CN106222747A - A kind of sapphire single-crystal furnace - Google Patents
A kind of sapphire single-crystal furnace Download PDFInfo
- Publication number
- CN106222747A CN106222747A CN201610777959.5A CN201610777959A CN106222747A CN 106222747 A CN106222747 A CN 106222747A CN 201610777959 A CN201610777959 A CN 201610777959A CN 106222747 A CN106222747 A CN 106222747A
- Authority
- CN
- China
- Prior art keywords
- crucible
- radiation shield
- sapphire single
- heater
- crystal furnace
- 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.)
- Pending
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
Abstract
The invention belongs to use kyropoulos to prepare sapphire crystal field, particularly to a kind of sapphire single-crystal furnace, including being provided with the body of heater of bell, the crucible of overlying crucible cover, heater, upper radiation shield, lateral reflection screen, lower radiation shield and seed rod, described crucible cover overlying heat protection screen, two heating plates it are provided with between described upper radiation shield and heat protection screen, said two heating plate is symmetrical set on seed rod both sides, and described bell is provided with vacuum component.The present invention reduces the deposition of volatile matter；Can realize the monitoring of infrared radiation thermometer and temperature sensor, the two cooperates simultaneously so that operator can understand and manipulate temperature field more easily；Along with the research and development of material, the decline of high temperature resistant temperature sensor cost so that infrared radiation thermometer is replaced completely so that kyropoulos realizes automatization and is possibly realized.
Description
Technical field
The invention belongs to use kyropoulos to prepare sapphire crystal field, particularly to a kind of sapphire single-crystal furnace.
Background technology
The growth course of kyropoulos sapphire crystal has mainly been carried by heat in control system, calandria
Producing heat by electric current and reach crucible outer wall with thermal-radiating form, crucible is the most respectively by conduction of heat and thermal-radiating shape
Heat is reached melt and crystal by formula, and crystal, along seeded growth, is connected with cooling water in seed rod, can be by thermal convection current
Form takes away the most heat of crystals.All there is a range of thermograde in melt in crucible and crystal, and one
Individual suitable thermograde determines the direction of transfer of heat and the growth of beneficially crystal.
The long brilliant process of kyropoulos has: the processes such as charging, melting charge, seeding, expansion shoulder, isodiametric growth and ending, at this
In serial procedures, the seeding stage is the most key, in the seeding stage, and Al in crucible2O3Liquation is in boiling stage, various in liquation
Impurity constantly volatilizees, and runs into low-temperature receiver, will be attached to above, owing to endoscopy glass temperature is relatively low, when opening visor baffle plate, and stove
Interior impurity adheres on endoscopy glass, and the long-time definition using endoscopy glass can slowly reduce, not aspect liquation face
The observation of color, owing to liquation different colours represents different temperature, visor is contaminated the judgement that can directly affect observer, leads
Cause seeding failure so that follow-up work cannot complete.
Existing single crystal growing furnace, the form on body of heater uses double-deck quartz glass, is provided with cold in the middle of double-deck quartz glass
But water circulation system.The weak point of existing window structure is: in the middle of (1) double-deck quartz glass, the flowing of water can produce ripple,
The accuracy that sapphire single-crystal completely generates is observed in impact；(2) sapphire single-crystal furnace in-furnace temperature is up to 2100 DEG C, once cools down
Water is uneven may result in the broken of sight glass；(3) the inside of form is concave structure, this not only difficulty of processing very big, and
And the form observation that can carry out is all unilateral observation, this just makes the observation of form have limitation, the operation not that sowing seed crystal
Convenient；(4) whole circumstances of crystal growth in stove can not be fully understood by by form.
Domestic present sapphire crystal growing furnace observation window, uses below upper bell more, heat screen top peace in stove
Fill a shielding plate, pass through；Rotating mechanism above bell blocks and exposes observation window, and this apparatus structure is complicated, and at stove
Interior high temperature to be born, is unfavorable for the sealing protection of shielding plate rotating mechanism, understands that the heat that shielding plate conduction comes up can have a strong impact on
In the life-span of rotating mechanism sealing ring, even in crystal growing furnace running, the situation of vacuum leak occurs.
Existing single crystal growing furnace is primarily directed to the improvement of observation window, improves the structure of observation window, increases the quantity of observation window
Deng, but to causing the unsharp volatile matter of observation window to dabble the fewest.Quite some meaning cured the symptoms, not the disease.
Volatile matter deposits, and volatile matter refers mainly to molybdenum, tungsten, melt and impurity therein etc..The crystal that is deposited on of volatile matter is given birth to
Growth process cannot be avoided, be mainly deposited at heat protection screen, pot cover and heater, due to the existence of volatile matter, raw at crystal
The long starting stage, need higher heating power；And the crystal growth later stage, volatile matter makes the high insulating effect in body of heater, with
Under sample heating power, temperature can raise, and therefore, for obtaining same crystal mass, then needs the bigger power range of decrease.
Owing under the high temperature conditions (1926 DEG C), the thermal decomposition of alumina melt trace discharges O2, calandria and crucible
Following chemical reaction is there is in tungsten with oxygen.
Mo+3/2O2=MoO3(gaseous state)；
W+3/2O2=WO3(gaseous state).
WO3Fusing point be 1469 DEG C, along with the continuous growth of crystal, power reduces, the temperature fall of upper heat protection screen middle
Low to WO3Fusing point below, WO3Deposit herein.Volatile matter, can completely plugged window when growing into about 2kg.Now
Power is reduced to about 827 DEG C in about 70kW, temperature herein, MoO3Deposit herein.At crystal growth early stage, volatile matter
Deposition can block up part observation window, makes top heat dissipation capacity reduce, causes crystal shouldering cannot even produce melt back；At crystal growth
In the later stage, volatile matter can block up observation window completely, cause in-furnace temperature to raise, and crucible bottom thermograde reduces, and easily causes crystalline substance
The too fast growth of body afterbody, produces viscous pot and bubble, affects crystal overall quality.
Al2O3Volatilize under the conditions of high temperature, coarse vacuum, form steam, owing to the temperature at pot cover is relatively low, Al2O3Steam is sent out
Raw condensation, forms Al2O3Crystal.The main component of the volatile matter at pot cover is Al2O3, owing to heat conductivity is relatively low, directly result in
The capacity of heat transmission at pot cover reduces so that the warm field in crucible controls difficulty.Volatile matter deposits at heating rod top (low-temperature space),
It is mainly composed of MoO3And WO3Mixture.It is mainly composed of tungsten due to what volatile matter deposited, consistent with the component of heater,
It is metal good conductor.After heating rod is thicker, causing the resistance of heating rod to reduce, caloric value reduces.At same growth conditions
Under, need bigger heating power, cause energy loss.
How to reduce volatile matter and deposit the adverse effect brought, the automatization how improving sapphire preparation process is to put
A difficult problem in face of people.
Summary of the invention
As known from the above, under current working condition, the generation of volatile matter is inevitable, how to alleviate volatile matter
How the adverse effect brought, promote automatic control level, is that the present invention attempts problem to be solved.The present invention intends providing one
Plant sapphire single-crystal furnace, including being provided with the body of heater 1 of bell 11, the crucible 3 of overlying crucible cover 2, heater 4, upper radiation shield 5, side
Radiation shield 6, lower radiation shield 7 and seed rod 8, described crucible cover 2 overlying heat protection screen 9, between described upper radiation shield 5 and heat protection screen 9
Being provided with two heating plates 10, said two heating plate (10) is symmetrical set on seed rod (8) both sides, and described bell 11 is provided with
Vacuum component 12.
Further, described crucible 3 is tungsten crucible, welding molybdenum crucible or sintering molybdenum crucible.Preferably tungsten crucible, because of
Fusing point for tungsten is higher than the fusing point of molybdenum, it is not easy to vaporization at high temperature out reacts with oxygen；The most conventional is sintering molybdenum earthenware
Crucible, but the performance of welding molybdenum crucible is better than sintering molybdenum crucible, the welding molybdenum crucible of same thickness and making of sintering molybdenum crucible tolerance
By temperature with to use time length be the same, the use time of the even significantly larger than sintered crucible having.This is because sintering
Density the highest, less than through all of consistency of molybdenum plate repeatedly rolled, therefore the molybdenum in welding molybdenum crucible is more not yet
Readily volatilized, and then produce MoO with oxygen reaction2。
Further, described lateral reflection screen 6, lower radiation shield 7 are tungsten radiation shield or tungsten radiation shield.In tungsten radiation shield
The quality accounting 50% of tungsten.Comparing molybdenum radiation shield, the probability of tungsten radiation shield and tungsten radiation shield vaporization at high temperature is lower, more not
Easily produce volatile matter deposition.
Further, the quantity of described vacuum component 12 is two, is symmetrical arranged.Dividing of sapphire single-crystal furnace middle temperature field
Cloth, control it is critical that, the change that single crystal growing furnace is done, all it is noted that keep in balance, the most easily change Varied Temperature Field
Distribution, in turn results in the adverse effects such as expansion uneven, the viscous pot of shoulder.
Further, described vacuum component 12 is provided with dust pelletizing system.After volatile matter produces, when arriving finite concentration, take out
Vacuum, takes away volatile matter in body of heater, does not the most allow volatile matter contact, adhere on observation window；Why setting removes
Dirt system, be because containing in volatile matter is all metal-oxide, if processing not in time, easily blocks the unit of vacuum component
Device, is unfavorable for producing continuously.
Further, described crucible 3, crucible cover 2, upper radiation shield 5 and heater 4 are provided with resistant to elevated temperatures temperature sensor.
Sapphire is during seeding, and the control to temperature is particularly important, and arranging of high temperature resistant temperature sensor can help operator
Member understands crucible 3, crucible cover 2, upper radiation shield 5 and the warm field of heater 4, crucible cover 2, the middle part of upper radiation shield 5 simultaneously in time
Being the position easily depositing volatile matter with the top of heater 4, had the help of temperature sensor, operator can be at not shadow
On the premise of ringing seeding progress, in time the temperature at above-mentioned position is intervened, and then reduce the deposition of volatile matter.
Further, described heater 4 is in parallel with heating plate 10.Why being arranged to parallel connection is to realize heating
The independent control of sheet 10, and then realize the regulation of the temperature to upper radiation shield 5 and heat protection screen 9, reduce the deposition of volatile matter.
Further, described heating plate 10 can move up and down.It is to operate for convenience that heating plate 10 can move up and down
Personnel specifically control heat protection screen 9 and the temperature of upper radiation shield 5, when needing the warm field regulating heat protection screen 9, can move heating plate
10 make it closer to heat protection screen 9, when needing the warm field of the upper radiation shield 5 of regulation, can move heating plate 10 and make it closer to upper
Radiation shield 5.
Compared with prior art, there is advantages that
(1) decrease the deposition of volatile matter on radiation shield, extend the time of observation；
(2) deposition of volatile matter on crucible cover is decreased so that the control of temperature field in crucible is relatively easy to；
(3) decrease the deposition of volatile matter on heater, reduce loss；
(4) can realize the monitoring of infrared radiation thermometer and temperature sensor, the two cooperates so that operator simultaneously
Can understand and manipulate temperature field more easily；Along with the research and development of material, the decline of high temperature resistant temperature sensor cost so that infrared
Temperature measurer is replaced completely so that kyropoulos realizes automatization and is possibly realized.
Accompanying drawing explanation
The structural representation of Fig. 1: the present invention；
In figure: 1, body of heater；2, crucible cover；3, crucible；4, heater；5, upper radiation shield；6, lateral reflection screen；7, lower reflection
Screen；8, seed rod；9, heat protection screen；10, heating plate；11, bell；12, vacuum component.
Detailed description of the invention
Embodiment one
A kind of sapphire single-crystal furnace, including:
Being provided with the body of heater 1 of bell 11, bell 11 is provided with observation window not shown in FIG.；Described bell 11 is provided with vacuum
Parts 12, the quantity of described vacuum component 12 is two, and the centrosymmetry around bell is arranged, and described vacuum component 12 is provided with and removes
Dirt system；Described vacuum component coordinates vacuometer to use, and determines the need for evacuation according to the sensing of vacuometer pointer；If
Vacuometer points to inaccurate or if being not provided with vacuometer, can come certainly according to the change in the response time of crystal or temperature field
Fixed the most whether extracting vacuum.
The crucible 3 of overlying crucible cover 2, crucible is tungsten crucible, and the pillar below crucible is tungsten pillar, in order to be incubated crucible cover
2 overlying heat protection screens 9；
Heater 4, heater 4 be shaped as common cage type；
Upper radiation shield 5, lateral reflection screen 6 and lower radiation shield 7, all use tungsten radiation shield；
Seed rod 8；
Being provided with two heating plates that can move up and down 10 between described upper radiation shield 5 and heat protection screen 9, said two heats
Sheet 10 is symmetrical set on seed rod 8 both sides, and said two heating plate 10 should be tried one's best away from seed rod 8, reduces seed rod 8
The impact of temperature, described heater 4 and heating plate 10 are in parallel, and operator can control heater 4 and heating plate 10 respectively
Open and close；
Described crucible 3, crucible cover 2, upper radiation shield 5 and heater 4 are provided with resistant to elevated temperatures temperature sensor.
Claims (8)
1. a sapphire single-crystal furnace, including being provided with the body of heater (1) of bell (11), the crucible (3) of overlying crucible cover (2), heating
Device (4), upper radiation shield (5), lateral reflection screen (6), lower radiation shield (7) and seed rod (8), it is characterised in that: described crucible cover (2)
Overlying heat protection screen (9), is provided with two heating plates (10), said two heating plate between described upper radiation shield (5) and heat protection screen (9)
(10) being symmetrical set on seed rod (8) both sides, described bell (11) is provided with vacuum component (12).
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: described crucible (3) is tungsten crucible, welding
Molybdenum crucible or sintering molybdenum crucible.
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: described lateral reflection screen (6), lower radiation shield
(7) it is tungsten radiation shield or tungsten radiation shield.
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: the quantity of described vacuum component (12) is
Two, it is symmetrical arranged.
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: described vacuum component (12) is provided with dedusting
System.
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: described crucible (3), crucible cover (2), on
Radiation shield (5) and heater (4) are provided with resistant to elevated temperatures temperature sensor.
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: described heater (4) and heating plate
(10) it is in parallel.
A kind of sapphire single-crystal furnace the most according to claim 1, it is characterised in that: described heating plate (10) can on move down
Dynamic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610777959.5A CN106222747A (en) | 2016-08-30 | 2016-08-30 | A kind of sapphire single-crystal furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610777959.5A CN106222747A (en) | 2016-08-30 | 2016-08-30 | A kind of sapphire single-crystal furnace |
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| Publication Number | Publication Date |
|---|---|
| CN106222747A true CN106222747A (en) | 2016-12-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610777959.5A Pending CN106222747A (en) | 2016-08-30 | 2016-08-30 | A kind of sapphire single-crystal furnace |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018129863A1 (en) * | 2017-01-13 | 2018-07-19 | 许昌天戈硅业科技有限公司 | Sapphire crystal growth furnace with low energy consumption |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2368710C1 (en) * | 2008-05-16 | 2009-09-27 | Николай Иванович Блецкан | Device for growing of volumetric rectangular monocrystals of sapphire |
| CN102677158A (en) * | 2011-03-15 | 2012-09-19 | 上海晨安电炉制造有限公司 | Kyropoulos crystal growing furnace with auxiliary chamber structure |
| CN202658264U (en) * | 2012-06-25 | 2013-01-09 | 上海嘉森真空科技有限公司 | Crystal growing furnace with thermal superposed field structure |
| CN203420008U (en) * | 2013-07-15 | 2014-02-05 | 哈尔滨工业大学 | Vacuum furnace for melt crystal growth |
| CN103806102A (en) * | 2014-02-14 | 2014-05-21 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN203728963U (en) * | 2014-02-14 | 2014-07-23 | 闽能光电集团有限公司 | Sapphire crystal growth thermal field structure |
| CN104514032A (en) * | 2014-12-18 | 2015-04-15 | 华中科技大学 | Thermal field coordination control Czochralski crystal growth furnace |
| CN204342916U (en) * | 2014-12-18 | 2015-05-20 | 华中科技大学 | A kind of method of crystal growth by crystal pulling stove of thermal field cooperation control |
| CN206052206U (en) * | 2016-08-30 | 2017-03-29 | 天通银厦新材料有限公司 | A kind of sapphire single-crystal furnace |
-
2016
- 2016-08-30 CN CN201610777959.5A patent/CN106222747A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2368710C1 (en) * | 2008-05-16 | 2009-09-27 | Николай Иванович Блецкан | Device for growing of volumetric rectangular monocrystals of sapphire |
| CN102677158A (en) * | 2011-03-15 | 2012-09-19 | 上海晨安电炉制造有限公司 | Kyropoulos crystal growing furnace with auxiliary chamber structure |
| CN202658264U (en) * | 2012-06-25 | 2013-01-09 | 上海嘉森真空科技有限公司 | Crystal growing furnace with thermal superposed field structure |
| CN203420008U (en) * | 2013-07-15 | 2014-02-05 | 哈尔滨工业大学 | Vacuum furnace for melt crystal growth |
| CN103806102A (en) * | 2014-02-14 | 2014-05-21 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN203728963U (en) * | 2014-02-14 | 2014-07-23 | 闽能光电集团有限公司 | Sapphire crystal growth thermal field structure |
| CN104514032A (en) * | 2014-12-18 | 2015-04-15 | 华中科技大学 | Thermal field coordination control Czochralski crystal growth furnace |
| CN204342916U (en) * | 2014-12-18 | 2015-05-20 | 华中科技大学 | A kind of method of crystal growth by crystal pulling stove of thermal field cooperation control |
| CN206052206U (en) * | 2016-08-30 | 2017-03-29 | 天通银厦新材料有限公司 | A kind of sapphire single-crystal furnace |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018129863A1 (en) * | 2017-01-13 | 2018-07-19 | 许昌天戈硅业科技有限公司 | Sapphire crystal growth furnace with low energy consumption |
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Application publication date: 20161214 |