CN114635183A - Directional crystallization device for guided mode method and growth method based on device - Google Patents
Directional crystallization device for guided mode method and growth method based on device Download PDFInfo
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- CN114635183A CN114635183A CN202210324134.3A CN202210324134A CN114635183A CN 114635183 A CN114635183 A CN 114635183A CN 202210324134 A CN202210324134 A CN 202210324134A CN 114635183 A CN114635183 A CN 114635183A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000007713 directional crystallization Methods 0.000 title abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 134
- 238000002425 crystallisation Methods 0.000 claims abstract description 27
- 230000008025 crystallization Effects 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 22
- 239000000155 melt Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000001816 cooling Methods 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
- 238000002109 crystal growth method 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
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000002156 mixing Methods 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
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- 238000000462 isostatic pressing Methods 0.000 claims description 4
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 239000011819 refractory material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 2
- 230000008901 benefit Effects 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
- 229910003443 lutetium oxide Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000005231 Edge Defined Film Fed Growth Methods 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 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
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- 238000013461 design Methods 0.000 description 1
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- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
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- -1 rare earth ions Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
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- 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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- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a directional crystallization device for a guide mold, which comprises: the crucible and the crucible cover are hoisted by the hoisting rod; the middle of the mould is provided with a vertical capillary channel, and the lower end of the mould extends into the crucible; and the seed crystal rod is positioned on the upper part of the crucible cover, the lower end of the seed crystal rod is fixed with seed crystals, and the seed crystals are close to the upper end die opening of the die. The middle of the die is provided with a vertical capillary channel for starting crystallization, and the crystal can grow directionally along the seed crystal to grow a high-quality crystal; the crucible cover is lifted by the hanging rod and is not stressed on the crucible, and in the crystallization process, the crucible moves downwards to separate the crystal crystallized on the mold from the crucible well, so that the expensive metal crucible is protected. The invention 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, reduced production cost, high working efficiency and larger economic use value.
Description
Technical Field
The invention belongs to the technical field of crystal material preparation, and particularly relates to an oriented crystallization device for a guide mold and a growth method based on the oriented crystallization device.
Background
Refractory oxide crystal (GdScO)3、Lu2O3、Sc2O3、Y2O3Etc.), in particular rare earth sesquioxide single crystals, have a series of advantages: the doping of various rare earth ions is easy to realize; the high thermal conductivity is 12.5-16.5W/mK; has the characteristic of strong field coupling; high impact resistance factor, high damage threshold; low phonon energy. Low phonon energy means that the non-radiative transition rate between metastable electron levels of the luminescent ion incorporated into the crystal lattice is low and therefore has a higher radiative probability and a higher optical transition quantum efficiency. Scientists have made clear that such laser crystals have a great application prospect in the field of multi-dimensional laser applications such as high-power lasers, mid-infrared and visible bands, scintillation crystals, disk lasers, and the like. The development of high-melting-point oxide crystals with excellent optical performance and the obtainment of high-performance laser crystal core components have great significance for promoting the development of laser manufacturing industry and breaking the technical barrier of developed countries.
It has been reported that refractory oxide crystals can be grown by flame, czochralski, float-zone, micro-pulldown, flux, hydrothermal methods, etc., but none of these techniques have achieved a mature growth process for large-diameter crystals. This is because the crystal has a high melting point and the raw material is expensive, and it is necessary to protect not only the expensive metal crucible but also the oxide melt, and therefore the crystal growth conditions are critical. Accordingly, the equipment requirements are also extremely high, and it is often necessary to separately design or modify the crystal growth furnace. In addition, for several crystal growth methods based on the melt method, the temperature field is distorted in the growth process, so that the temperature field is difficult to control, and the research on the crystal process is not delayed.
The guided mode method is one of the methods for artificially producing single crystal materials from a melt, namely, the "edge-defined film-fed growth" technique, which is actually a variation of the czochralski method. The working principle of the mold guiding method is that raw materials are put into a crucible to be heated and melted, a melt rises to the top end of a mold under the capillary action along a capillary feeding seam of the mold, a seed crystal is connected to the liquid level at the top of the mold to pull the melt, atoms or molecules are continuously rearranged on an interface between the seed crystal and the melt, and a single crystal is grown after the solidification along with the temperature reduction. The mold-guiding method has the advantages of short growth time, low power consumption, orientable/shape-fixed growth, simple crystal processing and the like.
Disclosure of Invention
The invention aims to solve the problems and provide an oriented crystallization device for a guided mode method and a growth method based on the oriented crystallization device, the device and the method are simple to operate, are effective and controllable, can effectively realize the growth and preparation of high-quality oxide crystals, effectively solve the problems that the high-melting-point oxide crystals are difficult to grow and a crucible is difficult to clean, and the grown crystals have high quality and large size, reduce the production cost, have high working efficiency and have higher economic use value.
The purpose of the invention is realized by the following technical scheme:
a guided mode epitaxial crystallization apparatus, comprising:
the crucible is used for containing crystallization raw materials;
the crucible cover is arranged at the upper part of the crucible and is hoisted by the hoisting rod;
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 extends into the crucible;
and the seed crystal rod is positioned on the upper part of the crucible cover, the lower end of the seed crystal rod is fixed with seed crystals, and the seed crystals are close to the upper end die opening of the die.
According to the directional crystallization device, the mold for crystallization is erected on the crucible cover, the crucible cover is lifted up through the lifting rod and is not stressed on the crucible, so that crystals crystallized on the mold are well separated from the crucible through downward movement of the crucible in the crystallization process, and the expensive metal crucible is protected; a vertical capillary channel is arranged in the middle of the die, the molten crystallization raw material moves upwards along the capillary channel and contacts with the seed crystal at the upper end to start crystallization, and the crystal can grow directionally along the seed crystal to grow a high-quality crystal.
Preferably, the width of the gap of the capillary channel is 0.3-0.5 mm.
Preferably, the seed crystal is obtained from high-quality crystals, and is required to have no cracking, no grain boundary and no bubble.
Preferably, the crucible cover, the mold and the hanger rod are made of iridium, molybdenum or tungsten high temperature resistant materials.
The crystal growth method based on the die-guided orientation crystallization device comprises the following steps:
s01, preparing materials: calculating the mass required by each raw material according to the stoichiometric ratio, accurately weighing, uniformly mixing, performing isostatic pressing, forming and sintering;
s02, assembling the crucible and the mold: putting raw materials into a crucible; a mould with a feeding seam width of 0.3-0.5 mm is erected on the crucible cover, and material particles are discharged from the mould opening; the crucible cover is lifted by the hanging rod and is not stressed on the crucible;
s03, seed crystal installation: fixing a seed crystal on a seed crystal rod chuck;
s04, the crucible is positioned in a closed furnace, the closed furnace is vacuumized and filled with protective gas: closing the furnace door, starting a mechanical pump to vacuumize, closing the mechanical pump when the vacuum degree reaches 3-10 Pa, and filling protective gas to the standard atmospheric pressure;
s05, heating and melting: turning on a heating power supply, heating to 2000-2500 ℃, keeping the temperature for 0.5-2 h, and completely melting the raw materials;
s06, seeding: continuing heating, shaking down the seed crystal after the material particles at the die opening begin to melt, baking the seed crystal, and then fully contacting the seed crystal with the melt at the die cutting edge for seeding;
s07, descending crucible growth: slowly cooling to enable the crystal to grow outwards from the middle of the mould along the seed crystal, and slowly lowering the crucible;
s08, ending the feeding and separating the crystal from the crucible: after the feeding is finished, the crystal naturally separates from the crucible;
s09, cooling and annealing: annealing in situ for 2-10 h, and cooling for 20-40 h to obtain the target product oxide crystal.
As a preferred embodiment, the purity of the raw material in step S01 is greater than 99.99%, and the sintering process conditions are as follows: sintering at 1300-1800 ℃ for 10-20 h.
In a preferred embodiment, the crucible cover, the mold, and the hanger bar in step S02 are made of a high temperature resistant material such as iridium, molybdenum, or tungsten.
As a preferred embodiment, the seed crystal in step S03 is made of high-quality crystal, and is required to have no crack, no grain boundary, and no bubble.
In a preferable embodiment, the temperature is continuously increased to 20-50 ℃ in S06, and the temperature is kept constant for 15min after temperature increase; when the seed crystal is baked, 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 seed crystal baking time is 10-30 min; the seed crystal is fully contacted with the melt at the cutting edge of the die, and the seed crystal is ensured to be soaked in the melt for 15-40 min.
As a preferred embodiment, in the S07 crystal growth process, firstly, the crucible descending speed is kept at 2-10 mm/h, and the temperature is reduced at the speed of 10-25 ℃/h to grow so that the crystal is transversely enlarged in size; then the crucible is cooled down at the speed of 5-15 mm/h and the temperature of 5-10 ℃/h for growth.
Compared with the prior art, the invention has the following advantages:
according to the invention, the directional crystallization device is structurally arranged, the mold for crystallization is erected on the crucible cover, the crucible cover is lifted by the hanging rod and is not stressed on the crucible, so that in the crystallization process, the crucible moves downwards to separate the crystal crystallized on the mold from the crucible well, and the problem that the crucible is difficult to clean is effectively solved; the vertical capillary channel is arranged in the middle of the die, the molten crystallization raw material moves upwards along the capillary channel and contacts with the seed crystal at the upper end to start crystallization, the crystal can grow directionally to grow a high-quality crystal, the problem of difficulty in growth of the high-melting-point oxide crystal is effectively solved, the grown crystal is high in quality and size, the production cost is reduced, the working efficiency is improved, and the economic use value is high.
Drawings
FIG. 1 is a schematic view of a directional crystallization profile of a guide mold;
FIG. 2 is a cross-sectional view of an oriented crystal of a guided mode;
in the figure: 1-a crucible; 2-crucible cover; 3-molding; 4-seed crystal; 5-seed rods; 6-a suspender.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Referring to fig. 1 and 2, a guide die method directional crystallization device comprises:
the crucible 1 is used for containing crystallization raw materials;
the crucible cover 2 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 extends into the crucible 1, and the gap width of the capillary channel is 0.3-0.5 mm;
and the seed crystal rod 5 is positioned at the upper part of the crucible cover 2, the lower end of the seed crystal rod 5 is fixed with the seed crystal 4, 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 the seed crystal is made of high-quality crystal and has no cracking, crystal boundary and air bubble.
According to the device, the mold 3 for crystallization is erected on the crucible cover 2, the crucible cover 2 is hoisted through the suspender 6 and is not stressed on the crucible 1, so that in the crystallization process, the crucible 1 moves downwards, crystals crystallized on the mold 3 are well separated from the crucible 1, and the expensive metal crucible is protected; 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 to start crystallization, and the crystal can grow directionally to grow a high-quality crystal. 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, reduced production cost, high working efficiency and larger economic use value.
The following are specific application examples:
example 1
Gadolinium scandate (GdScO) in the present example3) The process flow of the growth of the single crystal comprises the following steps: purity of99.99% Gd2O3And Sc2O3Accurately weighing the raw materials according to the stoichiometric ratio, uniformly mixing, performing isostatic pressing at 200MPa for forming, and sintering in an alumina crucible at 1500 ℃ for 10 h; putting sintered raw materials into an iraurita crucible, selecting a die with a gap width of 0.4mm for a capillary channel, and placing GdScO at the die opening as shown in figure 13A crystal grain; the crucible cover is hoisted by the molybdenum suspender and is not stressed on the crucible; selecting GdScO of (100) direction3The seed crystal is fixed on the chuck of the seed crystal rod; closing the furnace door, starting a mechanical pump to vacuumize, closing the mechanical pump when the vacuum degree reaches 5Pa, and filling protective gas to the standard atmospheric pressure; turning on a heating power supply, heating to 2140 ℃, and keeping the temperature for 1h to completely melt the raw materials; continuing to heat up to 25 ℃, shaking down the seed crystal after the material grains at the die opening begin to melt, keeping the distance between the seed crystal and the top end of the die to bake the seed crystal, immersing the seed crystal into the melt at the die cutting edge after 10min, and seeding after 20 min; then, firstly keeping the descending speed of the crucible at 5mm/h, and slowly cooling and growing at the speed of 15 ℃/h to ensure that the crystal grows outwards from the middle of the mould along the seed crystal and the size is enlarged transversely; then the crucible is cooled down at the speed of 8mm/h and the temperature of 10 ℃/h for growth; after the feeding is finished, the crystal naturally separates from the crucible; annealing in situ for 5h, and slowly cooling to room temperature for 24h to obtain high-quality GdScO3And (4) crystals.
Example 2
Lu is 1.0% Ho in this example2O3The process flow of the growth of the single crystal comprises the following steps: mixing Lu with purity of 99.99%2O3And Ho2O3Accurately weighing the raw materials according to the stoichiometric ratio, uniformly mixing, performing isostatic pressing at 200MPa for forming, and putting into an alumina crucible to sinter for 10h at 1600 ℃; putting the sintered raw materials into a tungsten crucible, selecting a die with a feeding gap width of 0.3mm to be erected on a crucible cover, and putting Lu at the die opening2O3A crystal grain; the crucible cover is hoisted by the molybdenum suspender and is not stressed on the crucible; lu in selected (100) direction2O3The seed crystal is fixed on the chuck of the seed crystal rod; closing the furnace door, starting a mechanical pump to vacuumize, closing the mechanical pump when the vacuum degree reaches 8Pa, and filling protective gas to the standard atmospheric pressure;turning on a heating power supply, heating to 2450 deg.C, and maintaining the temperature for 2 hr to completely melt the raw materials; continuing to heat up to 30 ℃, shaking down the seed crystal after the material grains at the die opening begin to melt, keeping the distance between the seed crystal and the top end of the die to bake the seed crystal, immersing the seed crystal into the melt at the die cutting edge after 10min, and seeding after 20 min; then, firstly keeping the descending speed of the crucible at 4mm/h, and slowly cooling and growing at the speed of 15 ℃/h to ensure that the crystal grows outwards from the middle of the mould along the seed crystal and the size is enlarged transversely; then the crucible is cooled down at the speed of 8mm/h and the temperature of 8 ℃/h for growth; after the feeding is finished, the crystal naturally separates from the crucible; annealing in situ for 6h, and slowly cooling to room temperature for 24h to obtain high-quality 1.0% Ho: Lu2O3And (4) crystals.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, 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 embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A guided mode epitaxial crystallization apparatus, comprising:
the crucible is used for containing crystallization raw materials;
the crucible cover is arranged at the upper part of the crucible and is hoisted by the hoisting rod;
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 extends into the crucible;
and the seed crystal rod is positioned on the upper part of the crucible cover, the lower end of the seed crystal rod is fixed with seed crystals, and the seed crystals are close to the upper end die opening of the die.
2. The apparatus of claim 1, wherein the capillary channel has a gap width of 0.3-0.5 mm.
3. The apparatus for guided mold orientation crystallization as claimed in claim 1, wherein the lower end of the seed rod is provided with a chuck, and the seed crystal is fixed to the chuck of the seed rod.
4. The guided mode orientational crystallization device of claim 1, wherein the crucible, crucible cover, mold and hanger rod are made of iridium, molybdenum or tungsten refractory material.
5. The apparatus of claim 1, wherein the seed crystal is made of high quality crystal, and has no crack, no grain boundary, and no bubble.
6. The method for growing a crystal in an oriented crystallization apparatus of a mold-guiding method according to claim 1, comprising the steps of:
s01, preparing materials: calculating the mass required by each raw material according to the stoichiometric ratio, accurately weighing, uniformly mixing, performing isostatic pressing, forming and sintering;
s02, assembling the crucible and the mold: putting the raw materials into a crucible, discharging particles at a die opening, and testing the temperature;
s03, seed crystal installation: fixing a seed crystal on a seed crystal rod chuck;
s04, the device is located in a closed furnace, the closed furnace is vacuumized and filled with protective gas: closing the furnace door, starting a mechanical pump to vacuumize, closing the mechanical pump when the vacuum degree reaches 3-10 Pa, and filling protective gas to the standard atmospheric pressure;
s05, heating and melting: turning on a heating power supply, heating to 2000-2500 ℃, keeping the temperature for 0.5-2 h, and completely melting the raw materials;
s06, seeding: continuing heating, shaking down the seed crystal after the material particles at the die opening begin to melt, baking the seed crystal, and then fully contacting the seed crystal with the melt at the die opening for seeding;
s07, descending crucible growth: slowly cooling to enable the crystal to grow outwards from the middle of the mould along the seed crystal, and slowly lowering the crucible;
s08, finishing feeding and separating the crystal from the crucible: after the feeding is finished, the crystal naturally separates from the crucible;
s09, cooling and annealing: in-situ annealing for 2-10 h, and cooling for 20-40 h to obtain the target product oxide crystal.
7. The crystal growth method of claim 6, wherein the purity of the raw material in step S01 is greater than 99.99%, and the sintering process conditions are as follows: sintering at 1300-1800 ℃ for 10-20 h.
8. The crystal growth method according to claim 6, wherein the temperature is continuously raised in step S06 to 20-50 ℃, and the temperature is kept constant for 15min after the temperature is raised.
9. The crystal growth method of claim 8, wherein the seed crystal is baked for 10-30 min, and is positioned above the top end of the mold and is 2-4 mm away from the top end; the seed crystal is fully contacted with the melt at the cutting edge of the die, and the seed crystal is ensured to be soaked in the melt for 15-40 min.
10. The crystal growth method of claim 6, wherein in the crystal growth process of step S07, the crucible descending speed is maintained at 2-10 mm/h, and the temperature is reduced at a rate of 10-25 ℃/h to grow the crystal in a laterally enlarged size; then the crucible is lowered at the speed of 5-10 mm/h and the temperature of 5-10 ℃/h for growth by cooling until the crystal is pulled off.
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| Title |
|---|
| 王东海等: "导模法晶体生长技术研究及应用", 《物理实验》 * |
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| CN114635183B (en) | 2023-11-24 |
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