CN114635183B - Guide die method oriented crystallization device and growth method based on device - Google Patents
Guide die method oriented crystallization device and growth method based on device Download PDFInfo
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- CN114635183B CN114635183B CN202210324134.3A CN202210324134A CN114635183B CN 114635183 B CN114635183 B CN 114635183B CN 202210324134 A CN202210324134 A CN 202210324134A CN 114635183 B CN114635183 B CN 114635183B
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000002425 crystallisation Methods 0.000 title claims abstract description 26
- 230000008025 crystallization Effects 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 claims abstract description 124
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000007713 directional crystallization Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 21
- 239000000155 melt Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 238000010899 nucleation Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000002109 crystal growth method Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 229910052741 iridium Inorganic materials 0.000 claims description 5
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 238000011065 in-situ storage Methods 0.000 claims description 4
- 238000000462 isostatic pressing Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011819 refractory material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052689 Holmium Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- TVFHPXMGPBXBAE-UHFFFAOYSA-N [Sc].[Gd] Chemical compound [Sc].[Gd] TVFHPXMGPBXBAE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000007716 flux method Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
- C30B15/24—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using mechanical means, e.g. shaping guides
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a guide die method directional crystallization device, comprising: a crucible, a crucible cover, and a hanging rod for hanging; the middle of the die is provided with a vertical capillary channel, and the lower end of the die stretches into the crucible; the seed rod is positioned at the upper part of the crucible cover, the seed crystal is fixed at the lower end of the seed rod, and the seed crystal is close to the upper end die opening of the die. The middle of the die is provided with a vertical capillary channel, crystallization is started, and crystals can grow along the seed crystal in an oriented manner, so that high-quality crystals can be grown; the crucible cover is lifted by the hanging rod and is not stressed by the crucible, and in the crystallization process, the crystal crystallized on the die is well separated from the crucible by the downward movement of the crucible, so that the protection of the expensive metal crucible is facilitated. The invention effectively solves the problems of difficult growth of high-melting-point oxide crystals and difficult cleaning of a crucible, and the grown crystals have high quality, large size, reduced production cost, high working efficiency and great economic use value.
Description
Technical Field
The invention belongs to the technical field of crystal material preparation, and particularly relates to a guide die method oriented crystallization device and a growth method based on the device.
Background
High melting point oxide Crystal (GdSco) 3 、Lu 2 O 3 、Sc 2 O 3 、Y 2 O 3 Etc.), especially rare earth sesquioxide single crystals, have a series of advantages: the doping of various rare earth ions is easy to realize; high heat conductivity of 12.5-16.5W/mK; has strong field coupling characteristics; high impact factor, high damage threshold; low phonon energy. The low phonon energy means that the non-radiative transition rate between metastable electron energy levels of luminescent ions incorporated into the lattice is low and therefore has a higher radiative probability and a higher optical transition quantum efficiency. Scientists have clear that the laser crystal has great application prospect in the laser application fields of high-power lasers, mid-infrared and visible wave bands, scintillation crystals, disc lasers and other multiple dimensions.The development of high-melting-point oxide crystals with excellent optical performance to obtain high-performance laser crystal core components has great significance in promoting the development of laser manufacturing industry and breaking the technical barriers of developed countries.
According to the published reports, the high-melting point oxide crystal can be grown by flame method, lifting method, floating zone method, micro-pulling method, flux method, hydrothermal method and other methods, but in the above technologies, no mature growth process of large-caliber crystal is obtained. This is because the crystal melting point is high, the raw material is expensive, and not only an expensive metal crucible but also an oxide melt is protected, so that the crystal growth conditions are severe. Accordingly, the equipment requirements are also extremely high, and it is often necessary to separately design, manufacture, or retrofit the crystal growth furnace. In addition, for several melt-based crystal growth methods, temperature field distortion during growth causes difficulty in temperature field control, and research on crystal processes remains elusive.
The guided mode method is one of the methods for artificially producing single crystal materials from a melt, namely the "edge defined film feed growth" technique, and is actually a modification of the Czochralski method. The working principle of the guided mode method is that the raw materials are put into a crucible for heating and melting, the melt rises to the top end of the mould along a capillary feed slot of the mould under the capillary action, and the liquid level at the top of the mould is connected with a seed crystal to lift the melt, so that atoms or molecules are rearranged continuously at the interface between the seed crystal and the melt, and the melt is gradually solidified along with cooling to grow single crystals. The guided mode method has the advantages of short growth time, low power consumption, directional/shaped growth, simple crystal processing and the like.
Disclosure of Invention
The invention aims to solve the problems and provide a guide die method oriented crystallization device and a growth method based on the device, which are simple to operate, effective and controllable, can effectively realize the growth and preparation of high-quality oxide crystals, effectively solve the problems of difficult growth of high-melting-point oxide crystals and difficult cleaning of a crucible, and have the advantages of high quality of the grown crystals, large size, reduced production cost, high working efficiency and higher economic use value.
The aim of the invention is achieved by the following technical scheme:
a guided-mode method oriented crystallization apparatus comprising:
the crucible is used for containing the crystallization raw materials;
the crucible cover is arranged at the upper part of the crucible and is lifted by a suspender;
the mold is erected on the crucible cover, a vertical capillary channel is arranged in the middle of the mold, and the lower end of the mold stretches into the crucible;
the seed rod is positioned at the upper part of the crucible cover, the seed crystal is fixed at the lower end of the seed rod, and the seed crystal is close to the upper end die opening of the die.
According to the directional crystallization device, the mold for crystallization is arranged on the crucible cover, the crucible cover is lifted by the hanging rod, and the crucible cover is lifted by the hanging rod and is not stressed by the crucible, so that in the crystallization process, the crystal crystallized on the mold is well separated from the crucible by the downward movement of the crucible, and the protection of the expensive metal crucible is facilitated; the middle of the die is provided with a vertical capillary channel, the melted crystallization raw material moves upwards along the capillary channel and contacts with the seed crystal at the upper end, crystallization starts, and the crystal can grow directionally along the seed crystal, so that high-quality crystal grows.
Preferably, the gap width of the capillary channel is 0.3-0.5 mm.
Preferably, the seed crystal is selected from high-quality crystals, and is required to be free of cracking, grain boundaries and bubbles.
Preferably, the crucible, crucible cover, mold and hanger rod are made of iridium, molybdenum or tungsten refractory materials.
The crystal growth method based on the above-mentioned guided-mode method directional crystallization device comprises the following steps:
s01, batching: calculating the required mass of each raw material according to the stoichiometric ratio, accurately weighing, uniformly mixing, isostatic pressing, forming and sintering;
s02, assembling a crucible and a die: feeding raw materials into a crucible; a die with a feed slit width of 0.3-0.5 mm is arranged on the crucible cover, and the die opening is used for discharging grains; the crucible cover is lifted by the suspension rod and is not stressed by the crucible;
s03, seed crystal loading: fixing seed crystal on the seed crystal rod clamp;
s04, the crucible is positioned in a closed furnace, and the closed furnace is vacuumized and filled with protective gas: closing a furnace door, opening a mechanical pump for vacuumizing, closing the mechanical pump when the vacuum degree reaches 3-10 Pa, and filling the protective gas to the standard atmospheric pressure;
s05, heating and melting: the heating power supply is turned on to heat up to 2000-2500 ℃, and the temperature is kept for 0.5-2 hours, so that the raw materials are completely melted;
s06, seeding: continuing to heat, shaking down the seed crystal after the material particles at the die opening start to melt, baking the seed crystal, and then seeding the melt at the position where the seed crystal fully contacts the die cutting edge;
s07, crucible growth is reduced: slowly cooling to enable the crystal to grow outwards from the middle of the mould along the seed crystal, and slowly descending the crucible;
s08, feeding is finished and the crystal is separated from the crucible: when the feeding is finished, the crystal naturally breaks away from the crucible;
s09, cooling and annealing: and (3) annealing for 2-10 h in situ, and cooling for 20-40 h to obtain the target product oxide crystal.
As a preferred embodiment, the raw material in step S01 has a purity of greater than 99.99%, and the sintering process conditions are as follows: sintering at 1300-1800 deg.c for 10-20 hr.
In a preferred embodiment, in step S02, the crucible cover, the mold, and the hanger rod are made of a high temperature resistant material such as iridium, molybdenum, or tungsten.
As a preferred embodiment, the seed crystal in the step S03 is a high-quality crystal, and is required to be free of cracks, grain boundaries and bubbles.
As a preferable embodiment, the temperature is continuously raised in the step S06 to 20-50 ℃, and the temperature is kept for 15min after the temperature is raised; when the seed crystal is roasted, the seed crystal is positioned above the top end of the die and is 2-4 mm away from the top end of the die, and the time for roasting the seed crystal is 10-30 min; the seed crystal fully contacts with the melt at the cutting edge of the die, and the seed crystal is soaked in the melt for 15-40 min.
As a preferred embodiment, in the S07 crystal growth process, the descending speed of a crucible is kept at 2-10 mm/h, and the temperature is reduced and grown at the speed of 10-25 ℃/h so as to transversely enlarge the size of the crystal; then the crucible is cooled and grown at a speed of 5-15 mm/h and a temperature of 5-10 ℃/h.
Compared with the prior art, the invention has the following advantages:
according to the invention, the structure of the directional crystallization device is provided, the mold for crystallization is erected on the crucible cover, and the crucible cover is lifted by the hanging rod and is not stressed by the crucible, so that in the crystallization process, the crystal crystallized on the mold is well separated from the crucible by downwards moving the crucible, and the problem that the crucible is difficult to clean is effectively solved; the middle of the die is provided with a vertical capillary channel, the melted crystallization raw material moves upwards along the capillary channel, contacts with the seed crystal at the upper end, starts crystallization, enables the crystal to grow directionally, grows high-quality crystals, effectively solves the problem that high-melting-point oxide crystals are difficult to grow, has high quality and large size, reduces the production cost, improves the working efficiency, and has larger economic use value.
Drawings
FIG. 1 is a diagram showing the outline of a directional crystallization by a guide mold method;
FIG. 2 is a cross-sectional view of a guide mold method oriented crystallization;
in the figure: 1-a crucible; 2-a crucible cover; 3-a mold; 4-seed crystal; 5-seed crystal rods; 6-hanging rod.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
Referring to fig. 1 and 2, a device for directional crystallization by using a guided mode method comprises:
the crucible 1 is used for containing crystallization raw materials;
a crucible cover 2 which is arranged at the upper part of the crucible 1 and is lifted by a hanging rod 6;
the mold 3 is erected on the crucible cover 2, a vertical capillary channel is arranged in the middle of the mold 3, the lower end of the mold 3 stretches into the crucible 1, and the gap width of the capillary channel is 0.3-0.5 mm;
the seed rod 5 is positioned at the upper part of the crucible cover 2, the seed crystal 4 is fixed at the lower end of the seed rod 5, and the seed crystal 4 is close to the upper end die opening of the die 3.
The lower end of the seed rod is provided with a chuck, and the seed crystal is fixed on the chuck of the seed rod. The crucible, the crucible cover, the mold and the suspender are made of iridium, molybdenum or tungsten high-temperature resistant materials, and seed crystals are obtained from high-quality crystals, and the crucible is free of cracking, grain boundaries and bubbles.
The device is characterized in that the mould 3 for crystallization is arranged on the crucible cover 2, the crucible cover 2 is lifted by the hanging rod 6, and the crucible cover 2 is lifted by the hanging rod 6 and is not stressed by the crucible 1, so that in the crystallization process, the crystal crystallized on the mould 3 is well separated from the crucible 1 by the downward movement of the crucible 1, and the protection of an expensive metal crucible is facilitated; the middle of the die 3 is provided with a vertical capillary channel, the melted crystallization raw material moves upwards along the capillary channel and contacts with the seed crystal at the upper end, crystallization is started, and the crystal can grow directionally, so that high-quality crystal can be grown. The device effectively solves the problems of difficult growth of high-melting-point oxide crystals and difficult cleaning of the crucible, and the grown crystals have high quality, large size, low production cost, high working efficiency and great economic use value.
The following are specific application examples:
example 1
Gadolinium scandium acid (GdSco) in this example 3 ) The growth process flow of the monocrystal specifically comprises the following steps: gd with purity of 99.99% 2 O 3 With Sc 2 O 3 Accurately weighing the raw materials according to the stoichiometric ratio, uniformly mixing, performing isostatic pressing forming under 200MPa, putting into an alumina crucible, and sintering at 1500 ℃ for 10 hours; putting the sintered material into an iridium crucible, selecting a die with a gap width of 0.4mm of a capillary channel, and placing GdScO at the die opening as shown in figure 1 3 A crystal grain; the crucible cover is lifted by the molybdenum suspender and is not stressed by the crucible; gdSco for selecting (100) direction 3 The seed crystal is fixed on the seed crystal rod clamp; closing the furnace door, opening a mechanical pump for vacuumizing, closing the mechanical pump when the vacuum degree reaches 5Pa, and filling the protective gas to the standard atmospheric pressure; starting a heating power supply to heat to 2140 ℃, and keeping the temperature for 1h to completely melt the raw materials; continuously heating to 25 ℃, shaking down the seed crystal after the material particles at the die opening start to melt, enabling the seed crystal to keep a distance of 3mm from the top end of the die to bake the seed crystal, immersing the seed crystal into a melt at the cutting edge of the die after 10min,seeding after 20 min; then, firstly keeping the descending speed of the crucible to be 5mm/h, and slowly cooling and growing at the speed of 15 ℃/h to enable the crystal to grow outwards from the middle of the mould along the seed crystal, and transversely expanding the size; then the crucible is cooled and grown at a speed of 8mm/h and a temperature of 10 ℃/h; when the feeding is finished, the crystal naturally breaks away from the crucible; annealing for 5h in situ, slowly cooling to room temperature for 24h to obtain high-quality GdScO 3 And (5) a crystal.
Example 2
1.0% Ho:Lu in this example 2 O 3 The growth process flow of the monocrystal specifically comprises the following steps: lu with purity of 99.99% 2 O 3 With Ho 2 O 3 Accurately weighing the raw materials according to the stoichiometric ratio, uniformly mixing, performing isostatic pressing forming under 200MPa, and placing the raw materials into an alumina crucible to sinter for 10 hours at 1600 ℃; putting the sintered raw materials into a tungsten crucible, selecting a die with a feeding seam width of 0.3mm to be supported on a crucible cover, and placing Lu at a die opening 2 O 3 A crystal grain; the crucible cover is lifted by the molybdenum suspender and is not stressed by the crucible; selecting Lu in (100) direction 2 O 3 The seed crystal is fixed on the seed crystal rod clamp; closing the furnace door, opening a mechanical pump for vacuumizing, closing the mechanical pump when the vacuum degree reaches 8Pa, and filling the protective gas to the standard atmospheric pressure; heating to 2450 ℃ by turning on a heating power supply, and keeping the temperature for 2 hours to completely melt the raw materials; continuously heating to 30 ℃, shaking down the seed crystal after the material particles at the die opening start to melt, enabling the seed crystal to keep a distance of 3mm from the top end of the die, baking the seed crystal, immersing the seed crystal into a melt at the cutting edge of the die after 10min, and seeding after 20 min; then, firstly keeping the descending speed of the crucible to be 4mm/h, and slowly cooling and growing at the speed of 15 ℃/h to enable the crystal to grow outwards from the middle of the mould along the seed crystal, and transversely expanding the size; then the crucible is cooled and grown at a speed of 8mm/h and a temperature of 8 ℃/h; when the feeding is finished, the crystal naturally breaks away from the crucible; annealing for 6h in situ, slowly cooling to room temperature for 24h to obtain the high-quality 1.0% Ho: lu 2 O 3 And (5) a crystal.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (9)
1. A guided-mode method oriented crystallization device, comprising:
the crucible is used for containing the crystallization raw materials;
the crucible cover is arranged at the upper part of the crucible and is lifted by a suspender;
the mold is erected on the crucible cover, a vertical capillary channel is arranged in the middle of the mold, and the lower end of the mold stretches into the crucible;
the seed rod is positioned at the upper part of the crucible cover, the lower end of the seed rod is fixed with seed crystals, and the seed crystals are close to the upper end die opening of the die;
the lower end of the seed rod is provided with a chuck, and the seed crystal is fixed on the chuck of the seed rod;
in the crystal growth method of the guide mold method directional crystallization device, crystals are grown outwards from the middle of a mold along a seed crystal, and a crucible is slowly lowered.
2. The device for direct crystallization according to claim 1, wherein the capillary channel has a gap width of 0.3 to 0.5mm.
3. The apparatus according to claim 1, wherein the crucible, the crucible cover, the mold and the hanger rod are made of iridium, molybdenum or tungsten refractory materials.
4. The apparatus according to claim 1, wherein the seed crystal is a high-quality crystal, and has no cracks, no grain boundaries, and no bubbles.
5. A crystal growth method based on a guided-mode method oriented crystallization apparatus as set forth in claim 1, comprising the steps of:
s01, batching: calculating the required mass of each raw material according to the stoichiometric ratio, accurately weighing, uniformly mixing, isostatic pressing, forming and sintering;
s02, assembling a crucible and a die: putting raw materials into a crucible, and placing material particles at a die opening for temperature test;
s03, seed crystal loading: fixing seed crystal on the seed crystal rod clamp;
s04, the device is positioned in a closed furnace, and the closed furnace is vacuumized and filled with protective gas: closing a furnace door, opening a mechanical pump for vacuumizing, closing the mechanical pump when the vacuum degree reaches 3-10 Pa, and filling the protective gas to the standard atmospheric pressure;
s05, heating and melting: heating to 2000-2500 deg.c with the heating power source for 0.5-2 hr to melt the material completely;
s06, seeding: continuing to heat, shaking down the seed crystal after the material particles at the die opening start to melt, baking the seed crystal, and then seeding the melt at the position where the seed crystal fully contacts the die opening;
s07, crucible growth is reduced: slowly cooling to enable the crystal to grow outwards from the middle of the mould along the seed crystal, and slowly descending the crucible;
s08, feeding is finished and the crystal is separated from the crucible: when the feeding is finished, the crystal naturally breaks away from the crucible;
s09, cooling and annealing: and (5) in-situ annealing for 2-10 h, and cooling for 20-40 h to obtain the target product oxide crystal.
6. The method according to claim 5, wherein the raw material in step S01 has a purity of more than 99.99%, and the sintering process conditions are as follows: sintering at 1300-1800 ℃ for 10-20 h.
7. The method according to claim 5, wherein the temperature is continuously raised in step S06 to a level of 20 to 50℃and the temperature is maintained for 15 minutes after the temperature is raised.
8. The crystal growth method according to claim 7, wherein the seed crystal is positioned above the top end of the mold and is 2 to 4mm away from the top end of the mold when the seed crystal is baked, and the time for baking the seed crystal is 10 to 30 minutes; the seed crystal fully contacts with the melt at the cutting edge of the die, and the seed crystal is soaked in the melt for 15-40 min.
9. The method according to claim 5, wherein in the step S07 crystal growth, the crucible is maintained at a lowering speed of 2-10 mm/h, and the crystal is grown at a lowering temperature of 10-25 ℃/h to expand the size laterally; then the crucible is cooled and grown at a speed of 5-10 mm/h and a temperature of 5-10 ℃/h until the crystal is pulled off.
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| CN104264215A (en) * | 2014-10-15 | 2015-01-07 | 江苏中电振华晶体技术有限公司 | Sapphire crystal growing device adopting edge defined film-fed growth techniques and growing method |
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| CN110453283A (en) * | 2019-09-11 | 2019-11-15 | 同济大学 | A kind of mold and method of the EFG technique growth sealing sapphire pipe of sealing cover type seeding |
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| JP2004059360A (en) * | 2002-07-26 | 2004-02-26 | Sharp Corp | Apparatus and process for manufacturing crystal sheet, and solar cell |
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|---|---|---|---|---|
| CN104264215A (en) * | 2014-10-15 | 2015-01-07 | 江苏中电振华晶体技术有限公司 | Sapphire crystal growing device adopting edge defined film-fed growth techniques and growing method |
| CN106498488A (en) * | 2016-10-28 | 2017-03-15 | 同济大学 | Multiple doping CaF are grown simultaneously2The device of crystal and the preparation method based on the device |
| CN110453283A (en) * | 2019-09-11 | 2019-11-15 | 同济大学 | A kind of mold and method of the EFG technique growth sealing sapphire pipe of sealing cover type seeding |
Non-Patent Citations (1)
| Title |
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| 导模法晶体生长技术研究及应用;王东海等;《物理实验》;第第42卷卷(第第1期期);第1-10页 * |
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