130.It is set between crystal growing crucible 200 and growth furnace 110
It is equipped with insulating layer 120.
Growth furnace 110 includes furnace body 111 and the chamber 112 being arranged in furnace body 111, and insulating layer 120 is arranged in chamber
In 112.
Crystal growing crucible 200 includes the crucible body 210 being arranged in chamber 112, and crucible body 210 is provided with crystal
Raw material.It is equipped with heating unit 230 in 210 external rings of crucible body, is additionally provided in crucible body 210 and wears crucible body 210
Heat exchanger 220.In the present embodiment, heat exchanger 220 is also arranged in insulating layer 120 and furnace body 111.
It is connected between heat exchanger 220 and furnace body 111 by magnetic seal, heat exchanger 220 realizes longitudinal movement.
Control centre 130 connect with heat exchanger 220, heating unit 230, and display is additionally provided in control centre 130
Device 131, for visualizing parameter.
120 material of insulating layer can be refractory material.
Refering to fig. 1, furnace body 111 is closed furnace body 111 in the present embodiment, spatially shape structure, in the present embodiment furnace
Body 111 is ellipsoid, but other any three-dimensional knots such as furnace body 111 or square, cuboid in other embodiments
Structure.
Chamber 112 is the hollow structure that furnace body 111 surrounds, and shape feature is identical as furnace body 111, when furnace body 111 is ellipse
When circle, chamber 112 is similarly ellipsoid.When furnace body 111 is other stereochemical structures, such as when furnace body 111 is cuboid,
Chamber 112 is similarly cuboid.
Referring to Fig.2, the upper end of crucible body 210 is openable to be provided with crucible cover 211, crucible further includes having 213 He of side wall
The crucible chamber 212 that bottom wall 214 and side wall 213 and bottom wall 214 surround.Crucible chamber 212 is raw for crystal for placing crystal raw material
Long place, and heat exchanger 220 wears crucible body 210 and carries out longitudinal movement in crucible chamber 212.Crucible chamber 212
It, can stereochemical structure identical with the chamber 112 of crystal growing apparatus 100 for the cavity structure of a variety of stereochemical structures, 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 cylindrical body
Structure.
Heating unit 230 includes primary heater 231 and secondary heater 232, and wherein 231 ring of primary heater is located at earthenware
Outside the side wall 213 of crucible ontology 210, secondary heater 232 is arranged in outside the bottom wall 214 of crucible body 210.Wherein primary heater
231 upper end is more than the top of crucible cover 211, the length of secondary heater 232 can be less than bottom wall 214 diameter, can also
To be greater than the diameter of bottom wall 214, the diameter of bottom wall 214 can also be equal to.In the present embodiment, the length of secondary heater 232
Greater than the diameter of bottom wall 214.
Referring to Fig. 2, heat exchanger 220 includes fluid supply unit 221, the stream for being connected to fluid supply unit 221
Body flow controlling unit 222, and be connected to 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 tube body 225 and outer tube body 224, cavity structure is heat exchanger channels 226.Interior tube body 225 is uniformly arranged
There is heat exchanging holes (not marking in figure), heat exchanging holes are connected to heat exchanger channels 226.Wherein one end of interior tube body 225 and fluid flow control
Unit 222 processed connects, and the other end of outer tube body 224 and interior tube body 225 is all set in crucible chamber 212, and outer tube body 224 is threaded through
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, and interior tube body 225 and outer tube body 224 specially can be achieved in crucible chamber
Longitudinal round-trip in 212.
Seed crystal 400 and the fixation of outer tube body 224 include being fixedly connected and being detachably connected, be detachably connected including clamping,
The means such as the bonding of chemical means are being detachably connected for plug-in between seed crystal 400 and outer tube body 224 in the present embodiment.
Seed crystal 400 and the contact relation of outer tube body 224 include that seed crystal 400 is completely attached to outer tube body 224, non-fully contacts and excessively connect
Touching, the cross-sectional area and 224 surface area phase of outer tube body of the seed crystal 400 that the meaning of full contact is and 224 junction of outer tube body
Together；The meaning non-fully contacted is that seed crystal 400 and the cross-sectional area of 224 junction of outer tube body are less than 224 surface face of outer tube body
Product；The meaning of excessive contact is that seed crystal 400 and the cross-sectional area of 224 contact surface of outer tube body are greater than 224 surface area of outer tube body.
In the present embodiment, the contact relation between seed crystal 400 and outer tube body 224 is to completely attach to.
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.For exchanging heat, cooling gas is introduced into interior tube body 225, then by interior heat exchanger channels 226
The heat exchanging holes being arranged on tube body 225 enter to heat exchanger channels 226 and carry out heat exchange, are then exhausted from heat exchange unit 223.
A kind of crystal growing apparatus 100 provided in this embodiment, realizes the growth of crystal.Crucible chamber 212 is raw for crystal
Long to provide place, heating unit 230 melts crystal raw material and promotes the growth of crystal for providing high temperature.Heat exchanger
220, which realize seed crystal 400, is in contact in the state that crystal raw material is completely melt with the crystalloid solution of fusing, and transmits heat exchange
Medium carries out the cooling growth for promoting crystal to the crystalloid solution of fusing.Heat exchange medium can be a variety of crystal growths of being not involved in
Gas, including a variety of inert gases, in the present embodiment, heat exchange medium is helium.Heat exchanger 220 can also realize for
The lifting of crystal keeps crystal upward to seed crystal 400 and is grown perpendicular to the direction of thermoisopleth 500.Pass through control centre
The 130 accurate control for heat exchanger 220 and heating unit 230, realize do not contacted between crystal and crucible body 210 from
And realize the effect for reducing vigilant internal flaw, the reduction of necking process time is still realized, crystal has been finally reached and has been not easy
The effect of cracking.
Referring to Fig. 1, matched control centre 130 can also be set as needed in crystal growing apparatus 100.Example
Such as, 131. control centre 130 of display device is provided in control centre 130 to connect respectively with heating unit 230 and heat exchanger 220
It connects, such as can make to connect by data by communication cable, or equipment is attached by wireless communication.In the present embodiment
In, temperature sensor can be set in the inside of crucible chamber 212, wherein temperature sensor is connect with control centre 130.Temperature passes
Sensor for realizing temperature in crucible chamber 212 real time monitoring.
The controlling terminal of 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 the convenience that control is made is improved, convenient for being adjusted according to vigilant specific growing state, to improve crystalline substance
The quality of body.
A kind of crystal growing apparatus 100 provided in this embodiment, realizes the growth of high-quality crystal.Accomplished crystal with
Crystal growing crucible 200 contacts to reduce the effect of matter crystal internal defect less.
All unlatchings and closed action are realized by the way that external control centre 130 is arranged in the present embodiment
, control centre 130 is connected with each component, including primary heater 231, secondary heater 232.And in the present embodiment,
Because the difference of the positional relationship between primary heater 231 and secondary heater 232, and act on difference.Then first adds
Hot device 231 and 232 control mode of secondary heater are because of the Bu Tong also different of positional relationship.It is molten when carrying out heating in crystal raw material
During change, primary heater 231 and secondary heater 232 are co- controlling.After heating fusing in crystal growing process,
Primary heater 231 can need to be adjusted with secondary heater 232 according to temperature, and the mode of adjusting is that individually control first adds
Hot device 231 and secondary heater 232, and increase the power of secondary heater 232 by the power for being greater than primary heater 231
Increase degree.
The present invention also provides a kind of growing methods based on above-mentioned crystal growing apparatus 100, first by crystal raw material
The center position being placed in crucible chamber 212, specially crystal raw material mode are at 214 medial center position of bottom wall, then
Seed crystal 400 is placed on to the center position of one end that interior tube body 225 is not connect with other devices.Then to crucible chamber 212 into
Row preheats, and uses the raw material that crystal raw material is 99.99% for purity in the present embodiment.
Keep crystal raw material completely molten by the power of enhancing primary heater 231 and secondary heater 232 after preheating
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, it is molten that one end that heat exchange unit 223 is provided with seed crystal 400 is longitudinally from top to bottom moved to crystal
The surface location of liquid, and turn-on flow rate supply unit and fluid flow control unit 222 are passed through heat-exchange gas helium.In this reality
It applies in example, the intake of helium at this time is 34L/min.
The intake of helium is kept to remain unchanged, until by seed crystal 400 diameter melt back to 57~63mm.
It keeps the power of primary heater 231 and secondary heater 232 constant, changes helium gas flow.The change of helium gas flow
It turns to increase the rate of 1L/min per hour and increase to 50L/min, then is increased to increasing the rate of 2L/min per hour
80L/min.Refering to figure, at this moment crystal will be grown down and perpendicular to 500 direction of thermoisopleth along seed crystal 400, realize seeding process.
When between crystal growth to 50%~60%, keeps the power of secondary heater 232 constant and increase by first adds
The power of hot device 231 carries out artificial necking down to crystal.
Then the intake for increasing helium makes crystal continue to grow up until crystal bottom touches bottom wall fastly to 100L/min
It is surveyed in 214.
Keep helium intake constant, 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, is kept the power of primary heater 231 constant, is made entire crystal
It is demoulded on the inside of 212 bottom wall 214 of crucible chamber, annealing cooling is entered after final crystal growth, obtains full-grown crystal.
In the present embodiment, after success seeding, by controlling 220 inside cooling gas flow of heat exchanger, heat exchanger
220 rates of climb, melt temperature realize necking down jointly, reduce by 400 internal flaw of seed crystal to crystals and breed extension.Long brilliant
When mid-term, i.e. crystal growth are to 50%~60%, crystal and 210 relative position of crucible body are kept, keeps or reduce side heating
Device power improves the isometrical stable growth of 220 inside cooling gas flow of heat exchanger realization crystal.Pass through control in the long brilliant later period
The power of 220 rate of climb of heat exchanger and bottom heater realizes that the bottom wall 214 of crystal and crucible body 210 demoulds jointly,
It is final to realize crystal and 210 Entirely contactless of crucible body.
The crystal that this method is grown and 213 bottom of crucible wall are contactless, are grown by crucible wall 213 and bottom wall 214
Grain boundary defects significantly reduce, and the defect of seed crystal 400 itself is since the process of the necking down of the crystal method is reduced, while final crystalline substance
Body and crucible wall 213 completely attach to, it is easy to crack for crystal.
Growth below by way of sapphire crystal illustrates growing method provided in this embodiment,
Sapphire crystal growth method specific embodiment of the present invention is successively as follows:
(1) 70kg high-purity mangesium oxide aluminum feedstock is put into center in the crucible chamber 212 in vacuum environment as requested
Place；
(2) primary heater 231 and secondary heater 232 are formed with tungsten metal；
(3) it opens primary heater 231 and secondary heater 232 heats crucible, through left and right for 24 hours, crucible chamber 212
Interior temperature reaches 2050 DEG C or more, and high-purity mangesium oxide aluminum feedstock is molten into pyrosol, and continue increase temperature to 2090 DEG C,
Keep temperature-resistant；
(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
The one end for making outer tube body 224 be provided with seed crystal 400 in crucible room 212 is contacted with high temperature crystal solution surface, and opens heat exchanger
220 keep the intake of helium for 34L/min, by 400 diameter melt back of seed crystal to 60mm；
(5) keep the power of primary heater 231 and secondary heater 232 constant, gradually increase helium intake, first with
The rate for increasing 1L/min per hour increases to 50L/min, then increases to 80L/min to increase the rate of 2L/min per hour,
Grow crystal down and perpendicular to 500 direction of thermoisopleth along seed crystal 400；
(6) it when crystal growth is to 50%~60%, keeps 232 power of secondary heater constant and increases 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 fastly to 100L/min
Portion；
(8) keep helium intake constant, when the 95% of crystalline solidification ad pond om, heat exchanger 220 is with certain speed
It is lifted up, while improving 232 power of secondary heater, demould entire crystal and crucible bottom；
(9) annealing cooling is carried out after crystal growth obtains final Shaped crystal 300.
Refering to Fig. 3 and Fig. 4 it is found that the Shaped crystal 300 produced through the invention and the side wall 213 in crucible chamber 212
It is not contacted with bottom wall 214, minimizes the defect of crystals.And it is brilliant by the final forming that traditional czochralski method is produced
Body 300a then in crucible chamber 212 side wall 213 and bottom wall 214 be in contact, this contact will cause the life of matter crystal internal defect
It is long, so that crystal is easy cracking.
Crystal growing apparatus 100, crystal growing crucible 200 and growing method provided in this embodiment can be used for giving birth to
The crystal of long sizes and type.For example, the biggish sapphire crystal of growth size can be used to.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of crystal growing crucible, including crucible body, which is characterized in that the crystal growing crucible further 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；The heat exchanger includes heat exchange unit and is provided with fluid flow control singly
The fluid supply unit of member；One end of the heat exchange unit is connect with the fluid supply unit, the heat exchange unit
The other end is through the crucible cover and protrudes into the crucible chamber, and the heat exchanger is optionally at the separate or close bottom
The place movement of wall；Heater is equipped with outside the crucible body, the heater includes being located on the first of the side wall to add
Hot device and the secondary heater being arranged in outside the bottom wall.
2. crystal growing crucible according to claim 1, which is characterized in that the heat exchange unit includes outer tube body and inner tube
Body, said inner tube body are arranged in the outer tube body, form heat exchanger channels between the outer tube body and said inner tube body；In described
Tube body offers the heat exchanging holes being connected to the heat exchanger channels；Said inner tube body and the outer tube body are arranged in the crucible cover simultaneously
Deeply to the crucible chamber.
3. a kind of crystal growing apparatus, which is characterized in that raw including crystal described in growth furnace and claim 1~2 any one
Long crucible；The growth furnace includes furnace body and chamber；The crucible is set in the chamber, the crucible and the furnace body it
Between be provided with insulating layer, the heat exchanger is successively arranged in the furnace body and the insulating layer.
4. crystal growing apparatus according to claim 3, which is characterized in that the heat exchanger and the furnace body pass through magnetic
Sealing.
5. a kind of growing method based on crystal growing crucible described in claim 1, which is characterized in that including following step
It is rapid:
Fusing is placed in the indoor crystal raw material of the crucible；
Contact the seed crystal in 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 processing successively is carried out to crystal, demoulding is handled.
6. growing method according to claim 5, which is characterized in that the method for melting the crystal raw material includes:
Simultaneously by the primary heater and the secondary heater in the indoor crystal raw material of the crucible into
Row heating.
7. growing method according to claim 5, which is characterized in that by the seed crystal and the institute for being in molten state
Stating crystal raw material, contiguously method includes:
The end that the heat exchanger protrudes into the crucible chamber is arranged in the seed crystal, the mobile heat exchanger makes the seed
Crystalline substance is contacted with the crystal raw material surface of molten state, and keeps the heating of the primary heater, the secondary heater
Temperature is constant.
8. growing method according to claim 5, which is characterized in that logical according to default rule in the heat exchanger
Enter in cooling gas step, the default rule are as follows:
The increase at any time of the intake of the cooling gas and increase.
9. growing method according to claim 5, which is characterized in that
To the crystal carry out demoulding processing method include:
It keeps the heating temperature of the primary heater constant, while increasing the heating temperature of the secondary heater, and by institute
It states heat exchanger and is moved in a manner of far from the crucible along the preset direction, make the crystal and the crucible of growth
It realizes and is detached from.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611243558.8A CN106854773B (en) | 2016-12-29 | 2016-12-29 | A kind of crystal growing crucible, device and its growing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611243558.8A CN106854773B (en) | 2016-12-29 | 2016-12-29 | A kind of crystal growing crucible, device and its growing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106854773A CN106854773A (en) | 2017-06-16 |
| CN106854773B true CN106854773B (en) | 2019-05-03 |
Family
ID=59126726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611243558.8A Active CN106854773B (en) | 2016-12-29 | 2016-12-29 | A kind of crystal growing crucible, device and its growing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106854773B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736395A (en) * | 2008-11-17 | 2010-06-16 | 中国科学院福建物质结构研究所 | Crystal growing and pulling device |
| CN201873779U (en) * | 2010-11-24 | 2011-06-22 | 中国科学院沈阳科学仪器研制中心有限公司 | Water-electricity connection mechanism |
| CN102677168A (en) * | 2011-03-15 | 2012-09-19 | 上海晨安电炉制造有限公司 | Thermal-field-adjustable furnace for growing crystals through kyropoulos method |
| CN202595336U (en) * | 2012-03-12 | 2012-12-12 | 徐州协鑫光电科技有限公司 | Seed crystal clamping structure |
| CN103103622A (en) * | 2011-11-11 | 2013-05-15 | 中国科学院沈阳科学仪器研制中心有限公司 | Water-cooled jacket capable of working in high-temperature environment of vacuum equipment for long time |
| CN103147121A (en) * | 2013-04-03 | 2013-06-12 | 中国科学院上海硅酸盐研究所 | Device for growing crystals by using lifting and Kyropoulos method |
| CN104499043A (en) * | 2014-12-15 | 2015-04-08 | 江苏苏博瑞光电设备科技有限公司 | 83kg-grade sapphire crystal furnace crystal-growing structure and crystal-growing method |
| CN104911708A (en) * | 2015-06-15 | 2015-09-16 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing square sapphire crystal by Kyropoulos process |
-
2016
- 2016-12-29 CN CN201611243558.8A patent/CN106854773B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736395A (en) * | 2008-11-17 | 2010-06-16 | 中国科学院福建物质结构研究所 | Crystal growing and pulling device |
| CN201873779U (en) * | 2010-11-24 | 2011-06-22 | 中国科学院沈阳科学仪器研制中心有限公司 | Water-electricity connection mechanism |
| CN102677168A (en) * | 2011-03-15 | 2012-09-19 | 上海晨安电炉制造有限公司 | Thermal-field-adjustable furnace for growing crystals through kyropoulos method |
| CN103103622A (en) * | 2011-11-11 | 2013-05-15 | 中国科学院沈阳科学仪器研制中心有限公司 | Water-cooled jacket capable of working in high-temperature environment of vacuum equipment for long time |
| CN202595336U (en) * | 2012-03-12 | 2012-12-12 | 徐州协鑫光电科技有限公司 | Seed crystal clamping structure |
| CN103147121A (en) * | 2013-04-03 | 2013-06-12 | 中国科学院上海硅酸盐研究所 | Device for growing crystals by using lifting and Kyropoulos method |
| CN104499043A (en) * | 2014-12-15 | 2015-04-08 | 江苏苏博瑞光电设备科技有限公司 | 83kg-grade sapphire crystal furnace crystal-growing structure and crystal-growing method |
| CN104911708A (en) * | 2015-06-15 | 2015-09-16 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing square sapphire crystal by Kyropoulos process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106854773A (en) | 2017-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2520472C2 (en) | Method and device for sapphire monocrystal growth | |
| CN102877117B (en) | Ingot furnace thermal field structure based on multi-heater and operation method | |
| CN101962798B (en) | Method and equipment for producing sapphire single crystal | |
| CN104499045B (en) | Kyropoulos-method sapphire crystal growth furnace | |
| CN103147121B (en) | The device of lift kyropoulos growing crystal | |
| CN102352530B (en) | Heat shield device for CZ-Si single crystal furnace | |
| CN104651934B (en) | A kind of energy-saving sapphire crystal growing furnace | |
| CN104651935B (en) | A kind of method that crucible rise method prepares high-quality sapphire crystal | |
| CN103060901B (en) | Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method | |
| CN104195640A (en) | Thermal field system for sapphire single crystal growth | |
| CN102628184A (en) | Method for growing gem crystals by way of vacuum induction heating and device realizing method | |
| CN202989351U (en) | Ingot furnace thermal field structure based on multiple heaters | |
| CN102534758A (en) | Growth method and growth device for bar-shaped sapphire crystals | |
| CN111020689A (en) | Crystal growth apparatus and method | |
| CN103966657B (en) | Ingotting furnace for polycrystalline silicon and quasi single crystal silicon and application method for ingotting furnace | |
| CN102560631A (en) | Growth method and equipment of sapphire crystal | |
| CN105088333A (en) | Kyropoulos sapphire crystal growth furnace | |
| CN104073875A (en) | Preparation method of large-size sapphire crystal dynamic temperature field | |
| CN104099660A (en) | Rotating shoulder-expanding stable pulling-up method for large-kilogram sapphire crystals | |
| CN102644113A (en) | Production method and equipment of c-oriented sapphire single crystal | |
| CN103255477B (en) | The growing method of a kind of shaped sapphire crystal and equipment | |
| KR101196445B1 (en) | Apparatus for Growing Sapphire Crystal and Method for Growing Sapphire Crystal Using the Same | |
| CN103469304B (en) | Branched shaping sapphire crystallization device and long crystal method thereof | |
| CN106854773B (en) | A kind of crystal growing crucible, device and its growing method | |
| CN104480527A (en) | Full-power control ingot casting process for polycrystalline silicon ingot furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
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. |