CN115573030A - Silicon carbide single crystal growth method and silicon carbide single crystal - Google Patents
Silicon carbide single crystal growth method and silicon carbide single crystal Download PDFInfo
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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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
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Abstract
The invention belongs to the technical field of crystal growth, and provides a silicon carbide single crystal growth method and a silicon carbide single crystal. Selecting silicon carbide powder with a set particle size as a raw material for growing silicon carbide single crystals, uniformly paving the silicon carbide powder at the bottom of a heating container, and bonding silicon carbide seed crystals to the top of the heating container; after the heating container is placed in the single crystal growth equipment, the single crystal growth equipment is sealed, and the interior of the single crystal growth equipment is vacuumized; heating the interior of the vacuumized single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset growth pressure, and preserving heat for a preset time to carry out crystal growth after heating to a preset growth temperature; the growth pressure is related to the granularity of the silicon carbide powder, and the larger the granularity of the powder is, the smaller the growth pressure is; and after the crystal growth is finished, cooling the interior of the single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset cooling pressure, and naturally cooling the crystal to obtain the silicon carbide single crystal.
Description
Technical Field
The invention belongs to the technical field of crystal growth, and particularly relates to a silicon carbide single crystal growth method and a silicon carbide single crystal.
Background
The statements in this section merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Silicon carbide, as an important third-generation semiconductor material at present, has excellent properties such as high thermal conductivity, large forbidden bandwidth, high breakdown field strength, high electronic saturation rate, high temperature resistance, radiation resistance, corrosion resistance and the like which are not possessed by traditional semiconductor materials such as Si and GaAs, so that a device can normally operate in a severe environment, and the silicon carbide has important applications in the fields of modern power electronics, microwave radio frequency, photoelectron and the like.
Methods for producing silicon carbide single crystals mainly include a Physical Vapor Transport (PVT) method, a Chemical Vapor Deposition (CVD) method, a flux (LPE) method, and the like. The most widely used and mature method at present is the physical vapor transport method. The crystal growth by adopting the method mainly comprises four stages: the chamber is vacuumized, preheated, grown at high temperature, cooled and the like. When the method is used for growing the silicon carbide crystals, silicon carbide powder serving as a raw material is required to be placed at the bottom of the graphite crucible, and silicon carbide seed crystal slices serving as seed crystals are required to be placed at the top of the graphite crucible. By heating the graphite crucible, a proper temperature field is constructed in the crucible, so that silicon carbide powder positioned at the bottom of the crucible is sublimated and decomposed into Si and Si 2 C、SiC 2 And the like, and the silicon carbide single crystal is crystallized and formed by the seed crystal conveyed from the bottom of the crucible to the top of the crucible under the action of the temperature gradient. The temperature field distribution in the crucible has important influence on the sublimation, transmission and recrystallization of the silicon carbide powder, and is a core factor influencing the growth of the silicon carbide single crystal.
The most common heating method for physical vapor transport is induction heating. The induction heating method is to generate a constantly changing magnetic field by a high frequency current whose direction is constantly changing in a coil, and then induce a current in a graphite crucible to generate heat. However, due to the skin effect of current, the heating positions of the graphite crucible are distributed on the side wall of the crucible, when a large-diameter silicon carbide single crystal grows, the radial temperature difference between the crucible wall and the crucible center is increased along with the increase of the diameter of the graphite crucible, a large radial temperature gradient is generated inside silicon carbide powder, so that after the powder on the two sides of the crucible is sublimated and decomposed, a part of the powder is transported into a growth cavity, and a large part of the powder is transported to the material center position with low temperature and crystallized, so that the utilization efficiency of the powder is influenced, and the crystal growth rate is reduced. Although the radial and axial temperature gradients in the material can be reduced by changing the relative position between the crucible and the induction coil, the axial temperature gradient in the growth cavity is increased along with the radial temperature gradient at the growth front edge, and the radial temperature gradient is reduced along with the axial temperature gradient, which is not beneficial to the growth of single crystal. Therefore, a method for improving the uniformity of the internal temperature distribution of the powder under the premise of not reducing the axial temperature gradient in the growth cavity and not increasing the radial temperature gradient of the growth front is needed.
Chinese patent document CN 115044969A discloses a growth apparatus for improving raw material transfer efficiency when growing silicon carbide crystals. In the invention, a graphite cylinder is arranged in a crystal growth crucible along the axis of the crucible, and a graphite plate is arranged in the graphite cylinder to divide a charging area in the crucible into three parts. The advantage of high thermal conductivity of the graphite cylinder and the graphite plate is utilized to achieve the purpose of reducing the radial temperature gradient in the raw material. Meanwhile, the graphite barrel and the graphite plate can prevent raw materials at the outer side from being transmitted to the center, so that the powder can be forced to be conveyed to the seed crystal positioned at the upper part of the crucible, the horizontal conveying of the silicon carbide powder is restrained, the powder conveying efficiency is improved, and the growth rate of the silicon carbide crystal is increased. Although the method can reduce the radial temperature gradient in the powder, the crucible assembly needs to be changed, and the process is complex. Furthermore, when the method is used for increasing the crystal growth rate, the charging height is strictly limited. The charging height is too high, and if the high-temperature area is positioned above, the transportation of raw materials at the lower part is not facilitated; if the high-temperature area is positioned below the high-temperature area, the upper part of the powder is crystallized, and the transportation of the raw material is blocked. Therefore, the charging amount in the method cannot be too high, namely, on the premise of not changing the charging height of the crucible, enough silicon carbide source material cannot be provided, so that the thickness of the grown crystal is limited, and the method cannot be used for growing large-size and thick crystals.
Chinese patent document CN113026095A discloses a growth method for increasing growth rate of silicon carbide crystal prepared by PVT method. The invention uses powder with different grain diameters to grow silicon carbide single crystal, the large size powder can provide enough grain gaps to promote the transportation of gas phase components, the small size powder has enough powder activity to generate enough reaction gas phase, and the growth rate (105 mu m/h) of the crystal is improved simultaneously in two aspects. However, in the method, the particle size of the used silicon carbide powder is generally small (10-500 μm), which can cause the accelerated decomposition of the powder, increase of silicon components in a growth system, easy corrosion of the inner wall of a graphite crucible and the like, and the corroded graphite crucible can provide a large amount of carbon particles in a growth cavity, thereby causing a large amount of carbon inclusions in crystals and influencing the quality of the grown crystals. In addition, the invention needs to mix the powder with different particle sizes according to different mass ratios, has relatively complex process and is not suitable for industrialized popularization.
In summary, the inventor finds that the existing silicon carbide crystal growth method needs to change the structure of a crucible, has relatively complex process, is not suitable for industrial popularization, and is not suitable for the growth of large-diameter (such as 6 inches and more in diameter) silicon carbide single crystals.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a silicon carbide single crystal growth method and a silicon carbide single crystal, wherein the method does not need to change the structure of a heating container, is compatible with the existing single crystal growth device, is simple and practical, and is beneficial to popularization.
In order to achieve the purpose, the invention adopts the following technical scheme:
a first aspect of the present invention provides a method for growing a silicon carbide single crystal.
In one or more embodiments, a silicon carbide single crystal growth method includes:
selecting silicon carbide powder with a set particle size as a raw material for growing silicon carbide single crystals, uniformly paving the silicon carbide powder at the bottom of a heating container, and bonding silicon carbide seed crystals at the top of the heating container;
after the heating container is placed in the single crystal growth equipment, the single crystal growth equipment is sealed, and the interior of the single crystal growth equipment is vacuumized;
heating the interior of the vacuumized single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset growth pressure, and preserving heat for a preset time to carry out crystal growth after heating to a preset growth temperature; the growth pressure is related to the granularity of the silicon carbide powder, and the larger the granularity of the powder is, the smaller the growth pressure is;
and after the crystal growth is finished, cooling the interior of the single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset cooling pressure, and naturally cooling the crystal to obtain the silicon carbide single crystal.
As an embodiment, the method for growing a silicon carbide single crystal further includes:
the thickness of the silicon carbide single crystal produced was measured to evaluate the growth height rate of the crystal.
Wherein, the thickness of the silicon carbide single crystal refers to the thickness of the thinnest part of the crystal. And the thickness of the crystal can be obtained by testing a vernier caliper, a micrometer screw gauge or a height gauge and the like.
As an embodiment, the method for growing a silicon carbide single crystal further includes:
observing the internal defects of the crystal, and preliminarily judging the crystallization quality of the crystal;
and performing cutting, grinding and polishing treatment on the grown crystal to obtain a silicon carbide wafer, and performing quality characterization on the wafer.
Wherein, the internal defects of the crystal are whether the defects of wrappage, polytype, microtubule and the like exist in the crystal. These can be observed by illuminating the crystal with a bright light source, a halogen lamp, or the like.
As an embodiment, the quality characterization of the wafer comprises: the crystal quality of the crystal is represented by an X-ray diffractometer, and defects (such as micropipes, inclusions, dislocation and the like) in the crystal are researched by a surface defect detector.
In one embodiment, the silicon carbide powder is silicon carbide particles having a diameter of 1 to 20 mm.
In one embodiment, the silicon carbide powder is paved at the bottom of the heating container to a thickness of 50-100 mm.
In one embodiment, the silicon carbide seed crystal has a diameter of at least 2 inches.
In one embodiment, the silicon carbide seed crystal has a diameter of 6 inches or 8 inches.
As an embodiment, after the inside of the single crystal growth apparatus is vacuumized, the inside of the single crystal growth apparatus is not more than 0.01Pa.
In one embodiment, the carrier gas is argon, hydrogen, nitrogen, helium, or a mixture thereof.
In one embodiment, the silicon carbide single crystal is grown under a pressure of 1 to 50mbar.
As an embodiment, when the powder granularity is 10-20 mm, the growth pressure is 1-30 mbar; when the powder granularity is 1-10 mm, the growth pressure is 5-50 mbar.
In one embodiment, the material is heated to the set growth temperature at a preset temperature-raising rate.
In one embodiment, the temperature increase rate is 300 to 300 ℃/h.
In one embodiment, the silicon carbide single crystal is grown at a temperature of 2100 to 2500 ℃.
In one embodiment, the silicon carbide single crystal is grown for 30 to 100 hours.
In one embodiment, the cooling pressure is 300 to 1000mbar.
A second aspect of the present invention provides a silicon carbide single crystal.
In one or more embodiments, a silicon carbide single crystal obtained by the silicon carbide single crystal growth method as described above.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the silicon carbide single crystal growth method disclosed by the invention, the silicon carbide powder with the set particle size is used for growing the large-diameter silicon carbide single crystal, so that the growth temperature field of the large-diameter silicon carbide single crystal is effectively improved: the problem that the edge temperature inside the powder is inconsistent with the central temperature inside the powder due to the skin effect of current in induction heating is solved to a certain extent, the radial temperature gradient inside the powder and the axial temperature gradient inside the powder are reduced, the axial temperature gradient in a growth cavity is improved, the problem that the powder in a crucible is recrystallized at the position close to the center inside the powder and on the surface of the powder is solved, the utilization rate of silicon carbide powder is improved, the transport speed of gas-phase components in the growth cavity is increased, the thickness of the silicon carbide single crystal is increased in the same time, and the productivity of the silicon carbide single crystal is improved.
(2) The method for growing the silicon carbide single crystal effectively transmits the heat of the crucible wall to the center of the powder, improves the temperature uniformity in the large-diameter silicon carbide single crystal growing powder, improves the heating efficiency of a heating system, effectively reduces the energy consumption for growing the silicon carbide single crystal and reduces the single crystal growing cost.
(3) The silicon carbide single crystal growth method fully utilizes the corresponding relation between the granularity of the powder and the growth pressure, and can reduce the axis ladder of heat preservation assembly as much as possible while ensuring the growth rate of the single crystal, so that the crystal can grow under a close-to-equilibrium state, the quality of the grown crystal is better, and particularly, secondary phase inclusions such as silicon drops, carbon inclusions and the like in the crystal can be obviously reduced.
(4) According to the method, the uniformity of a temperature field in the material is effectively improved by limiting the charging height of the crucible while the growth thickness of the single crystal is ensured, and both the axial temperature gradient in the powder and the radial temperature gradient on the surface of the powder are reduced to be less than 0.5 ℃/cm.
(5) The silicon carbide single crystal growth method does not need to change the structure of a heating container (such as a crucible), is compatible with the existing single crystal growth device, is simple and practical, and is beneficial to popularization; the method of the present invention is suitable for growing a silicon carbide single crystal having a large diameter (6 inches or more), and is also suitable for growing a single crystal having a diameter of 6 inches or less.
Advantages of additional aspects of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are included to illustrate an exemplary embodiment of the invention and not to limit the invention.
FIG. 1 is a schematic view of an apparatus for growing a silicon carbide single crystal according to the present invention.
FIG. 2 is a temperature field diagram of the inside of a graphite crucible for growing a silicon carbide single crystal obtained in example 1 of the present invention.
FIG. 3 is a photograph of a silicon carbide crystal grown in example 1 of the present invention and having a thickness of 33mm and a diameter of 150 mm.
FIG. 4 is a temperature field diagram in a graphite crucible for growing a silicon carbide single crystal obtained in comparative example 1 of the present invention.
Wherein, 1 is an induction heating coil, 2 is a graphite crucible, 3 is a heat insulation material, 4 is a silicon carbide seed crystal, 5 is a growing silicon carbide single crystal, and 6 is silicon carbide powder. T1 is the temperature of the center of the silicon carbide seed crystal, T2 is the temperature of the edge of the silicon carbide seed crystal, T3 is the temperature of the center of the surface of the silicon carbide powder, T4 is the temperature of the edge of the surface of the silicon carbide powder, T5 is the temperature of the center of the bottom of the silicon carbide powder, and T6 is the temperature of the edge of the bottom of the silicon carbide powder. The radial temperature gradient of the surface of the seed crystal is (T2-T1)/R, the axial temperature gradient in the growth cavity is (T3-T1)/L, the axial temperature gradient in the powder is (T5-T3)/H, and the radial temperature gradient of the surface of the powder is (T4-T3)/R. Wherein R is the radius of the used silicon carbide seed crystal, L is the length of a growth cavity of the used crucible, H is the paving thickness of the used silicon carbide powder at the bottom of the graphite crucible, and R is the radius of the paved surface of the used silicon carbide powder.
Detailed Description
The invention is further described with reference to the following figures and examples.
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Interpretation of terms:
growth front radial temperature gradient: the present invention refers to the temperature difference between the edge of the silicon carbide seed crystal and the center of the silicon carbide seed crystal per unit length. Generally, the radial temperature gradient of the growth front is too large, and the more convex the appearance of the grown crystal, the greater the stress in the crystal.
Axial temperature gradient of temperature in the growth chamber: the temperature difference between the surface center of the silicon carbide powder and the center of the silicon carbide seed crystal under the unit length represents the driving force of single crystal growth. The larger the temperature axial temperature gradient in the growth cavity is, the faster the single crystal growth rate is.
Material internal radial temperature gradient: the invention refers to the temperature difference between the center of the surface of the silicon carbide powder and the edge of the surface of the silicon carbide powder under unit length. The larger the radial temperature gradient in the material is, the easier the powder material at the edge is to agglomerate towards the center, and the more unfavorable the growth component is to be transmitted into the growth cavity. From the crystal growth point of view, the smaller the radial temperature gradient in the ingot, the better.
In-material axial temperature gradient: the present invention refers to the temperature difference between the center of the surface of the silicon carbide powder and the center of the bottom of the silicon carbide powder per unit length. The larger the axial temperature gradient in the material is, the easier the components in the material released by material sublimation are to crystallize on the surface of the material, and the more unfavorable the growth components are to be transmitted to the growth cavity. From the crystal growth perspective, the smaller the in-charge axial temperature gradient, the better.
Large-diameter silicon carbide single crystal: meaning 6 inches and more in diameter.
< method for growing silicon carbide Single Crystal >
In one or more embodiments, provided is a silicon carbide single crystal growth method including:
step 1: selecting silicon carbide powder with a set grain size as a raw material for growing the silicon carbide single crystal, uniformly spreading the silicon carbide powder at the bottom of the heating container, and bonding the silicon carbide seed crystal at the top of the heating container.
Wherein the silicon carbide powder is silicon carbide particles with the diameter of 1-20 mm.
The paving thickness of the silicon carbide powder at the bottom of the heating container is 50-100 mm.
The silicon carbide seed crystal has a diameter of at least 2 inches.
Preferably, the silicon carbide seed crystal has a diameter of 6 inches or 8 inches.
Step 2: and after the heating container is placed in the single crystal growth equipment, the single crystal growth equipment is sealed, and the interior of the single crystal growth equipment is vacuumized.
Wherein, after the interior of the single crystal growth equipment is vacuumized, the interior of the single crystal growth equipment is not more than 0.01Pa.
In this step, the carrier gas is argon, hydrogen, nitrogen, helium or a mixture thereof.
And step 3: heating the interior of the vacuumized single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset growth pressure, and preserving heat for a preset time to grow crystals after the single crystal growth equipment is heated to a preset growth temperature; the growth pressure is related to the granularity of the silicon carbide powder, and the larger the granularity of the powder is, the smaller the growth pressure is.
Specifically, the growth pressure of the silicon carbide single crystal is 1-50 mbar.
When the powder granularity is 10-20 mm, the growth pressure is 1-30 mbar; when the powder granularity is 1-10 mm, the growth pressure is 5-50 mbar.
Specifically, heating is carried out at a preset temperature rise speed to a set growth temperature. For example, the temperature rise rate is 300 to 300 ℃/h.
Wherein the growth temperature of the silicon carbide single crystal is 2100-2500 ℃. The growth time of the silicon carbide single crystal is 30-100 h.
And 4, step 4: and after the crystal growth is finished, cooling the interior of the single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset cooling pressure, and naturally cooling the crystal to obtain the silicon carbide single crystal.
Wherein the cooling pressure is 300 to 1000mbar.
In some other embodiments, the silicon carbide single crystal growth method further includes:
the thickness of the silicon carbide single crystal produced was measured to evaluate the growth height rate of the crystal.
Wherein, the thickness of the silicon carbide single crystal refers to the thickness of the thinnest part of the crystal. And the thickness of the crystal can be obtained by testing a vernier caliper, a micrometer screw gauge or a height gauge and the like.
In some other embodiments, the method of growing a silicon carbide single crystal further comprises:
observing the internal defects of the crystal, and preliminarily judging the crystallization quality of the crystal;
and performing cutting, grinding and polishing treatment on the grown crystal to obtain a silicon carbide wafer, and performing quality characterization on the wafer.
Wherein, the internal defects of the crystal are whether the defects of wrappage, polytype, microtubule and the like exist in the crystal. These can be observed by illuminating the crystal with a bright light source, a halogen lamp, or the like.
As an embodiment, the quality characterization of the wafer comprises: the crystal quality of the crystal is represented by an X-ray diffractometer, and defects (such as micropipes, inclusions, dislocation and the like) in the crystal are researched by a surface defect detector.
The following examples will be given by taking a graphite crucible as a heating vessel and a single crystal growth furnace as a single crystal growth apparatus.
It should be noted that the heating vessel and the single crystal growth furnace are both of the existing structure, and those skilled in the art can specifically select the corresponding devices or equipment according to the needs of actual situations.
The silicon carbide single crystal growth apparatus of the present example is shown in FIG. 1.
The method of the present invention is suitable for growing a silicon carbide single crystal having a large diameter (6 inches or more), and is also suitable for growing a single crystal having a diameter of 6 inches or less.
Example 1
The embodiment provides a silicon carbide single crystal growth method, which specifically comprises the following steps:
(1) Charging: selecting silicon carbide powder with the grain size of 1mm as a raw material for growing silicon carbide single crystals, uniformly spreading the silicon carbide powder at the bottom of a graphite crucible with the spreading thickness of 100mm, placing 4H-SiC seed crystals with the diameter of 6 inches at the top of the graphite crucible,
(2) Vacuumizing: the graphite crucible is put into a single crystal growth furnace and is vacuumized to 0.01Pa by a mechanical pump.
(3) Heating and growing: argon is filled into the furnace until the pressure is 50mbar, the graphite crucible is heated, the temperature is raised to 2100 ℃ at the speed of 300 ℃/h, and the temperature is maintained for 100h. The temperature field in the graphite crucible for growing the silicon carbide single crystal is shown in FIG. 2.
(4) Cooling: and reducing the heating power of the system, cooling, and introducing argon to the pressure of 1000mbar for natural cooling to obtain the silicon carbide single crystal.
(5) Opening the furnace: and taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, wherein the silicon carbide powder is completely in a bulk state, and no crystal exists in the powder or on the surface of the powder. Indicating a uniform temperature field distribution within the material, as shown in fig. 4.
(6) And (3) testing and characterizing: as shown in FIG. 3, the thickness of the silicon carbide single crystal was measured by a vernier caliper at 36.32mm, the crystal growth height rate was about 363 μm/h, and defects such as micropipes and inclusions in the crystal were not observed by using a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test a wafer (004) surface rocking curve, the half-peak width is only 20 arcsec, and the crystal crystallization quality is high; the surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, secondary phase defects such as silicon drops, carbon inclusions and the like do not exist, and the total dislocation density is 3200cm -2 . The 6-inch silicon carbide single crystal prepared by the method has high growth rate, thick crystal and high quality.
Example 2
The difference from example 1 is:
the embodiment provides a silicon carbide single crystal growth method, which specifically comprises the following steps:
(1) Charging: selecting silicon carbide powder with the grain diameter of 10mm as a raw material for growing the silicon carbide single crystal, uniformly spreading the silicon carbide powder at the bottom of a graphite crucible with the spreading thickness of 80mm, placing 4H-SiC seed crystals with the diameter of 8 inches at the top of the graphite crucible,
(2) Vacuumizing: the graphite crucible is put into a single crystal growth furnace, and is pumped to 0.001Pa by a molecular pump.
(3) Heating and growing: charging Ar and N into the furnace 2 The flow ratio of the mixed gas to the mixed gas is 20 to 5mbar, the graphite crucible is heated, the temperature is raised to 2500 ℃ at the speed of 300 ℃/h, and the temperature is kept for 30h.
(4) Cooling: and reducing the heating power of the system, cooling, and introducing argon to the pressure of 300mbar for natural cooling to obtain the silicon carbide single crystal.
(5) Opening the furnace: and taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, wherein the silicon carbide powder is completely in a bulk state, and no crystal exists in the powder or on the surface of the powder. Indicating that the temperature field in the material is uniformly distributed.
(6) And (3) testing and characterizing: the thickness of the silicon carbide single crystal measured by a vernier caliper is 15.6mm, the growth height rate of the crystal is about 520 mu m/h, and defects such as micropipes and inclusions in the crystal are not observed by a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test a wafer (004) surface swing curve, the half-peak width is only 28 arc seconds, and the crystal quality is high; the surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, secondary phase defects such as silicon drops, carbon inclusions and the like do not exist, and the total dislocation density is 4580cm -2 . The 8-inch silicon carbide single crystal prepared by the method has high growth rate and high quality.
Example 3
The difference from example 1 is:
the embodiment provides a silicon carbide single crystal growth method, which specifically comprises the following steps:
(1) Charging: selecting 20 mm-grain-size silicon carbide powder as a raw material for growing silicon carbide single crystals, uniformly spreading the silicon carbide powder at the bottom of a graphite crucible with the spreading thickness of 50mm, placing 4H-SiC seed crystals with the diameter of 8 inches at the top of the graphite crucible,
(2) Vacuumizing: the graphite crucible is put into a single crystal growth furnace, and is pumped to 0.001Pa by a molecular pump.
(3) Heating and growing: ar and H are charged into the furnace 2 Heating the graphite crucible to 2500 ℃ at a speed of 500 ℃/h, and keeping the temperature for 50h, wherein the flow ratio of the mixed gas to the gas is 20.
(4) Cooling: and reducing the heating power of the system, cooling, and introducing argon to the pressure of 800mbar for natural cooling to obtain the silicon carbide single crystal.
(5) Opening the furnace: and taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, wherein the silicon carbide powder is completely in a bulk state, and no crystal exists in the powder or on the surface of the powder. Indicating that the temperature field in the material is uniformly distributed.
(6) And (3) testing and characterizing: the thickness of the silicon carbide single crystal is measured to be 25.0mm by using a vernier caliper, the growth height rate of the crystal is about 500 mu m/h, and defects such as micropipes and inclusions in the crystal are not observed by using a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test a wafer (004) surface swing curve, the half-peak width is only 26 arc seconds, and the crystal quality is high; the surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, secondary phase defects such as silicon drops, carbon inclusions and the like do not exist, and the total dislocation density is 3860cm -2 . The 8-inch silicon carbide single crystal prepared by the method has high growth rate and high quality.
Comparative example 1
In this example, a silicon carbide powder having a particle size of 0.3mm was selected to grow a large-diameter silicon carbide single crystal, and the other growth conditions were the same as those in example 1. And after the growth is finished, taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, and finding out crystals in the silicon carbide powder and in the middle of the surface of the silicon carbide powder. Indicating that the axial temperature gradient and the radial temperature gradient in the material are larger. Furthermore, the graphite crucible was found to be severely corroded. The thickness of the silicon carbide single crystal is 10.2mm by using a vernier caliper, the growth height rate of the crystal is about 102 mu m/h, and the existence of microtubules and packages in the crystal are observed by using a halogen lampAnd (4) defects such as objects. Cutting, grinding and polishing the crystal, and testing a wafer (004) surface rocking curve by using an X-ray diffractometer, wherein the half-peak width is 82 arcsec, which indicates that the crystal quality is poor; the defects of micropipes, inclusions, dislocation and the like in the crystal are researched by adopting a surface defect detector, and the result shows that the density of the micropipes in the wafer is 0.33cm -2 The defect of the carbon inclusion exists, and the carbon inclusion causes a large amount of micropipes and dislocation defects in the crystal, and the density of the micropipes in the crystal is 12.5cm -2 Total dislocation density of over 10000cm -2 The 6-inch silicon carbide single crystal prepared in this example is slow in growth rate and poor in quality.
Comparative example 2
In this example, a silicon carbide powder having a particle size of 30mm was selected to grow a large-diameter silicon carbide single crystal, and the other growth conditions were the same as those in example 2. Opening the furnace: and taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, wherein the silicon carbide powder is completely in a bulk state, and no crystal exists in the powder or on the surface of the powder. Indicating that the temperature field in the material is uniformly distributed. The crystal diameter is only 160mm, and the 20mm of the edge of the seed crystal is seriously decomposed; the thickness of the silicon carbide single crystal is 3.3mm by using a vernier caliper, the growth height rate of the crystal is about 110 mu m/h, and defects such as micropipes, inclusions and the like in the crystal are observed by using a halogen lamp. Cutting, grinding and polishing the crystal, and testing a wafer (004) surface rocking curve by using an X-ray diffractometer, wherein the half-peak width is 62 arcsec, which indicates that the crystal quality is poor; the surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, and secondary phase defects such as silicon drops, carbon inclusions and the like do not exist, but the total dislocation density in the crystal is 8580cm -2 . The problem that the diameter of the prepared silicon carbide crystal is unqualified due to serious decomposition of the seed crystal edge, and the problems of slow crystal growth rate, high dislocation density and the like exist simultaneously.
Comparative example 3
In this example, the pressure of argon gas introduced into the furnace during thermal growth was 1mbar, and the growth conditions were the same as those in example 1. Opening the furnace: taking out the graphite crucible from the growth furnace to obtain silicon carbide single crystal, and finding carbonizationThe silicon powder is completely in a bulk state, and no crystal exists in the powder or on the surface of the powder. Indicating that the temperature field in the material is uniformly distributed. The thickness of the silicon carbide single crystal is measured by a vernier caliper to be 48.53mm, the growth height rate of the crystal is about 486 mu m/h, and defects such as micropipes and inclusions in the crystal are observed by a halogen lamp. Cutting, grinding and polishing the crystal, and testing a wafer (004) surface rocking curve by using an X-ray diffractometer, wherein the half-peak width is 85 arc seconds, which indicates that the crystal quality is poor; the surface defect detector is adopted to research the defects of micropipes, wrappings, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is 0.41cm -2 The crystal has a large number of micro-tubes and dislocation defects caused by carbon inclusions in the crystal, and the wafer has large-area mist inclusions with total dislocation density over 10000cm -2 The 6-inch silicon carbide single crystal prepared in this example was of a poor quality despite a fast growth rate.
Comparative example 4
In this example, the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 150mm, and the rest growth conditions are completely the same as those in example 1. Opening the furnace: and taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, and finding that the silicon carbide powder is blocky and crystals appear in the powder and on the surface of the powder. Indicating that the temperature field within the material is not uniformly distributed. The fact that the crystal diameter is only 140mm, the decomposition is serious when the edge of the seed crystal is 5mm is found, and growth components cannot be effectively conveyed into a growth cavity due to the fact that a temperature field in the material is not uniform; the thickness of the silicon carbide single crystal is 15.2mm by using a vernier caliper, the growth height rate of the crystal is about 152 mu m/h, and defects such as micropipes and inclusions in the crystal are observed by using a halogen lamp. Cutting, grinding and polishing the crystal, and testing a wafer (004) surface swing curve by using an X-ray diffractometer, wherein the half-peak width is 82 arc seconds, which indicates that the crystallization quality of the crystal is poor; a surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, and secondary phase defects such as silicon drops, carbon inclusions and the like do not exist, but the crystal does not reach the standard due to the decomposition of the edge of the seed crystal. The problems of unqualified diameter, slow crystal growth rate and the like caused by serious decomposition of the edge of the seed crystal in the preparation of the silicon carbide crystal in the method are explained.
Comparative example 5
The paving thickness of the silicon carbide powder at the bottom of the graphite crucible in the embodiment is 30mm, and the rest growth conditions are completely the same as those in the embodiment 1. Opening the furnace: taking the graphite crucible out of the growth furnace to obtain the silicon carbide single crystal, and finding that although the silicon carbide powder is completely in a loose state, no crystal exists in the powder or on the surface of the powder, the rest of the powder is less, and the surface of the crystal is decomposed and carbonized. It is shown that the temperature field in the material is distributed uniformly, but the charging amount is insufficient. The thickness of the silicon carbide single crystal is measured to be 12.36mm by using a vernier caliper, the growth height rate of the crystal is about 124 mu m/h, and defects such as micropipes, inclusions and the like in the crystal are observed by using a halogen lamp. Cutting, grinding and polishing the crystal, and testing a wafer (004) surface swing curve by using an X-ray diffractometer, wherein the half-peak width is 29 arc seconds; a surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, and secondary phase defects such as silicon drops, carbon inclusions and the like do not exist. This indicates that the method has a problem that a relatively thick crystal cannot be grown with a small amount of charge.
Comparative example 6
In this example, the pressure of argon gas introduced into the furnace during the thermal growth was 100mbar, and the other growth conditions were the same as those in example 1. Opening the furnace: and taking out the graphite crucible from the growth furnace to obtain the silicon carbide single crystal, wherein the silicon carbide powder is completely in a bulk state, and no crystal exists in the powder or on the surface of the powder. Indicating that the temperature field in the material is uniformly distributed. The crystal diameter is only 130mm, and the 10mm decomposition of the edge of the seed crystal is serious; the thickness of the silicon carbide single crystal is 1.34mm by using a vernier caliper, the growth height rate of the crystal is about 134 mu m/h, and defects such as micropipes and inclusions in the crystal are observed by using a halogen lamp. Cutting, grinding and polishing the crystal, and testing a wafer (004) surface rocking curve by using an X-ray diffractometer, wherein the half-peak width is 69 arc seconds, which indicates that the crystal quality is poor; the surface defect detector is adopted to research the defects of micropipes, inclusions, dislocation and the like in the crystal, and the result shows that the density of the micropipes in the wafer is zero, and secondary phase defects such as silicon drops, carbon inclusions and the like do not exist, but the total dislocation density in the crystal is 9160cm -2 . Illustrating that the silicon carbide crystal prepared by the method is seriously degraded due to the edge decomposition of the seed crystalThe diameter is unqualified, and the problems of slow crystal growth rate, high dislocation density and the like exist at the same time. Table 1 shows the temperature gradient and growth power results between the different examples and comparative examples calculated using numerical simulation software.
TABLE 1 temperature gradient and growth power results between different examples and comparative examples
The invention discovers that the temperature field distribution in the crucible can be obviously changed by only changing the granularity of silicon carbide powder under the condition of not changing the structure of the crucible when the silicon carbide single crystal is grown by adopting a physical vapor transport method by means of numerical simulation software. A preferable scheme capable of effectively improving the temperature field of the large-diameter silicon carbide single crystal growth crucible is determined through a large number of experimental verifications and simulation simulations. According to the invention, by adopting the silicon carbide powder with a proper particle size as a source material, the temperature field in the cavity and the temperature field in the material for growing the large-diameter silicon carbide single crystal can be effectively adjusted, so that the quality of the silicon carbide single crystal is improved, and the large-diameter silicon carbide single crystal is grown. The method effectively overcomes the problem that the axial temperature gradient of the growth chamber and the axial temperature gradient in the powder are coupled in the same direction when the silicon carbide crystal grows by an induction heating method, and realizes that the axial temperature gradient of the growth chamber is increased on the premise of reducing the axial temperature gradient in the powder. According to the invention, on one hand, by selecting a proper powder particle size, the temperature uniformity in the powder is improved, the crystallization at the center of the powder is weakened while the surface crystallization phenomenon of the powder is reduced, the transmission utilization efficiency of the powder is improved, the growth rate of crystals is increased, and thick crystals can grow in a short time. On the other hand, the method of the invention has low energy consumption of single crystal growth and can effectively reduce the single crystal growth cost because the heat of the side wall of the crucible is fully utilized. And the grown silicon carbide crystal is observed and analyzed, and the method does not introduce obvious defects such as inclusions, polytypes, micropipes and the like.
< Large-diameter silicon carbide Single Crystal >
In one or more embodiments, a large-diameter silicon carbide single crystal is obtained by the silicon carbide single crystal growth method as described above.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for growing a silicon carbide single crystal, comprising:
selecting silicon carbide powder with a set particle size as a raw material for growing silicon carbide single crystals, uniformly spreading the silicon carbide powder at the bottom of a heating container, and bonding silicon carbide seed crystals to the top of the heating container;
after the heating container is placed in the single crystal growth equipment, the single crystal growth equipment is sealed, and the interior of the single crystal growth equipment is vacuumized;
heating the interior of the vacuumized single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset growth pressure, and preserving heat for a preset time to grow crystals after the single crystal growth equipment is heated to a preset growth temperature; the growth pressure is related to the granularity of the silicon carbide powder, and the larger the granularity of the powder is, the smaller the growth pressure is;
and after the crystal growth is finished, cooling the interior of the single crystal growth equipment, filling carrier gas into the single crystal growth equipment to a preset cooling pressure, and naturally cooling the crystal to obtain the silicon carbide single crystal.
2. A silicon carbide single crystal growth method according to claim 1, further comprising:
the thickness of the silicon carbide single crystal produced was measured to evaluate the growth height rate of the crystal.
3. The silicon carbide single crystal growth method according to claim 1 or 2, further comprising:
observing the internal defects of the crystal, and preliminarily judging the crystallization quality of the crystal;
and performing cutting, grinding and polishing treatment on the grown crystal to obtain a silicon carbide wafer, and performing quality characterization on the wafer.
4. The method for growing a silicon carbide single crystal according to claim 1, wherein the silicon carbide powder is silicon carbide particles having a diameter of 1 to 20 mm.
5. The method for growing a silicon carbide single crystal according to claim 1, wherein the silicon carbide powder is spread to a thickness of 50 to 100mm at the bottom of the heating vessel.
6. A silicon carbide single crystal growth method according to claim 1 wherein the silicon carbide seed crystal has a diameter of at least 2 inches;
or the diameter of the silicon carbide seed crystal is 6 inches or 8 inches.
7. A silicon carbide single crystal growth method according to claim 1, wherein after the inside of the single crystal growth apparatus is vacuumized, the inside of the single crystal growth apparatus is not more than 0.01Pa;
or
The carrier gas is argon, hydrogen, nitrogen, helium or a mixture gas thereof;
or
The growth pressure of the silicon carbide single crystal is 1-50 mbar.
8. The method of growing a silicon carbide single crystal according to claim 1, wherein the growth pressure is 1 to 30mbar when the powder particle size is 10 to 20 mm; when the powder granularity is 1-10 mm, the growth pressure is 5-50 mbar.
9. A silicon carbide single crystal growth method according to claim 1, wherein heating is carried out at a predetermined rate of temperature rise to a predetermined growth temperature;
or
Heating to a set growth temperature at a preset heating rate of 300-300 ℃/h;
or
The growth temperature of the silicon carbide single crystal is 2100-2500 ℃;
or
The growth time of the silicon carbide single crystal is 30-100 h;
or
The cooling pressure is 300 to 1000mbar.
10. A silicon carbide single crystal obtained by the method for growing a silicon carbide single crystal according to any one of claims 1 to 9.
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