CN115573030B - 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
- Publication number
- CN115573030B CN115573030B CN202211312028.XA CN202211312028A CN115573030B CN 115573030 B CN115573030 B CN 115573030B CN 202211312028 A CN202211312028 A CN 202211312028A CN 115573030 B CN115573030 B CN 115573030B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- single crystal
- growth
- crystal
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 313
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 213
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 156
- 238000002109 crystal growth method Methods 0.000 title description 17
- 239000000843 powder Substances 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 57
- 238000010438 heat treatment Methods 0.000 claims abstract description 52
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000012159 carrier gas Substances 0.000 claims abstract description 11
- 238000009489 vacuum treatment Methods 0.000 claims abstract 3
- 230000007547 defect Effects 0.000 claims description 50
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 229910052786 argon Inorganic materials 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 235000012431 wafers Nutrition 0.000 claims 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000011049 filling Methods 0.000 abstract description 12
- 230000007480 spreading Effects 0.000 abstract description 9
- 238000003892 spreading Methods 0.000 abstract description 9
- 238000007789 sealing Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 59
- 229910002804 graphite Inorganic materials 0.000 description 45
- 239000010439 graphite Substances 0.000 description 45
- 239000000463 material Substances 0.000 description 32
- 238000002425 crystallisation Methods 0.000 description 15
- 230000008025 crystallization Effects 0.000 description 15
- 229910052799 carbon Inorganic materials 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 102000029749 Microtubule Human genes 0.000 description 11
- 108091022875 Microtubule Proteins 0.000 description 11
- 229910052736 halogen Inorganic materials 0.000 description 11
- 150000002367 halogens Chemical class 0.000 description 11
- 210000004688 microtubule Anatomy 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000006698 induction Effects 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 238000011068 loading method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000002500 effect on skin Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000005571 horizontal transmission Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
本发明属于晶体生长技术领域，提供了一种碳化硅单晶生长方法及碳化硅单晶。其中，该方法包括选用设定粒径的碳化硅粉料作为碳化硅单晶生长的原料，均匀摊铺在加热容器底部，将碳化硅籽晶粘接在加热容器顶部；将加热容器放入单晶生长设备后，密封单晶生长设备，对单晶生长设备内部进行抽真空处理；对抽真空处理后的单晶生长设备的内部进行加热，向单晶生长设备内充入载气至预设生长压力，当加热至设定生长温度后，保温预设时间进行晶体生长；其中生长压力与碳化硅粉料粒度有关，粉料粒度越大，生长压力越小；当晶体生长完成后，对单晶生长设备的内部进行降温，向单晶生长设备内充入载气至预设冷却压力，自然冷却晶体，得到碳化硅单晶。
The present invention belongs to the technical field of crystal growth, and provides a method for growing a silicon carbide single crystal and a silicon carbide single crystal. The method includes selecting silicon carbide powder with a set particle size as a raw material for growing a silicon carbide single crystal, evenly spreading it on the bottom of a heating container, and bonding a silicon carbide seed crystal to the top of the heating container; after placing the heating container into a single crystal growth device, sealing the single crystal growth device, and performing a vacuum treatment on the inside of the single crystal growth device; heating the inside of the single crystal growth device after the vacuum treatment, filling the single crystal growth device with a carrier gas to a preset growth pressure, and when heated to a set growth temperature, keeping the temperature for a preset time to grow the crystal; wherein the growth pressure is related to the particle size of the silicon carbide powder, and the larger the particle size of the powder, the smaller the growth pressure; after the crystal growth is completed, cooling the inside of the single crystal growth device, filling the single crystal growth device with a carrier gas to a preset cooling pressure, and naturally cooling the crystal to obtain a 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 is used as an important third-generation semiconductor material at present, has excellent properties which are not possessed by traditional semiconductor materials such as Si, gaAs and the like, such as high heat conductivity, large forbidden band width, high breakdown field strength, high electron saturation rate, high temperature resistance, radiation resistance, corrosion resistance and the like, so that the device can normally operate in a severe environment, and has important application in the fields of modern power electronics, microwave radio frequency, photoelectrons 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 transmission method. The method for crystal growth mainly comprises four stages, namely, vacuumizing a chamber, preheating, growing at high temperature, cooling and the like. When the method is used for growing the silicon carbide crystal, silicon carbide powder serving as a raw material is required to be placed at the bottom of a graphite crucible, and a silicon carbide seed crystal sheet serving as a seed crystal is 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, silicon carbide powder at the bottom of the crucible is sublimated and decomposed into chemical components such as Si, si 2C、SiC2 and the like, and the silicon carbide single crystal is formed by crystallization from the bottom of the crucible to a seed crystal at the top of the crucible under the action of a temperature gradient. The temperature field distribution in the crucible has important influence on sublimation, transmission and recrystallization of silicon carbide powder, and is a core factor influencing the growth of silicon carbide single crystals.
The most common heating method for physical vapor transport is induction heating. The induction heating method is to generate a magnetic field which is changed continuously by a high-frequency current which is changed continuously in the direction of a coil, and then to 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 the large-diameter silicon carbide single crystal grows, the radial temperature difference between the crucible wall and the center of the crucible is increased along with the increase of the diameter of the graphite crucible, a larger radial temperature gradient is generated in the silicon carbide powder, and after the powder on two sides of the crucible is sublimated and decomposed, a part of the powder is transported into a growth cavity, and a larger part of the powder is transported to the position of the center of the material with lower temperature and crystallized, so that the utilization efficiency of the powder is influenced, and the crystal growth rate is reduced. The radial and axial temperature gradients in the material can be reduced by changing the relative positions of the crucible and the induction coil, but the axial temperature gradient in the growth cavity is increased and the radial temperature gradient at the growth front is reduced, which are unfavorable for single crystal growth. Therefore, there is a need for a method of improving the uniformity of the internal temperature distribution of the powder without decreasing the axial temperature gradient in the growth chamber and without increasing the radial temperature gradient before growth.
Chinese patent document CN 115044969A discloses a growth apparatus for improving the efficiency of raw material transport when growing silicon carbide crystals. In the invention, a graphite cylinder is placed in a crystal growth crucible along the axis of the crucible, and a graphite plate is placed in the graphite cylinder to divide the charging area in the crucible into three parts. The purpose of reducing radial temperature gradient in the raw material is achieved by utilizing the advantage of high heat conductivity of the graphite cylinder and the graphite plate. Simultaneously, the graphite cylinder and the graphite plate can prevent the outside raw materials from being transmitted to the center, so that powder materials can be forced to be transmitted to seed crystals positioned at the upper part of the crucible, and the horizontal transmission of silicon carbide powder materials can be restrained, thereby improving the powder material transmission efficiency and increasing the growth rate of silicon carbide crystals. The method can reduce the radial temperature gradient in the powder, but the crucible assembly is required to be changed, and the process is complex. And there is a strict limitation on the charge height when the method is used to increase the crystal growth rate. The loading height is too high, if the high temperature area is positioned at an upper position, the lower raw material transportation is not facilitated, and if the high temperature area is positioned at a lower position, the upper part of the powder is crystallized, and the raw material transportation is blocked. Therefore, the loading amount in the method cannot be too high, namely, on the premise of not changing the loading 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 the growth rate of silicon carbide crystals prepared by PVT method. According to the invention, silicon carbide single crystal growth is carried out by using powder with different particle sizes, and large-size powder can provide enough particle gaps to promote gas phase component transportation, and small-size powder has enough powder activity to generate enough reaction gas phase, so that the growth rate of crystals is improved (to 105 mu m/h) in both aspects. However, the silicon carbide powder used in the method has generally smaller particle size (10-500 μm), so that the powder is accelerated to decompose, silicon components in a growth system are increased, the inner wall of a graphite crucible is easily corroded, and the corroded graphite crucible can provide a large amount of carbon particles in a growth cavity, so that a large amount of carbon inclusion is generated in crystals, and the quality of the grown crystals is affected. In addition, the invention needs to mix the powder materials with different particle sizes according to different mass ratios, has relatively complex process and is not suitable for industrialized popularization.
In summary, the inventors have found that the current silicon carbide crystal growth methods require a change in crucible structure, are relatively complex in process, are not suitable for industrial popularization, and are not suitable for growth of large-diameter (e.g., 6 inches in diameter and above) 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 is compatible with the existing single crystal growth device without changing the structure of a heating container, is simple and practical, and is beneficial to popularization.
In order to achieve the above purpose, the present 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 method of growing a silicon carbide single crystal includes:
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 at the top of the heating container;
after the heating container is put into 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 single crystal growth equipment subjected to the vacuumizing treatment, 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, wherein the growth pressure is related to the granularity of silicon carbide powder, and the larger the granularity of the powder is, the smaller the growth pressure is;
and after the crystal growth is completed, 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 one embodiment, the silicon carbide single crystal growth method further comprises:
the thickness of the prepared silicon carbide single crystal was measured, and the growth height rate of the crystal was evaluated.
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 vernier calipers, screw micrometers or height gauges and the like.
As one embodiment, the silicon carbide single crystal growth method further comprises:
Observing the internal defect of the crystal, and primarily judging the crystallization quality of the crystal;
And cutting, grinding and polishing the grown crystal to obtain a silicon carbide wafer, and carrying out quality characterization on the wafer.
Wherein, the defects inside the crystal are whether the defects such as wrappage, polytype, microtubule and the like exist inside the crystal. These can be observed by irradiating the crystal with a strong light source, a halogen lamp, or the like.
As one embodiment, the quality characterization of the wafer comprises characterizing the crystal quality using an X-ray diffractometer and investigating defects in the crystal (e.g., micropipes, inclusions, dislocations, etc. in the crystal) using a surface defect detector.
As one embodiment, the silicon carbide powder is silicon carbide particles with the diameter of 1-20 mm.
As an implementation mode, the paving thickness of the silicon carbide powder at the bottom of the heating container is 50-100 mm.
As one embodiment, the silicon carbide seed crystal has a diameter of at least 2 inches.
As one embodiment, the silicon carbide seed crystal has a diameter of 6 inches or 8 inches.
As one embodiment, the interior of the single crystal growth apparatus is not more than 0.01Pa after the interior of the single crystal growth apparatus is subjected to the vacuum-pumping treatment.
As one embodiment, the carrier gas is argon, hydrogen, nitrogen, helium or a mixture thereof.
As one embodiment, the silicon carbide single crystal has a growth pressure of 1 to 50 mbar.
As an implementation mode, when the granularity of the powder is 10-20 mm, the growth pressure is 1-30 mbar, and when the granularity of the powder is 1-10 mm, the growth pressure is 5-50 mbar.
As one embodiment, heating to a set growth temperature is performed at a preset ramp rate.
As one implementation mode, the temperature rising speed is 300-700 ℃ per hour.
As one embodiment, the growth temperature of the silicon carbide single crystal is 2100 to 2500 ℃.
As one embodiment, the silicon carbide single crystal has a growth time of 30 to 100 hours.
As an embodiment, the cooling pressure is 300 to 1000 mbar.
In a second aspect of the present invention, there is provided a silicon carbide single crystal.
In one or more embodiments, a silicon carbide single crystal is obtained using 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 growth method of the silicon carbide single crystal, 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 temperature of the inner edge of the powder is inconsistent with the temperature of the inner center of the powder due to the skin effect of current in induction heating is solved to a certain extent, the radial temperature gradient and the axial temperature gradient in the powder are reduced, the axial temperature gradient in a growth cavity is improved, the problem that the powder in a crucible is recrystallized near the inner center of the powder and on the surface of the powder is inhibited, the utilization rate of the 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 at the same time, and the productivity of the silicon carbide single crystal is improved.
(2) According to the silicon carbide single crystal growth method, the heat of the crucible wall is effectively transmitted to the center of the powder, so that the temperature uniformity in the large-diameter silicon carbide single crystal growth powder is improved, the heating efficiency of a heating system is improved, the energy consumption for growing the silicon carbide single crystal is effectively reduced, and the single crystal growth cost is reduced.
(3) According to the silicon carbide single crystal growth method, the corresponding relation between the powder granularity and the growth pressure is fully utilized, and the shaft ladder assembled in a heat preservation manner can be reduced as much as possible while the single crystal growth rate is ensured, so that the crystal can grow in a state close to equilibrium, the quality of the grown crystal is better, and particularly, secondary phase inclusions such as silicon drops and carbon wrappage in the crystal can be remarkably reduced.
(4) The method of the invention effectively improves the uniformity of the temperature field in the material by limiting the charging height of the crucible while ensuring the growth thickness of the single crystal, and reduces the axial temperature gradient in the powder and the radial temperature gradient on the surface of the powder to be less than 0.5 ℃ per 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 large-diameter (6 inches or more) silicon carbide single crystals, and is also suitable for growing single crystals of 6 inches or less.
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 included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain 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 Wen Changtu in a graphite crucible for growing a silicon carbide single crystal obtained in example 1 in the present invention.
FIG. 3 is a photograph of a silicon carbide crystal of thickness 37 mm and diameter 150 mm grown in example 1 of the present invention.
FIG. 4 is a view showing the interior Wen Changtu of a graphite crucible for growing a silicon carbide single crystal obtained in comparative example 1 in the present invention.
Wherein 1 is an induction heating coil, 2 is a graphite crucible, 3 is a thermal insulation material, 4 is a silicon carbide seed crystal, 5 is a grown silicon carbide single crystal, and 6 is silicon carbide powder. T1 is the center temperature of the silicon carbide seed crystal, T2 is the edge temperature of the silicon carbide seed crystal, T3 is the center temperature of the surface of the silicon carbide powder, T4 is the edge temperature of the surface of the silicon carbide powder, T5 is the center temperature of the bottom of the silicon carbide powder, and T6 is the edge temperature of the bottom of the silicon carbide powder. The radial temperature gradient of the seed crystal surface 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 powder surface is (T4-T3)/R. Wherein R is the radius of the silicon carbide seed crystal, L is the length of a growth cavity of the crucible, H is the paving thickness of the silicon carbide powder on the bottom of the graphite crucible, and R is the radius of the paved surface of the silicon carbide powder.
Detailed Description
The invention will be further described with reference to the drawings and examples.
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. 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 present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
Term interpretation:
The radial temperature gradient before growth refers to the temperature difference between the edge of the silicon carbide seed crystal and the center of the silicon carbide seed crystal in unit length. In general, the larger the radial temperature gradient before growth, the more convex the grown crystal shape, and the greater the stress in the crystal.
The axial temperature gradient of the temperature in the growth cavity refers to the temperature difference between the center of the surface of the silicon carbide powder and the center of the silicon carbide seed crystal in unit length, and represents the driving force of single crystal growth. The larger the temperature axial temperature gradient in the growth chamber, the faster the single crystal growth rate.
The inner diameter temperature gradient of the material 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 in unit length. The larger the radial temperature gradient of the material, the easier the edge powder material is to agglomerate towards the center, and the less favorable the growth component is to be transferred into the growth cavity. From the viewpoint of growing crystals, the smaller the radial temperature gradient in the material, the better.
The in-material axial temperature gradient 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 in unit length. The larger the in-material axial temperature gradient is, the easier the material inner component released by sublimation of the material is crystallized on the surface of the material, and the more unfavorable the transmission of the growth component into the growth cavity is. From the perspective of growing crystals, the smaller the in-material axial temperature gradient, the better.
Large diameter silicon carbide single crystal refers to a diameter of 6 inches or more.
< Method for growing silicon carbide Single Crystal >
In one or more embodiments, a method of growing a silicon carbide single crystal is provided, comprising:
step1, 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 at the top of the heating container.
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.
And 2, after the heating container is placed into the single crystal growth equipment, sealing the single crystal growth equipment, and vacuumizing the interior of the single crystal growth equipment.
Wherein, after the vacuum pumping treatment is carried out on the inside of the single crystal growth equipment, the inside 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 3, heating the interior of the single crystal growth equipment subjected to the vacuumizing treatment, 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, wherein the growth pressure is related to the granularity of 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 granularity of the powder is 10-20 mm, the growth pressure is 1-30 mbar, and when the granularity of the powder is 1-10 mm, the growth pressure is 5-50 mbar.
Specifically, heating to a set growth temperature at a preset heating rate. For example, the temperature rising speed is 300-700 ℃ per hour.
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, cooling the interior of the single crystal growth equipment after the crystal growth is completed, 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 300-1000 mbar.
In some other embodiments, the silicon carbide single crystal growth method further comprises:
the thickness of the prepared silicon carbide single crystal was measured, and the growth height rate of the crystal was evaluated.
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 vernier calipers, screw micrometers or height gauges and the like.
In some other embodiments, the silicon carbide single crystal growth method further comprises:
Observing the internal defect of the crystal, and primarily judging the crystallization quality of the crystal;
And cutting, grinding and polishing the grown crystal to obtain a silicon carbide wafer, and carrying out quality characterization on the wafer.
Wherein, the defects inside the crystal are whether the defects such as wrappage, polytype, microtubule and the like exist inside the crystal. These can be observed by irradiating the crystal with a strong light source, a halogen lamp, or the like.
As one embodiment, the quality characterization of the wafer comprises characterizing the crystal quality using an X-ray diffractometer and investigating defects in the crystal (e.g., micropipes, inclusions, dislocations, etc. in the crystal) using a surface defect detector.
In the following, a graphite crucible is used as a heating container, and a single crystal growth apparatus using a single crystal growth furnace is used as an example to give corresponding specific examples.
It should be noted that, the heating container and the single crystal growing furnace are both existing structures, and those skilled in the art can specifically select corresponding devices or apparatuses according to actual situation requirements.
The silicon carbide single crystal growth apparatus of the present embodiment is shown in fig. 1.
The method of the present invention is suitable for growing large-diameter (6 inches or more) silicon carbide single crystals, and is also suitable for growing single crystals 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, namely selecting silicon carbide powder with the grain diameter 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, spreading the silicon carbide powder with the thickness of 100mm, placing 4H-SiC seed crystals with the diameter of 6 inches at the top of the graphite crucible,
(2) And vacuumizing, namely placing the graphite crucible into a single crystal growth furnace, and vacuumizing to 0.01Pa by adopting a mechanical pump.
(3) And (3) heating and growing, namely filling argon into the furnace until the pressure is 50 mbar, heating the graphite crucible, heating to 2100 ℃ at the speed of 300 ℃ per hour, and preserving heat for 100 hours. The temperature field in a graphite crucible for growing silicon carbide single crystals is shown in fig. 2.
(4) And cooling, namely reducing the heating power of the system, cooling, and filling argon to the pressure of 1000mbar for natural cooling to obtain the silicon carbide single crystal.
(5) And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is found to be all 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 batch, as shown in figure 4.
(6) As shown in FIG. 3, the silicon carbide single crystal was measured with a vernier caliper to have a thickness of 36.72mm and a crystal growth height rate of about 367 μm/h, and defects such as micropipes and inclusions in the crystal were not observed with a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test the swing curve of the surface of the wafer (004), the half-peak width is only 20 arc seconds, the crystal crystallization quality is higher, a surface defect detector is adopted to research defects such as microtubules, wrappage, dislocation and the like in the crystal, and the result shows that the density of the microtubules in the wafer is zero, no secondary phase defects such as silicon drops, carbon wrappage and the like exist, and the total dislocation density is 3200cm -2. The method has the advantages of high growth rate, thick crystal and high quality of the 6-inch silicon carbide single crystal.
Example 2
Unlike example 1, the following is:
The embodiment provides a silicon carbide single crystal growth method, which specifically comprises the following steps:
(1) Charging, namely selecting silicon carbide powder with the grain diameter of 10mm as a raw material for growing silicon carbide single crystals, uniformly spreading the silicon carbide powder at the bottom of a graphite crucible, spreading the silicon carbide powder with the thickness of 80mm, placing 4H-SiC seed crystals with the diameter of 8 inches at the top of the graphite crucible,
(2) And vacuumizing, namely placing the graphite crucible into a single crystal growth furnace, and vacuumizing to 0.001Pa by adopting a molecular pump.
(3) And (3) heating and growing, namely filling a mixed gas of Ar and N 2 into a furnace, heating the graphite crucible at a speed of 700 ℃ per hour to 2500 ℃ at a flow ratio of 20:1 to a pressure of 5 mbar, and preserving heat for 30 hours.
(4) And cooling, namely reducing the heating power of the system, cooling, and filling argon to the pressure of 300mbar for natural cooling to obtain the silicon carbide single crystal.
(5) And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is found to be all 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) The test characterization shows that the thickness of the silicon carbide single crystal is 15.6mm by adopting a vernier caliper, the height rate of crystal growth is about 520 mu m/h, and defects such as microtubes, wrappers and the like in the crystal are not observed by adopting a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test the swing curve of the surface of the wafer (004), the half-peak width is only 28 arc seconds, the crystal crystallization quality is higher, a surface defect detector is adopted to research defects such as microtubules, wrappage, dislocation and the like in the crystal, and the result shows that the density of the microtubules in the wafer is zero, no secondary phase defects such as silicon drops, carbon wrappage and the like 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
Unlike example 1, the following is:
The embodiment provides a silicon carbide single crystal growth method, which specifically comprises the following steps:
(1) Charging, namely selecting silicon carbide powder with the grain diameter of 20 mm as a raw material for growing silicon carbide single crystals, uniformly spreading the silicon carbide powder at the bottom of a graphite crucible, spreading the silicon carbide powder with the thickness of 50mm, placing 4H-SiC seed crystals with the diameter of 8 inches at the top of the graphite crucible,
(2) And vacuumizing, namely placing the graphite crucible into a single crystal growth furnace, and vacuumizing to 0.001Pa by adopting a molecular pump.
(3) And (3) heating and growing, namely filling a mixed gas of Ar and H 2 into a furnace, heating the graphite crucible at a speed of 500 ℃ per hour to 2500 ℃ at a flow ratio of 20:1 to a pressure of 1:1 mbar, and preserving heat for 50 hours.
(4) And cooling, namely reducing the heating power of the system, cooling, and filling argon to the pressure of 800mbar for natural cooling to obtain the silicon carbide single crystal.
(5) And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is found to be all 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) The test characterization shows that the thickness of the silicon carbide single crystal is 25.0mm by adopting a vernier caliper, the height rate of crystal growth is about 500 mu m/h, and defects such as microtubes, wrappers and the like in the crystal are not observed by adopting a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test the swing curve of the surface of the wafer (004), the half-peak width is only 26 arc seconds, the crystal crystallization quality is higher, a surface defect detector is adopted to research defects such as micropipes, wrappage, dislocation and the like in the crystal, and the result shows that the micropipe density in the wafer is zero, no secondary phase defects such as silicon drops, carbon wrappage and the like exist, and the total dislocation density is 3830 cm -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, silicon carbide powder having a grain diameter of 0.3mm was used to grow a large-diameter silicon carbide single crystal, and the remaining growth conditions were exactly the same as in example 1. And taking out the graphite crucible in the growth furnace after the growth is finished to obtain silicon carbide single crystals, and finding that crystallization occurs in the silicon carbide powder and the middle part of the material surface. Indicating that the axial temperature gradient and the radial temperature gradient in the material are larger. In addition, graphite crucibles were found to be severely corroded. The thickness of the silicon carbide single crystal is 10.2mm by adopting a vernier caliper to test, the growth height rate of the crystal is about 102 mu m/h, and defects such as microtubes, wrappage and the like in the crystal are observed by adopting a halogen lamp. The method is characterized in that the crystal is cut, ground and polished, an X-ray diffractometer is adopted to test the swing curve of the wafer (004) surface, the half-peak width is 82 arc seconds, the crystal crystallization quality is poor, a surface defect detector is adopted to research defects such as micropipes, wrappage and dislocation in the crystal, the result shows that the micropipe density in the wafer is 0.33 cm -2, more carbon wrappage defects exist, a large number of micropipe and dislocation defects are induced in the crystal by the carbon wrappage, the micropipe density in the wafer is 12.5 cm -2, the total dislocation density exceeds 10000cm -2, and the method cannot be used for preparing related devices.
Comparative example 2
In this example, silicon carbide powder having a grain diameter of 30mm was used to grow a large-diameter silicon carbide single crystal, and the remaining growth conditions were exactly the same as in example 2. And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is found to be all 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 3.3mm, the growth height rate of the crystal is about 110 mu m/h, and defects such as microtubes, wrappage and the like in the crystal are observed by adopting a halogen lamp. The crystal is cut, ground and polished, the swing curve of the surface of the wafer (004) is tested by an X-ray diffractometer, the half-peak width is 62 arc seconds, the crystal crystallization quality is poor, the defects of microtubules, wrappage, dislocation and the like in the crystal are researched by a surface defect detector, and the result shows that the density of the microtubules in the wafer is zero, and secondary phase defects such as silicon drops and carbon wrappage are avoided, but the total dislocation density in the crystal is 8580cm -2. The method has the advantages that the silicon carbide crystal prepared by the method has the problems of disqualification of diameter, slow crystal growth rate, high dislocation density and the like due to serious decomposition of the edge of the seed crystal.
Comparative example 3
In this example, the pressure of argon gas introduced into the furnace during the heating growth was 1mbar, and the other growth conditions were exactly the same as in example 1. And (3) opening the furnace, namely taking out the graphite crucible from the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is found to be all 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 48.57mm by adopting a vernier caliper to test, the growth height rate of the crystal is about 486 mu m/h, and defects such as microtubes, wrappage and the like in the crystal are observed by adopting a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test the swing curve of the wafer (004) surface, the half-peak width is 85 arc seconds, the crystal crystallization quality is poor, a surface defect detector is adopted to research the defects of microtubes, wrappage, dislocation and the like in the crystal, the result shows that the density of the microtubes in the wafer is 0.41 cm -2, more carbon wrappage defects exist, a large number of microtubes and dislocation defects are induced in the crystal by the carbon wrappage, a large-area mist inclusion exists in the wafer, and the total dislocation density exceeds 10000cm -2.
Comparative example 4
In the embodiment, the paving thickness of the silicon carbide powder on the bottom of the graphite crucible is 150mm, and the rest of growth conditions are completely the same as those in the embodiment 1. And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is in a block shape, and crystallization occurs in the powder and on the surface of the powder. Indicating that the temperature field in the material is unevenly distributed. The thickness of the silicon carbide single crystal is 15.2mm when being tested by a vernier caliper, the growth height rate of the crystal is about 152 mu m/h, and defects such as microtubes, wrappage and the like in the crystal are observed by adopting a halogen lamp. The crystal is cut, ground and polished, an X-ray diffractometer is adopted to test the swing curve of the surface of the wafer (004), the half-peak width is 82 arc seconds, the crystallization quality of the crystal is poor, a surface defect detector is adopted to research defects such as microtubules, wrappage, dislocation and the like in the crystal, and the result shows that the density of the microtubules in the wafer is zero, and secondary phase defects such as silicon drops, carbon wrappage and the like are avoided, but the crystal does not reach the standard due to the decomposition of the edge of the seed crystal. The method solves the problems of unqualified diameter, slow crystal growth rate and the like of the silicon carbide crystal prepared by the method due to serious decomposition of the edge of the seed crystal.
Comparative example 5
In the embodiment, the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 30mm, and the rest of growth conditions are completely the same as those in the embodiment 1. And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is in a bulk state, and the powder is not crystallized at all in the powder or on the surface of the powder, but the powder allowance is less, and the surface of the crystal is decomposed and carbonized. The temperature field in the material is uniformly distributed, but the material loading is insufficient. The thickness of the silicon carbide single crystal is 12.36mm by adopting a vernier caliper to test, the growth height rate of the crystal is about 124 mu m/h, and defects such as microtubes, wrappage and the like in the crystal are observed by adopting a halogen lamp. The crystal is cut, ground and polished, the swing curve of the surface of the wafer (004) is tested by an X-ray diffractometer, the half-peak width is 29 arc seconds, and defects such as microtubes, wrappage, dislocation and the like in the crystal are researched by a surface defect detector, so that the result shows that the density of the microtubes in the wafer is zero, and secondary phase defects such as silicon drops, carbon wrappage and the like are avoided. The method has the problem that thicker crystals cannot be grown due to small loading.
Comparative example 6
In this example, the pressure of argon gas introduced into the furnace during the heating growth was 100mbar, and the other growth conditions were exactly the same as in example 1. And (3) opening the furnace, namely taking out the graphite crucible in the growth furnace to obtain silicon carbide single crystals, wherein the silicon carbide powder is found to be all 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 1.34mm, the growth height rate of the crystal is about 134 mu m/h, and defects such as microtubes, wrappage and the like in the crystal are observed by adopting a halogen lamp. The crystal is cut, ground and polished, the swing curve of the surface of the wafer (004) is tested by an X-ray diffractometer, the half-peak width is 69 arc seconds, the crystallization quality of the crystal is poor, the defects of microtubes, wrappage, dislocation and the like in the crystal are researched by a surface defect detector, and the result shows that the density of the microtubes in the wafer is zero, and secondary phase defects such as silicon drops and carbon wrappage are avoided, but the total dislocation density in the crystal is 9160cm -2. The method has the advantages that the silicon carbide crystal prepared by the method has the problems of disqualification of diameter, slow crystal growth rate, high dislocation density and the like due to serious decomposition of the edge of the seed crystal. Table 1 shows the temperature gradients 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 when the silicon carbide monocrystal is grown by adopting a physical vapor transmission method by means of numerical simulation software, 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 crucible structure. A great number of experimental verification and simulation experiments prove that a preferable scheme capable of effectively improving the temperature field of the large-diameter silicon carbide single crystal growth crucible is determined. According to the invention, the silicon carbide powder with proper particle size is used as a source material, so that the temperature field in a growth cavity and the temperature field in the material of the large-diameter silicon carbide single crystal can be effectively regulated, and the quality of the silicon carbide single crystal is improved, and the large-diameter silicon carbide single crystal is grown. The method effectively solves the difficulty of the same-direction coupling of the axial temperature gradient of the growth chamber and the axial temperature gradient inside the powder, which is faced by growing the silicon carbide crystal by the induction heating method, and increases the axial temperature gradient of the growth chamber on the premise of reducing the axial temperature gradient inside the powder. According to the invention, on one hand, by selecting proper powder particle size, the temperature uniformity in the powder is improved, the crystallization phenomenon on the surface of the powder is reduced, the crystallization in the center of the powder is weakened, the transmission utilization efficiency of the powder is improved, the growth rate of crystals is increased, and thick crystals can be grown in a short time. On the other hand, the method has low energy consumption for 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. The grown silicon carbide crystal is observed and analyzed, and the method does not introduce obvious defects such as wrapping, polytype, microtubule and the like.
< Large diameter silicon carbide Single Crystal >
In one or more embodiments, a large diameter silicon carbide single crystal is obtained using the silicon carbide single crystal growth method as described above.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211312028.XA CN115573030B (en) | 2022-10-25 | 2022-10-25 | Silicon carbide single crystal growth method and silicon carbide single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211312028.XA CN115573030B (en) | 2022-10-25 | 2022-10-25 | Silicon carbide single crystal growth method and silicon carbide single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115573030A CN115573030A (en) | 2023-01-06 |
| CN115573030B true CN115573030B (en) | 2025-03-07 |
Family
ID=84586659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211312028.XA Active CN115573030B (en) | 2022-10-25 | 2022-10-25 | Silicon carbide single crystal growth method and silicon carbide single crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115573030B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2025030917A (en) * | 2023-08-24 | 2025-03-07 | 株式会社レゾナック | SiC substrate and SiC epitaxial wafer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190323A (en) * | 2017-06-06 | 2017-09-22 | 宝鸡文理学院 | A kind of method for growing low defect single-crystal silicon carbide |
| CN113403688A (en) * | 2021-06-22 | 2021-09-17 | 山东天岳先进科技股份有限公司 | Seed crystal and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8410488B2 (en) * | 2006-09-14 | 2013-04-02 | Cree, Inc. | Micropipe-free silicon carbide and related method of manufacture |
| KR102331308B1 (en) * | 2018-10-16 | 2021-11-24 | 에스아이씨씨 컴퍼니 리미티드 | Large size, high-purity silicon carbide single crystal, substrate, and manufacturing method and device for the same |
| CN113026095A (en) * | 2021-03-15 | 2021-06-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for improving growth rate of silicon carbide crystal prepared by PVT method |
| CN115044969A (en) * | 2022-07-21 | 2022-09-13 | 广州南砂晶圆半导体技术有限公司 | A device for improving the transfer efficiency of raw materials during the growth of silicon carbide crystals |
-
2022
- 2022-10-25 CN CN202211312028.XA patent/CN115573030B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190323A (en) * | 2017-06-06 | 2017-09-22 | 宝鸡文理学院 | A kind of method for growing low defect single-crystal silicon carbide |
| CN113403688A (en) * | 2021-06-22 | 2021-09-17 | 山东天岳先进科技股份有限公司 | Seed crystal and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115573030A (en) | 2023-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11421343B2 (en) | Method and apparatus for producing bulk silicon carbide using a silicon carbide seed | |
| US11591714B2 (en) | Apparatus for producing bulk silicon carbide | |
| EP2336399B1 (en) | Method of producing high quality silicon carbide single crystal in a seeded growth system | |
| US11505876B2 (en) | Method for producing bulk silicon carbide | |
| TWI723579B (en) | Large-size and high-purity silicon carbide single crystal, base material, and preparation method and device for preparation thereof | |
| TWI774929B (en) | Manufacturing method of silicon carbide single crystal | |
| US11434582B2 (en) | Method for producing bulk silicon carbide by sublimation of a silicon carbide precursor prepared from silicon and carbon particles or particulate silicon carbide | |
| CN108138359A (en) | Sic single crystal ingot | |
| CN110331438B (en) | Method for inhibiting defect generation of carbon inclusion in growth of conductive silicon carbide crystal | |
| CN214572367U (en) | Silicon carbide crystal growing device | |
| CN104947182A (en) | Method for rapidly growing large-size high-purity semi-insulating silicon carbide single crystal | |
| CN106968018A (en) | A kind of growing method for the single-crystal silicon carbide material that germanium nitrogen is co-doped with | |
| CN108468089B (en) | Process for high-efficiency high-temperature curing of silicon carbide seed crystal | |
| CN115573030B (en) | Silicon carbide single crystal growth method and silicon carbide single crystal | |
| CN114262936B (en) | Silicon carbide single crystal growth method and crack closure growth method | |
| CN116163009A (en) | Method for growing silicon carbide single crystal | |
| CN114182357A (en) | Method for regrowing silicon carbide single crystal by using broken crystal grains of silicon carbide crystal | |
| TWI703242B (en) | Semi-insulating silicon carbide single crystal doped with a small amount of vanadium, substrate and preparation method | |
| CN211420368U (en) | Apparatus for growing large diameter silicon carbide crystals | |
| Wang et al. | Study on carbon particle inclusions during 4H-SiC growth by using physical vapor transport system | |
| US9512542B2 (en) | Bulk silicon carbide having low defect density | |
| CN118127615A (en) | Method for filling silicon carbide crystal growth raw material | |
| CN113026093B (en) | Semi-insulating silicon carbide wafer with uniform resistivity and preparation method thereof | |
| CN116145243A (en) | A crucible and method for p-type SiC single crystal growth | |
| CN115573029A (en) | Large-size silicon carbide growth device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |