CN104532342B - A kind of EFG technique grows the growing method of micropore sapphire crystal - Google Patents
A kind of EFG technique grows the growing method of micropore sapphire crystal Download PDFInfo
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- CN104532342B CN104532342B CN201410765560.6A CN201410765560A CN104532342B CN 104532342 B CN104532342 B CN 104532342B CN 201410765560 A CN201410765560 A CN 201410765560A CN 104532342 B CN104532342 B CN 104532342B
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Abstract
The invention discloses the growing method that a kind of EFG technique grows micropore sapphire crystal, S01, assembly jig：Mould wool opening is carefully stitched, the molybdenum filament or 3~15, tungsten filament of equidistant a diameter of below the 0.5mm of filling in capillary seam, and molybdenum filament or tungsten filament expose 1 mm of die top~10mm, and fixed molybdenum filament or tungsten filament are vertically arranged molybdenum filament or tungsten filament；S02, shove charge；S03, vacuumizes and applying argon gas；S04, heats up；S05, seeding；S06, shouldering；S07, isodiametric growth；S08, cooling；The present invention can grow below diameter 0.5mm on sapphire crystal, the micropore of length more than 15mm, be that common drilling method and laser boring to be realized；The length of micropore can accomplish several meters or more than ten meters long, be limited with the stroke of long crystal furnace.
Description
Technical field
The life of micropore sapphire crystal is grown the present invention relates to sapphire production technical field, more particularly to a kind of EFG technique
Method long.
Background technology
Can grow to be processed with standard machinery and include the laser boring micropore to be processed, microcell length can be with
More than 15mm is reached, common boring method processes sapphire crystal, the hole for below 0.5mm, when drilling depth is more than 15mm
During the above, drill bit intensity is not reached, and after laser boring, micropore makes melt be still present in micropore due to capillarity, it is impossible to
Achieve the goal.
There is sapphire crystal good through performance to be used for many measurements in visible ray to 5.6um spectral regions
The optical window material of analytical instrument.The anisotropy of sapphire crystal, is applied to waveguide laser cavity, surface acoustic wave filtering
Device, delay line, ultrasonic wave transport element；The hardness (Mohs degree 9) of sapphire crystal is only second to diamond, he have hardness and
The series of characteristics such as the characteristics of intensity is high, wear-resistant, heat-resisting ability is strong and stable chemical nature, acid-alkali-corrosive-resisting are wide
It is general to be applied to high power laser light window, high temperature resistant, high pressure, resistance to high-speed friction, the observation of container or the vacuum tank such as be able to bear strong corrosion
Heat sink of window and optical window and projecting apparatus etc..
In the prior art, flame method growth micropore sapphire due to thermograde it is excessive and cannot growth diameter be more than 50mm
Monocrystalline and crystal defect and inner-stress value it is higher, range of application is greatly limited.Czochralski method, kyropoulos, heat are handed over
Change the methods such as method, Bridgman-Stockbarger method can growing large-size sapphire crystal, but they need by multiple high rigidity cut, into
After a series of heavy machinings such as type, grinding, applicable shape and size can be made, operation is more complicated；High cost and
It is time-consuming；Crystalline material utilization rate is relatively low, and operating efficiency is not high, and cost remains high.
The hardness (Mohs degree 9) of sapphire crystal is only second to diamond, just because of its high rigidity and high intensity
Characteristic, sapphire is difficult to be processed, the hole for below 0.5mm, and when drilling depth is more than more than 15mm, drill bit intensity is not up to
Arrive, after laser boring, micropore makes melt be still present in micropore due to capillarity, it is impossible to achieve the goal.
The content of the invention
Instant invention overcomes the deficiencies in the prior art, there is provided a kind of EFG technique grows the growth side of micropore sapphire crystal
Method, can process below diameter 0.5mm on sapphire crystal, and the micropore of length more than 15mm, the length of micropore can be done
It is long to several meters or more than ten meters, it is limited with the stroke of long crystal furnace.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of EFG technique grows the growing method of micropore sapphire crystal, comprises the following steps：
S01, assembly jig：Mould wool opening is carefully stitched, the molybdenum filament or tungsten of equidistant a diameter of below the 0.5mm of filling in capillary seam
Silk 3~15, molybdenum filament or tungsten filament expose 1 mm of die top~10mm, and fixed molybdenum filament or tungsten filament make molybdenum filament or tungsten filament set vertically
Put；
S02, shove charge：From M to or C to seed crystal, seed crystal is fixed on seedholder, load molybdenum crucible 5kg~7kg flames
Molten method particle, mould mouthful blowing grain；
S03, vacuumizes and applying argon gas：Close fire door, open mechanical pump vacuumized, vacuum reach 3Pa~
Vacuum equipment, applying argon gas to standard atmospheric pressure are closed during 10Pa；
S04, heats up：Open heating power supply and be warmed up to 2100 DEG C~2300 DEG C, melt mould mouthful material grain；
S05, seeding：Seed crystal is turned down after after the material grain fusing of mould mouthful, seeding is carried out after roasting crystalline substance is carried out to seed crystal, make seed
Crystal block and melt welding, and upwards with 5mm/h~20mm/h lifting seed crystals；
S06, shouldering：The seed rod rate of pulling is adjusted to shouldering and limits speed, crystal is made along seed crystal from mould by shouldering
To outgrowth in the middle of tool；
S07, isodiametric growth：After shouldering terminates, isodiametric growth is carried out, improve pulling rate to 30 mm/h~40mm/h；
S08, cooling：Crystal break away from moulds is pulled, starts cooling, room temperature dropped to after 10h and is come out of the stove.
More preferably, shouldering limits speed as 20mm/h ~ 30mm/h.
More preferably, mould is that flat-die has or oblique angle mould.
More preferably, mold material is molybdenum or tungsten or iridium.
Compared with prior art, beneficial effects of the present invention have：The present invention can grow diameter on sapphire crystal
The micropore of below 0.5mm, more than length 15mm, is that common drilling method and laser boring to be realized；Micropore
Length can accomplish several meters or more than ten meters long, be limited with the stroke of long crystal furnace.
Brief description of the drawings
Fig. 1 is the growing method schematic flow sheet that a kind of EFG technique of the invention grows micropore sapphire crystal；
Fig. 2 is invention assembling mold structure schematic diagram.
Specific embodiment
The present invention is further described below in conjunction with the accompanying drawings.
As shown in figure 1, a kind of EFG technique grows the growing method of micropore sapphire crystal, comprise the following steps：
S01, assembly jig：As shown in Fig. 2 the wool opening of mould 1 is carefully stitched, in capillary seam the equidistant a diameter of 0.5mm of filling with
Under molybdenum filament 2（The present embodiment uses molybdenum filament, it is also possible to use tungsten filament）3~15, molybdenum filament or tungsten filament expose the mm of die top 1
~10mm, fixed molybdenum filament 2, is vertically arranged molybdenum filament 2；
S02, shove charge：From M to or C to seed crystal, seed crystal is fixed on seedholder, load molybdenum crucible 5kg~7kg flames
Molten method particle, mould mouthful blowing grain；
S03, vacuumizes and applying argon gas：Close fire door, open mechanical pump vacuumized, vacuum reach 3Pa~
Vacuum equipment, applying argon gas to standard atmospheric pressure are closed during 10Pa；
S04, heats up：Open heating power supply and be warmed up to 2100 DEG C~2300 DEG C, melt mould mouthful material grain；
S05, seeding：Seed crystal is turned down after after the material grain fusing of mould mouthful, seeding is carried out after roasting crystalline substance is carried out to seed crystal, make seed
Crystal block and melt welding, and upwards with 5mm/h~20mm/h lifting seed crystals；
S06, shouldering：The seed rod rate of pulling is adjusted to shouldering and limits speed 20mm/h ~ 30mm/h, crystal is made by shouldering
Along seed crystal from the middle of mould to outgrowth；
S07, isodiametric growth：After shouldering terminates, isodiametric growth is carried out, improve pulling rate to 30 mm/h~40mm/h；
S08, cooling：Crystal break away from moulds is pulled, starts cooling, room temperature dropped to after 10h and is come out of the stove.
Mould is that flat-die has or oblique angle mould, and mold material is molybdenum or tungsten or iridium.
The above is only the preferred embodiment of the present invention, it should be pointed out that：Come for those skilled in the art
Say, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (2)
1. a kind of EFG technique grows the growing method of micropore sapphire crystal, it is characterised in that comprise the following steps：
S01, assembly jig：Mould wool opening is carefully stitched, if the equidistant molybdenum filament or tungsten filament for clogging a diameter of below 0.5mm in capillary seam
Dry root, molybdenum filament or tungsten filament expose die top 1mm~10mm, and fixed molybdenum filament or tungsten filament are vertically arranged molybdenum filament or tungsten filament；
S02, shove charge：From M to or C to seed crystal, seed crystal is fixed on seedholder, load molybdenum crucible 5kg~7kg flame melt methods
Particle, mould mouthful blowing grain；
S03, vacuumizes and applying argon gas：Fire door is closed, mechanical pump is opened and is vacuumized, vacuum is closed when reaching 3Pa~10Pa
Close vacuum equipment, applying argon gas to standard atmospheric pressure；
S04, heats up：Open heating power supply and be warmed up to 2100 DEG C~2300 DEG C, melt mould mouthful material grain；
S05, seeding：Seed crystal is turned down after after the material grain fusing of mould mouthful, seeding is carried out after roasting crystalline substance is carried out to seed crystal, make seed crystal blocks
With melt welding, and upwards with 5mm/h~20mm/h lift seed crystal；
S06, shouldering：The seed rod rate of pulling is adjusted to shouldering and limits speed, being lowered the temperature by shouldering makes crystal along seed crystal from mould
To outgrowth in the middle of tool；
S07, isodiametric growth：After shouldering terminates, isodiametric growth is carried out, improve pulling rate to 30mm/h~40mm/h；
S08, cooling：Crystal break away from moulds is pulled, starts cooling, room temperature dropped to after 10h and is come out of the stove；
The shouldering limits speed as 20mm/h~30mm/h；
The mould is that flat-die has or oblique angle mould；
The mold material is molybdenum or tungsten or iridium.
2. a kind of EFG technique according to claim 1 grows the growing method of micropore sapphire crystal, it is characterised in that institute
State the molybdenum filament or 3~15, tungsten filament of equidistant a diameter of below the 0.5mm of filling in step S01 capillarys seam.
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| CN107059114A (en) * | 2017-03-08 | 2017-08-18 | 同济大学 | The mould and method of a kind of EFG technique growth crystal optical fibre |
| CN108456926B (en) * | 2018-02-27 | 2020-08-14 | 同济大学 | Method for growing crystal fiber core in crystal cladding |
| CN109338467A (en) * | 2018-10-31 | 2019-02-15 | 江苏师范大学 | A kind of preparation method of coloring uniform color jewel |
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| CN103469305A (en) * | 2013-08-23 | 2013-12-25 | 江苏中电振华晶体技术有限公司 | Sapphire crystal nucleation method and special nucleation equipment therefor |
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| CN202482487U (en) * | 2012-01-18 | 2012-10-10 | 鸿福晶体科技(安徽)有限公司 | Crystal multi-die growth device through adopting EFG (edge-defined, film-fed growth) method |
| CN102586866A (en) * | 2012-02-09 | 2012-07-18 | 上海施科特光电材料有限公司 | Method for restraining bulbs in process of growing slice-shaped sapphire in guiding mold mode |
| CN103469305A (en) * | 2013-08-23 | 2013-12-25 | 江苏中电振华晶体技术有限公司 | Sapphire crystal nucleation method and special nucleation equipment therefor |
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