CN110777430A - Method for growing large-size silicon carbide single crystal - Google Patents

Method for growing large-size silicon carbide single crystal Download PDF

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Publication number
CN110777430A
CN110777430A CN201910969170.3A CN201910969170A CN110777430A CN 110777430 A CN110777430 A CN 110777430A CN 201910969170 A CN201910969170 A CN 201910969170A CN 110777430 A CN110777430 A CN 110777430A
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China
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induction coil
crystal growth
coil
growing
silicon carbide
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CN201910969170.3A
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方帅
高超
刘圆圆
周敏
张虎
姜岩鹏
黄治成
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Jining Tianyue New Material Technology Co Ltd
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Jining Tianyue New Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/36Carbides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials

Abstract

The invention provides a method for growing large-size silicon carbide single crystals, which comprises the step of heating a crystal growth chamber by using an induction coil, wherein in the process of growing the single crystals, the induction coil is controlled to rotate by arranging a rotating mechanism, and the uniformity of a temperature field of the crystal growth chamber is controlled by reducing the turn pitch of the induction coil and increasing the ratio of the height of the coil to the diameter of the coil. The invention improves the uniformity of the magnetic field generated by the induction coil by optimizing the arrangement of the induction coil, can ensure that the temperature around the crystal growth chamber is as uniform as possible, effectively reduces the phenomenon of uneven thickness around the crystal, effectively reduces the collapse of the charge level in a certain direction, ensures that the erosion rates of the crystal growth chamber in all directions are the same, increases the use times of consumables and the stability of crystal growth, reduces the uneven heat productivity of the crucible and improves the uniformity of the grown crystal.

Description

Method for growing large-size silicon carbide single crystal
Technical Field
The invention relates to a method for growing large-size silicon carbide single crystals, belonging to the technical field of crystal growth.
Background
Silicon carbide (SiC) single crystal has excellent semiconductor physical properties such as high thermal conductivity, high breakdown voltage, extremely high carrier mobility, high chemical stability and the like, can be manufactured into high-frequency and high-power electronic devices and optoelectronic devices which work under the conditions of high temperature and strong radiation, has great application value in the fields of national defense, high technology, industrial production, power supply and power transformation, and is regarded as a third-generation wide-bandgap semiconductor material with great development prospect.
Despite the great advances made in recent years by Physical Vapor Transport (PVT) growth of silicon carbide crystals, the stability of the grown crystals needs to be further investigated. For example, the reduction of the use times and the fluctuation of the crystal growth stability caused by the uneven heating of the crucible, and the enlargement of the size of the silicon carbide crystal can greatly reduce the cost of power devices and electronic and electric devices.
At present, in the method for growing crystal by PVT, the medium frequency induction coil heating is widely used, the induction coil is in a spiral shape, and the spiral induction coil heating has many limitations, such as: 1. a large gap exists between each turn of the coil; 2. the height of the coil is not much higher than its diameter; this causes the magnetic field generated by the induction coil to be offset from the central axis of the coil and to be non-uniform. Such non-uniformity of the magnetic field causes non-uniform variation of magnetic flux in each small region of the crucible, resulting in non-uniform heating of the crucible, most directly resulting in non-uniform thickness of the grown crystal, non-uniform loss of the crucible and the heat preservation to affect the subsequent use effect, and non-uniform evaporation of the growth raw material to collapse the charge level, which all cause instability of the grown crystal. Particularly, for the growth of large-size silicon carbide (6-8 inches) crystals, the stability of the grown crystals is more required. Any one point of fluctuation may cause crystal defects.
In the prior art, CN105256371B discloses a device for improving the temperature field uniformity of a crystal growth furnace by a physical vapor transport method, which comprises a crystal growth furnace, wherein the crystal growth furnace comprises a radio frequency power supply, a contact electrode, a coil, a heat insulation layer and a graphite single crystal growth device, the coil is uniformly arranged outside the heat insulation layer in a horizontal axis symmetry manner, and the coil can rotate around the heat insulation layer through a rotating device; the number of the coils is single, and the single coil is wound on the outer side of the heat insulation layer in a bow-shaped mode; or the number of the coils is two, and the two coils are wound in a bow-shaped mode and are symmetrically arranged on the outer side of the heat preservation layer. The coil is wound in a bow-shaped mode, and the bent part of the coil exists, so that the temperature of the bent part is concentrated, a magnetic field generated by the induction coil can deviate from the central axis of the coil, the uniformity of the temperature can be influenced due to the fact that the magnetic field is uneven, and the stability of crystal growth is influenced.
The temperature field provided in the motion process is a dynamic change process, and the dynamic change process also has a problem of controlling the whole process, so that the PVT method can obtain better single crystals. Because the crystallization process suffers from the problems of temperature field uniformity, temperature control of the whole field, pressure control and the like, in the prior art, no specific and feasible process parameters are provided for achieving the purpose of obtaining the large-size silicon carbide single crystal meeting the requirements.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for growing a large-sized silicon carbide single crystal, which reduces the crystal growth stress by improving the distribution uniformity of the temperature field in the crystal growth chamber, thereby improving the crystal growth stability.
The technical scheme adopted by the application is as follows:
a method for growing large-size silicon carbide single crystal comprises the step of heating a crystal growing chamber by using an induction coil, wherein in the process of growing the single crystal, the induction coil is controlled to rotate by arranging a rotating mechanism, and the distribution uniformity of a temperature field of the crystal growing chamber is improved by reducing the turn pitch of the induction coil and increasing the ratio of the height of the coil to the diameter of the coil.
Furthermore, the turn pitch of the induction coil is 0-6 mm, and the ratio of the height of the coil to the diameter of the coil is 1.2-3. Preferably, the turn pitch of the induction coil is 4mm, and the ratio of the height of the coil to the diameter of the coil is 2; the magnetic field generated by the induction coil is parallel to the central axis of the coil by further reducing the turn-to-turn distance of the coil and increasing the ratio of the height of the coil to the diameter of the coil, and the uniformity of the magnetic field ensures that the heat productivity of each small area in the crystal growth chamber is uniform.
Furthermore, a first quartz tube is arranged on the inner side of the induction coil, the induction coil rotates around the first quartz tube, and a second quartz tube is arranged on the outer side of the induction coil; preferably, circulating cooling water flows through both the first quartz tube and the second quartz tube. The first quartz tube and the second quartz tube are internally and uniformly circulated with circulating cooling water to cool the induction coil, so that the service life and the heating stability of the coil are improved. In the crystal growth process, the circulating water is directly communicated.
Further, the axial section of the induction coil is olive-shaped or dumbbell-shaped; preferably, the difference between the maximum diameter of the coil and the minimum diameter thereof is not greater than the horizontal distance between the first and second quartz tubes.
Further, the magnitude of the power supply current of the induction coil is controlled by a current control component; preferably, the current control assembly comprises a sliding contact, a contact ring and a medium-frequency power supply, and two ends of the induction coil are respectively connected with the medium-frequency power supply through the sliding contact and the contact ring; preferably, the current control assembly is controlled by a control system.
Further, the rotating mechanism comprises a motor for controlling the induction coil to rotate; preferably, two ends of the induction coil are inserted on the insulating disc, and the insulating disc is connected with a rotating shaft of the motor; preferably, the motor is controlled by a control system.
Further, the induction coil is spirally wound outside the crystal growth chamber; preferably, the crystal growth chamber is a graphite crucible; preferably, the crystal growth chamber is located substantially in the center of the induction coil; preferably, the temperature of the crystal growth chamber is measured by a temperature measuring device, which is connected to the control system.
Further, before crystal growth, under the rotation condition of the induction coil, the current of the induction coil is increased, and the crystal growth chamber is heated to the temperature required by crystal growth; when crystal growth occurs, the rotating speed of the induction coil is increased, and the current of the induction coil is kept stable; after crystal growth is finished, the current in the induction coil is slowly reduced, meanwhile, the rotating speed of the induction coil is increased, and the temperature of the crystal growth chamber is reduced to room temperature.
Further, before crystal growth, the rotating speed of the induction coil is 3-30r/min, the temperature of the crystal growth chamber is controlled to 1800-2000k, and the pressure is controlled to 8000-12000 pa; during crystal growth, the rotating speed of the induction coil is 10-70r/min, the temperature of the crystal growth chamber is controlled to 2200-; after crystal growth is finished, the rotating speed of the induction coil is 3-30 r/min; preferably, the cooling rate is 6-10 k/h.
The invention also provides a large-size silicon carbide single crystal prepared by the method.
The invention has the beneficial effects that:
(1) the invention improves the uniformity of the magnetic field generated by the induction coil by optimizing the arrangement of the induction coil, reducing the turn pitch of the coil and increasing the ratio of the height of the coil to the diameter of the coil, can ensure that the temperature around the crystal growth chamber is as uniform as possible, effectively reduces the phenomenon of uneven thickness around the crystal, effectively reduces the collapse of the material surface in a certain direction, ensures that the erosion rate of the crystal growth chamber in all directions is the same, and increases the use times of consumables and the stability of crystal growth.
(2) The invention also controls the induction coil to rotate by arranging the rotating mechanism, thereby further reducing the uneven heat productivity of the crucible and improving the uniformity of the grown crystal.
(3) The method for growing the large-size silicon carbide single crystal is simple, high in automation degree, low in overall cost and high in economic benefit.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a schematic structural view of a growth apparatus for growing a large-sized silicon carbide single crystal according to the present invention;
FIG. 2 is a schematic diagram of an induction coil according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of an induction coil in another embodiment of the present invention;
FIG. 4 is a high resolution XRD image of a sample of an embodiment of the present invention;
wherein, 1, graphite crucible; 2. a first quartz tube; 3. an induction coil; 4. a second quartz tube; 5. a temperature measuring device; 6. a sliding contact; 7. a contact ring; 8. a control system; 9. a motor; 10. and an intermediate frequency power supply.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited by the specific embodiments disclosed below.
In addition, in the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "coupled," and the like are to be construed broadly and include, for example, fixed or removable connections or integral parts; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. In the description herein, reference to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Unless otherwise specified, the raw materials and reagents in the examples of the present application were purchased commercially.
Example 1: the application is used for growing the specific structure of the large-size silicon carbide single crystal growing device:
as shown in fig. 1, the growing apparatus for growing a large-sized silicon carbide single crystal comprises, in order from the inside to the outside: the large-size crystal growing device comprises a crystal growing chamber, a first quartz tube 2, an induction coil 3 and a second quartz tube 4, wherein the crystal growing chamber is used for growing large-size crystals; the induction coil 3 is wound on the outer side of the first quartz tube 2 and used for heating the crystal growth chamber, and the uniformity of a magnetic field generated by the induction coil 3 is improved by reducing the turn pitch of the coil and increasing the ratio of the height of the coil to the diameter of the coil, so that the distribution uniformity of a temperature field in the crystal growth chamber is improved; the induction coil 3 is also rotated around the first quartz tube 2 by a rotation mechanism provided.
Specifically, the turn pitch of the induction coil 3 is 0-6 mm, the ratio of the height of the coil to the diameter of the coil is 1.2-3, preferably, the turn pitch of the induction coil 3 is 4mm, and the ratio of the height of the coil to the diameter of the coil is 2. The inventor finds that the coil turn-to-turn ratio is more than 6mm, which influences the uniformity of a temperature field and further influences the crystal growth quality of the silicon carbide crystal; the larger the ratio of the height to the diameter of the coil is, the closer the magnetic field is to a uniform magnetic field, so that the more uniform the heating of the crucible is, the more uniform the crystal growth is.
In a specific embodiment, circulating cooling water flows through both the first quartz tube 2 and the second quartz tube 4 for cooling the induction coil 3. The first quartz tube 2 and the second quartz tube 4 are both double-layer quartz tubes. Circulating water is introduced into the first quartz tube 2, so that heat can be effectively dissipated to the furnace chamber and the induction coil. The induction coil 3 is a solid copper coil, has strong thermoplasticity, is easy to deform when heated to a higher temperature, and influences the service life of the induction coil, the first quartz tube 2 is circulated with cooling water to cool the inner side of the induction coil, and the induction coil is solid, so that the induction coil is unevenly cooled; circulating cooling water flowing through the second quartz tube 4 can cool the outer side of the induction coil, so that the induction coil is cooled more uniformly; if the temperature of the induction coil is too high, the temperature field generated by the induction coil fluctuates, and the uniformity of crystal growth is indirectly influenced; therefore, circulating cooling water through the second quartz tube 4 can improve the uniformity of crystal growth.
In a preferred embodiment, the induction coil 3 can be a coil with an olive-shaped axial cross-section, as shown in fig. 2, in order to accommodate different requirements, such as a large intrinsic temperature gradient of the crucible during heating, i.e. to adjust the shape of the coil. Accordingly, in order to make the coil have a small intrinsic temperature gradient, the induction coil 3 may be a coil having a dumbbell-shaped axial cross section, as shown in fig. 3. Accordingly, the shapes of the first quartz tube 2 and the second quartz tube 4 are also changed similarly.
In a specific embodiment, the rotation mechanism includes a motor for controlling the rotation of the induction coil 3; preferably, two ends of the induction coil 3 are inserted on an insulating disc, and the insulating disc is connected with a rotating shaft of the motor 9; preferably, the motor 9 is controlled by the control system 8.
The magnitude of the power supply current in the induction coil 3 is controlled by a current control component; preferably, the current control assembly comprises a sliding contact 6, a contact ring 7 and a medium frequency power supply 10, and two ends of the induction coil 3 are respectively connected with the medium frequency power supply 10 through the sliding contact 6 and the contact ring 7; preferably, the current control assembly is controlled by a control system 8. The temperature of the crystal growth chamber is measured by a temperature measuring device 5, and the temperature measuring device 5 is connected with a control system 8. The control system 8 adjusts the magnitude of the intermediate frequency power supply current through the sliding contact 6 according to the set temperature and the temperature magnitude of the temperature measuring device 5.
The induction coil 3 is spirally wound outside a crystal growth chamber, wherein the crystal growth chamber is a graphite crucible 1, and the graphite crucible 1 is heated after the induction coil 3 is electrified.
In order to ensure the heating uniformity of the graphite crucible 1, the graphite crucible 1 is placed at the center of the induction coil 3 as much as possible before crystal growth, and even if there is a small deviation, an error can be avoided by the rotation of the induction coil 3.
Example 2: growth of silicon carbide single crystal
According to an embodiment of the present application, a growth method of growing a large-size silicon carbide single crystal includes:
(1) and (3) assembling: placing raw materials and seed crystals in a crystal growth chamber, namely a graphite crucible 1, and placing heat preservation felts at the bottom and the side part of a growth device, and replacing the atmosphere of the crystal growth chamber with a protective gas atmosphere;
(2) a heating temperature-rising stage: vacuumizing the growth device, introducing protective gas, and maintaining the absolute pressure in the growth device at 0.8X 10 4-1.2×10 4Pa; controlling the medium-frequency power supply to be electrified by the control system, simultaneously starting the temperature measuring device, and starting to rotate the induction coil at the rotating speed of 3-30r/min until the crystal growth chamber reaches 1800-2000 k;
(3) crystal growth stage: the temperature uniformity determines the quality of the long crystal and the number of times of using consumable materials, therefore, the rotating speed of the induction coil is increased, 10-70r/min is kept, the heating is kept stable, the control system can automatically adjust the magnitude of the intermediate frequency power supply current and the rotating speed of the coil according to the set temperature, the temperature is continuously controlled to be 2200-. In the crystal growth process, circulating cooling water uniformly flows through the first quartz tube 2 and the second quartz tube 4.
(4) And (3) cooling: the crystal is cooled at a very slow speed and in a very uniform temperature environment, which reduces the residual stress in the crystal. Therefore, the cooling speed is set, the heating current is slowly reduced, the cooling speed is kept at 6-10k/h, the rotating speed of the induction coil is kept at 3-30r/min, the flow rate of the internal and external circulating water is controlled to be increased to 200L/min, the temperature of the furnace chamber is quickly reduced to the room temperature, and crystal growth is completed.
(5) And (3) a blow-in stage: crystals were obtained.
Specific implementation conditions are shown in table 1:
TABLE 1 Process parameters of samples of examples of the invention
In addition, 3 comparative examples were provided, and the induction coil of comparative example 1 was not rotated. The turn pitch of the induction coil in the comparative example 2 is 7mm, and the coil is set to rotate; the ratio of the height to the diameter of the induction coil in the comparative example 3 is 1, and the coil is set to rotate; the outer layer of the induction coil in the comparative example 4 is not provided with a second quartz tube, and only the first quartz tube circulates circulating cooling water; the remaining preparation processes in comparative examples 1 to 4 are the same as those of sample 1.
The crystal quality of all samples 1 to 6 and comparative samples 1 to 4 were examined. The thicknesses of four points of the crystal are respectively measured by a vernier caliper after the crystal growth is finished, the crystal quality is measured by high-resolution XRD, the high-resolution XRD image of the sample 1 is shown in figure 4, and the test results of all the samples are shown in table 2.
As shown in fig. 4, the high-resolution XRD pattern of sample 1, having a full width at half maximum of 14.4, was visually recognized in the case of collapse of the starting material, and phase change cracks on the crystal surface were visually recognized. As shown in table 2, the comparison between sample 1 and comparative sample 1 can be obtained, and the rotating coil has a significant improvement in crystal quality for crystal growth. Comparing the sample 1 with the comparative sample 2, it can be concluded that too large a coil turn-to-turn distance results in non-uniform temperature field and thus affects the crystal growth quality of the silicon carbide crystal. Comparing the sample 1 with the comparative sample 3 to obtain the influence of the ratio of the height to the diameter of the coil on the quality of the crystal; wherein, in the coils with the same diameter, the higher the coil is, the closer the magnetic field is to the uniform magnetic field, so that the more uniform the heating of the crucible is, the more uniform the crystal growth is; and comparing the sample 1 with the comparative sample 4 to obtain circulating cooling water circulating outside the induction coil, so that the crystal growth quality of the silicon carbide crystal can be improved.
TABLE 2 results of crystal quality measurements for all samples
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present application, and the protection scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.

Claims (10)

1. A method for growing large-size silicon carbide single crystal comprises the step of heating a crystal growing chamber by using an induction coil, and is characterized in that in the process of growing the single crystal, the induction coil is controlled to rotate by arranging a rotating mechanism, and the uniformity of the temperature field of the crystal growing chamber is controlled by reducing the turn pitch of the induction coil and increasing the ratio of the height of the coil to the diameter of the coil.
2. A method for growing a large-sized silicon carbide single crystal according to claim 1, wherein the pitch of the turns of the induction coil is 0 to 6mm, and the ratio of the height of the coil to the diameter of the coil is 1.2 to 3, preferably, the pitch of the turns of the induction coil is 4mm, and the ratio of the height of the coil to the diameter of the coil is 2.
3. A method for growing a large-sized silicon carbide single crystal according to claim 1, wherein a first quartz tube is provided inside the induction coil, the induction coil rotates around the first quartz tube, and a second quartz tube is provided outside the induction coil; preferably, circulating cooling water flows through both the first quartz tube and the second quartz tube.
4. A method for growing a large-size silicon carbide single crystal according to claim 3, wherein the axial section of the induction coil is olive-shaped or dumbbell-shaped; preferably, the difference between the maximum diameter of the coil and the minimum diameter thereof is not greater than the horizontal distance between the first and second quartz tubes.
5. A method for growing a large-size silicon carbide single crystal according to claim 1, wherein the magnitude of the power supply current of the induction coil is controlled by a current control assembly; preferably, the current control assembly comprises a sliding contact, a contact ring and a medium-frequency power supply, and two ends of the induction coil are respectively connected with the medium-frequency power supply through the sliding contact and the contact ring; preferably, the current control assembly is controlled by a control system.
6. A method for growing a large-size silicon carbide single crystal according to claim 1, wherein the rotating mechanism includes a motor for controlling rotation of an induction coil; preferably, two ends of the induction coil are inserted on the insulating disc, and the insulating disc is connected with a rotating shaft of the motor; preferably, the motor is controlled by a control system.
7. A method for growing a large-size silicon carbide single crystal according to claim 1, wherein the induction coil is disposed outside the crystal growth chamber in a spirally wound manner; preferably, the crystal growth chamber is a graphite crucible; preferably, the crystal growth chamber is located substantially in the center of the induction coil; preferably, the temperature of the crystal growth chamber is measured by a temperature measuring device, which is connected to the control system.
8. A method for growing a large-size silicon carbide single crystal according to claim 1, wherein before the crystal growth, the current of the induction coil is increased under the rotation condition of the induction coil to heat the crystal growth chamber to a temperature required for the crystal growth; when crystal growth occurs, the rotating speed of the induction coil is increased, and the current of the induction coil is kept stable; after crystal growth is finished, the current in the induction coil is slowly reduced, meanwhile, the rotating speed of the induction coil is increased, and the temperature of the crystal growth chamber is reduced to room temperature.
9. The method as claimed in claim 8, wherein before the growth, the rotation speed of the induction coil is 3-30r/min, the temperature of the crystal growth chamber is controlled to 1800-2000k, and the pressure is controlled to 8000-12000 pa; during crystal growth, the rotating speed of the induction coil is 10-70r/min, the temperature of the crystal growth chamber is controlled to 2200-; after crystal growth is finished, the rotating speed of the induction coil is 3-30 r/min; preferably, the cooling rate is 6-10 k/h.
10. A large-size silicon carbide single crystal produced by the method for growing a large-size silicon carbide single crystal according to any one of claims 1 to 9.
CN201910969170.3A 2019-10-12 2019-10-12 Method for growing large-size silicon carbide single crystal Pending CN110777430A (en)

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CN113622029A (en) * 2021-08-12 2021-11-09 山东天岳先进科技股份有限公司 Crucible assembly having polycrystalline block, method of manufacturing the same, and silicon carbide single crystal manufactured therefrom
CN114411264A (en) * 2022-01-20 2022-04-29 南京晶升装备股份有限公司 Rotatory long brilliant stove induction heating system of carborundum and long brilliant stove
CN115198366A (en) * 2022-09-14 2022-10-18 青禾晶元(天津)半导体材料有限公司 Growth device and growth method of large-size silicon carbide crystals

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CN203546207U (en) * 2013-11-20 2014-04-16 河北同光晶体有限公司 Induction coil for growth of large-size silicon carbide crystal
CN104498901A (en) * 2015-01-06 2015-04-08 北京华进创威电子有限公司 Method and device for plating silicon carbide single crystal
CN105200515A (en) * 2015-09-24 2015-12-30 山东大学 Induction coil for SiC single-crystal growth furnace and application thereof
CN105256371A (en) * 2015-11-30 2016-01-20 山东省科学院能源研究所 Device for improving temperature field uniformity of crystal growing furnace of physical vapor transport method
CN107142520A (en) * 2017-05-17 2017-09-08 中国科学院电工研究所 One kind control silicon carbide monocrystal growth device
CN208717470U (en) * 2018-08-27 2019-04-09 山东大学 A kind of low nitrogen content SiC single crystal grower
CN109518275A (en) * 2018-11-02 2019-03-26 山东天岳先进材料科技有限公司 A kind of method of uniform distribution of temperature field degree during raising silicon carbide monocrystal growth

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CN113622029B (en) * 2021-08-12 2022-11-29 山东天岳先进科技股份有限公司 Crucible assembly having polycrystalline block, method of manufacturing the same, and silicon carbide single crystal manufactured therefrom
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Application publication date: 20200211