CN101760774A - Post-heater for reduction of internal thermal stress of crystal grown in Czochralski method - Google Patents
Post-heater for reduction of internal thermal stress of crystal grown in Czochralski method Download PDFInfo
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- CN101760774A CN101760774A CN200810072460A CN200810072460A CN101760774A CN 101760774 A CN101760774 A CN 101760774A CN 200810072460 A CN200810072460 A CN 200810072460A CN 200810072460 A CN200810072460 A CN 200810072460A CN 101760774 A CN101760774 A CN 101760774A
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Abstract
The invention adopts a post-heater to substitute the commonly used single-layer or multi-layer alumina and zirconia insulation tube in the prior art. The post-heater adopts a shaping upper insulation cover processed with zirconia fiber, the upper insulation cover consists of an inner layer of zirconia fiber and an outer layer of zirconia fiber, and a hot chrome-alumina high-temperature resistance heating wire is embedded between the two layers. During the early period of the crystal growth, the resistance heating wire does not work for heating; when most of the grown crystal extends into the upper insulation cover, the heating wire starts heating, and an annealing zone with a low temperature gradient is formed in the upper insulation cover, thereby making the temperature gradient between the head part and the tail part of the crystal low, ensuring that the whole crystal can be annealed in the space with a relatively constant temperature, and realizing the effect of reducing the internal thermal stress of the crystal. After growing up and being annealed, the crystal can be directly aligned and cut without annealing outside the furnace for a long term, thereby greatly reducing the internal stress of the crystal, decreasing the internal defects and significantly enhancing the efficiency. Moreover, the device has the advantages of simple structure and low manufacturing cost, and is applicable to mass production.
Description
Technical field
The invention belongs to the artificial lens preparing technical field, particularly relate to a kind of post-heater Design of device principle and apparatus structure that reduces the Czochralski grown crystal built-in thermal stress.
Background technology
Adopting crystal pulling method growing crystal from pure melt, is one of at present general growing method.This method is applicable to the growth congruent melting and does not have the crystal of destructive phase transformation to room temperature that such as laser crystal Nd-doped vanadic acid yttrium, vanadic acid gadolinium, yttrium iron garnet, yttrium aluminate, and scintillation crystal is mixed cerium yttrium luetcium silicate etc.Adopt Czochralski grown crystal, have fast growth, crystal wraps up problems such as defective is few.
In general, a temperature design requirements of method of crystal growth by crystal pulling system is axisymmetric, adopt single or multiple lift aluminum oxide, zirconium white heat-preservation cylinder, metal plate washer and after-heater form one can flexible combination heat-insulation system, satisfy the general requirement of crystal growth, the thermograde (the solution-air temperature difference) that is bath surface wants big, vertically gradient is bigger near the liquid level, and the after heat chambers temp gradient of melt top is little.
The design of big gradient temperature directly causes the crystal thermal stresses of being grown higher in the method for crystal growth by crystal pulling, occurs easily ftractureing, dissociating and defective such as dislocation.The method that generally adopts is after crystal growth finishes at present, adopts modes such as the outer atmosphere annealing of stove, alleviates the unrelieved stress in the crystal, improves the crystalline quality.Because annealing temperature is more much lower than crystal growth temperature, and after crystal growth finished, many defectives had cured, and are difficult to adopt the mode of post annealed to eliminate.It is not only consuming time very long to carry out the outer atmosphere annealing of stove simultaneously, and needs the annealing device of more complicated.
Summary of the invention
The present invention relates to a kind of post-heater Design of device that reduces the Czochralski grown crystal built-in thermal stress.
The present invention adopts the post-heater device to substitute single or multiple lift aluminum oxide, zirconium white heat-preservation cylinder commonly used at present.This post-heater device is to adopt stay-warm case in the typing that Zirconium oxide fibre is processed into, and last insulation is covered with inside and outside 2 layers of Zirconium oxide fibre tube 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 realize the adjusting of thermograde by the power of heater strip by the thermograde of 2 thermocouple measurement chambers on whole annealed, realizes the controllability of annealing process.
Description of drawings:
Fig. 1 is the structural representation of the method for crystal growth by crystal pulling post-heater device of this elimination crystal stress
The 1st, 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 in the ectonexine stay-warm case;
5 and 6 is double platinum rhodium thermopairs.
Embodiment
Embodiment 1: the Nd-doped yttrium vanadate crystal growth
Laser crystals be meant a kind of can stimulated radiation under light or electric equal excitation, launch the crystal of laser.The Nd-doped yttrium vanadate crystal is a kind of laser crystals that is widely used at present, and its molecular formula is Nd
xY
1-xV0
4(x is the content of neodymium ion in the crystal).
Growing apparatus: homemade DJL-400 type pulling method monocrystal growing furnace, the heating of 25KW thyristor medium frequency induction power supply, double platinum rhodium (Pt/Rh30-Pt/Rh10) thermopair, Britain Continental Europe 818 type thermoswitchs, growth container is
The shallow type iridium crucible of level.
The technical parameter that crystal growth is adopted: seed orientation a axle, growth atmosphere is nitrogen (containing 0.5% oxygen), air pressure is 50KPa, crystal growth rate is 1.5～2.5mm/h, Crystal Rotation speed is 5～10rpm, the inner chamber height of post-heater device is 80mm, and the rate of temperature fall that crystal growth finishes is 15 ℃/h～25 ℃/h.
Embodiment 2: the growth of neodymium-doped vanadic acid gadolinium crystal
Neodymium-doped vanadic acid gadolinium crystal is a kind of laser crystals that is widely used at present, and its molecular formula is Nd
xGd
1-xVO
4(x is the content of neodymium ion in the crystal).
Growing apparatus: homemade DJL-400 type pulling method monocrystal growing furnace, the heating of 25KW thyristor medium frequency induction power supply, double platinum rhodium (Pt/Rh30-Pt/Rh10) thermopair, Britain Continental Europe 818 type thermoswitchs, growth container is
The shallow type iridium crucible of level.
The technical parameter that crystal growth is adopted: seed orientation a axle, growth atmosphere is nitrogen (containing 0.5% oxygen), air pressure is 50KPa, crystal growth rate is 2～3mm/h, Crystal Rotation speed is 10～15rpm, the inner chamber height of post-heater device is 80mm, and the rate of temperature fall that crystal growth finishes is 20 ℃/h～30 ℃/h.
Embodiment 3: the neodymium-doped yttrium-aluminum garnet crystal growth
The neodymium-doped yttrium-aluminum garnet crystal is a kind of laser crystals that is widely used at present, and its molecular formula is Nd
xY
3-xAl
5O
12(x is the content of neodymium ion in the crystal).
Growing apparatus: 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, growth container is a bore
Internal depth is the iridium crucible of 120mm.
The technical parameter that crystal growth is adopted: seed orientation＜111〉direction, growth atmosphere is a pure nitrogen gas, air pressure is 100KPa, crystal growth rate is 0.5～1.5mm/h, Crystal Rotation speed is 15～30rpm, the inner chamber height of post-heater device is 250mm, and the rate of temperature fall that crystal growth finishes is 15 ℃/h～30 ℃/h.
Embodiment 4: the growth of neodymium-doped yttrium aluminate crystal
The neodymium-doped yttrium aluminate crystal is a kind of laser crystals that is widely used at present, and its molecular formula is Nd
xY
1-xA1O
3(x is the content of neodymium ion in the crystal).
Growing apparatus: 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, growth container is a bore
Internal depth is the iridium crucible of 120mm.
The technical parameter that crystal growth is adopted: seed orientation＜111〉direction, growth atmosphere is a pure nitrogen gas, air pressure is 100KPa, crystal growth rate is 0.5～1.5mm/h, Crystal Rotation speed is 15～30rpm, the inner chamber height of post-heater device is 250mm, and the rate of temperature fall that crystal growth finishes is 15 ℃/h～30 ℃/h.
Embodiment 5: mix the crystal growth of cerium yttrium luetcium silicate
Mixing cerium yttrium luetcium silicate crystal is a kind of scintillation crystal that is widely used at present, and its molecular formula is C
eXLu
2-xSi
2O
5(x is the content of cerium ion in the crystal).
Growing apparatus: 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, growth container is a bore
Internal depth is the iridium crucible of 120mm.
The technical parameter that crystal growth is adopted: seed orientation＜111〉direction, growth atmosphere is a pure nitrogen gas, air pressure is 100KPa, crystal growth rate is 0.5～1.5mm/h, Crystal Rotation speed is 15～30rpm, the inner chamber height of post-heater device is 250mm, and the rate of temperature fall that crystal growth finishes is 15 ℃/h～30 ℃/h.
Claims (3)
1. post-heater device that reduces the Czochralski grown crystal built-in thermal stress, it is characterized in that: this post-heater device is to adopt stay-warm case in the typing that Zirconium oxide fibre is processed into, last insulation is covered with inside and outside 2 layers of Zirconium oxide fibre tube and forms, imbed hot chromium aluminium high temperature resistance heater strip between two-layer, by regulating the heating power of heater strip, an additional 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 post-heater device that reduces the Czochralski grown crystal built-in thermal stress according to claim 1 is characterized in that: the stay-warm case material can be aluminum oxide, yttrium oxide.
3. a kind of post-heater device that reduces the Czochralski grown crystal built-in thermal stress according to claim 1, it is characterized in that: this device can be used for laser crystal Nd-doped vanadic acid yttrium, vanadic acid gadolinium, yttrium aluminum garnet, yttrium aluminate crystal growth, and scintillation crystal is mixed the crystal growth of cerium yttrium luetcium silicate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810072460A CN101760774A (en) | 2008-12-25 | 2008-12-25 | Post-heater for reduction of internal thermal stress of crystal grown in Czochralski method |
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|---|---|---|---|
| CN200810072460A CN101760774A (en) | 2008-12-25 | 2008-12-25 | Post-heater for reduction of internal thermal stress of crystal grown in Czochralski method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160931A (en) * | 2011-12-09 | 2013-06-19 | 福州高意光学有限公司 | Heat-insulating cover structure for crystal growth furnace and production method for same |
| CN103266346A (en) * | 2013-05-22 | 2013-08-28 | 嘉兴和讯光电科技有限公司 | Growing equipment for growing YVO4 (Yttrium Vanadate) crystal with drawing method and growing method based on same |
| CN103436962A (en) * | 2013-08-08 | 2013-12-11 | 巢湖市环宇光学技术有限公司 | Large-volume neodymium-doped yttrium vanadate crystal and preparation method thereof |
| CN108893780A (en) * | 2018-07-19 | 2018-11-27 | 中山大学 | A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof |
-
2008
- 2008-12-25 CN CN200810072460A patent/CN101760774A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160931A (en) * | 2011-12-09 | 2013-06-19 | 福州高意光学有限公司 | Heat-insulating cover structure for crystal growth furnace and production method for same |
| CN103266346A (en) * | 2013-05-22 | 2013-08-28 | 嘉兴和讯光电科技有限公司 | Growing equipment for growing YVO4 (Yttrium Vanadate) crystal with drawing method and growing method based on same |
| CN103266346B (en) * | 2013-05-22 | 2016-12-28 | 嘉兴和讯光电科技有限公司 | The growth apparatus of a kind of crystal Pulling YVO4 crystal and growing method based on this growth apparatus |
| CN103436962A (en) * | 2013-08-08 | 2013-12-11 | 巢湖市环宇光学技术有限公司 | Large-volume neodymium-doped yttrium vanadate crystal and preparation method thereof |
| CN108893780A (en) * | 2018-07-19 | 2018-11-27 | 中山大学 | A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof |
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Application publication date: 20100630 |