CN115233299A - Seeding method for growing sapphire by kyropoulos method - Google Patents
Seeding method for growing sapphire by kyropoulos method Download PDFInfo
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- CN115233299A CN115233299A CN202210832932.7A CN202210832932A CN115233299A CN 115233299 A CN115233299 A CN 115233299A CN 202210832932 A CN202210832932 A CN 202210832932A CN 115233299 A CN115233299 A CN 115233299A
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- seed crystal
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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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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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
- 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
- C30B29/20—Aluminium oxides
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a seeding method for sapphire growth by a kyropoulos method, which comprises the following steps: (1) After a blocking annular groove is formed at the lower part of the cylindrical seed crystal, the seed crystal is arranged on a clamp; (2) Heating the alumina raw material in the crucible, and lowering the clamp after the alumina raw material is melted to enable the seed crystal to be inserted below the liquid level of the melt; (3) Controlling the temperature of the melt to enable the liquid level temperature of the melt to be slightly higher than the melting point, and rotating the clamp; (4) After the surface of the seed crystal is slightly melted, reducing the surface temperature of the seed crystal to a melting point, pulling and rotating the clamp, controlling the pulling speed and the rotating speed, and growing the cylindrical crystal in the continuous pulling process. The invention can effectively avoid the phenomenon of eccentric disc polycrystal in the seeding process, lead all the pulled crystal crystals to be in a single crystal state, and greatly improve the crystal quality and the production efficiency.
Description
Technical Field
The invention relates to the technical field of sapphire production, in particular to a seeding method for growing high-quality sapphire by a kyropoulos method.
Background
The second generation semiconductor sapphire crystal growth adopts a kyropoulos method, and the crystal growth process comprises the steps of material melting, seeding, shoulder-expanding growth, equal-diameter growth, ending and annealing.
The seeding method by the kyropoulos method comprises the following steps: placing an aluminum oxide raw material in a crucible in a thermal field, heating to a melting point, melting to form a melt (liquid state), contacting the surface of the melt with a seed crystal of a single crystal, starting to grow the single crystal with the same crystal structure as the seed crystal on a solid-liquid interface of the seed crystal and the melt, pulling the seed crystal upwards at a very slow speed, pulling for a period of time to form a crystal neck, and finishing seeding after the solidification rate of the melt and the seed crystal interface is stable.
In the crystal growth process by the kyropoulos method, the seeding process is the most critical, and the quality of the seeding directly determines the quality of the crystal in the later period, which is taken as the core process of the seeding of the sapphire. For example, chinese patent application publication No. CN104674345a, application publication date 2015, 6-month 3-day, discloses a seeding control method for growing large-size sapphire crystals by kyropoulos method.
In the seeding process, the clean degree of seed crystal washing plays a key role in the seeding process, because in the seeding process, especially a special thermal field of zirconium oxide, a large amount of volatile matters are generated and adhered to the surface of the whole seed crystal in the material melting process, and the volatile matters adhered to the surface of the seed crystal cannot be washed away in the seed crystal washing process (the volatile matters on the surface are difficult to remove at high and low temperatures in the crystal washing process), so that the seed crystal is not in a single crystal state, and the phenomenon of disopy and polycrystal can occur in the seeding process.
The partial discolouration polycrystallization refers to the polycrystallization phenomenon that the seed crystal (with volatile substances adhered to the seed crystal) is contacted with an alumina raw material solution in the seeding process, and the seed crystal grows while not growing. The lower part of the seed crystal is completely in an empty state in the upward pulling process, and the crystal junction led out is not in a vertical state with the seed crystal, so that the stress of the seed crystal and the crystal at the later stage is uneven, the phenomenon of seed crystal breakage is generated in the crystal growing process or the annealing process, if the seed crystal is broken, the crystal in the furnace can not continue to grow, the furnace needs to be opened for restarting, a large amount of labor is wasted, the electricity charge, the time and the like are greatly improved, the production cost is greatly reduced, and the production efficiency is seriously reduced.
Disclosure of Invention
The seeding method for growing sapphire by the kyropoulos method is provided to solve the problem that the phenomenon of disc-biased polycrystal is cracked when the seeding method in the prior art is used for seeding, and the phenomenon of disc-biased polycrystal is avoided in the seeding process, so that all the led crystal crystals are in a single crystal state, and the crystal quality and the production efficiency are greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme: a seeding method for growing sapphire by a kyropoulos method comprises the following steps:
(1) After a blocking annular groove is formed at the lower part of the cylindrical seed crystal, the seed crystal is arranged on the clamp.
(2) Heating the alumina raw material in the crucible, and lowering the clamp after the alumina raw material is molten to ensure that the seed crystal is inserted below the liquid level of the melt.
(3) Controlling the temperature of the melt to ensure that the liquid level temperature of the melt is slightly higher than the melting point, and rotating the clamp.
(4) After the surface of the seed crystal is slightly melted, reducing the surface temperature of the seed crystal to a melting point, pulling and rotating the clamp, controlling the pulling speed and the rotating speed, and growing the cylindrical crystal in the continuous pulling process.
Preferably, in the step (1), the width W of the blocking annular groove is 1 ± 0.1mm.
Preferably, in step (1), the depth D of the blocking annular groove is 10.1mm.
Preferably, in the step (1), the distance H from the blocking annular groove to the lower end of the seed crystal is 30 +/-1 mm.
Preferably, in step (2), the depth L of the seed crystal inserted below the liquid level of the melt is 35. + -.1 mm.
Preferably, in the step (4), the thickness of the melted surface of the seed crystal is 0.3 to 0.5mm.
Therefore, the invention has the following beneficial effects: the blocking ring groove is formed in the bottom of the seed crystal, in the seed crystal washing process, the volatile matter blocking the inside of the ring groove is far less than the volatile matter on the surface of the seed crystal, so that the sticky volatile matter generated in the temperature rising and material melting process of the seed crystal can be divided into two sections, the effect of segmenting the volatile matter is achieved, the volatile matter located below the blocking ring groove and stuck on the surface of the seed crystal can fall off along with the epidermis of the seed crystal, the outer surface of the seed crystal located below the blocking ring groove is quite clean, the state of the single crystal is achieved, the phenomenon of partial disc polycrystal can not occur in the seeding process, all the led crystal junctions are in the single crystal state and are quite stable, crystals can not fall in the middle-stage crystal growth and later-stage annealing processes, the production efficiency is improved, and the crystal quality is guaranteed.
Drawings
FIG. 1 is a schematic view of a state in which a seed crystal is inserted below the liquid level of a melt in the present invention.
Fig. 2 is an enlarged view at a in fig. 1.
In the figure: seed crystal 1, blocking ring groove 2, and clamp 3.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
(1) After a blocking annular groove 2 (shown in figure 1) is formed in the lower part of a cylindrical seed crystal 1, the seed crystal is arranged on a clamp 3, the distance L from the blocking annular groove to the lower end of the seed crystal is 30mm, the width W of the blocking annular groove is 1mm, and the depth D of the blocking annular groove is 1 +/-0.1 mm;
(2) Heating the alumina raw material in the crucible, and after the alumina raw material is melted, lowering the clamp to enable the seed crystal to be inserted below the liquid level of the melt, wherein the depth L of the seed crystal inserted below the liquid level of the melt is 35mm;
(3) Controlling the temperature of the melt to enable the liquid level temperature of the melt to be slightly higher than the melting point, and rotating the clamp;
(4) After the surface of the seed crystal is slightly melted, reducing the surface temperature of the seed crystal to a melting point, pulling and rotating the clamp, controlling the pulling speed and the rotating speed, and growing the cylindrical crystal in the continuous pulling process.
According to the invention, the blocking annular groove is formed at the bottom of the seed crystal, when the seed crystal is washed, volatile matters in the blocking annular groove are far less than volatile matters on the surface of the seed crystal, and the volatile matters below the blocking annular groove and adhered to the surface of the seed crystal can fall off along with the surface of the seed crystal, so that the outer surface of the seed crystal below the blocking annular groove is very clean, the phenomenon of biased disc polycrystal in the seeding process is effectively avoided, the all the led crystal junctions are in a single crystal state and are very stable, crystals can not fall off in the middle-stage crystal growth and later-stage annealing processes, the production efficiency is improved, and the crystal quality is ensured.
The above-described embodiment is a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. A seeding method for growing sapphire by a kyropoulos method is characterized by comprising the following steps:
the method comprises the following steps that (1) after a blocking annular groove (2) is formed in the lower portion of a cylindrical seed crystal (1), the seed crystal is installed on a clamp (3);
(2) Heating the alumina raw material in the crucible, and lowering the clamp after the alumina raw material is melted to enable the seed crystal to be inserted below the liquid level of the melt;
(3) Controlling the temperature of the melt to enable the liquid level temperature of the melt to be slightly higher than the melting point, and rotating the clamp;
(4) After the surface of the seed crystal is slightly melted, reducing the surface temperature of the seed crystal to a melting point, pulling and rotating the clamp, controlling the pulling speed and the rotating speed, and growing the cylindrical crystal in the continuous pulling process.
2. A seeding method for sapphire growth by kyropoulos method according to claim 1, wherein in step (1), the width W of the blocking annular groove is 1 ± 0.1mm.
3. A seeding method for sapphire growth by kyropoulos method according to claim 1, wherein in step (1), the depth D of the blocking annular groove is 1 ± 0.1mm.
4. A seeding method for sapphire growth by kyropoulos method according to claim 1, 2 or 3, wherein in step (1), the distance H between the blocking annular groove and the lower end of the seed crystal is 30 ± 1mm.
5. A seeding method for sapphire growth by kyropoulos method according to claim 1, wherein in step (2), the seed crystal is inserted to a depth L of 35 ± 1mm below the liquid level of the melt.
6. The seeding method for sapphire growth by kyropoulos method according to claim 1, wherein in the step (4), the thickness of the melted surface of the seed crystal is 0.3 to 0.5mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210832932.7A CN115233299A (en) | 2022-07-14 | 2022-07-14 | Seeding method for growing sapphire by kyropoulos method |
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| CN202210832932.7A CN115233299A (en) | 2022-07-14 | 2022-07-14 | Seeding method for growing sapphire by kyropoulos method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116575114A (en) * | 2023-07-14 | 2023-08-11 | 内蒙古晶环电子材料有限公司 | Seeding method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877120A (en) * | 2012-09-29 | 2013-01-16 | 浙江东晶光电科技有限公司 | Automatic seeding technique for growing sapphire crystal by Kyropoulos method |
| JP2013209257A (en) * | 2012-03-30 | 2013-10-10 | Sumco Corp | Sapphire single crystal and method for producing the same |
| CN104674345A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Seeding control method for large-size sapphire crystals growing through Kyropulos method |
| CN113652748A (en) * | 2021-08-18 | 2021-11-16 | 山东天岳先进科技股份有限公司 | Seed crystal with annular barrier belt and processing method thereof |
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2022
- 2022-07-14 CN CN202210832932.7A patent/CN115233299A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013209257A (en) * | 2012-03-30 | 2013-10-10 | Sumco Corp | Sapphire single crystal and method for producing the same |
| CN102877120A (en) * | 2012-09-29 | 2013-01-16 | 浙江东晶光电科技有限公司 | Automatic seeding technique for growing sapphire crystal by Kyropoulos method |
| CN104674345A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Seeding control method for large-size sapphire crystals growing through Kyropulos method |
| CN113652748A (en) * | 2021-08-18 | 2021-11-16 | 山东天岳先进科技股份有限公司 | Seed crystal with annular barrier belt and processing method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116575114A (en) * | 2023-07-14 | 2023-08-11 | 内蒙古晶环电子材料有限公司 | Seeding method |
| CN116575114B (en) * | 2023-07-14 | 2023-11-28 | 内蒙古晶环电子材料有限公司 | Seeding method |
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