CN116791190A - Quasi-closed tube kyropoulos crucible and use method thereof - Google Patents
Quasi-closed tube kyropoulos crucible and use method thereof Download PDFInfo
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- CN116791190A CN116791190A CN202310812387.XA CN202310812387A CN116791190A CN 116791190 A CN116791190 A CN 116791190A CN 202310812387 A CN202310812387 A CN 202310812387A CN 116791190 A CN116791190 A CN 116791190A
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- crucible
- sleeve
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- quasi
- seed rod
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- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000013078 crystal Substances 0.000 claims abstract description 87
- 238000007789 sealing Methods 0.000 claims abstract description 74
- 239000007788 liquid Substances 0.000 claims abstract description 68
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 239000010453 quartz Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 239000000155 melt Substances 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 238000010899 nucleation Methods 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000565 sealant Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000011449 brick Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000009347 mechanical transmission Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a quasi-closed tube kyropoulos crucible and a use method thereof, comprising the following steps: the lower end of the seed rod is provided with a clamping part for clamping seed crystals, and the side surface of the seed rod extends outwards along the circumferential direction of the seed rod to form a liquid seal groove; the sleeve is sleeved outside the seed rod, one end of the sleeve is operatively arranged in the liquid seal groove, a first gap is formed between the inner surface of the sleeve and the outer surface of the seed rod, the first gap is communicated with the liquid seal groove, and the sleeve can move relative to the seed rod along the axial direction; the crucible device is provided with an operably closed accommodating space, and the lower end of the seed rod, the liquid sealing groove and the lower end of the sleeve are operably arranged in the accommodating space. The liquid seal design of the invention has the advantages of both the open pipe method and the closed pipe method, and can simultaneously meet the transmission requirement of seed crystal pulling and the control requirement of component vapor pressure.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a quasi-closed tube kyropoulos crucible and a manufacturing method thereof.
Background
In the prior art, an open-tube crucible is adopted to realize the seeding requirement of the growth of crystals by a bubble growth method. For the compound crystal with volatile components, a layer of liquid sealing agent is added above the crystal, and the crucible is still in open-tube design. Open-pipe designs still suffer from the following drawbacks and disadvantages:
the open-tube type growth equipment has a complex structure, and the heating module is exposed in the crystal growth atmosphere and has higher requirements on the material and the sealing performance of the furnace chamber;
the temperature of the cold point in the furnace chamber is too low, and volatile components are easy to condense, so that the partial pressure of the volatile components and the proportion of the compound components cannot be regulated;
the liquid sealing agent needs to be covered above the crystal thickly, the usage amount is very large, and meanwhile, the crystal is grown by contact, so that defects such as dislocation and the like are easy to introduce;
disclosure of Invention
In view of the above, the invention aims to provide a quasi-closed tube kyropoulos crucible adopting a liquid seal, which can realize the advantages of an open tube method and a closed tube method and can simultaneously meet the transmission requirement of seed crystal pulling and the control requirement of component vapor pressure.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a quasi-closed tube kyropoulos method crucible, comprising:
the seed rod is provided with a clamping part at the lower end for clamping seed crystals, and the side surface of the seed rod extends outwards along the circumferential direction to form a liquid seal groove;
the sleeve is sleeved outside the seed rod, one end of the sleeve is operably arranged in the liquid seal groove, a first gap is formed between the inner surface of the sleeve and the outer surface of the seed rod, the first gap is communicated with the liquid seal groove, and the sleeve can move along the axial direction relative to the seed rod;
the crucible device is provided with an operably closed accommodating space, and the lower end of the seed rod, the liquid seal groove and the lower end of the sleeve are operably arranged in the accommodating space.
The above-mentioned quasi-closed tube kyropoulos method crucible, wherein, the crucible device includes: the device comprises a crystal growth crucible and a PBN crucible arranged in the crystal growth crucible, wherein the outer wall of the sleeve is in sealing connection with the inner wall of the crystal growth crucible through a sealing piece.
The quasi-closed tube kyropoulos method crucible comprises a first part and a second part which are connected with each other, wherein the first part is positioned at the upper part of the second part, and the inner diameter of the first part is larger than the inner diameter of the second part;
the PBN crucible is disposed within the first portion;
the outer wall of the sleeve is in sealing connection with the inner wall of the first part through a sealing piece.
The quasi-closed tube kyropoulos method crucible is characterized in that the sealing piece is a quartz plug, the quartz plug is annular, the inner side of the quartz plug is fixedly connected with the outer wall of the sleeve, and the outer side of the quartz plug is propped against the inner wall of the first part.
The quasi-closed tube kyropoulos method crucible is characterized in that a liquid sealing agent is arranged in the liquid sealing groove;
the interior of the crystal growth crucible is filled with an atmosphere of a set pressure, which is greater than one atmosphere, to press the liquid sealing agent in a liquid state into the first gap.
The quasi-closed tube kyropoulos method crucible is characterized in that a sealing orifice is arranged at the upper part of the sleeve.
The quasi-closed tube kyropoulos method crucible, further comprising: and the crystal pulling rod is fixedly connected with the upper end of the seed crystal rod, and a second gap is formed between the inner surface of the sleeve and the outer surface of the crystal pulling rod.
The quasi-closed tube kyropoulos method crucible is characterized in that a wax seal is arranged in the second gap.
A method of using a quasi-closed tube kyropoulos method crucible, wherein a quasi-closed tube kyropoulos method crucible is used, the quasi-closed tube kyropoulos method crucible comprising:
the seed rod is provided with a clamping part at the lower end for clamping seed crystals, and the side surface of the seed rod extends outwards along the circumferential direction to form a liquid seal groove;
the sleeve is sleeved outside the seed rod, one end of the sleeve is operably arranged in the liquid seal groove, a first gap is formed between the inner surface of the sleeve and the outer surface of the seed rod, the first gap is communicated with the liquid seal groove, and the sleeve can move along the axial direction relative to the seed rod;
the crystal pulling rod is fixedly connected with the upper end of the seed rod, and a second gap is formed between the inner surface of the sleeve and the outer surface of the seed rod;
the device comprises a crystal growth crucible and a PBN crucible arranged in the crystal growth crucible, wherein the outer wall of the sleeve is in sealing connection with the inner wall of the crystal growth crucible through a sealing piece;
the using method comprises the following steps:
clamping a seed crystal at the lower end of the seed rod;
mounting the upper end of the seed rod to the lower end of the pull rod;
inserting the seed rod into the sleeve;
adjusting the height position and the center position of the seed rod relative to the sleeve, and arranging a wax seal between the seed rod and the sleeve, wherein the wax seal is positioned above the liquid seal groove;
arranging a liquid sealing agent in the liquid sealing groove;
and obtaining a seed crystal mechanism.
The quasi-closed tube kyropoulos method crucible, wherein the using method further comprises the following steps:
placing an atmosphere source in the crystal growth crucible; placing the PBN crucible in the crystal growth crucible; placing a polycrystalline material into the PBN crucible;
placing the seed crystal mechanism above the polycrystalline material;
the pipe orifice of the crystal growth crucible is connected into a vacuumizing device, vacuumized and deaerated;
welding the sealing piece of the seed crystal mechanism and the long crystal crucible to finish primary tube sealing;
breaking vacuum, and removing the part of the crystal growth crucible above the sealing element;
the pipe sealing port at the upper part of the sleeve is connected into a vacuumizing device, vacuumized and deaerated;
and (5) burning and melting the tube sealing port to finish secondary tube sealing.
The quasi-closed tube kyropoulos method crucible, wherein the using method further comprises the following steps:
at a growth temperature, the liquid sealing agent melts, the atmosphere source provides an atmosphere of a set pressure, the wax seal melts, the liquid sealing agent in a liquid state is pressed into the first gap, and relative movement among the seed rod, the pull rod and the sleeve is allowed;
and (3) descending the seed crystal to contact with the molten polycrystal material, so as to finish seeding.
The invention adopts the technology, so that compared with the prior art, the invention has the positive effects that:
(1) The liquid seal design of the invention has the advantages of both the open pipe method and the closed pipe method, and can simultaneously meet the transmission requirement of seed crystal pulling and the control requirement of component vapor pressure;
(2) The crystal growth furnace has simple structure and thermal field design requirements, and can be suitable for crystal growth furnaces of a vertical Bridgman method and a vertical temperature gradient solidification method;
(3) The sealing material has small demand, and the crystal is grown after being separated from contact, so that defects are not introduced;
(4) The invention can realize the atmosphere sealing in the crucible at the same time, and the seed crystal is controlled to rise and fall by an external mechanical transmission device;
(5) The invention adopts the design of unsealing the pipe orifice on the side wall of the sleeve and sealing the upper end gap wax seal, and can realize the vacuumizing and pipe sealing of the crucible system at room temperature.
Drawings
FIG. 1 is a schematic view of a quasi-closed tube kyropoulos crucible of the present invention.
FIG. 2 is an enlarged partial schematic view of a quasi-closed tube kyropoulos crucible of the present invention.
FIG. 3 is a schematic diagram of the closing orifice of the quasi-closed tube kyropoulos crucible of the present invention.
FIG. 4 is a schematic view of a seed rod and a pull rod of a quasi-closed tube kyropoulos crucible of the present invention.
FIG. 5 is a schematic view of the bushing of the quasi-closed tube kyropoulos crucible of the present invention.
FIG. 6 is a schematic view of a seed mechanism of the quasi-closed tube kyropoulos crucible of the present invention.
FIG. 7 is a schematic view of a growth crucible of the quasi-closed tube kyropoulos crucible of the present invention.
FIG. 8 is a schematic view of a quasi-closed tube kyropoulos crucible of the present invention.
FIG. 9 is a schematic view of a quasi-closed tube kyropoulos crucible of the present invention.
In the accompanying drawings: 1. seed rods; 10. seed crystal; 11. a clamping part; 12. a liquid seal groove; 2. a sleeve; 21. sealing the pipe orifice; 3. growing a crystal crucible; 31. a first portion; 32. a second portion; 4. a PBN crucible; 5. a quartz plug; 6. pulling the crystal bar; 7. sealing with wax; 8. an atmosphere source; 91. a furnace tube of a crystal growth furnace; 92. and (5) insulating bricks.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "upper," "lower," "left," "right," "inner," "outer," "front," "rear," "transverse," "vertical," and the like are used for convenience in describing the present invention based on the orientation or positional relationship shown in the drawings, and do not denote or imply that the device or element to be referred to must have a specific orientation, and thus should not be construed as limiting the present invention.
In the present invention, "horizontal" and "vertical" are used to describe a general positional relationship, and are not strictly "horizontal" or "vertical".
Referring to fig. 1 to 9, a quasi-closed tube kyropoulos crucible of a preferred embodiment is shown, comprising: the seed rod 1, the lower end of the seed rod 1 is provided with a clamping part 11 for clamping a seed crystal 10, and the side surface of the seed rod 1 extends outwards along the circumferential direction to form a liquid seal groove 12.
Further, as a preferred embodiment, the quasi-closed tube kyropoulos method crucible further comprises: the sleeve 2 is sleeved outside the seed rod 1, one end of the sleeve 2 is operatively arranged in the liquid seal groove 12, a first gap is formed between the inner surface of the sleeve 2 and the outer surface of the seed rod 1, the first gap is communicated with the liquid seal groove 12, and the sleeve 2 can move relative to the seed rod 1 along the axial direction.
Preferably, the seed rod 1 and the liquid seal tank 12 are made of an integrated quartz material.
Further, as a preferred embodiment, the quasi-closed tube kyropoulos method crucible further comprises: the crucible device is provided with an operably closed accommodating space, and the lower end of the seed rod 1, the liquid seal groove 12 and the lower end of the sleeve 2 are operably arranged in the accommodating space.
Further, as a preferred embodiment, the crucible apparatus includes: the crystal growth crucible 3 and the PBN crucible 4 arranged in the crystal growth crucible 3 are hermetically connected through a sealing piece, and the outer wall of the sleeve 2 is hermetically connected with the inner wall of the crystal growth crucible 3.
Further, as a preferred embodiment, the growth crucible 3 includes a first portion 31 and a second portion 32 connected to each other, the first portion 31 being located at an upper portion of the second portion 32, the first portion 31 having an inner diameter larger than an inner diameter of the second portion 32.
Further, as a preferred embodiment, the PBN crucible 4 is provided in the first portion 31.
Preferably, the growth crucible 3 has a variable diameter between the first portion 31 and the second portion 32, where the PBN crucible 4 is erected.
Further, as a preferred embodiment, the outer wall of the sleeve 2 is sealingly connected to the inner wall of the first portion 31 by a seal.
Further, as a preferred embodiment, the sealing member is a quartz plug 5, the quartz plug 5 is annular, the inner side of the quartz plug 5 is fixedly connected with the outer wall of the sleeve 2, and the outer side of the quartz plug 5 abuts against the inner wall of the first portion 31.
Further, as a preferred embodiment, a liquid sealant is provided in the liquid seal tank 12.
Preferably, the liquid sealing agent is B 2 O 3。
Further, as a preferred embodiment, the inside of the long crystal crucible 3 is filled with an atmosphere of a set pressure, which is greater than one atmosphere, to press the liquid sealing agent in a liquid state into the first gap.
Preferably, the atmosphere is provided by an atmosphere source, which is typically an elemental substance of a component of the compound crystal.
Further, as a preferred embodiment, the upper part of the sleeve 2 has a closing nozzle 21.
Specifically, the sealing nozzle 21 is located at the side of the upper portion of the sleeve 2, and the sealing nozzle 21 has a tubular structure and communicates with the interior of the sleeve 2.
More specifically, the axis of the nozzle 21 is perpendicular to the axis of the sleeve 2.
Further, as a preferred embodiment, the quasi-closed tube kyropoulos method crucible further comprises: the crystal pulling rod 6 is fixedly connected with the upper end of the seed rod 1, and a second gap is formed between the inner surface of the sleeve 2 and the outer surface of the crystal pulling rod 6.
Preferably, the pull rod 6 is made of a material having high heat conductivity and strength.
More preferably, the top of the pull rod 6 may be water cooled or air cooled to conduct away the heat flow.
Further, as a preferred embodiment, a wax seal 7 is provided in the second gap.
Specifically, the liquid seal design principle is shown in fig. 2. At the growth temperature, the liquid sealing agent melts, filling the liquid sealing tank 12. The atmosphere pressure is controlled by controlling the temperature at the atmosphere source 8. Under atmospheric pressure control, the growth crucible 3 is filled with an atmosphere of a pressure, typically greater than one atmosphere, so that the liquid sealant is pressed into the gap between the seed rod 1 and the sleeve 2.
Further, along with the increase of the pressing-in distance, the front edge of the liquid sealing agent is far away from the growth temperature area, the temperature is reduced, the viscosity is increased, the liquid sealing agent is prevented from being pushed in the gap, and finally, the balance is achieved, so that the liquid sealing is realized. At the same time, the pull rod 1 can move up and down relative to the sleeve 2.
Furthermore, since the liquid sealing agent is solid at room temperature, the sealing effect cannot be achieved, and another set of sealing scheme at room temperature needs to be designed at the top. The schematic diagram of the top seal is shown in fig. 3, wax with lower melting point is smeared at the gap between the top of the pull rod 6 and the sleeve 2, and the sealing effect is achieved at low temperature. And simultaneously, vacuumizing, degassing and secondary tube sealing are carried out through the tube sealing opening 21 of the sleeve 2. At the growth temperature, heat conduction is up, and the wax seal is melted again, so that the crystal pulling rod 6 can move up and down relative to the sleeve 2.
The invention also provides a use method of the quasi-closed tube kyropoulos method crucible, which comprises the following steps:
clamping a seed crystal 10 at the lower end of a seed rod 1;
the upper end of the seed rod 1 is mounted to the lower end of the crystal pulling rod 6;
specifically, the seed rod 1 and the crystal pulling rod 6 can be connected by adopting a threaded connection or a mortise-tenon structure;
inserting the seed rod 1 into the sleeve 2;
adjusting the height position and the center position of the seed rod 1 relative to the sleeve 2, arranging a wax seal 7 between the seed rod 1 and the sleeve 2, and positioning the wax seal 7 above the liquid seal groove 12;
specifically, the wax is heated to melt, and is dropped into a gap between the pull rod 6 and the upper end of the sleeve 2, and solidified to form a wax seal 7.
Disposing a liquid sealant within the liquid seal tank 12;
and obtaining a seed crystal mechanism.
Further, as a preferred embodiment, the method of use further comprises:
placing an atmosphere source 8 in the crystal growth crucible 3; placing a PBN crucible 4 in the crystal growing crucible 3; placing polycrystalline materials into a PBN crucible 4;
placing a seed crystal mechanism above the polycrystalline material;
the pipe orifice of the crystal growth crucible 3 is connected into a vacuum pumping device, and the vacuum pumping and degassing are carried out;
welding a sealing piece of the seed crystal mechanism and the long crystal crucible 3 to finish primary tube sealing;
breaking vacuum, and removing the part of the crystal growth crucible 3 above the sealing element;
the sealing pipe orifice 21 at the upper part of the sleeve 2 is connected into a vacuumizing device, vacuumized and deaerated;
and (5) burning and melting the sealing pipe orifice 21 to finish secondary sealing.
Further, as a preferred embodiment, the method of use further comprises:
at the growth temperature, the liquid sealing agent melts, the atmosphere source provides an atmosphere of set pressure, the wax seal 7 melts, the liquid sealing agent in the liquid state is pressed into the first gap, and the relative movement among the seed rod 1, the crystal pulling rod 6 and the sleeve 2 is allowed;
and (3) descending the seed crystal to contact with the molten polycrystal material, so as to finish seeding.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, and it will be appreciated by those skilled in the art that equivalent substitutions and obvious variations may be made using the description and illustrations of the present invention, and are intended to be included within the scope of the present invention.
Claims (11)
1. A quasi-closed tube kyropoulos crucible comprising:
the seed rod is provided with a clamping part at the lower end for clamping seed crystals, and the side surface of the seed rod extends outwards along the circumferential direction to form a liquid seal groove;
the sleeve is sleeved outside the seed rod, one end of the sleeve is operably arranged in the liquid seal groove, a first gap is formed between the inner surface of the sleeve and the outer surface of the seed rod, the first gap is communicated with the liquid seal groove, and the sleeve can move along the axial direction relative to the seed rod;
the crucible device is provided with an operably closed accommodating space, and the lower end of the seed rod, the liquid seal groove and the lower end of the sleeve are operably arranged in the accommodating space.
2. The quasi-closed tube kyropoulos method crucible as claimed in claim 1, wherein the crucible apparatus comprises: the device comprises a crystal growth crucible and a PBN crucible arranged in the crystal growth crucible, wherein the outer wall of the sleeve is in sealing connection with the inner wall of the crystal growth crucible through a sealing piece.
3. The quasi-closed tube kyropoulos method crucible of claim 1, wherein the growing crucible comprises a first portion and a second portion connected to each other, the first portion being located at an upper portion of the second portion, an inner diameter of the first portion being greater than an inner diameter of the second portion;
the PBN crucible is disposed within the first portion;
the outer wall of the sleeve is in sealing connection with the inner wall of the first part through a sealing piece.
4. A quasi-closed tube kyropoulos method crucible as in claim 3 wherein the seal is a quartz plug, the quartz plug is ring-shaped, the inside of the quartz plug is fixedly connected with the outer wall of the sleeve, the outside of the quartz plug is in abutment with the inner wall of the first portion.
5. The quasi-closed tube kyropoulos method crucible of claim 1, wherein a liquid sealing agent is provided in the liquid sealing tank;
the interior of the crystal growth crucible is filled with an atmosphere of a set pressure, which is greater than one atmosphere, to press the liquid sealing agent in a liquid state into the first gap.
6. The quasi-closed tube kyropoulos method crucible of claim 1, wherein the upper portion of the sleeve has a closing orifice.
7. The quasi-closed tube kyropoulos method crucible of claim 1, further comprising: and the crystal pulling rod is fixedly connected with the upper end of the seed rod, and a second gap is formed between the inner surface of the sleeve and the outer surface of the seed rod.
8. The quasi-closed tube kyropoulos method crucible of claim 9, wherein a wax seal is provided in the second gap.
9. A method of using a quasi-closed tube kyropoulos method crucible, characterized in that a quasi-closed tube kyropoulos method crucible is used, the quasi-closed tube kyropoulos method crucible comprising:
the seed rod is provided with a clamping part at the lower end for clamping seed crystals, and the side surface of the seed rod extends outwards along the circumferential direction to form a liquid seal groove;
the sleeve is sleeved outside the seed rod, one end of the sleeve is operably arranged in the liquid seal groove, a first gap is formed between the inner surface of the sleeve and the outer surface of the seed rod, the first gap is communicated with the liquid seal groove, and the sleeve can move along the axial direction relative to the seed rod;
the crystal pulling rod is fixedly connected with the upper end of the seed crystal rod, and a second gap is formed between the inner surface of the sleeve and the outer surface of the crystal pulling rod;
the device comprises a crystal growth crucible and a PBN crucible arranged in the crystal growth crucible, wherein the outer wall of the sleeve is in sealing connection with the inner wall of the crystal growth crucible through a sealing piece;
the using method comprises the following steps:
clamping a seed crystal at the lower end of the seed rod;
mounting the upper end of the seed rod to the lower end of the pull rod;
inserting the seed rod into the sleeve;
adjusting the height position and the center position of the seed rod relative to the sleeve, and arranging a wax seal between the seed rod and the sleeve, wherein the wax seal is positioned above the liquid seal groove;
arranging a liquid sealing agent in the liquid sealing groove;
and obtaining a seed crystal mechanism.
10. The quasi-closed tube kyropoulos method crucible of claim 9, wherein the method of use further comprises:
placing an atmosphere source in the crystal growth crucible; placing the PBN crucible in the crystal growth crucible; placing a polycrystalline material into the PBN crucible;
placing the seed crystal mechanism above the polycrystalline material;
the pipe orifice of the crystal growth crucible is connected into a vacuumizing device, vacuumized and deaerated;
welding the sealing piece of the seed crystal mechanism and the long crystal crucible to finish primary tube sealing;
breaking vacuum, and removing the part of the crystal growth crucible above the sealing element;
the pipe sealing port at the upper part of the sleeve is connected into a vacuumizing device, vacuumized and deaerated;
and (5) burning and melting the tube sealing port to finish secondary tube sealing.
11. The quasi-closed tube kyropoulos method crucible of claim 10, wherein the method of use further comprises:
at a growth temperature, the liquid sealing agent melts, the atmosphere source provides an atmosphere of a set pressure, the wax seal melts, the liquid sealing agent in a liquid state is pressed into the first gap, and relative movement among the seed rod, the pull rod and the sleeve is allowed;
and (3) descending the seed crystal to contact with the molten polycrystal material, so as to finish seeding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310812387.XA CN116791190A (en) | 2023-07-04 | 2023-07-04 | Quasi-closed tube kyropoulos crucible and use method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310812387.XA CN116791190A (en) | 2023-07-04 | 2023-07-04 | Quasi-closed tube kyropoulos crucible and use method thereof |
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