CN109402724A - The undoped and Eu of one kind2+Adulterate the orientation growing by zone melting device and method of iodate strontium crystal - Google Patents
The undoped and Eu of one kind2+Adulterate the orientation growing by zone melting device and method of iodate strontium crystal Download PDFInfo
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- CN109402724A CN109402724A CN201710703145.1A CN201710703145A CN109402724A CN 109402724 A CN109402724 A CN 109402724A CN 201710703145 A CN201710703145 A CN 201710703145A CN 109402724 A CN109402724 A CN 109402724A
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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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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Abstract
The present invention provides one kind undoped and Eu2+Adulterate the orientation growing by zone melting device and method of iodate strontium crystal, the device includes: liftable support, the roller bearing screw rod platform supported by the liftable support, by step motor control with the mobile thermal field mobile relative to the roller bearing screw rod platform, the roller bearing screw rod platform is fixed on by fixed bracket and crosses the quartz glass boiler tube of the mobile thermal field, the growing container being placed in inside the quartz glass boiler tube.The present invention is advantageously implemented the dynamic or observation in real time of crystal growth, and seed crystal inoculating process can be used, the crystal of specific direction is obtained, simultaneously, the crystal top grown is in untethered state, space has been reserved to the expansion of crystal, has been conducive to the timely release of crystals stress, reduces the cracking of crystal, this method speed of growth is fast, the success rate of crystal growth is high, monocrystal good quality obtained, therefore greatly reduces the production cost of crystal.
Description
Technical field
The invention belongs to halide crystal preparation fields, and in particular to the undoped and Eu of one kind2+Adulterate strontium iodide (SrI2)
The orientation growing by zone melting device and method of crystal.
Background technique
Scintillation crystal refer to can be issued under the irradiation of high energy particle (such as X or gamma-rays) ultraviolet light, visible light or
A kind of light functional crystal material of infrared light, is widely used in the scientific experiments such as high-energy physics, nuclear physics, astrophysics, and
The necks closely related with national economy such as nuclear medicine, oil well detection, industry CT (Computed Tomography) and safety inspection
Domain.
1969, U.S. Robert Hofstadter application Eu2+Adulterate iodate strontium crystal (SrI2: Eu) as radiation
The patent of material is detected, but due to preparing the second-rate of crystal at that time, performance is compared to commercialized Tl+Ion is mixed
Miscellaneous NaI crystal has no advantage, its subsequent correlative study falls into nearly 40 years silence.Until 2008, in Homeland Security office, the U.S.
Under supporting with department outlays such as Ministry of Energy, Nerine Cherepy et al. is prepared for the SrI of high quality2: Eu crystal studies table
It is bright, SrI2: the light output of Eu is the highest inorganic scintillator of known light output up to 120,000 ph/MeV, is had splendid
Energy resolution (< 3%) has preferable energy linearity in wider energy range.Undoped and Eu2+Strontium iodide is adulterated to make
For a kind of scintillator again attention by inorganic scintillator field, associated research rapidly becomes inorganic scintillator research
Hot spot and forward position.Country's outgrowth strontium iodide crystal mainly uses Bridgman-Stockbarger method at present, and this method is in the presence of the device is complicated, growth
Process is not easy to observe, the drawbacks such as larger, easy to crack that grow crystal stress.
SrI2Fusing point (538 DEG C) is lower, no cleavage surface, within the scope of from melting temperature to room temperature without phase-change, is suitble to including
The melt method of Bridgman-Stockbarger method is grown.Due to SrI2For alkaline-earth halide, easily deliquesces and aoxidize, at present in the world
Generally use following growth technique: by anhydrous high-purity SrI2And EuI2Raw material weighing is packed into high purity quartz earthenware after mixing in proportion
After crucible, high-purity silica pot is sealed after vacuumizing, carries out crystal growth in crucible decline furnace.
But there are the following problems for Bridgman-Stockbarge method for growing iodate strontium crystal:
1) thermal expansion coefficient (0.6 × 10 of silica crucible-6℃-1) with thermal expansion coefficient (0.9-2.1 × 10 of iodate strontium crystal-5
℃-1) there are larger differences, in crystal growing process, crystals can gather biggish stress, and crystal is be easy to cause seriously to open
It splits；
2) strontium iodide melt easily reacts etch quartz crucible with silica crucible, and silica crucible is easy to produce in growth or temperature-fall period
Raw cracking phenomena, causes crystal growth to fail, I is caused when serious2The pollution of the nuisances such as steam, endangers health of human body；
3) iodate strontium crystal can only be enclosed in growth in silica crucible, can not be grown using seed crystal seeding mode, while also can not
Using reaction atmosphere (Reactive Atmosphere Processing abbreviation RAP) technology growth crystal, silica crucible is taken out
When vacuum, the denier water of internal residual, oxygen also can quality to crystal and performance cause to seriously affect；
4) growth cycle is longer, is suitble to growing large-size crystal, but be unsuitable for quickly preparing crystal.
Summary of the invention
Based on the above shortcomings, fast, crystal growth success rate that the purpose of the present invention is to provide a kind of speeds of growth
Monocrystal good quality high, obtained, the undoped and Eu for substantially reducing crystal production cost2+Adulterate strontium iodide (SrI2) crystal
Orientation growing by zone melting device and method.
The object of the present invention is achieved like this: the present invention provides the undoped and Eu of one kind2+Adulterate iodate strontium crystal
Orient growing by zone melting device, comprising: liftable support, the roller bearing screw rod platform supported by the liftable support, by stepping electricity
Machine control is fixed on the roller bearing screw rod by fixed bracket and is put down with the mobile thermal field mobile relative to the roller bearing screw rod platform
Platform and the quartz glass boiler tube for crossing the mobile thermal field, the growing container being placed in inside the quartz glass boiler tube.
Orientation growing by zone melting device provided by the invention, as protection cavity, can be determined using transparent quartz tube using seed crystal
To growth crystal, be conducive to the dynamic and observation in real time of crystal growing process, the crystal purity grown is high, stress is small and complete
Degree is high, has significant technical advantage.
Preferably, quartz glass boiler tube both ends are sealed using steel flange, and can connect vacuum pump or logical
Enter inert protective gas.
Preferably, the liftable support is equipped with multiple, and the height by adjusting each liftable support makes the life
It long vessel level or is tilted a certain angle.
Preferably, the mobile thermal field includes: insulating layer of furnace body；It is embedded in the heater of the insulating layer of furnace body；It is removable
It is installed on the light heat insulation material of the inside of the insulating layer of furnace body with unloading；With for in the mobile thermal field temperature carry out
Thermometric and the thermocouple for feeding back to temperature control system.
Preferably, the insulating layer of furnace body gathers light material using high purity aluminium oxide, and the heater is resistance wire heater.
Another aspect of the present invention provides one kind undoped and Eu2+The orientation growing by zone melting method of iodate strontium crystal is adulterated,
Include the following steps:
(1) anhydrous strontium iodide and iodate europium raw material are adequately mixed and are placed among the molten crucible in area, crucible is melted into area and is placed in
In the quartz glass boiler tube of above-mentioned orientation growing by zone melting device；
(2) the quartz glass boiler tube is vacuumized, or is passed through inertia or protective gas containing iodine；
(3) mobile thermal field is opened；
(4) step motor control program is set, the mobile thermal field is made to be moved to the other end from quartz glass boiler tube one end,
Then quick correcting action, so as to form polycrystal material ingot.
(5) polycrystal material ingot will be formed by be packed into such as growth crucible of target shape or grow the growing container of boat
It is interior, repeat above step (1)~(3)；
(6) step motor control program is set, is moved to the mobile thermal field from one end of the quartz glass boiler tube another
End；
(7) after crystal growth, the crystal grown is made to be in light heat insulation material region, in-situ annealing；
(8) crystal temperature effect is down to room temperature by setting cooling process, to obtain perfect crystal identical with the growing container shape.
After above (1) ~ (4) step process, raw material becomes the polycrystal material ingot with the transparent crystal grain of certain size, can be with
It effectively reduces raw material volume and excludes objectionable impurities.
This method is advantageously implemented the dynamic or observation in real time of crystal growth, and can use seed crystal inoculating process, obtains
The crystal of specific direction, meanwhile, the crystal top grown is in untethered state, has reserved space to the expansion of crystal, has had
Conducive to the timely release of crystals stress, the cracking of crystal is reduced, this method speed of growth is fast, the success rate of crystal growth
Height, monocrystal good quality obtained, therefore greatly reduce the production cost of crystal.
Detailed description of the invention
Fig. 1 is the undoped and Eu of an implementation form according to the present invention2+Adulterate strontium iodide crystal orientation growing by zone melting device
Structural schematic diagram；
Fig. 2 is the undoped and Eu of an implementation form according to the present invention2+It is moved in doping strontium iodide crystal orientation growing by zone melting device
Dynamic temperature field schematic diagram of internal structure；
1-1. stepper motor
1-2. roller bearing screw rod platform
1-3. Slider platform
1-4. liftable support
1-5. steel flange
1-6. fixes bracket
1-7. quartz glass boiler tube
1-8. moves thermal field
2-1. thermocouple
2-2. high purity aluminium oxide gathers light material
2-3. resistance wire heater
2-4. light heat insulation material
2-5. light heat insulation material
2-6. quartz glass boiler tube
2-7. crystal
2-8. melt
2-9. polycrystal material.
Specific embodiment
One embodiment of the invention is further described with reference to the accompanying drawing.
It, can be using transparent quartz tube as protection chamber when orienting area's clinkering crystalline substance since the fusing point of iodate strontium crystal is lower
Body is conducive to the dynamic or observation in real time of crystal growing process in this way；Crystal growth can carry out in inertia or reaction atmosphere,
It can also carry out in a vacuum；Crystal growth vessel can use silica crucible, can also use metal or graphite crucible, due to
The crucible top laid flat is opening-wide state, and the crystal top grown is in untethered state, has reserved sky to the expansion of crystal
Between, be conducive to the timely release of crystals stress；When orienting growing by zone melting, seed crystal can be placed in the side of crucible, adopted
It is inoculated with growth crystal with seed crystal, improves the success rate of crystal growth, and the crystal of specific direction can be obtained.
Based on the above advantages, the present invention provides one kind undoped and Eu2+Strontium iodide crystal orientation growing by zone melting device is adulterated,
Its overall structure is as shown in Figure 1.
The device includes liftable support 1-4, is supported by liftable support 1-4 and stepper motor 1-1 is used to control
Roller bearing screw rod platform 1-2, the rotation of roller bearing screw rod can drive Slider platform 1-3 to move back and forth, and mobile thermal field 1-8 is fixed on sliding block
On platform 1-3, by step motor control movement speed.The quartz glass both ends boiler tube 1-7 are by being fixed on roller bearing screw rod platform 1-2
The fixation bracket 1-6 at both ends is fixed, and crosses among mobile thermal field 1-8 as burner hearth.Growing container is placed in quartzy glass
Inside glass boiler tube 1-7.
Liftable support 1-4 is equipped with multiple, such as Fig. 1 show three, can by adjusting each bracket 1-4 height so that
Growth platform is in level or is inclined at an angle.
The quartz glass both ends boiler tube 1-7 are sealed using steel flange 1-5, can connect vacuum pump or logical inertia protection gas
Body.
Mobile thermal field 1-8 internal structure as shown in Fig. 2, gather light material 2-2 as insulating layer of furnace body using high purity aluminium oxide,
It is embedded in resistance wire heater 2-3.Light heat insulation material 2-4,2-5 are removably installed in the inside of insulating layer of furnace body.By thermoelectricity
Even 2-1 thermometric simultaneously feeds back to temperature control system.
By changing the thickness and length size of light heat insulation material 2-4,2-5, melting zone and crystallization sector width, shape is adjusted
Temperature field and temperature gradient at suitable crystal growth.
Also as shown in Fig. 2, the growth crucible equipped with polycrystal material 2-9 is placed in quartz glass boiler tube 2-6, it is appropriate to adjust
Temperature polycrystal material 2-9 can be realized and switch to melt 2-8 and then shape by the relative movement of mobile thermal field 1-8 and growth crucible
At the crystal growing process of crystal 2-7.
The present invention also provides the undoped and Eu of one kind2+The orientation growing by zone melting method of iodate strontium crystal is adulterated, to realize height
Quality is undoped and Eu2+Adulterate the controllable preparation of iodate strontium crystal.Crystal growing process includes the following steps.
1) anhydrous strontium iodide and iodate europium raw material are adequately mixed and are placed among the molten crucible in area, area melts crucible and is placed in
In the quartz ampoule burner hearth of above-mentioned orientation growing by zone melting device, burner hearth can be horizontal, can also be tilted a certain angle.
2) it opens vacuum pump to vacuumize quartz ampoule burner hearth, is generally kept in vacuum degree 1 × 10-2Pa or so, can also
To be passed through inertia or protective gas containing iodine.
3) the mobile thermal field as heating device is opened, so that melting zone temperature is higher than 100~200 DEG C of fusing point, preheating zone, crystallization
Area's temperature is lower than 50~100 DEG C of fusing point, melting zone 20~100mm of width.
4) step motor control program is set, so that mobile thermal field is moved to the other end from quartz ampoule burner hearth one end, then fastly
Fast correcting action.Wherein, it is mobile with 10~20mm/ hours speed preferably to move thermal field.It is displaced program by setting,
The process can be repeated several times.
After above step is handled, raw material becomes the polycrystal material ingot with the transparent crystal grain of certain size, can effectively subtract
Few raw material volume and exclusion objectionable impurities.
5) the polycrystal material ingot of certain mass is packed into the growth crucible or growth boat of target shape, repeats above step
1)~3).
6) step motor control program is set, mobile thermal field is made to be moved to the other end from one end of quartzy burner hearth.It is wherein excellent
Selection of land, the rate that rate travel is 0.1~5mm/ hours, more preferably 0.1-2mm/h.
7) after crystal growth, so that the crystal grown is in light heat insulation material region, crystal is in 400-500
In-situ annealing at DEG C, to eliminate as much as crystals thermal stress；
8) crystal temperature effect is down to room temperature by setting cooling process, can be obtained identical with aforementioned growth crucible or growth boat-shaped shape
Perfect crystal is preferably advisable with 5-20 DEG C/h of rate of temperature fall.
Orientation growing by zone melting device provided by the invention, as protection cavity, can be determined using transparent quartz tube using seed crystal
To growth crystal, be conducive to the dynamic and observation in real time of crystal growing process, the crystal purity grown is high, stress is small and complete
Degree is high, has significant technical advantage.
Technical solution of the present invention is elaborated by following examples further below.
Embodiment 1
Undoped SrI2Monocrystal orientation area's clinkering crystalline substance preparation process includes the following steps:
By height 90mm, length 300mm, thickness 2.5mm, bottom is placed in internal diameter 120mm, length with the quartz boat of 90 ° of cone angles
In the suprasil burner hearth of 1500mm, thickness 3mm.
By the SrI of 1kg purity >=99.99%2Powder is added in quartz boat, opens vacuum pump and vacuumizes quartzy burner hearth
To 1 × 10-2Pa。
Mobile thermal field internal lightweight thermal insulation material is removed, entire quartz boat is made to be in heating zone, opens heating system, heating
To 200 DEG C and 4 hours are kept the temperature, sufficiently excludes the absorption water in raw material.
Heating system is closed, light heat insulation material is placed inside mobile thermal field heating device, adjusts melting zone width 30mm,
And it is in melting zone at the cone angle of quartz boat bottom.
Heating system is opened, 600 DEG C of melting zone temperature is warming up to, melts raw material at quartz boat cone angle sufficiently, crystal region temperature
Degree is maintained at 450 DEG C.
Step motor control program is set, so that melting zone is moved to the other end from quartz boat cone angle with 10mm/h speed, so
Afterwards with 600mm/h speed correcting action, start to move with 10mm/h speed again after pause 30min, and repeat it is above into
Journey 10 times.
Step motor control program is set, melting zone is made to be moved to the other end from quartz boat cone angle with 2mm/h speed, quartz
Crystal enters light heat insulation material region in boat, and setting program, which cools down, carries out in-situ annealing to crystal, can be obtained and quartz boat
The identical perfect crystal of shape.
Embodiment 2
Eu2+Adulterate SrI2Clinkering crystalline substance preparation process in crystal orientation area includes the following steps:
By the SrI of 800g purity >=99.99%2The EuI of powder and 20g purity >=99.99%2After mixing, it is added to platinum
In golden crucible, platinum crucible diameter 30mm × length 300mm, thickness 0.3mm, bottom belt have capillary structure；Then by platinum earthenware
Crucible is placed in internal diameter 40mm × length 1500mm, in the suprasil burner hearth of thickness 3mm；Platinum crucible and quartz ampoule contact surface are placed
One layer of 2mm thickness ceramic fiber blanket prevents quartz ampoule hot-spot, and prevents platinum crucible mobile.
Liftable support is adjusted, quartzy burner hearth is made to tilt 30 °, at this point, platinum crucible top and capillary end are tilted in 30 °,
Be conducive to melt and fill full entire crucible.
Mobile thermal field internal lightweight thermal insulation material is removed, entire platinum crucible is made to be in heating zone.Vacuum pump is opened by stone
English burner hearth is evacuated to 1 × 10-2Pa opens heating system, is warming up to 200 DEG C and keeps the temperature 4 hours, sufficiently excludes the suction in raw material
Attached water.
Heating system is closed, high-purity Ar gas is filled with into burner hearth, makes to keep micro-positive pressure inside burner hearth.Then in mobile thermal field
Inside addition light heat insulation material, adjusts melting zone width 30mm.
Heating system is opened, 600 DEG C of melting zone temperature is warming up to, melts raw material in platinum crucible sufficiently, crystal region temperature
It is maintained at 450 DEG C.
Step motor control program is set, is moved to melting zone from platinum crucible capillary structure with 10mm/h speed another
End starts to move with 10mm/h speed again then with 600mm/h speed correcting action after pause 30min, and repeat with
Upper process 15 times.
Step motor control program is set, is moved to melting zone from platinum crucible capillary structure with 1mm/h speed another
It holds, crystal enters light heat insulation material region in crucible, and setting program, which cools down, carries out in-situ annealing to crystal, can be obtained
SrI2: Eu crystal.
Implementation of the invention is not limited to the example above.According to the above description, the present invention is illustrated in those skilled in the art
More improvement and other implementation forms.Therefore, above description is only used as example for illustrating, and is with to art technology
It is provided for the purpose of the optimal modality that personnel instruct implementation of the invention.Purport that as long as it does not depart from the spirit of the invention, can be substantive
It is changed to other structures and/or function to property.
For example, the quartz boat in embodiment 1, can also be used graphite boat or metal boat, only it need to ensure material at high temperature not
With strontium iodide or Eu2+Doping strontium iodide melt chemically reacts.
It is also possible to platinum crucible bottom wicking portion in embodiment 2 being changed to placement oriented seed, that is, seed crystal can be used
Inoculation growth；Depending on crucible size growth crystalline size needed for, suprasil size of burner hearth can then change according to crucible size.
Claims (6)
1. the undoped and Eu of one kind2+Adulterate the orientation growing by zone melting device of iodate strontium crystal characterized by comprising
Liftable support (1-4),
The roller bearing screw rod platform (1-2) supported by the liftable support,
It is controlled by stepper motor (1-1) with the mobile thermal field (1-8) mobile relative to the roller bearing screw rod platform (1-2),
The roller bearing screw rod platform is fixed on by fixed bracket (1-6) and crosses the quartz glass of the mobile thermal field (1-8)
Boiler tube (1-7),
It is placed in the internal growing container of the quartz glass boiler tube (1-7).
2. according to claim 1 undoped and Eu2+The orientation growing by zone melting device of iodate strontium crystal is adulterated, feature exists
In,
The quartz glass boiler tube both ends (1-7) are sealed using steel flange, and can be connected vacuum pump or be passed through inertia
Protective gas.
3. according to claim 1 undoped and Eu2+The orientation growing by zone melting device of iodate strontium crystal is adulterated, feature exists
It is equipped in, the liftable support (1-4) multiple, the height by adjusting each liftable support (1-4) makes the growth
Vessel level or inclination.
4. as claimed in any of claims 1 to 3 undoped and Eu2+Adulterate the orientation growing by zone melting of iodate strontium crystal
Device, which is characterized in that
The mobile thermal field (1-8) includes: insulating layer of furnace body；It is embedded in the heater of the insulating layer of furnace body；Removably pacify
The light heat insulation material of inside loaded on the insulating layer of furnace body；With for in the mobile thermal field temperature carry out thermometric simultaneously
Feed back to the thermocouple (2-1) of temperature control system.
5. according to claim 4 undoped and Eu2+The orientation growing by zone melting device of iodate strontium crystal is adulterated, feature exists
In,
The insulating layer of furnace body gathers light material using high purity aluminium oxide, and the heater is resistance wire heater (2-3).
6. the undoped and Eu of one kind2+Adulterate the orientation growing by zone melting method of iodate strontium crystal, which is characterized in that including walking as follows
It is rapid:
(1) anhydrous strontium iodide and iodate europium raw material are adequately mixed and are placed among the molten crucible in area, crucible is melted into area and is placed in
In the quartz glass boiler tube of orientation growing by zone melting device as described in claim 1；
(2) the quartz glass boiler tube is vacuumized, or is passed through inertia or protective gas containing iodine；
(3) mobile thermal field is opened；
(4) step motor control program is set, is moved to the mobile thermal field from one end of the quartz glass boiler tube another
It holds, then quick correcting action, so as to form polycrystal material ingot；
(5) polycrystal material ingot will be formed by be packed into the growing container of target shape, repeats above step (1)~(3)；
(6) step motor control program is set, is moved to the mobile thermal field from one end of the quartz glass boiler tube another
End；
(7) after crystal growth, the crystal grown is made to be in light heat insulation material region, in-situ annealing；
(8) crystal temperature effect is down to room temperature by setting cooling process, to obtain perfect crystal identical with the growing container shape.
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| CN201710703145.1A CN109402724B (en) | 2017-08-16 | 2017-08-16 | Non-doped and Eu2+Directional zone-melting growth device and method for doped strontium iodide crystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877785A (en) * | 2020-12-31 | 2021-06-01 | 云南农业大学 | Crystal material zone melting purification device |
| CN114525590A (en) * | 2022-01-26 | 2022-05-24 | 深圳先进电子材料国际创新研究院 | Multifunctional crystal growth device |
| CN116676669A (en) * | 2023-08-03 | 2023-09-01 | 北京奇峰蓝达光学科技发展有限公司 | Equipment and method for purifying and treating calcium fluoride crystal growth raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899716A (en) * | 2012-09-14 | 2013-01-30 | 北京京运通科技股份有限公司 | Bidirectionally translational mechanism and zone-melting monocrystal furnace |
| CN103789832A (en) * | 2014-02-17 | 2014-05-14 | 中国科学院上海硅酸盐研究所 | Nested crucible for growing strontium iodide crystal and method for growing strontium iodide crystal |
| CN103818942A (en) * | 2014-01-22 | 2014-05-28 | 中国科学院上海硅酸盐研究所 | Method for preparing high-purity anhydrous strontium iodide |
-
2017
- 2017-08-16 CN CN201710703145.1A patent/CN109402724B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899716A (en) * | 2012-09-14 | 2013-01-30 | 北京京运通科技股份有限公司 | Bidirectionally translational mechanism and zone-melting monocrystal furnace |
| CN103818942A (en) * | 2014-01-22 | 2014-05-28 | 中国科学院上海硅酸盐研究所 | Method for preparing high-purity anhydrous strontium iodide |
| CN103789832A (en) * | 2014-02-17 | 2014-05-14 | 中国科学院上海硅酸盐研究所 | Nested crucible for growing strontium iodide crystal and method for growing strontium iodide crystal |
Non-Patent Citations (1)
| Title |
|---|
| RAJA ARUMUGAM等: "The Purification Process On Scintillator Material (SrI2: Eu) By Zone-refinement Technique", 《AIP CONF.PROC.》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877785A (en) * | 2020-12-31 | 2021-06-01 | 云南农业大学 | Crystal material zone melting purification device |
| CN114525590A (en) * | 2022-01-26 | 2022-05-24 | 深圳先进电子材料国际创新研究院 | Multifunctional crystal growth device |
| CN116676669A (en) * | 2023-08-03 | 2023-09-01 | 北京奇峰蓝达光学科技发展有限公司 | Equipment and method for purifying and treating calcium fluoride crystal growth raw material |
| CN116676669B (en) * | 2023-08-03 | 2023-12-08 | 北京奇峰蓝达光学科技发展有限公司 | Equipment and method for purifying and treating calcium fluoride crystal growth raw material |
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|---|---|
| CN109402724B (en) | 2020-12-11 |
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