CN111607823A - Sapphire single crystal pulling method preparation device and method - Google Patents
Sapphire single crystal pulling method preparation device and method Download PDFInfo
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- CN111607823A CN111607823A CN202010566637.2A CN202010566637A CN111607823A CN 111607823 A CN111607823 A CN 111607823A CN 202010566637 A CN202010566637 A CN 202010566637A CN 111607823 A CN111607823 A CN 111607823A
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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
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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
- C30B15/10—Crucibles or containers for supporting the 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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
Abstract
The invention relates to the technical field of sapphire preparation, in particular to a device and a method for preparing a sapphire single crystal by a pulling method. The device comprises a crucible, a heating system, a driving system, a heat preservation system and a vacuum system; the heating system comprises a heater; the driving system comprises a seed shaft, and the seed shaft is connected with the rotary lifting device; the heat preservation system comprises a heat preservation layer, the heat preservation layer is arranged between the furnace wall and the heater, and the heat preservation layer comprises a zirconium oxide heat insulation layer, a molybdenum sheet heat insulation screen and a nano tungsten film reflection layer; the heat preservation system also comprises an argon supply device, wherein the argon supply device comprises an air supply pipe arranged on the furnace wall and an argon gas storage tank connected with the air supply pipe. On the basis of improving the production efficiency, the quality of the obtained crystal is obviously improved, for example, the crystallization quality is more uniform, and the integrity and the optical transmittance of the crystal are obviously improved.
Description
Technical Field
The invention relates to the technical field of sapphire preparation, in particular to a device and a method for preparing a sapphire single crystal by a pulling method.
Background
The sapphire crystal has high hardness of 9-grade Mohs hardness, the melting point of 2050 ℃ and the boiling point of 3500 ℃, and can be used as an important technical crystal. It has excellent light transmission, heat conductivity, electric insulation and mechanical performance, and is widely used in scientific technology, national defense and civil industry, and many fields of electronic technology, such as laser matrix, substrate, optical element, etc.
At present, the manufacturing method of the artificial sapphire comprises a kyropoulos method, a heat exchange method, a mold guiding method, a pulling method and the like, and various methods respectively have advantages and disadvantages aiming at different characteristics. In the growth of sapphire crystals, after in-situ annealing and pulling-off, the furnace temperature can be reduced to the blow-in condition by depending on the circulating water cooling of the furnace body within about 5 days, and nearly half of the time is reduced in the growth period of 45 kg crystals within 12 days, so that the production efficiency is limited, the time is long and the efficiency is low.
The applicant provides a sapphire single crystal pulling method preparation device and method through the structure, process steps, parameter control and the like of an adjusting device aiming at the research and improvement of the pulling method.
Disclosure of Invention
Aiming at the defects of long cooling time, low production quality and the like of the sapphire production method in the prior art, the invention provides a pulling method preparation device and method of sapphire single crystal.
The technical scheme of the invention is as follows:
a pulling method preparation device of sapphire single crystal comprises a crucible, a heating system, a driving system, a heat preservation system and a vacuum system;
the heating system comprises a heater;
the driving system comprises a seed shaft, and the seed shaft is connected with the rotary lifting device;
the heat preservation system comprises a heat preservation layer, the heat preservation layer is arranged between the furnace wall and the heater, and the heat preservation layer comprises a zirconium oxide heat insulation layer, a molybdenum sheet heat insulation screen and a nano tungsten film reflection layer; the heat preservation system also comprises an argon supply device, wherein the argon supply device comprises an air supply pipe arranged on the furnace wall and an argon gas storage tank connected with the air supply pipe.
Furthermore, the heater comprises two parts, wherein one part is a side wall annular heater matched with the side plate of the crucible, and the other part is a bottom sheet heater matched with the bottom of the crucible; the two parts of heaters are adopted, so that the temperature of different parts can be flexibly controlled, the problem that the central area at the bottom of the crucible is uniformly heated is solved, and favorable temperature regulation conditions are provided for uniform growth of crystals.
Furthermore, the crucible is an iridium crucible, the crucible is in the shape of a cylinder with a spherical crown at the bottom, and the bottom of the crucible is in the shape of a spherical crown, so that the crucible is matched with a crystal growth interface in the crystal growth process, the temperature uniformity of the molten liquid is more favorably ensured, and favorable conditions are further provided for the uniform growth of the crystal.
Furthermore, the rotary lifting device comprises a worm gear speed reducer, a synchronous belt, a precise planetary speed reducer and a servo motor; and a precise transmission mode is adopted, so that precise rotation and lifting are realized, and precise equipment conditions are provided for the Czochralski method growth of the crystal.
Furthermore, the seed shaft rotary seal adopts magnetic fluid seal, the vertical motion seal adopts a stainless steel corrugated pipe, and the vacuum environment is effectively kept through precise seal.
Furthermore, a temperature sensor and a gas flowmeter are arranged on the gas supply pipe, so that the flow and the problem of supplied argon can be conveniently controlled, conditions are provided for the cooling step in the furnace, the cooling time can be greatly reduced, and the production efficiency is improved.
Furthermore, the vacuum system adopts a direct-connection rotary vane vacuum pump and a high-vacuum gate valve, so that the vacuum degree of the equipment is improved, and the quality of crystals is improved.
The invention also aims to provide a method for preparing the sapphire single crystal by the pulling method, which comprises the steps of raw material preparation, vacuumizing, heating and melting, crystal growth and cooling, and specifically comprises the following steps:
raw material preparation: the method comprises the following steps of (1) adopting a mixture of high-purity alumina powder with the purity of 5 grade and crushed crystals, wherein the weight ratio of the high-purity alumina powder to the crushed crystals is 5:1, the crushed crystals need to be cleaned for multiple times by ultrasonic waves, and the high-purity alumina powder needs to be pressed into cylindrical blocks; the gas contained in the raw materials can be discharged as far as possible after pressing, the quality of the raw materials is improved, in addition, the crushed crystals are placed at the bottom, the quality of the raw materials is good, and the quality improvement during bottom melt crystallization is facilitated.
Vacuumizing step, namely vacuumizing the furnace to 1-5 × 10 vacuum degree-4Pa。
Heating and melting: heating is started, the temperature is raised to 2500 ℃ for 1-3 hours, and the raw materials are ensured to be completely melted.
A crystal growth step: lowering the seed shaft to start seeding, controlling the temperature to be 1800-plus 2300 ℃, necking, shouldering, growing the crystal to a proper size, and then annealing; the rotating speed of the seed crystal shaft is 3-15 r/min.
And (3) cooling: argon is introduced into the furnace through an air supply pipe to cool the crystal, and the cooling time lasts for 1.5 to 3 hours. Through letting in the argon gas cooling, properly accelerated the cooling speed, shortened the cooling time, effectively improved production efficiency.
Further, a heating and melting step: the temperature is raised to 2400-.
The beneficial effect of the invention is that,
the device of the invention optimizes and improves the structure of the heater, the driving mode of the driving system, the heat preservation system and the like, and sets the argon cooling mode, thereby effectively shortening the cooling time, predicting that the cooling time can be shortened by 2 days from 5 days, reducing the growth cycle of 45 kg crystals from 12 days to 10 days, saving 1500 ℃ electricity in each furnace, and producing 5 more crystals in each furnace year.
Direct benefit: 1500 degrees can be saved in each furnace, 3 furnaces are produced per month, 40 × 3 × 1500 ═ 18 ten thousand degrees can be saved in 40 furnaces per month, 180000 degrees × 0.68 yuan ═ 122400 yuan can be saved, and 12.24 × 11 ≈ 135 ten thousand yuan can be saved each year. In addition, more crystals 40 x 5-200 can be produced in the year, and the economic benefit is better.
After the device is adopted, the method optimizes and innovates the selection of raw materials, the vacuum degree, the heating and melting temperature and time, the crystal growth process and the like, and obviously improves the quality of the obtained crystal on the basis of improving the production efficiency, for example, the crystallization quality is more uniform, and the integrity and the optical transmittance of the crystal are obviously improved.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic view of the apparatus of the present invention;
the device comprises a crucible 1, a side wall annular heater 21, a bottom sheet heater 22, a seed crystal shaft 3, a zirconium oxide heat insulation layer 51, a molybdenum sheet heat shield 52, a nano tungsten film reflection layer 53, an argon gas storage tank 6, a temperature sensor 61, a gas flowmeter 62, a rotary lifting device 7 and a vacuum pump 8.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment 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.
Example 1 device for producing sapphire single crystal by Czochralski method
The technical scheme is as follows: comprises a crucible 1, a heating system, a driving system, a heat preservation system and a vacuum system;
the crucible 1 is an iridium crucible, the shape of the crucible is a cylinder with a spherical crown shape at the bottom, the bottom is arranged into the spherical crown shape, and the crucible is matched with an interface for crystal growth in the process of crystal growth, so that the temperature uniformity of molten liquid is more favorably ensured, and favorable conditions are further provided for the uniform growth of crystals.
The heating system comprises a heater; the heater comprises two parts, one part is a side wall annular heater 21 matched with a crucible side plate, and the other part is a bottom sheet heater 22 matched with the bottom of the crucible; the two parts of heaters are adopted, so that the temperature of different parts can be flexibly controlled, the problem that the central area at the bottom of the crucible is uniformly heated is solved, and favorable temperature regulation conditions are provided for uniform growth of crystals.
The driving system comprises a seed shaft 3, the seed shaft is connected with a rotary lifting device 7, and the rotary lifting device comprises a worm gear speed reducer, a synchronous belt, a precise planetary speed reducer and a servo motor; and a precise transmission mode is adopted, so that precise rotation and lifting are realized, and precise equipment conditions are provided for the Czochralski method growth of the crystal. The seed shaft rotary seal adopts magnetic fluid seal, the vertical motion seal adopts stainless steel corrugated pipe, the precision seal can effectively keep the vacuum environment.
The heat preservation system comprises a heat preservation layer, the heat preservation layer is arranged between the furnace wall and the heater, and the heat preservation layer comprises a zirconium oxide heat preservation layer 51, a molybdenum sheet heat shield 52 and a nano tungsten film reflection layer 53; this heat preservation system still includes argon gas supply device, and this argon gas supply device is equipped with temperature sensor 61 and gas flowmeter 62 including setting up the air supply pipe on the oven, the gaseous storage tank 6 of argon gas that is connected with the air supply pipe on the air supply pipe, be convenient for to the argon gas control flow and the problem of infeeding, for the step of cooling down provides the condition in the stove, the time of reduction cooling that can be great provides production efficiency.
The vacuum system adopts the direct-connection rotary vane vacuum pump 8 and the high-vacuum gate valve, so that the vacuum degree of the equipment is improved, and the quality of crystals is improved.
Example 2 Czochralski method for producing sapphire single crystal
The method comprises the steps of raw material preparation, vacuumizing, heating and melting, crystal growth and cooling, and specifically comprises the following steps:
raw material preparation: the method comprises the following steps of (1) adopting a mixture of high-purity alumina powder with the purity of 5 grade and crushed crystals, wherein the weight ratio of the high-purity alumina powder to the crushed crystals is 5:1, the crushed crystals need to be cleaned for multiple times by ultrasonic waves, and the high-purity alumina powder needs to be pressed into cylindrical blocks; the gas contained in the raw materials can be discharged as far as possible after pressing, the quality of the raw materials is improved, in addition, the crushed crystals are placed at the bottom, the quality of the raw materials is good, and the quality improvement during bottom melt crystallization is facilitated.
Vacuumizing step, namely vacuumizing the furnace to a vacuum degree of 3 × 10-4Pa。
Heating and melting: heating is started, the temperature is increased to 2300-2400 ℃, and the temperature is kept for 2.5 hours to ensure that the raw materials are completely melted.
A crystal growth step: lowering the seed crystal shaft to start seeding, controlling the temperature at 1900-2000 ℃, necking, shouldering, growing the crystal to a proper size, and then annealing; the rotating speed of the seed crystal shaft is 10 r/min.
And (3) cooling: argon is introduced into the furnace through the gas supply pipe, the temperature of the crystal is reduced, and the temperature reduction time lasts for 2 hours. Through letting in the argon gas cooling, properly accelerated the cooling speed, shortened the cooling time, effectively improved production efficiency.
Example 3 Czochralski method for producing sapphire single crystal
The method comprises the steps of raw material preparation, vacuumizing, heating and melting, crystal growth and cooling, and specifically comprises the following steps:
raw material preparation: the method comprises the following steps of (1) adopting a mixture of high-purity alumina powder with the purity of 5 grade and crushed crystals, wherein the weight ratio of the high-purity alumina powder to the crushed crystals is 5:1, the crushed crystals need to be cleaned for multiple times by ultrasonic waves, and the high-purity alumina powder needs to be pressed into cylindrical blocks; the gas contained in the raw materials can be discharged as far as possible after pressing, the quality of the raw materials is improved, in addition, the crushed crystals are placed at the bottom, the quality of the raw materials is good, and the quality improvement during bottom melt crystallization is facilitated.
Vacuumizing step, namely vacuumizing the furnace to 5 × 10 vacuum degree-4Pa。
Heating and melting: heating is started, the temperature is raised to 2500 ℃ and 2500 ℃, and the temperature is kept for 1.5 hours to ensure that the raw materials are completely melted.
A crystal growth step: descending a seed crystal shaft to start seeding, controlling the temperature to be 2200-; the rotating speed of the seed crystal shaft is 8 r/min.
And (3) cooling: argon is introduced into the furnace through the gas supply pipe, the temperature of the crystal is reduced, and the temperature reduction time lasts for 2 hours. Through letting in the argon gas cooling, properly accelerated the cooling speed, shortened the cooling time, effectively improved production efficiency.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A pulling method preparation device of sapphire single crystal comprises a crucible, a heating system, a driving system, a heat preservation system and a vacuum system;
the heating system comprises a heater;
the driving system comprises a seed shaft, and the seed shaft is connected with the rotary lifting device;
the heat preservation system comprises a heat preservation layer, the heat preservation layer is arranged between the furnace wall and the heater, and the heat preservation layer comprises a zirconium oxide heat insulation layer, a molybdenum sheet heat insulation screen and a nano tungsten film reflection layer; the heat preservation system also comprises an argon supply device, wherein the argon supply device comprises an air supply pipe arranged on the furnace wall and an argon gas storage tank connected with the air supply pipe.
2. The apparatus of claim 1, wherein the heater comprises two parts, one part being a side wall ring heater fitted to a side plate of the crucible, and the other part being a bottom plate heater fitted to a bottom of the crucible.
3. The apparatus of claim 1, wherein the crucible is an iridium crucible, and the crucible is in the shape of a cylinder with a spherical crown at the bottom.
4. The device of claim 1, wherein the rotary lifting device comprises a worm gear reducer, a synchronous belt, a precision planetary reducer and a servo motor.
5. The device according to claim 1, wherein the seed shaft rotary seal is a magnetic fluid seal, and the vertical motion seal is a stainless steel bellows.
6. The apparatus as claimed in claim 1, wherein a temperature sensor and a gas flow meter are provided on the gas supply tube.
7. The apparatus of claim 1, wherein the vacuum system employs a direct rotary vane vacuum pump and a high vacuum gate valve.
8. The method for producing a sapphire single crystal by the Czochralski method according to claim 1 to claim 7, comprising a raw material preparation step, a vacuum-pumping step, a heating and melting step, a crystal growth step, and a cooling step, wherein the method comprises the following steps:
raw material preparation: the method comprises the following steps of (1) adopting a mixture of high-purity alumina powder with the purity of 5 grade and crushed crystals, wherein the weight ratio of the high-purity alumina powder to the crushed crystals is 5:1, the crushed crystals need to be cleaned for multiple times by ultrasonic waves, and the high-purity alumina powder needs to be pressed into cylindrical blocks; the gas contained in the raw materials can be discharged as far as possible after pressing, the quality of the raw materials is improved, in addition, the crushed crystals are placed at the bottom, the quality of the raw materials is good, and the quality improvement during bottom melt crystallization is facilitated.
Vacuumizing step, namely vacuumizing the furnace to 1-5 × 10 vacuum degree-4Pa。
Heating and melting: heating is started, the temperature is raised to 2500 ℃ for 1-3 hours, and the raw materials are ensured to be completely melted.
A crystal growth step: lowering the seed shaft to start seeding, controlling the temperature to be 1800-plus 2300 ℃, necking, shouldering, growing the crystal to a proper size, and then annealing; the rotating speed of the seed crystal shaft is 3-15 r/min.
And (3) cooling: argon is introduced into the furnace through an air supply pipe to cool the crystal, and the cooling time lasts for 1.5 to 3 hours. Through letting in the argon gas cooling, properly accelerated the cooling speed, shortened the cooling time, effectively improved production efficiency.
9. The method of claim 8, wherein the heating and melting step: the temperature is raised to 2400 ℃ and 2500 ℃, and the temperature is maintained for 1.5 hours.
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| CN112458533A (en) * | 2020-10-30 | 2021-03-09 | 山东新升光电科技有限责任公司 | Sapphire single crystal growth system and method |
| CN112779535A (en) * | 2020-12-07 | 2021-05-11 | 上海航天设备制造总厂有限公司 | Laser ablation resistant coating for substrate surface and preparation method thereof |
| CN114739171A (en) * | 2022-05-05 | 2022-07-12 | 湖南江滨机器（集团）有限责任公司 | Composite material preparation device and preparation method |
| CN116949563A (en) * | 2023-09-19 | 2023-10-27 | 内蒙古晶环电子材料有限公司 | Thermal insulation structure and sapphire crystal growth furnace |
| CN116949557A (en) * | 2023-09-18 | 2023-10-27 | 内蒙古晶环电子材料有限公司 | Thermal insulation structure and sapphire crystal growth furnace |
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| CN116949563A (en) * | 2023-09-19 | 2023-10-27 | 内蒙古晶环电子材料有限公司 | Thermal insulation structure and sapphire crystal growth furnace |
| CN116949563B (en) * | 2023-09-19 | 2024-02-13 | 内蒙古晶环电子材料有限公司 | Thermal insulation structure and sapphire crystal growth furnace |
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Application publication date: 20200901 |