CN220012886U - Growth device for preparing large-size gallium oxide crystals by cold crucible pulling method - Google Patents

Growth device for preparing large-size gallium oxide crystals by cold crucible pulling method Download PDF

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CN220012886U
CN220012886U CN202321613577.0U CN202321613577U CN220012886U CN 220012886 U CN220012886 U CN 220012886U CN 202321613577 U CN202321613577 U CN 202321613577U CN 220012886 U CN220012886 U CN 220012886U
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gallium oxide
crucible
water
pulling method
ganguo
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唐皇哉
承刚
胡树金
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Beijing Houpusi Technology Co ltd
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Beijing Houpusi Technology Co ltd
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Abstract

The utility model discloses a growth device for preparing large-size gallium oxide crystals by a cold crucible pulling method, which comprises a crucible wall of a water-cooled crucible, a high-frequency induction coil, a base of the water-cooled crucible and a fireproof base, wherein the crucible wall of the water-cooled crucible is formed by a plurality of water-cooled pipes which are arranged at equal intervals around the axis of the base of the water-cooled crucible, the high-frequency induction coil is arranged around the crucible wall of the water-cooled crucible and surrounds the crucible wall of the water-cooled crucible, the base of the water-cooled crucible is arranged on the fireproof base, the growth device for preparing large-size gallium oxide crystals by the cold crucible pulling method further comprises a gallium oxide seed chuck, and the lower end of the gallium oxide seed chuck is positioned in the center of a thermal field formed by the high-frequency induction coil. The utility model works in an oxygen-enriched environment without using an iridium crucible.

Description

Growth device for preparing large-size gallium oxide crystals by cold crucible pulling method
Technical Field
The utility model relates to the field of crystal production, in particular to a growth device for preparing large-size gallium oxide crystals by a cold crucible pulling method.
Background
Gallium oxide (beta-Ga) 2 O 3 ) The crystal is an ultra-wide band-gap semiconductor material, and has the advantages of large band gap (eg=4.8-5.2 eV), short absorption cut-off edge (260 nm), high breakdown electric field strength (8 MV/cm), stable chemical performance, suitability for melt growth and the like. Thus, beta-Ga 2 O 3 The material is one of the preferable materials of high-voltage, high-power devices and deep ultraviolet optoelectronic devices, and can be applied to Field Effect Transistors (FETs), solar blind ultraviolet detectors, schottky diodes, gas sensors and the like.
Gallium oxide has five crystal structures of alpha, beta, epsilon, delta and gamma, wherein the beta-type structure is the most stable, and other phases are uniformly converted into beta phase at the temperature higher than 850 ℃. beta-Ga 2 O 3 To uniformly melt the compound, the beta-Ga can be obtained by melt growth 2 O 3 Bulk crystals. The difficulty in growing gallium oxide crystals is: g a in a growth atmosphere which is anoxic at high temperature 2 O 3 The decomposition reaction can occur to generate products such as low-valence gallium oxide, simple substance gallium and the like; the gallium and the iridium can form alloy, so that noble metal loss is caused; and beta-Ga 2 O 3 It is easy to produce contracture crystal, mosaic structure, cleavage and cracking, screw dislocation and other defects. Thus, large-size, high-quality beta-Ga is obtained 2 O 3 Crystals are extremely difficult.
The pulling method and the guided mode method are the successful methods for growing large-size gallium oxide crystals at present. The Czochralski method adopted by Germany Laibunitz crystal growth research institute successfully grows 2 inches beta-Ga 2 O 3 Crystals, tamura, japan Takara and light wave Co., ltd, were first commercialized with 2 inch beta-Ga using the guided-mode technique 2 O 3 A substrate and a 6 inch crystal ingot was grown. However, these two growth methods have the disadvantages: growth of beta-Ga by pulling method and guided mode method 2 O 3 The crystal adopts an iridium crucible, on one hand, gallium can cause serious corrosion to the inner wall of the iridium crucible, and the iridium loss is relatively highLarge; to suppress Ga during growth 2 O 3 Is decomposed and volatilized, and the high pressure CO of 7bar is adopted by the research institute of the crystal growth of the Laibunitz 2 The atmosphere grows crystals, which puts more stringent demands on the pressure resistance of the device. On the other hand, the global yield of noble metal iridium is 7 tons/year, 10 kg of iridium is needed for preparing an iridium crucible with 2 inches of gallium oxide, the yield of iridium cannot meet the production requirement of the future global electronics industry on gallium oxide, the price of iridium rises by more than 10 times in the past 5 years, iridium accounts for more than half of the preparation cost of gallium oxide, and the commercial application of gallium oxide is greatly limited by the high cost of gallium oxide. More importantly, the iridium crucible can not work gallium oxide crystals in an oxygen-enriched environment, and crystal defects caused by an iridium crucible method can not be overcome.
Disclosure of Invention
The utility model provides a growth device for preparing large-size gallium oxide crystals by a cold crucible pulling method.
The technical proposal is as follows: the utility model provides a cold crucible pulling method preparation jumbo size gallium oxide crystal's growth load, leng Ganguo pulling method preparation jumbo size gallium oxide crystal's growth device includes water-cooled crucible's crucible wall, high frequency induction coil, water-cooled crucible's base and fire-resistant base, water-cooled crucible's crucible wall is surrounded by a plurality of water-cooled tubes equidistance about water-cooled crucible's base axis, high frequency induction coil sets up around water-cooled crucible's crucible wall, with water-cooled crucible's crucible wall encirclement in, water-cooled crucible's base is placed on fire-resistant base, cold crucible pulling method preparation jumbo size gallium oxide crystal's growth device still includes gallium oxide seed chuck, the lower extreme of gallium oxide seed chuck is located the thermal field center that high frequency induction coil formed.
In one or more specific embodiments of the present utility model, the growth apparatus for preparing large-size gallium oxide crystals by the Leng Ganguo pulling method further includes a plurality of support columns and a support frame, the plurality of support columns are distributed outside the high-frequency induction coil, the support frame is connected to the upper ends of the plurality of support columns, the gallium oxide seed chuck passes through the support frame and is mounted on the support frame, and the upper end of the gallium oxide seed chuck is connected to the gallium oxide seed transmission shaft.
In one or more embodiments of the present utility model, the growth apparatus for preparing large-sized gallium oxide crystals by the Leng Ganguo Czochralski method is further provided with a heat insulation plate, which is disposed on top of the water-cooled crucible.
In one or more embodiments of the present utility model, the Leng Ganguo crystal growth apparatus for preparing large-sized gallium oxide crystals is further provided with an insulating layer.
In one or more embodiments of the present utility model, the growth apparatus for preparing large-size gallium oxide crystals by the Leng Ganguo Czochralski method further comprises a plurality of annular concave reflecting screens.
In one or more embodiments of the utility model, the plurality of annular concave reflective screens are coupled to a reflective screen drive shaft.
In one or more embodiments of the utility model, the annular concave reflective screen is focused at a maximum diameter position for crystal growth.
In one or more embodiments of the utility model, the water-cooled tube has a diameter of 2-40mm.
In one or more embodiments of the utility model, the water-cooled tube has a height of 20-200mm.
Drawings
FIG. 1 is a schematic diagram of a growth apparatus for preparing large-size gallium oxide crystals by a cold crucible pulling method according to the present utility model;
FIG. 2 is a schematic view of the support frame of FIG. 1;
FIG. 3 is a schematic diagram showing a structure of a growth apparatus for preparing large-size gallium oxide crystals by another cold crucible pulling method according to the present utility model;
FIG. 4 is a temperature profile formed by the growth apparatus of FIG. 1;
FIG. 5 is a temperature profile formed by the growth apparatus of FIG. 3;
in the figure, 1, the crucible wall of a water-cooled crucible, 2, a high-frequency induction coil, 3, the base of the water-cooled crucible, 4, a fireproof base, 5, a gallium oxide seed chuck, 6, a gallium oxide seed transmission shaft, 7, a support column, 8, a support frame, 9, an annular concave reflecting screen, 10, a heat insulation plate, 11, a heat insulation layer, 12 and a reflecting screen transmission shaft.
Detailed Description
The utility model will be further described with reference to the accompanying drawings.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a growth apparatus for preparing large-size gallium oxide crystals by a cold crucible pulling method according to the present utility model, and fig. 2 is a schematic structural diagram of a support frame.
The utility model provides a cold crucible pulling method prepares growing device of jumbo size gallium oxide crystal, including water-cooling crucible's crucible wall 1, high frequency induction coil 2, water-cooling crucible's base 3 and fire-resistant base 4, water-cooling crucible's crucible wall 1 is surrounded by a plurality of water-cooling pipes around water-cooling crucible's base 3 axis equidistance, high frequency induction coil 2 sets up around water-cooling crucible's crucible wall 1, with water-cooling crucible's crucible wall 1 encirclement in, water-cooling crucible's base 3 is placed on fire-resistant base 4, cold crucible pulling method prepares growing device of jumbo size gallium oxide crystal still includes gallium oxide seed chuck 5, the lower extreme of gallium oxide seed chuck 5 is located the thermal field center that high frequency induction coil 2 formed.
In one or more specific embodiments of the present utility model, the growth apparatus for preparing large-sized gallium oxide crystals by the cold crucible pulling method further includes a plurality of support columns 7 and a support frame 8, the plurality of support columns 7 are distributed outside the high-frequency induction coil 2, the support frame 8 is connected to the upper ends of the plurality of support columns 7, the gallium oxide seed chuck 5 passes through the support frame 8 and is mounted on the support frame 8, the upper end of the gallium oxide seed chuck 5 is connected to the gallium oxide seed transmission shaft 6, and the other end of the gallium oxide seed transmission shaft 6 is connected to an existing power transmission mechanism (not shown in the figure).
In one or more embodiments of the present utility model, the top of the water-cooled crucible is provided with a heat shield 10, and it will be appreciated by those skilled in the art that the heat shield 10 is provided for the purpose of heat insulation and not for the purpose of preventing the flow of gas.
In one or more embodiments of the present utility model, the water-cooled crucible is provided with a heat insulating layer 11, and it should be appreciated by those skilled in the art that the heat insulating layer 11 is provided for heat insulation, not for preventing gas flow.
Since the crucible wall 1 of the water-cooled crucible is formed by a plurality of water-cooled pipes which are equidistantly arranged around the axis of the base 3 of the water-cooled crucible, gaps are reserved among the water-cooled pipes, and the upper part of the water-cooled pipes is also in an open structure, thus when the water-cooled pipes are in a spherical Ga shape 2 O 3 When the raw material grows gallium oxide crystals in a thermal field, the raw material is equivalent to directly contacting oxygen in air, high-temperature oxygen deficiency does not exist, and an expensive iridium crucible is not needed, so that the production cost is reduced. More importantly, in the whole work, the growing device for preparing the large-size gallium oxide crystals by the cold crucible pulling method greatly reduces impurities in the generated crystals because the generated melt and crystals are not contacted with other metals and the like except gallium oxide seed crystals.
The schematic structural diagram of the growth apparatus for preparing large-size gallium oxide crystals by the cold crucible pulling method shown in fig. 1 solves the problem of oxygen deficiency and expensive iridium crucible, but the growth apparatus shown in fig. 1 is easy to form a temperature distribution with high middle and low periphery when the growth apparatus shown in fig. 1 works because the crucible wall 1 of the water-cooled crucible is cooled by circulating water, and the pulling method is used for growing crystals, and needs a temperature distribution with low middle and high periphery temperature.
Referring to fig. 3, fig. 3 is a schematic structural diagram of a growth apparatus for preparing large-size gallium oxide crystals by using a cold crucible pulling method according to another embodiment of the present utility model.
The utility model provides a cold crucible pulling method prepares growing device of jumbo size gallium oxide crystal, including the crucible wall 1 of water-cooling crucible, high frequency induction coil 2, the base 3 and the fire-resistant base 4 of water-cooling crucible, the crucible wall 1 of water-cooling crucible is surrounded by a plurality of water-cooling tubes around the equidistant range of the base 3 axis of water-cooling crucible, high frequency induction coil 2 sets up around the crucible wall 1 of water-cooling crucible, surround the crucible wall 1 of water-cooling crucible inside, the base 3 of water-cooling crucible is placed on fire-resistant base 4, the growing device of jumbo size gallium oxide crystal still includes gallium oxide seed chuck 5, the lower extreme of gallium oxide seed chuck 5 is located the thermal field center that high frequency induction coil 2 formed, the growing device of jumbo size gallium oxide crystal is still included a plurality of annular concave reflection screens 9, annular concave reflection screens 9 collect the heat reflection all around, form the temperature distribution that satisfies the long crystal.
In one or more embodiments of the utility model, the annular concave reflective screen is coupled to a reflective screen drive shaft 12, and the other end of the reflective screen drive shaft 12 is coupled to an existing power transmission mechanism (not shown).
In one or more specific embodiments of the present utility model, the growth apparatus for preparing large-sized gallium oxide crystals by the cold crucible pulling method further includes a plurality of support columns 7 and a support frame 8, the plurality of support columns 7 are distributed outside the high-frequency induction coil 2, the support frame 8 is connected to the upper ends of the plurality of support columns 7, the gallium oxide seed chuck 5 passes through the support frame 8 and is mounted on the support frame 8, the upper end of the gallium oxide seed chuck 5 is connected to the gallium oxide seed transmission shaft 6, and the other end of the gallium oxide seed transmission shaft 6 is connected to an existing power transmission mechanism (not shown in the figure).
In one or more embodiments of the present utility model, the top of the water-cooled crucible is provided with a heat shield 10, and it will be appreciated by those skilled in the art that the heat shield 10 is provided for the purpose of heat insulation and not for the purpose of preventing the flow of gas.
In one or more embodiments of the present utility model, the water-cooled crucible is provided with a heat insulating layer 11, and it should be appreciated by those skilled in the art that the heat insulating layer 11 is provided for heat insulation, not for preventing gas flow.
Experiment 1 thermal field distribution test
The temperature distribution was measured for the growth apparatuses of fig. 1 and 3, respectively, and the growth apparatuses of fig. 1 and 3 were identical in structure and size and shape, except for the annular concave reflecting screen 9 of fig. 3, and the methods and conditions used for the measurement were not different.
The growth apparatus of fig. 1 forms a temperature profile as shown in fig. 4, and the growth apparatus of fig. 3 forms a temperature profile as shown in fig. 5.
The following examples 2-6 employ the growth apparatus of FIG. 3, but the components of FIG. 3 employed in the different examples are different.
Example 2
A growth method for preparing large-size gallium oxide crystals by a cold crucible pulling method comprises the following steps:
placing beta-Ga on a base 3 of a water-cooled crucible 2 O 3 Seed crystal, stacking high purity Ga 2 O 3 The spherical raw material forms a raw material pile.
The heating power supply of the induction coil is started.
And (5) material melting.
And (5) seeding. The seed crystal slowly enters a position 10-20mm above the melt, the weight starts to drop, and the seed crystal melts and cannot enter the next step.
In example 2, the device of fig. 3 has the heat shield 10, heat insulating layer 11 and annular concave reflective screen 9 and reflective screen drive shaft 12 not activated.
The results are shown in Table 1 below.
Example 3
A growth method for preparing large-size gallium oxide crystals by a cold crucible pulling method comprises the following steps:
placing beta-Ga on a base 3 of a water-cooled crucible 2 O 3 Seed crystal, stacking high purity Ga 2 O 3 The spherical raw material forms a raw material pile.
The heating power supply of the induction coil is started.
And (5) material melting.
And (5) seeding. The seed crystal slowly rotates into the melt, the weight is unchanged, and the seed crystal does not develop. The next step cannot be entered.
In example 3, the insulation 11 was removed from the device of fig. 3 and the annular concave reflective screen 9 and reflective screen drive shaft 12 were not activated.
Example 4
A growth method for preparing large-size gallium oxide crystals by a cold crucible pulling method comprises the following steps:
placing beta-Ga on a base 3 of a water-cooled crucible 2 O 3 Seed crystal, build-up Ga 2 O 3 The spherical raw material forms a raw material pile. The seed rod is connected with water cooling, and the water temperature of the connected water cooling is room temperature.
The heating power supply of the induction coil is started.
And (5) material melting.
And (5) seeding. The seed crystal slowly enters the melt, the seed crystal rotates to slowly enter the melt, the diameter of a seeding neck is smaller than 15mm, and the crystal stops growing and cannot shoulder.
And growing in equal diameter. The isodiametric growth rate is not more than 10g per hour.
In example 3, the insulation 11 was removed from the device of fig. 3 and the annular concave reflective screen 9 and reflective screen drive shaft 12 were not activated.
The results are shown in Table 1 below.
Example 5
A growth method for preparing large-size gallium oxide crystals by a cold crucible pulling method, which adopts a growth device of fig. 2, comprising the following steps:
placing beta-Ga on a base 3 of a water-cooled crucible 2 O 3 Seed crystal, stacking high purity Ga 2 O 3 The spherical raw material forms a raw material pile. The seed rod is connected with water cooling, and the water temperature is room temperature.
The heating power supply of the induction coil is started.
And (5) material melting.
And (5) seeding. The seed crystal slowly rotates into the melt, the diameter of the seeding neck is smaller than 20mm, and the length is larger than 50mm.
And (5) putting the shoulder. Can be scaled up to 25mm but not continue to grow.
And growing in equal diameter. The isodiametric growth rate is not more than 20g per hour.
In example 3, the annular concave reflective screen 9 and reflective screen drive shaft 12 are not enabled in the device of fig. 3.
The results are shown in Table 1 below.
Example 6 a growth method for preparing large-size gallium oxide crystals by a cold crucible pulling method, which adopts negative feedback power control, comprises the following steps:
placing beta-Ga on a base 3 of a water-cooled crucible 2 O 3 Seed crystal, stacking high purity Ga 2 O 3 The spherical raw material forms a raw material pile. The seed rod is connected with water cooling, and the water temperature is room temperature.
The heating power supply of the induction coil is started.
And (5) material melting.
And (5) seeding. The seed crystal slowly rotates into the melt, the diameter of the seeding neck is smaller than 20mm, and the length is larger than 50mm.
And (5) putting the shoulder. The crystal growth rate is slowly increased from 10g to 100g, and the focusing position of the reflecting mirror is the maximum diameter position of the crystal growth. Shoulder placement is stopped at this position.
And growing in equal diameter. The isodiametric growth rate is not greater than 100g per hour.
The results are shown in Table 1 below.
TABLE 1
The above description is only of the preferred embodiments of the present utility model and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.

Claims (9)

1. The utility model provides a cold crucible pulling method prepares growing device of jumbo size gallium oxide crystal, a serial communication port, leng Ganguo pulling method prepares growing device of jumbo size gallium oxide crystal includes crucible wall (1) of water-cooling crucible, high frequency induction coil (2), base (3) and fire-resistant base (4) of water-cooling crucible, crucible wall (1) of water-cooling crucible are surrounded by a plurality of water-cooling tubes around the equidistant range of base (3) axis of water-cooling crucible, high frequency induction coil (2) set up around crucible wall (1) of water-cooling crucible, with crucible wall (1) of water-cooling crucible encircleing inside, base (3) of water-cooling crucible are placed on fire-resistant base (4), growing device of jumbo size gallium oxide crystal is still including gallium oxide seed chuck (5) of cold crucible pulling method preparation, the lower extreme of gallium oxide seed chuck (5) is located the thermal field center that high frequency induction coil (2) formed.
2. The device for preparing large-size gallium oxide crystals by using the Leng Ganguo pulling method according to claim 1, wherein the device for preparing large-size gallium oxide crystals by using the Leng Ganguo pulling method further comprises a plurality of support columns (7) and a support frame (8), the support columns (7) are distributed outside the high-frequency induction coil (2), the support frame (8) is connected to the upper ends of the support columns (7), the gallium oxide seed chuck (5) passes through the support frame (8) and is mounted on the support frame (8), and the upper end of the gallium oxide seed chuck (5) is connected with the gallium oxide seed transmission shaft (6).
3. The device for growing large-size gallium oxide crystals by the Leng Ganguo pulling method according to claim 1, wherein the device for growing large-size gallium oxide crystals by the Leng Ganguo pulling method is further provided with a heat insulating plate (10), and the heat insulating plate (10) is arranged on the top of the water-cooled crucible.
4. The apparatus for growing large-size gallium oxide crystals by the Leng Ganguo pulling method according to claim 1, wherein the apparatus for growing large-size gallium oxide crystals by the Leng Ganguo pulling method is further provided with an insulating layer (11).
5. A growth apparatus for producing large-size gallium oxide crystals according to the Leng Ganguo pulling method as defined in any one of claims 1 to 4, wherein the growth apparatus for producing large-size gallium oxide crystals according to the Leng Ganguo pulling method further comprises a plurality of annular concave reflecting screens (9).
6. The Leng Ganguo pulling method as claimed in claim 5, wherein the plurality of annular concave reflecting screens (9) are connected with a reflecting screen transmission shaft (12).
7. A growth apparatus for producing large-size gallium oxide crystals according to the Leng Ganguo pulling method of claim 5, wherein the positions at which the plurality of annular concave reflecting screens (9) are focused are positions of maximum diameter of crystal growth.
8. A growth apparatus for producing large-size gallium oxide crystals according to the Leng Ganguo pulling method of claim 1, wherein the water-cooled tube has a diameter of 2 to 40mm.
9. A growth apparatus for producing large-size gallium oxide crystals according to the Leng Ganguo pulling method of claim 1, wherein the water-cooled tube has a height of 20 to 200mm.
CN202321613577.0U 2023-06-25 2023-06-25 Growth device for preparing large-size gallium oxide crystals by cold crucible pulling method Active CN220012886U (en)

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