CN110820043A - Crystal growth apparatus and growth method - Google Patents
Crystal growth apparatus and growth method Download PDFInfo
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- CN110820043A CN110820043A CN201810900366.2A CN201810900366A CN110820043A CN 110820043 A CN110820043 A CN 110820043A CN 201810900366 A CN201810900366 A CN 201810900366A CN 110820043 A CN110820043 A CN 110820043A
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- 239000013078 crystal Substances 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title description 15
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000010453 quartz Substances 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002109 crystal growth method Methods 0.000 claims abstract description 12
- 239000000155 melt Substances 0.000 claims abstract description 11
- 239000012774 insulation material Substances 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 239000007789 gas Substances 0.000 claims description 29
- 239000000498 cooling water Substances 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 230000001681 protective effect Effects 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 230000017525 heat dissipation Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- ANDNPYOOQLLLIU-UHFFFAOYSA-N [Y].[Lu] Chemical compound [Y].[Lu] ANDNPYOOQLLLIU-UHFFFAOYSA-N 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- PSNPEOOEWZZFPJ-UHFFFAOYSA-N alumane;yttrium Chemical compound [AlH3].[Y] PSNPEOOEWZZFPJ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- -1 lutetium aluminum Chemical compound 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
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
- C30B27/00—Single-crystal growth under a protective fluid
- C30B27/02—Single-crystal growth under a protective fluid by pulling from a melt
-
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
-
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
-
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
Abstract
The invention relates to a crystal growth device, which comprises a quartz furnace, a base, a top cover, a lifting mechanism and a seed crystal; the base and the top cover are respectively fixed on the lower surface and the upper surface of the quartz furnace; the quartz furnace comprises a crucible, a heat insulation material for coating the crucible, a heater surrounding the crucible, an air inlet pipe, a corrugated pipe, a seed crystal rod and an air outlet pipe; the crucible is internally provided with a melt, and the seed crystal is connected with the liquid level of the melt; the upper part of the heat insulation material is provided with a first through hole which penetrates through the top cover up and down, the top cover is provided with a second through hole which penetrates through the top cover up and down, the corrugated pipe is connected between the top cover and the lifting mechanism, the quartz furnace, the top cover, the corrugated pipe and the lifting mechanism together form a furnace chamber, the seed rod penetrates through the first through hole and the second through hole up and down, and two ends of the seed rod are respectively connected with the seed crystal and the lifting mechanism; the air inlet pipe penetrates through the base and is communicated with the furnace chamber; the air outlet pipe penetrates through the top cover, and one end of the air outlet pipe is communicated with the furnace chamber. The invention also relates to a crystal growth method.
Description
Technical Field
The invention relates to the field of preparation of crystals, in particular to a crystal growth device and a crystal growth method.
Background
The Czochralski method is a method for growing high quality single crystals by pulling from a melt. The pulling method is characterized in that raw materials for forming crystals are put in a crucible to be heated and melted, seed crystals are welded on the surface of a melt and pulling is started, and the melt is gradually solidified on a solid-liquid interface under a certain condition to grow single crystals. The Czochralski method has become the crystal growth method with the widest application range.
The single crystal pulling furnace is a device for growing crystal by pulling method, and generally comprises a furnace chamber, a heating system, a pulling system, an atmosphere control system and the like. Wherein, the furnace chamber is a container for crystal growth and is an important component of the single crystal pulling furnace. The furnace chamber plays the roles of isolating air, isolating heat radiation and the like. Generally, the furnace chamber is made of double-layer stainless steel, and cooling water is filled in the furnace chamber for protection. Most single crystal pulling furnaces require an opening in the furnace chamber for observing the growth of the crystal. Due to the complex structure of the furnace chamber, the single crystal pulling furnace has higher cost and is not beneficial to large-scale production; the cooling circulating water takes away a large amount of heat, which is not beneficial to energy conservation; because the furnace chamber is formed by welding stainless steel with fixed size, the furnace chambers with different sizes are needed to be customized for growing crystals with different sizes, and the additional cost is higher.
Therefore, there is a need for a crystal growing apparatus and a crystal growing method that can simplify the furnace chamber and reduce the cost.
Disclosure of Invention
The invention aims to provide a crystal growing device and a crystal growing method which simplify a furnace chamber and reduce the cost.
In order to achieve the purpose, the invention adopts the following technical scheme: a crystal growing device comprises a quartz furnace, a base, a top cover, a lifting mechanism and a seed crystal; the base and the top cover are respectively fixed on the lower surface and the upper surface of the quartz furnace; the quartz furnace comprises a crucible, a heat insulation material for coating the crucible, a heater surrounding the crucible, an air inlet pipe, a corrugated pipe, a seed crystal rod and an air outlet pipe; the crucible is internally provided with a melt, and the seed crystal is connected with the liquid level of the melt; the upper part of the heat insulation material is provided with a first through hole which penetrates through the top cover up and down, the top cover is provided with a second through hole which penetrates through the top cover up and down, the corrugated pipe is connected between the top cover and the lifting mechanism, the quartz furnace, the top cover, the corrugated pipe and the lifting mechanism together form a furnace chamber, the seed rod penetrates through the first through hole and the second through hole up and down, and two ends of the seed rod are respectively connected with the seed crystal and the lifting mechanism; the air inlet pipe penetrates through the base and is communicated with the furnace chamber; the air outlet pipe penetrates through the top cover, and one end of the air outlet pipe is communicated with the furnace chamber.
As a further improvement of the invention, a plurality of clamping blocks are convexly arranged on the upper surface of the base; the quartz furnace is fixedly connected with the base through a clamping block.
As a further improvement of the invention, the base is connected with a first water inlet pipe and a first water outlet pipe.
As a further improvement of the invention, the top cover is connected with a second water inlet pipe and a second water outlet pipe.
As a further improvement of the invention, the crystal growing apparatus further includes a support for supporting the pulling mechanism.
As a further improvement of the invention, the crystal growth device also comprises a liquid tank, the liquid tank is filled with absorption liquid, and the other end of the air outlet pipe is positioned in the absorption liquid.
As a further improvement of the invention, the absorption liquid is water.
The invention also provides a crystal growth method, which adopts the crystal growth device and comprises the following steps:
s1: and (3) charging: fixing the quartz furnace in the base; the raw materials are put into a crucible, and a heater is installed; mounting the top cover on a quartz furnace, and inserting an air outlet pipe into a liquid tank containing absorption liquid; cooling water is introduced into the base through the first water inlet pipe, and cooling water is introduced into the top cover through the second water inlet pipe; the cooling water of the base is discharged by a first water outlet pipe; the cooling water of the top cover is discharged by a second water outlet pipe;
s2: crystal growth stage: introducing first protective gas into the furnace chamber from the gas inlet pipe; after the crystal growth is maintained for 0.5-2h, starting a crystal growth program, introducing second protective gas into the furnace chamber from the gas inlet pipe, starting crystal growth on the basis of seed crystals, and adjusting the position of a seed crystal rod by the pulling mechanism as required along with the crystal growth until the crystal growth is finished.
As a further improvement of the invention, the first protective gas is argon
As a further improvement of the invention, the second protective gas is one or a mixture of several of nitrogen and inert gas.
The crystal growth device and the crystal growth method greatly simplify the structure of the furnace chamber, the same furnace chamber can be used for growing crystals with different sizes, the crystal growth cost is also reduced, and good crystal growth effect can be realized.
Drawings
FIG. 1 is a schematic view of the overall structure of an embodiment of a crystal growth apparatus of the present invention.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a crystal growth apparatus, which includes a quartz furnace 1, a base 2, a lid 3, a pulling mechanism 4 and a seed crystal 5. The base 2 and the top cover 3 are respectively fixed on the lower surface and the upper surface of the quartz furnace 1.
The quartz furnace 1 includes a crucible 11, a heat insulating material 12 covering the crucible 11, a heater 13 surrounding the crucible 11, an inlet pipe 14, a bellows 15, a seed rod 16, and an outlet pipe 17.
The crucible 11 is internally provided with a melt 18, and the seed crystal 5 is connected with the liquid level of the melt 18. The upper part of the heat insulation material 12 is provided with a first through hole 121 which penetrates through the top cover up and down, the top cover 3 is provided with a second through hole 33 which penetrates through the top cover up and down, the corrugated pipe 15 is connected between the top cover 3 and the lifting mechanism 4, the quartz furnace 1, the top cover 3, the corrugated pipe 15 and the lifting mechanism 4 jointly form a furnace chamber 19, the seed rod 16 penetrates through the first through hole 121 and the second through hole 33 up and down, and two ends of the seed rod 16 are respectively connected with the seed crystal 5 and the lifting mechanism 4. The air inlet pipe 14 penetrates through the base 2 and is communicated with the furnace chamber 19; an air outlet pipe 17 penetrates through the top cover 3, and one end of the air outlet pipe 17 is communicated with the oven cavity 19.
Centers of the first through hole 121 and the second through hole 33 are located on the same vertical line.
When heating is required, the heater 13 forms a certain thermal field for crystal growth.
The base 2 is connected with a first water inlet pipe 21 and a first water outlet pipe 22, and the first water inlet pipe 21, the first water outlet pipe 22 and the base 2 can form cooling water circulation to maintain the heat dissipation of the base 2. A plurality of blocks 23 are convexly arranged on the upper surface of the base 2. The quartz furnace 1 is fixedly connected with the base 2 through a fixture block 23.
The top cover 3 is connected with a second water inlet pipe 31 and a second water outlet pipe 32, and the second water inlet pipe 31, the second water outlet pipe 32 and the top cover 3 can form cooling water circulation to maintain the heat dissipation of the top cover 3.
The pulling mechanism 4 can adjust the position of the seed rod 16 as needed for crystal growth. In some embodiments of the invention, the crystal growing apparatus further comprises a support 7, the support 7 being configured to support the pulling mechanism 4.
The liquid tank 6 is filled with absorption liquid 61, the other end of the air outlet pipe 17 is positioned in the absorption liquid 61, and the tail gas is absorbed by the absorption liquid and then discharged, so that the environmental pollution is avoided. In certain embodiments of the present invention, the absorption liquid is water.
The invention also relates to a crystal growth method, which adopts the crystal growth device and comprises the following steps:
s1: and (3) charging: fixing the quartz furnace in the base; the raw materials are put into a crucible, and a heater is installed; mounting the top cover on a quartz furnace, and inserting an air outlet pipe into a liquid tank containing absorption liquid; cooling water is introduced into the base through the first water inlet pipe, and the cooling water of the base is discharged through the first water outlet pipe; cooling water is introduced into the top cover through a second water inlet pipe, and the cooling water of the top cover is discharged through a second water outlet pipe;
s2: crystal growth stage: introducing first protective gas into the furnace chamber from the gas inlet pipe at a certain flow rate; after the crystal growth is maintained for 0.5-2h, starting a crystal growth program, introducing second protective gas into the furnace chamber at a certain flow rate from the gas inlet pipe, starting the crystal growth on the basis of seed crystals, and adjusting the position of a seed crystal rod by the pulling mechanism as required along with the crystal growth until the crystal growth is finished.
In certain embodiments of the present invention, the first protective gas is argon. The argon gas has a higher density than air, so that the air in the furnace chamber can be replaced more easily.
In some embodiments of the present invention, the second shielding gas is one or a mixture of nitrogen and an inert gas. The second protective gas forms a protective atmosphere, which is convenient for crystal growth.
The crystal growth device and the crystal growth method can be applied to growth of germanium crystals, silicon crystals, bismuth germanate crystals, tellurium dioxide crystals, yttrium vanadate-doped crystals, gadolinium vanadate-doped crystals, lithium niobate-doped crystals, lithium tantalate-doped crystals, yttrium aluminum garnet-doped crystals, yttrium aluminate-doped crystals, lutetium aluminate-doped crystals, gadolinium gallium aluminum garnet-doped crystals, lutetium aluminum garnet-doped crystals and yttrium lutetium silicate-doped crystals.
Example 1.
By adopting the crystal growth device, the quartz furnace with the inner diameter of 800mm is respectively fixed with the base and the top cover, and the air outlet pipe is inserted into the liquid tank filled with water; the first water inlet pipe, the first water outlet pipe and the base can form cooling water circulation to maintain the heat dissipation of the base; the second water inlet pipe, the second water outlet pipe and the top cover can form cooling water circulation to maintain the heat dissipation of the top cover; 15kg of raw material of the doped lutetium yttrium silicate crystal is put into an iridium crucible with the diameter of 160mm, and a zirconium oxide heater is started; the heating mode of the zirconia heater is medium-frequency induction heating. 5N argon is introduced from the air inlet to the bottom of the furnace chamber; after maintaining for 0.5h, turning on a power supply, entering a crystal growth procedure, and introducing 5N nitrogen with a certain flow rate from an air inlet to the bottom of the furnace chamber; the tail gas enters the liquid tank through the gas outlet pipe and is discharged after being absorbed by water.
During the crystal growth, the growth condition of the crystal is observed through the furnace chamber and is used as the basis for setting the crystal growth procedure.
The prepared lutetium yttrium silicate crystal has no defects of cracking, bubbles, inclusion, scattering and the like, the diameter reaches 80mm, the length of the constant diameter is 200mm, the weight is 9kg, and a good crystal growth effect is achieved.
Example 2.
By adopting the crystal growth device, the quartz furnace with the inner diameter of 600mm is respectively fixed with the base and the top cover, and the air outlet pipe is inserted into the liquid tank filled with water; the first water inlet pipe, the first water outlet pipe and the base can form cooling water circulation to maintain the heat dissipation of the base; the second water inlet pipe, the second water outlet pipe and the top cover can form cooling water circulation to maintain the heat dissipation of the top cover; loading 8kg of yttrium aluminum garnet doped crystal raw material into an iridium crucible with the diameter of 150mm, and starting a zirconia heater; the heating mode of the zirconia heater is medium-frequency induction heating. 5N argon is introduced from the air inlet to the bottom of the furnace chamber; after maintaining for 1h, turning on a power supply, entering a crystal growth procedure, and introducing 5N argon gas to the bottom of the furnace chamber from an air inlet; the tail gas enters the liquid tank through the gas outlet pipe and is discharged after being absorbed by water.
During the crystal growth, the growth condition of the crystal is observed through the furnace chamber and is used as the basis for setting the crystal growth procedure.
The prepared yttrium aluminum garnet crystal has no defects of cracking, bubbles, inclusion, scattering and the like, the diameter reaches 60mm, the length of the equal diameter reaches 150mm, and a good crystal growth effect is achieved.
Example 3.
By adopting the crystal growth device, the quartz furnace with the inner diameter of 600mm is respectively fixed with the base and the top cover, and the air outlet pipe is inserted into the liquid tank filled with water; the first water inlet pipe, the first water outlet pipe and the base can form cooling water circulation to maintain the heat dissipation of the base; the second water inlet pipe, the second water outlet pipe and the top cover can form cooling water circulation to maintain the heat dissipation of the top cover; loading 10kg of germanium crystal raw material into a graphite crucible with the diameter of 100mm, and starting a zirconium oxide heater; the heating mode of the zirconia heater is medium-frequency induction heating. 5N argon is introduced from the air inlet to the bottom of the furnace chamber; after maintaining for 2 hours, turning on a power supply, entering a crystal growth procedure, and introducing 5N helium gas from an air inlet to the bottom of the furnace chamber; the tail gas enters the liquid tank through the gas outlet pipe and is discharged after being absorbed by water.
During the crystal growth, the growth condition of the crystal is observed through the furnace chamber and is used as the basis for setting the crystal growth procedure.
The prepared germanium crystal has no defects of cracking, bubbles, inclusion, scattering and the like, the diameter reaches 50mm, the equal-diameter length reaches 500mm, and a good crystal growth effect is achieved.
The crystal growth device and the crystal growth method greatly simplify the structure of the furnace chamber, the same furnace chamber can be used for growing crystals with different sizes, the crystal growth cost is also reduced, and good crystal growth effect can be realized.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (10)
1. A crystal growth apparatus, comprising: the crystal growth device comprises a quartz furnace, a base, a top cover, a lifting mechanism and a seed crystal; the base and the top cover are respectively fixed on the lower surface and the upper surface of the quartz furnace; the quartz furnace comprises a crucible, a heat insulation material for coating the crucible, a heater surrounding the crucible, an air inlet pipe, a corrugated pipe, a seed crystal rod and an air outlet pipe; the crucible is internally provided with a melt, and the seed crystal is connected with the liquid level of the melt; the upper part of the heat insulation material is provided with a first through hole which penetrates through the top cover up and down, the top cover is provided with a second through hole which penetrates through the top cover up and down, the corrugated pipe is connected between the top cover and the lifting mechanism, the quartz furnace, the top cover, the corrugated pipe and the lifting mechanism together form a furnace chamber, the seed rod penetrates through the first through hole and the second through hole up and down, and two ends of the seed rod are respectively connected with the seed crystal and the lifting mechanism; the air inlet pipe penetrates through the base and is communicated with the furnace chamber; the air outlet pipe penetrates through the top cover, and one end of the air outlet pipe is communicated with the furnace chamber.
2. The crystal growth apparatus of claim 1, wherein: a plurality of clamping blocks are convexly arranged on the upper surface of the base; the quartz furnace is fixedly connected with the base through a clamping block.
3. The crystal growth apparatus of claim 2, wherein: the base is connected with a first water inlet pipe and a first water outlet pipe.
4. The crystal growth apparatus of claim 3, wherein: the top cover is connected with a second water inlet pipe and a second water outlet pipe.
5. The crystal growth apparatus of claim 4, wherein: the crystal growing apparatus also includes a support for supporting the pulling mechanism.
6. The crystal growth apparatus of claim 5, wherein: the crystal growth device also comprises a liquid tank, the liquid tank is filled with absorption liquid, and the other end of the air outlet pipe is positioned in the absorption liquid.
7. The crystal growth apparatus of claim 6, wherein: the absorption liquid is water.
8. A crystal growth method using the crystal growth apparatus according to any one of claims 4 to 7, characterized in that: the crystal growth method comprises the following steps:
s1: and (3) charging: fixing the quartz furnace in the base; the raw materials are put into a crucible, and a heater is installed; mounting the top cover on a quartz furnace, and inserting an air outlet pipe into a liquid tank containing absorption liquid; cooling water is introduced into the base through the first water inlet pipe, and cooling water is introduced into the top cover through the second water inlet pipe; the cooling water of the base is discharged by a first water outlet pipe; the cooling water of the top cover is discharged by a second water outlet pipe;
s2: crystal growth stage: introducing first protective gas into the furnace chamber from the gas inlet pipe; after the crystal growth is maintained for 0.5-2h, starting a crystal growth program, introducing second protective gas into the furnace chamber from the gas inlet pipe, starting crystal growth on the basis of seed crystals, and adjusting the position of a seed crystal rod by the pulling mechanism as required along with the crystal growth until the crystal growth is finished.
9. The crystal growth method of claim 8, wherein: the first protective gas is argon.
10. The crystal growth method of claim 8, wherein: the second protective gas is one or a mixture of nitrogen and inert gas.
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| CN201810900366.2A CN110820043A (en) | 2018-08-09 | 2018-08-09 | Crystal growth apparatus and growth method |
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| CN112725890A (en) * | 2020-12-25 | 2021-04-30 | 清远先导材料有限公司 | Crystal growth apparatus and crystal growth method |
| CN114045557A (en) * | 2021-10-25 | 2022-02-15 | 安徽光智科技有限公司 | Method and equipment for preparing ultra-high purity germanium single crystal |
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