CN208517586U - Top seed crystal heat-exchanging method growing sapphire crystal - Google Patents
Top seed crystal heat-exchanging method growing sapphire crystal Download PDFInfo
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- CN208517586U CN208517586U CN201820505891.XU CN201820505891U CN208517586U CN 208517586 U CN208517586 U CN 208517586U CN 201820505891 U CN201820505891 U CN 201820505891U CN 208517586 U CN208517586 U CN 208517586U
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- Prior art keywords
- crystal
- heat
- seed crystal
- heat exchanger
- growth
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- 239000013078 crystal Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 20
- 239000010980 sapphire Substances 0.000 title claims abstract description 19
- 239000001307 helium Substances 0.000 claims abstract description 18
- 229910052734 helium Inorganic materials 0.000 claims abstract description 18
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 7
- 239000010937 tungsten Substances 0.000 claims abstract description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000009413 insulation Methods 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 239000011733 molybdenum Substances 0.000 claims abstract description 3
- 238000012544 monitoring process Methods 0.000 claims abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000024241 parasitism Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model relates to a kind of top seed crystal heat-exchanging method growing sapphire crystals, it mainly includes a tubular tungsten heater, there is a liftable heat exchanger in its top, circulated in heat exchanger through the compressed helium of helium compressor, in crystal growth by technique require can pressure to compressed gas and flow be adjusted and be combined seed crystal preferably with the melt in crucible by adjusting the position of heat exchange bar；Heat exchange bar lower end has a collet, and seed crystal is housed thereon.The fixation of the achievable seed crystal of heat exchanger, the rotation and lifting of crystal.With molybdenum crucible, heat-insulation system is tungsten insulating layer.External photoelectric pyrometer, monitoring in-furnace temperature variation.Helium gas flow in crystal growing process in heating power and heat exchanger is respectively by programmable automatic control system independent control.Melt, seeding, crystal growth initial stage, cooling growth are specifically included that using the method for above-mentioned apparatus growing sapphire crystal.
Description
Technical field
The utility model relates to sapphire crystal growth technical fields, are a kind of top seed crystal heat-exchanging method growing sapphires
The technology of crystal.
Background technique
Synthetic sapphire crystal (α-Al2O3) it is a kind of crystalline material haveing excellent performance, there is high rigidity, high-melting-point, steady
Fixed chemical property, good mechanical performance, excellent heat conductivity and electric insulating quality.In ultraviolet, visible, infrared band model
High transmittance is all had in enclosing, is up to 85% in 3~5 mu m waveband transmitances, thus is widely used in high-end technology field, such as
Various jewels, optical element, laser, microelectronics, the substrate material of photoelectronic industry and the ideal window of military installation
Material etc..In recent years, the rapid development of national defence, military affairs and infrared technique proposes higher quality to sapphire crystal material
It is required that.
Currently, the mainstream technology of production high quality LED substrate sapphire crystal mainly has heat-exchanging method, temperature gradient method
With Bridgman-Stockbarger method etc..Heat-exchanging method growing sapphire have thermal field is stable, crucible internal temperature gradient is small, control precision with from
The advantages that dynamicization degree is high.But existing hot swapping seed crystal is located at crucible bottom, and when seeding is not easy to observe, and is easy to appear more
Brilliant phenomenon；The top that melt is in growth interface is unfavorable for the discharge of impurity.Meanwhile the heap of the carbon and other impurities at the top of thermal field
Product object can be deposited in solid liquid interface when falling into crucible, form other nucleus crystallizations so as to cause polycrystalline generation；Crystal growth is whole
In be passed through helium, cause there are a large amount of bubbles in crystal, the presence of bubble causes light to scatter and reduces the photopermeability energy of crystal.
Summary of the invention
The object of the present invention is to provide a kind of methods of growing sapphire crystal, blue precious to solve traditional heat-exchanging method growth
There are a large amount of bubbles and the problem for being easy to crack for stone, and the present invention uses improved heat exchanger, in new growing system, in crystalline substance
Body early growth period uses top seed crystal heat-exchanging method seeding to cause polycrystalline to generate to avoid parasitism nucleation；Crystal seeding is put
Accurately control in-furnace temperature and temperature gradient by adjusting heater helium gas flow and heater power after shoulder, promote crystal after
Continuous growth, realizes the control to crystal growth.
A kind of sapphire crystal growth method, key step include:
(1) high purity aluminium oxide powder is pressed into the cylindric material block that diameter is slightly less than crucible internal diameter, at 800 DEG C ~ 1500 DEG C
Sintering；Broken grain material is dried for standby after should carefully being cleaned using ultrasonic wave.
(2) raw material is packed into crucible, and crucible is placed in heat-exchanging furnace, increased resistance heater power, make in crucible
Melting sources, while being passed through helium in heat exchanger and guaranteeing that seed crystal is not melted.
(3) incrementally increase helium intake, reduce seed temperature, under shake seed crystal make its with obtained at melt contacts it is good
Solid liquid interface, seed crystal and melt contacts start crystalline growth, realize the necking down and shouldering to crystal by control helium gas flow
Control.
(4) continue to increase helium gas flow, control rate of crystalline growth, seed crystal and liquid level contact position start crystalline growth；When
When crystal growth is to certain size, stop the power for being passed through helium and slowly reducing crystal heater, promotes crystallization completely；In this way
It avoids whole process and is passed through the generation that helium causes a large amount of bubbles in crystals, improve sapphire crystal quality, reduce hot friendship
Method production cost is changed, growth cycle is shortened.
(5) crystal growth terminates, and furnace temperature is down to room temperature with the rate of 30 45 DEG C/h, takes out crystal.
By above technical scheme as it can be seen that the utility model patent provides new heat-exchanging furnace device and new growing system,
Crystal growth initial stage use at the top of seed crystal heat-exchanging method seeding to avoid sidewall of crucible spontaneous nucleation；After crystal seeding, shouldering
Promote crystal continued growth by control heater helium gas flow and reduction heater power, realizes the control to crystal growth
System,
Advantages of the present invention are as follows: avoid traditional heat-exchanging method whole process and be passed through a large amount of bubbles in crystals caused by helium
It generates, improves sapphire crystal quality, and reduce the production cost of heat-exchanging method, shorten growth cycle.
Detailed description of the invention
Fig. 1 is the main view of top seed crystal heat exchange sapphire crystal growing furnace.
Specific embodiment
A kind of sapphire crystal growth device, it mainly includes a tubular tungsten heater, and there is stretchable heat in top
Exchanger has a collet in heat exchanger lower end, seed crystal is housed thereon.Using molybdenum crucible, heat-insulation system is tungsten heat preservation
Layer.External photoelectric pyrometer, monitoring in-furnace temperature variation.Helium stream in crystal growing process in heating power and heat exchanger
Amount is respectively by programmable automatic control system independent control.
The growth of sapphire crystal is carried out with above-mentioned improvement heat-exchanging method growing technology, comprising the following steps:
(1) selection and processing of raw material
High purity aluminium oxide powder is pressed into the cylindric material block that diameter is slightly less than crucible internal diameter, is sintered at 1000 DEG C；Broken grain
Material is dried for standby after should carefully being cleaned using ultrasonic wave.
(2) raw material shove charge
The processed raw material 80kg of step 1 is put into bottom size to be 380 × 400 crucible of φ and crucible is placed in heat exchange
In furnace.
(3) using improvement heat-exchanging method growing sapphire monocrystalline
Heat-exchanging furnace is evacuated to 10Pa, is started to warm up to 2030 DEG C, is filled with high-purity argon gas as protective gas to being
Unite positive pressure 3000pa；It keeps helium gas flow 1.5L/min constant, increase heater power and is warming up to 2070 DEG C, constant temperature 2 hours
It is completely melt to raw material；Under shake seed crystal and make it and obtain good solid liquid interface at melt contacts, persistently increased with the speedup of 1L/h
Add helium throughput, promotes crystal preliminary growth；When it is 2,050 2055 DEG C that crystal cooling, which grows into temperature, stopping is passed through helium
Gas slowly reduces the power of heater, crystal structure is promoted to complete；After to crystal growth, it is cooled to 45 DEG C/h rate
Room temperature takes out crystal.
Claims (1)
1. a kind of top seed crystal heat-exchanging method growing sapphire crystal includes mainly a tubular tungsten heater, is provided with one
A molybdenum crucible, outside are equipped with tungsten insulating layer, it is characterised in that: have a liftable heat exchanger, heat exchange above crucible
Device lower end has a collet, and sapphire seed crystal is housed thereon, and heat-insulation system is tungsten insulating layer, external photoelectric pyrometer, monitoring
In-furnace temperature changes, and the helium gas flow in crystal growing process in heating power and heat exchanger is automatically controlled by programmable respectively
System independent control.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820505891.XU CN208517586U (en) | 2018-04-11 | 2018-04-11 | Top seed crystal heat-exchanging method growing sapphire crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820505891.XU CN208517586U (en) | 2018-04-11 | 2018-04-11 | Top seed crystal heat-exchanging method growing sapphire crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN208517586U true CN208517586U (en) | 2019-02-19 |
Family
ID=65341847
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201820505891.XU Expired - Fee Related CN208517586U (en) | 2018-04-11 | 2018-04-11 | Top seed crystal heat-exchanging method growing sapphire crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN208517586U (en) |
-
2018
- 2018-04-11 CN CN201820505891.XU patent/CN208517586U/en not_active Expired - Fee Related
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| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190219 |