CN108866619A - The oriented growth device and technique of large scale magnesium fluoride monocrystalline - Google Patents
The oriented growth device and technique of large scale magnesium fluoride monocrystalline Download PDFInfo
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- CN108866619A CN108866619A CN201810706570.0A CN201810706570A CN108866619A CN 108866619 A CN108866619 A CN 108866619A CN 201810706570 A CN201810706570 A CN 201810706570A CN 108866619 A CN108866619 A CN 108866619A
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- graphite
- insulation cover
- heater
- magnesium fluoride
- large scale
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Classifications
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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
-
- 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
- C30B29/12—Halides
Abstract
The invention belongs to monocrystalline production fields, and in particular to the oriented growth device and technique of large scale magnesium fluoride monocrystalline, including furnace shell, heat preservation mechanism, heating mechanism, magnetism servo-electric motor water-cooling and crystal growth mechanism；Heat preservation mechanism includes top graphite insulation cover, side graphite insulation cover and bottom insulation cover, and a keeping warmth space is collectively formed in top graphite insulation cover, side graphite insulation cover and bottom insulation cover；Heating mechanism includes electrode stem and graphite heater；The surface of graphite heater is equipped with several heater apertures, and the closeness for being located at the heater aperture on graphite heater top is greater than the closeness of the heater aperture of lower part；Relative to furnace shell displacement upward or downward can occur for graphite crucible together with magnetism servo-electric motor water-cooling.The crystalline size that it grows is big, and required simple process is controllable, and production cost is low.
Description
Technical field
The invention belongs to monocrystalline production fields, and in particular to the oriented growth device and technique of large scale magnesium fluoride monocrystalline.
Background technique
UV grade magnesium fluoride monocrystalline has wider through range and high transmitance, there is certain double refractive inde, can
It is wide for optical elements, the large scale UV grade magnesium fluoride monocrystalline such as fiber optic communication field and production optical prism, lens and window
It is general to be applied to laser, infrared, ultraviolet optics, high energy detection, light communication system and military industry field, it is generally used in industry at present
Bridgman-Stockbarger method is produced, by resistance heating, the mixed raw material being melted in crucible, and by sowing, necking down, isometrical equal operation,
Grow the crystal of certain orientation；In addition using the orientable growth fluoride single crystal of temperature gradient method, the terraced method of temperature for passing on a skill from a master to a single disciple system is brilliant
Body furnace growth single crystal size is smaller, using tungsten insulation cover higher cost.
To realize the above-mentioned technical purpose, Chinese patent CN105603506B discloses a kind of terraced method growing large-size of dynamic temperature
The device and method of monocrystalline, the device of the terraced method growing large-size monocrystalline of dynamic temperature, is fixed with top in the top end part of circumference insulation cover
Portion's insulation cover is fixed with cricoid bottom insulation cover in the bottom end of circumference insulation cover, peace is slidingly sealed in the insulation cover of bottom
Equipped with center insulation cover, at center, the bottom end of insulation cover is equipped with center insulation cover lifting drive, is fixed in single crystal growing furnace
Crucible pole is fixed with bottom in crucible pole.Thermocouple is fixed with crucible in the top end part of crucible pole, solid in the outside of crucible
Surely there is heater, be fixed with top thermocouple on the insulation cover of top.But above-mentioned technical proposal is made due to the restriction of insulation cover
The single crystal size that must be grown is limited.
Summary of the invention
The present invention provides the oriented growth device and technique of large scale magnesium fluoride monocrystalline, and the crystalline size of growth is big, institute
Need simple process controllable, production cost is low.
To realize the above-mentioned technical purpose, the technical scheme adopted by the invention is as follows, the oriented growth of large scale magnesium fluoride monocrystalline
Device, including furnace shell, heat preservation mechanism, heating mechanism, magnetism servo-electric motor water-cooling and crystal growth mechanism；
Heat preservation mechanism includes top graphite insulation cover, side graphite insulation cover and bottom insulation cover, top graphite insulation cover, side
Portion's graphite insulation cover and bottom insulation cover are set to inside furnace shell jointly, and a keeping warmth space is collectively formed；
Heating mechanism includes electrode stem and graphite heater, and electrode stem is connected to external power supply, and for heating graphite heater,
Graphite heater is placed in keeping warmth space, and close to side graphite insulation cover；The surface of graphite heater is equipped with several fevers
Body aperture, and the closeness for being located at the heater aperture on graphite heater top is greater than the intensive of the heater aperture of lower part
Degree；
Crystal growth mechanism includes graphite crucible, and graphite crucible is placed in the middle position of keeping warmth space, and can thermally equivalent；
Magnetism servo-electric motor water-cooling includes water cooling seed rod protective case and water cooling seed rod, and water cooling seed rod protective case is located at the bottom of graphite crucible
Portion, and it is located at the end of water cooling seed rod；The intermediate position of water cooling seed rod is equipped with water inlet pipe, water inlet pipe and water cooling seed rod
Outlet pipe is formed between tube wall；
Relative to furnace shell displacement upward or downward can occur for graphite crucible together with magnetism servo-electric motor water-cooling.
As the improved technical solution of the present invention, the diameter of graphite heater is 500mm.
As the improved technical solution of the present invention, the diameter of graphite crucible is 350mm.
As the improved technical solution of the present invention, the wall thickness of graphite crucible is 10mm.
Another object of the present invention is to provide the oriented growth techniques of large scale magnesium fluoride monocrystalline, include the following steps：
S1, the polycrystalline particle raw material by the magnesium fluoride seed crystal and purity of orientation greater than 99.99% are fitted into graphite crucible；
S2, keeping warmth space is vacuumized, until keeping warmth space pressure is 3 × 10-3MPa, meanwhile, open electrode stem, graphite
Heater heat production, control growth temperature gradient is 60-90 DEG C/cm, until keeping warmth space temperature reaches 1250 DEG C, constant temperature 2-4h；
S3, the long brilliant rate of observation, and the long brilliant time is set, specially rate of temperature fall is 1-2 DEG C/h, until keeping warmth space temperature is
1220 DEG C, constant temperature reduces graphite crucible 80mm, and graphite crucible fall off rate is 0.5-1.3mm/h；
S4, in-situ high temperature annealing is carried out to crystal, the rate of temperature fall of annealing stage guarantees that anneal duration is 70h.
Beneficial effect
The device of the application uses graphite insulation cover, and the insulation cover of graphite insulation cover device compared with the existing technology is used for a long time
Graphite insulation cover is unlikely to deform, and thermal field is relatively more uniform, and advantage of lower cost；Heater diameter increases to 500mm；Warm area
Increase, maximum can place the graphite crucible of 350mm diameter；Guarantee that crystal can be grown bigger, and the device of the prior art due to
Temperature field makes it produce large-sized magnesium fluoride monocrystalline inferior quality respectively, and quality cannot also control.
During long brilliant, the tungsten heat protection screen of conventional temperature gradient method is compared, the device in this method uses graphite temperature
, thermal field can have deformation caused by high temperature, and thermal field uniformity is high, and graphite heater uses ad hoc aperture, be more advantageous to manufacture
Crystal growth required temperature gradient.The method that annealing uses in-situ annealing, technique simplify, and save the production time.
Crystal is in high temperature protection area always, is more advantageous to reduction crystals relative to czochralski method and Bridgman-Stockbarger method and answers
Power, and temperature-fall period is slow, this process, which is equivalent to, anneals to magnesium fluoride crystal；It will not be generated in crystal growing process because of rotation
Turn and decline bring crystal defect.This method uses graphite crucible and graphite insulation cover, relative to czochralski method and tradition temperature ladder
Production cost greatly reduces in method.
Detailed description of the invention
The structural schematic diagram of Fig. 1 the application device；
Fig. 2 the application graphite heater structural schematic diagram；
In figure：1, electrode stem；2, water cooling seed rod；3, bottom insulation cover；4, water cooling seed rod protective case；5, side graphite is kept the temperature
Cover；6, graphite heater；7, graphite crucible；8, top graphite insulation cover；9, furnace shell；10, heater aperture；11, water inlet pipe；
12, outlet pipe.
Specific embodiment
To keep purpose and the technical solution of the embodiment of the present invention clearer, below in conjunction with the attached of the embodiment of the present invention
Figure, is clearly and completely described the technical solution of the embodiment of the present invention.Obviously, described embodiment is of the invention
A part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, those of ordinary skill in the art
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of being not necessarily to creative work.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein（Including technology art
Language and scientific term）With meaning identical with the general understanding of those of ordinary skill in fields of the present invention.Should also
Understand, those terms such as defined in the general dictionary, which should be understood that, to be had and the meaning in the context of the prior art
The consistent meaning of justice, and unless defined as here, it will not be explained in an idealized or overly formal meaning.
The oriented growth device of large scale magnesium fluoride monocrystalline, including furnace shell, heat preservation mechanism, heating mechanism, magnetism servo-electric motor water-cooling with
And crystal growth mechanism；
Heat preservation mechanism includes top graphite insulation cover, side graphite insulation cover and bottom insulation cover, top graphite insulation cover, side
Portion's graphite insulation cover and bottom insulation cover are set to inside furnace shell jointly, and a keeping warmth space is collectively formed；
Heating mechanism includes electrode stem and graphite heater, and electrode stem is connected to external power supply, and for heating graphite heater,
Graphite heater is placed in keeping warmth space, and close to side graphite insulation cover；The surface of graphite heater is equipped with several fevers
Body aperture, and the closeness for being located at the heater aperture on graphite heater top is greater than the intensive of the heater aperture of lower part
Degree；
Crystal growth mechanism includes graphite crucible, and graphite crucible is placed in the middle position of keeping warmth space, and can thermally equivalent；
Magnetism servo-electric motor water-cooling includes water cooling seed rod protective case and water cooling seed rod, and water cooling seed rod protective case is located at the bottom of graphite crucible
Portion, and it is located at the end of water cooling seed rod；The intermediate position of water cooling seed rod is equipped with water inlet pipe, water inlet pipe and water cooling seed rod
Outlet pipe is formed between tube wall；
Relative to furnace shell displacement upward or downward can occur for graphite crucible together with magnetism servo-electric motor water-cooling.
Due to the special designing of the application graphite heater, so that the diameter of the graphite heater of the application is 500mm；Stone
The diameter of black crucible is 350mm；The wall thickness of graphite crucible is 10mm.
Another object of the present invention is to provide the oriented growth techniques of large scale magnesium fluoride monocrystalline, include the following steps：
S1, the polycrystalline particle raw material by the magnesium fluoride seed crystal and purity of orientation greater than 99.99% are fitted into graphite crucible；The seed
Crystalline substance by screening without crystal boundary, envelope, scattering, stress the defects of [001] to seed crystal；MgF2 material purity >=99. 99%.
S2, keeping warmth space is vacuumized, until keeping warmth space pressure is 3 × 10-3MPa, meanwhile, electrode stem is opened,
Graphite heater heat production, control growth temperature gradient is 60-90 DEG C/cm, until keeping warmth space temperature reaches 1250 DEG C, constant temperature 2-
4h；
S3, the long brilliant rate of observation, and the long brilliant time is set, specially rate of temperature fall is 1-2 DEG C/h, until keeping warmth space temperature is
1220 DEG C, constant temperature reduces graphite crucible 80mm, and graphite crucible fall off rate is 0.5-1.3mm/h；
S4, in-situ high temperature annealing is carried out to crystal, the rate of temperature fall of annealing stage guarantees that anneal duration is 70h.
Concrete application
The seed crystal of [001] direction MgF2 is put into the seed slot of graphite crucible bottom, the polycrystalline by purity greater than 99. 99% is former
Material 15kg is put into diameter 300mm, wall thickness with a thickness of in the graphite crucible of 10mm.
Graphite crucible is put into single crystal growing furnace according to charging technique and adjusts geometric center, pumping high vacuum to 3x10-3Pa, heating
To 1250 °C constant temperature 2 hours, melt seed crystal position sufficiently to crucible seed crystal groove location, set cooling process and start long crystalline substance, drop
1-2 DEG C of warm rate/h to 1220 DEG C, crucible 80mm, crucible fall off rate 0.5-1.3mm/h, long crystalline substance process duration drop in constant temperature later
70-120h is later annealing stage, and setting cooling process is annealed, anneal duration 70h, and growth cycle is 6-10 days, cooling
After obtain deep ultraviolet magnesium fluoride monocrystalline, crystal weight is 14kg after polishing, and material crystal rate reaches 93%, after detecting really
Determine the defects of crystals are without crystal boundary, optical path, stress.
Measured crystal Mohs' hardness be 6, Young's modulus be 138. 8Gp, density be 3. 18g/cm3,0.11-7 μm
The transmitance of wave band is 90. 8%
The above is only embodiments of the present invention, and the description thereof is more specific and detailed, and but it cannot be understood as to this hair
The limitation of bright the scope of the patents.It should be pointed out that for those of ordinary skill in the art, not departing from present inventive concept
Under the premise of, various modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Claims (5)
1. the oriented growth device of large scale magnesium fluoride monocrystalline, which is characterized in that including furnace shell, heat preservation mechanism, heating mechanism, water
Cold structure and crystal growth mechanism；
Heat preservation mechanism includes top graphite insulation cover, side graphite insulation cover and bottom insulation cover, top graphite insulation cover, side
Portion's graphite insulation cover and bottom insulation cover are set to inside furnace shell jointly, and a keeping warmth space is collectively formed；
Heating mechanism includes electrode stem and graphite heater, and electrode stem is connected to external power supply, and for heating graphite heater,
Graphite heater is placed in keeping warmth space, and close to side graphite insulation cover；The surface of graphite heater is equipped with several fevers
Body aperture, and the closeness for being located at the heater aperture on graphite heater top is greater than the intensive of the heater aperture of lower part
Degree；
Crystal growth mechanism includes graphite crucible, and graphite crucible is placed in the middle position of keeping warmth space, and can thermally equivalent；
Magnetism servo-electric motor water-cooling includes water cooling seed rod protective case and water cooling seed rod, and water cooling seed rod protective case is located at the bottom of graphite crucible
Portion, and it is located at the end of water cooling seed rod；The intermediate position of water cooling seed rod is equipped with water inlet pipe, water inlet pipe and water cooling seed rod
Outlet pipe is formed between tube wall；
Relative to furnace shell displacement upward or downward can occur for graphite crucible together with magnetism servo-electric motor water-cooling.
2. the oriented growth device of large scale magnesium fluoride monocrystalline according to claim 1, which is characterized in that graphite heater
Diameter be 500mm.
3. the oriented growth device of large scale magnesium fluoride monocrystalline according to claim 1, which is characterized in that graphite crucible
Diameter is 350mm.
4. the oriented growth device of large scale magnesium fluoride monocrystalline according to claim 1, which is characterized in that graphite crucible
Wall thickness is 10mm.
5. the oriented growth technique based on any large scale magnesium fluoride monocrystalline of claim 1-4, which is characterized in that including
Following steps：
S1, the polycrystalline particle raw material by the magnesium fluoride seed crystal and purity of orientation greater than 99.99% are fitted into graphite crucible；
S2, keeping warmth space is vacuumized, until keeping warmth space pressure is 3 × 10-3MPa, meanwhile, open electrode stem, graphite
Heater heat production, control growth temperature gradient is 60-90 DEG C/cm, until keeping warmth space temperature reaches 1250 DEG C, constant temperature 2-4h；
S3, the long brilliant rate of observation, and the long brilliant time is set, specially rate of temperature fall is 1-2 DEG C/h, until keeping warmth space temperature is
1220 DEG C, constant temperature reduces graphite crucible 80mm, and graphite crucible fall off rate is 0.5-1.3mm/h；
S4, in-situ high temperature annealing is carried out to crystal, the rate of temperature fall of annealing stage guarantees that anneal duration is 70h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810706570.0A CN108866619A (en) | 2018-07-02 | 2018-07-02 | The oriented growth device and technique of large scale magnesium fluoride monocrystalline |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810706570.0A CN108866619A (en) | 2018-07-02 | 2018-07-02 | The oriented growth device and technique of large scale magnesium fluoride monocrystalline |
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| CN108866619A true CN108866619A (en) | 2018-11-23 |
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| CN201810706570.0A Pending CN108866619A (en) | 2018-07-02 | 2018-07-02 | The oriented growth device and technique of large scale magnesium fluoride monocrystalline |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110030828A (en) * | 2019-04-23 | 2019-07-19 | 西安航空制动科技有限公司 | A kind of vaccum sensitive stove |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766901A (en) * | 2012-08-20 | 2012-11-07 | 元亮科技有限公司 | Device for growing large-size and high-temperature crystals with real-time adjustable temperature gradient method and method |
| JP2013060335A (en) * | 2011-09-14 | 2013-04-04 | Tokuyama Corp | METHOD FOR PRODUCING MgF2 SINGLE CRYSTAL |
| CN103060891A (en) * | 2013-01-31 | 2013-04-24 | 长春理工大学 | Device and method for directionally growing fluoride single crystal via lifting small-gradient thermal field |
| CN103526279A (en) * | 2013-10-25 | 2014-01-22 | 北京华进创威电子有限公司 | Sleeve type graphite heater used for GaAs (gallium arsenide) crystal growth |
| CN106149051A (en) * | 2015-04-03 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | The thermal control Bridgman method single-crystal growing apparatus of fluoride single crystal body and method |
-
2018
- 2018-07-02 CN CN201810706570.0A patent/CN108866619A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013060335A (en) * | 2011-09-14 | 2013-04-04 | Tokuyama Corp | METHOD FOR PRODUCING MgF2 SINGLE CRYSTAL |
| CN102766901A (en) * | 2012-08-20 | 2012-11-07 | 元亮科技有限公司 | Device for growing large-size and high-temperature crystals with real-time adjustable temperature gradient method and method |
| CN103060891A (en) * | 2013-01-31 | 2013-04-24 | 长春理工大学 | Device and method for directionally growing fluoride single crystal via lifting small-gradient thermal field |
| CN103526279A (en) * | 2013-10-25 | 2014-01-22 | 北京华进创威电子有限公司 | Sleeve type graphite heater used for GaAs (gallium arsenide) crystal growth |
| CN106149051A (en) * | 2015-04-03 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | The thermal control Bridgman method single-crystal growing apparatus of fluoride single crystal body and method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110030828A (en) * | 2019-04-23 | 2019-07-19 | 西安航空制动科技有限公司 | A kind of vaccum sensitive stove |
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Application publication date: 20181123 |