CN101831712A - Crystal annealing device in growth furnace - Google Patents
Crystal annealing device in growth furnace Download PDFInfo
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- CN101831712A CN101831712A CN200910111250A CN200910111250A CN101831712A CN 101831712 A CN101831712 A CN 101831712A CN 200910111250 A CN200910111250 A CN 200910111250A CN 200910111250 A CN200910111250 A CN 200910111250A CN 101831712 A CN101831712 A CN 101831712A
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Abstract
The invention relates to a crystal annealing device in a growth furnace. The heating power of a heat chromium-aluminum high-temperature heating wire which is wound on an inner layer and an outer layer of heat insulating covers is adjusted by measuring the temperatures of two double platinum-rhodium thermocouples, and a heating source is provided; and an annealing space with the relatively small temperature gradient is formed in the upper heat insulating cover, and then the temperature gradients on a head part and a tail part of the crystal are smaller, so that an inner thermal stress of the crystal can be reduced. By using the method, the high-temperature crystal with the low internal stress can be grown, the crystal can be directly oriented and cut after annealing of crystal growth and crystal elements with all kinds of specifications are prepared without long-time annealing outside the furnace, so that the internal stress of the crystal is greatly reduced, the internal defects are reduced, the efficiency is greatly improved, and the device has simple structure and low manufacturing cost and is suitable for batch production.
Description
Technical field
The invention belongs to the artificial lens preparing technical field, particularly relate to a kind of structure and principle of crystal annealing device in growth furnace.
Background technology
Growing crystal is one of the most general growing method from pure melt.The biggest advantage of pure crystal growth from melt is the speed of growth more much higher than additive method, secondly is that the relative impurity parcel of crystal that grows lacks, but higher with the crystal thermal stresses of this method growth, phenomenons such as dislocation and crystal boundary are comparatively serious.
Adopt pure melt method of pulling up can grow dystectic functional crystal, mix cerium yttrium luetcium silicate etc. such as laser crystals yttrium iron garnet and scintillation crystal, these crystal growth temperatures are generally near 2000 ℃.After crystal growth finishes, need progressively reduce heating power, slowly drop to room temperature.In temperature-fall period, the crystalline head and tail temperature difference is very big, and reason is: also in crucible or the crucible oral area, crucible is subjected to Medium frequency induction, is heating element for crystal bottom, is surrounded by lagging material layer by layer simultaneously, and its temperature is very high; And the crystal head has gone out last stay-warm case or on the mouth of last stay-warm case, itself do not produce heat, and its temperature is well below mouth of pot.A whole like this crystal is at head low temperature, slowly cools to room temperature under the afterbody pyritous state, and the main stress of crystalline is just very big like this.Such crystal stress can cause the generation of various microdefects, and these defectives are fixed along with the crystalline cooling.Subsequent anneal is carried out in the crystal growth back that finishes outside stove because the annealed temperature is difficult to higher (generally following at 1300 degree), so the crystalline internal stress and can't outside follow-up stove, anneal because of the defective that thermal stresses causes in discharged fully and solved.The extra outer annealing of stove simultaneously also needs long annealing time.
If can search out a kind of method, reduce head and tail temperature difference in the crystal temperature-fall period, just can effectively reduce the crystal thermal stresses, crystal does not need extra stove to anneal outward yet simultaneously.
Summary of the invention
The present invention relates to a kind of design of crystal annealing device in growth furnace.The present invention adopts stay-warm case in the typing that Zirconium oxide fibre is processed into, and last insulation is covered with inside and outside 2 layer materials composition, imbeds hot chromium aluminium high temperature resistance heater strip between two-layer.In Frequency Induction Heating crystal growth early stage, resistance heating wire's heating of not working; To the crystal major part of growth when entering stay-warm case, heater strip begins heating, like this between the less annealed zone of thermograde of the inner formation of last stay-warm case, make that the thermograde of crystal head and afterbody is less, guarantee that whole crystal anneal in more isothermal relatively space, thereby played the effect that reduces the crystals thermal stresses.
Because the temperature in the last stay-warm case has certain temperature head than melt, can not make that the crystalline temperature gradient of solid-liquid interface is too small, crystal growth can't continue.
Adopt method of the present invention growing the high temperature crystal of low internal stress, after finishing, crystal growth annealing can directly carry out orientation and cutting, preparation becomes the crystal element and device of all size, do not need the outer long term annealing of stove, not only greatly reduce the crystalline internal stress, reduce subsurface defect, can raise the efficiency greatly simultaneously, and apparatus structure is simple, and cost of manufacture is low, and this method is fit to produce in batches.
This device has the following advantages:
(1) crystal growing process carries out under a relative demulcent thermograde with the middle crystalline annealing that finishes, and the internal stress and the lattice defect that itself produce are just fewer;
(2) the stay-warm case system can be by the thermograde of 2 thermocouple measurement chambers on whole annealed; Can realize the adjusting of thermograde by the power of heater strip, realize the controllability of annealing process.
Description of drawings:
Accompanying drawing is the structural representation of the method for crystal growth by crystal pulling post-heater device of this elimination crystal stress: wherein: the 1st, and the outer stay-warm case of the cotton preparation of Zirconium oxide fibre, the 2nd, the internal layer stay-warm case of the cotton preparation of Zirconium oxide fibre, the 3rd, the stay-warm case upper cover plate of the cotton preparation of Zirconium oxide fibre, the 4th, be wrapped in the hot chromium aluminium heat silk on the ectonexine stay-warm case, 5 and 6 is double platinum rhodium thermopairs.
Embodiment
Embodiment 1: laser crystal Nd-doped yag crystal growth
Adopt homemade DJL-600 type pulling method monocrystal growing furnace, the heating of 50KW thyristor medium frequency induction power supply, double platinum rhodium (Pt/Rh30-Pt/Rh10) thermopair, Britain Continental Europe 818 type thermoswitchs.
The technical parameter that crystal growth is adopted: 1) seed orientation: a axle; 2) growth atmosphere and pressure: N
2, 50KPa; 3) rate of pulling: 0.5～1.0m/h; 4) slewing rate: 10～15rpm; 5) the inner chamber height of post-heater: 160～200mm; 6) annealing rate: 10～15K/h (＞1200 ° of c), 30～50K/h (＜1200 ℃).
Adopt and use
The shallow type iridium crucible of level, and by Al
2O
3Pipe, Pt radiative cylinder, the back hot cell that Pt plate washer etc. are formed.By regulating the relative position and the last stay-warm case internal heating silk power of crucible and ruhmkorff coil, can realize that the solution-air temperature difference of bath surface both sides reaches 50～100 ℃, and the thermograde in the 60mm of bath surface top is≤25 ℃/cm.When the crystal growth end, after cooling was solidified liquid level, the thermograde in the post-heater at crystal place can drop in the 18 ℃/cm.
Embodiment 2: scintillation crystal is mixed the crystal growth of cerium yttrium luetcium silicate
Adopt homemade DJL-600 type pulling method monocrystal growing furnace, the heating of 50KW thyristor medium frequency induction power supply, double platinum rhodium (Pt/Rh30-Pt/Rh10) thermopair, Britain Continental Europe 818 type thermoswitchs.
The technical parameter that crystal growth is adopted: 1) seed orientation: a axle; 2) growth atmosphere and pressure: N
2, 50KPa; 3) rate of pulling: 0.5～1.0m/h; 4) slewing rate: 10～15rpm; 5) the inner chamber height of post-heater: 160～200mm; 6) annealing rate: 10～15K/h (＞1200 ° of c), 30～50K/h (＜1200 ℃).
Adopt and use
The shallow type iridium crucible of level, and by Al
2O
3Pipe, Pt radiative cylinder, the back hot cell that Pt plate washer etc. are formed.By regulating the relative position and the last stay-warm case internal heating silk power of crucible and ruhmkorff coil, can realize that the solution-air temperature difference of bath surface both sides reaches 50～100 ℃, and the thermograde in the 60mm of bath surface top is≤25 ℃/cm.When the crystal growth end, after cooling was solidified liquid level, the thermograde in the post-heater at crystal place can drop in the 18 ℃/cm.
Claims (3)
1. crystal annealing device in growth furnace, it is characterized in that: by measuring 2 double platinum rhodium electric thermo-couple temperatures, adjusting is wrapped in the heating power of the hot chromium aluminium heat silk on the ectonexine stay-warm case, a heating source is provided, in annealing space that thermograde is relatively little of the inner formation of last stay-warm case, make that the thermograde of crystal head and afterbody is less, thereby played the effect that reduces the crystals thermal stresses.
2. a kind of crystal annealing device in growth furnace according to claim 1 is characterized in that: the stay-warm case material can be aluminum oxide.
3. a kind of crystal annealing device in growth furnace according to claim 1 is characterized in that: this device can be used for neodymium-doped yttrium-aluminum garnet, mix the crystal growth of cerium yttrium luetcium silicate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910111250A CN101831712A (en) | 2009-03-13 | 2009-03-13 | Crystal annealing device in growth furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910111250A CN101831712A (en) | 2009-03-13 | 2009-03-13 | Crystal annealing device in growth furnace |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101831712A true CN101831712A (en) | 2010-09-15 |
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ID=42715922
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910111250A Pending CN101831712A (en) | 2009-03-13 | 2009-03-13 | Crystal annealing device in growth furnace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102856231A (en) * | 2011-06-27 | 2013-01-02 | 东京毅力科创株式会社 | Heat treatment furnace and heat treatment apparatus |
| CN108559834A (en) * | 2018-06-19 | 2018-09-21 | 宝钢湛江钢铁有限公司 | A kind of fixed hot rolling heat preservation annealing device |
-
2009
- 2009-03-13 CN CN200910111250A patent/CN101831712A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102856231A (en) * | 2011-06-27 | 2013-01-02 | 东京毅力科创株式会社 | Heat treatment furnace and heat treatment apparatus |
| CN102856231B (en) * | 2011-06-27 | 2016-03-09 | 东京毅力科创株式会社 | Heat-treatment furnace and annealing device |
| TWI560418B (en) * | 2011-06-27 | 2016-12-01 | Tokyo Electron Ltd | Heat treatment furnace and heat treatment apparatus |
| CN108559834A (en) * | 2018-06-19 | 2018-09-21 | 宝钢湛江钢铁有限公司 | A kind of fixed hot rolling heat preservation annealing device |
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Application publication date: 20100915 |