CN113026095A - Method for improving growth rate of silicon carbide crystal prepared by PVT method - Google Patents
Method for improving growth rate of silicon carbide crystal prepared by PVT method Download PDFInfo
- Publication number
- CN113026095A CN113026095A CN202110276280.9A CN202110276280A CN113026095A CN 113026095 A CN113026095 A CN 113026095A CN 202110276280 A CN202110276280 A CN 202110276280A CN 113026095 A CN113026095 A CN 113026095A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- carbide powder
- graphite crucible
- growth rate
- crystal growth
- 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.)
- Pending
Links
Images
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
The invention relates to a method for improving the growth rate of silicon carbide crystals prepared by a PVT method, belonging to the technical field of silicon carbide crystal preparation. In order to solve the problem of slow growth rate of silicon carbide crystals prepared by the conventional PVT method, the invention provides a method for improving the growth rate of silicon carbide crystals prepared by the PVT method, silicon carbide powder materials with different particle sizes are mixed to prepare silicon carbide powder, the silicon carbide powder materials are heated to 400-800 ℃ under a vacuum condition and kept for 2 hours, argon is filled, the heating is continued to the crystal growth temperature to start crystal growth, and the natural cooling is carried out after the crystal growth is completed, so that the silicon carbide crystals are obtained. According to the invention, silicon carbide powders with different particle sizes are mixed according to different proportions and then subjected to PVT method silicon carbide crystal growth, large-particle silicon carbide powders provide enough particle gaps to promote gas phase material transportation, and small-particle silicon carbide powders provide enough active surfaces to generate enough reaction gas phases, so that the two aspects are simultaneously improved, and the crystal growth rate is remarkably improved.
Description
Technical Field
The invention belongs to the technical field of silicon carbide crystal preparation, and particularly relates to a method for improving the growth rate of silicon carbide crystals prepared by a PVT (physical vapor transport) method.
Background
The silicon carbide serving as a third-generation semiconductor material has the characteristics of wide forbidden band, high breakdown field strength, high thermal conductivity and the like, and can be applied to the fields of new energy automobiles, photovoltaic inverters, charging piles and the like to achieve the aims of reducing power consumption, improving switching frequency, reducing overall cost and the like.
Since silicon carbide is decomposed before being heated to a melting point under normal pressure, a method similar to the growth of silicon crystal cannot be directly used. At present, the growth methods of the large-size silicon carbide crystal mainly comprise two methods: one is to add a flux to form a melt containing silicon carbide and grow crystals using the melt. The other is the PVT method. Since the first method is accompanied by a large number of crystal defects due to the introduction of a cosolvent into the crystals to be produced, the method currently used for mass production is the second PVT method.
The PVT process for growing silicon carbide crystals is very slow compared to the czochralski method used for crystalline silicon growth and the kyropoulos method used for sapphire growth, and fewer crystals grow per furnace. In order to increase the growth rate of silicon carbide crystals, researchers have proposed various improvement approaches, such as increasing the temperature of the frit region to promote the decomposition and transportation of the frit, adding a doping gas to promote nucleation, introducing an additional carbon source and a silicon source, and the like. However, these methods have their own drawbacks, such as increased lateral temperature differential and increased stress, and the introduction of dopant gases causes impurity defects in the crystal. In the same way, because the reaction system structure or parameters are changed greatly in these methods, it is necessary to search for conditions for growing high quality crystals with a great deal of effort.
Disclosure of Invention
In order to solve the problem of slow growth rate of silicon carbide crystals prepared by the existing PVT method, the invention provides a method for improving the growth rate of silicon carbide crystals prepared by the PVT method.
The technical scheme of the invention is as follows:
a method for improving growth rate of silicon carbide crystals prepared by a PVT method comprises the steps of mixing silicon carbide powder with different particle sizes to prepare silicon carbide powder, putting the silicon carbide powder into a graphite crucible, bonding a silicon carbide seed crystal to a graphite crucible cover, putting the graphite crucible into a crystal growth furnace, heating to 400-800 ℃ under a vacuum condition, keeping for 2 hours, filling argon gas, continuing to heat to a crystal growth temperature to start crystal growth, naturally cooling to 500 ℃ after crystal growth is completed, filling argon gas to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystals.
Furthermore, the silicon carbide powder with different particle sizes is prepared by mixing silicon carbide powder with the particle size of 10-200 mu m and silicon carbide powder with the particle size of 50-500 mu m.
Furthermore, the silicon carbide powder with the particle size of 10-200 mu m accounts for 5-60% of the total weight of the powder.
Furthermore, the silicon carbide powder with the particle size of 10-200 μm accounts for 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55% or 60% of the total weight of the powder.
Further, the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 50-150 mm.
Further, the vacuum condition is that the interior of the graphite crucible is vacuumized to 10 DEG-4torr。
Further, the pressure of the argon gas is 0.1-1 atm.
Further, the heating rate is 200-800 ℃/h.
Further, the crystal growth temperature is 1800-2300 ℃ of the central temperature of the upper cover of the crucible.
The invention has the beneficial effects that:
according to the invention, silicon carbide powders with different particle sizes are mixed according to different proportions and then subjected to PVT method silicon carbide crystal growth, large-particle silicon carbide powders provide enough particle gaps to promote gas phase material transportation, and small-particle silicon carbide powders provide enough active surfaces to generate enough reaction gas phases, so that the two aspects are simultaneously improved, and the crystal growth rate is remarkably improved.
The method improves the crystal growth speed by improving the powder decomposition rate, is simple, has small change to a growth system, further has small workload of exploring new process parameters, and can be combined with different heating modes, different thermal field modes and different heating modes of different growth process modes. In addition, the invention does not introduce additional additives and can not cause the generation of defects.
Drawings
FIG. 1 is a graph showing the decomposition ratio of silicon carbide powder consisting of silicon carbide powders having different particle diameters according to the present invention as a function of time.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention. The process equipment or apparatus not specifically mentioned in the following examples are conventional in the art, and if not specifically mentioned, the raw materials and the like used in the examples of the present invention are commercially available; unless otherwise specified, the technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the grain size of 50 microns and silicon carbide powder with the grain size of 100 microns, the obtained silicon carbide powder is put into a graphite crucible, and the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG-4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
The porosity and the particle size of the silicon carbide powder have important influence on the growth speed of the silicon carbide crystal. When the powder particles are smaller, the stacking among the particles is denser, the gaps among the powder are smaller, gas phase substances generated by the decomposition of the silicon carbide are not smoothly transported, and the crystal growth speed is slowed down. On the contrary, when the particle size is larger, the specific surface area of the silicon carbide particles is smaller, the decomposition reaction activity is poorer, the gas phase generation rate is slower, and the crystal growth speed is also slowed down.
The embodiment utilizes different particle size silicon carbide powders to carry out PVT method silicon carbide crystal growth after mixing according to different proportions, and the silicon carbide powder of large granule provides sufficient granule clearance and promotes gaseous phase material and transport, and the silicon carbide powder of small granule provides sufficient active surface and produces sufficient reaction gaseous phase for two aspects obtain promoting simultaneously, are showing and have promoted crystal growth rate.
Example 2
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 5% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 3
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 10% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4torr, heating to 700 deg.C at a heating rate of 800 deg.C/h and holding for 2h, filling argon to 0.1atm, and heating to the upper cover of the crucibleAnd starting crystal growth at the core temperature of 2200 ℃, naturally cooling to 500 ℃ after the crystal growth is finished for 20 hours, introducing argon to normal pressure, and continuously naturally cooling to obtain the silicon carbide crystal.
Example 4
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 15% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 5
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 20% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 6
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 30% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 7
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 40% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 8
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 60 percent of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
FIG. 1 is a graph showing the decomposition ratios of silicon carbide powders composed of silicon carbide powders having different particle diameters according to examples 2 to 8 with respect to time, wherein curves 1 to 7 show the decomposition ratios of the silicon carbide powders according to examples 2 to 8 when the argon pressure is 1000Pa and the center temperature of the upper lid of the crucible is 2200 ℃ respectively. As can be seen from FIG. 1, the silicon carbide powders having different particle diameters in which silicon carbide powder having a particle diameter of 50 μm accounts for 10% by weight of the total powder have the highest decomposition ratio.
Example 9
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 10 microns and silicon carbide powder with the particle size of 50 microns, wherein the silicon carbide powder with the particle size of 10 microns in the silicon carbide powder accounts for 25% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 50 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4torr, heating to 400 ℃ at a heating rate of 200 ℃/h and keeping for 2h, filling argon to 0.2atm, continuing to heat until the central temperature of the upper cover of the crucible is 1800 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, continuing to perform self-heatingThen cooling to obtain the silicon carbide crystal.
Example 10
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 10 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 10 microns in the silicon carbide powder accounts for 35% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 70 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And (3) torr, heating to 500 ℃ at the heating rate of 300 ℃/h, keeping for 2h, filling argon to the pressure of 0.4atm, continuing to heat until the central temperature of the upper cover of the crucible is 1900 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 11
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 100 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 45 percent of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 90 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And (3) torr, heating to 600 ℃ at the heating rate of 500 ℃/h, keeping for 2h, filling argon to the pressure of 0.6atm, continuing to heat until the central temperature of the upper cover of the crucible is 2000 ℃, starting crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 12
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 50 microns and silicon carbide powder with the particle size of 200 microns, wherein the silicon carbide powder with the particle size of 50 microns in the silicon carbide powder accounts for 50% of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 120 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And (3) torr, heating to 700 ℃ at a heating rate of 600 ℃/h, keeping for 2h, filling argon to the pressure of 0.8atm, continuing to heat until the central temperature of the upper cover of the crucible is 2100 ℃, starting crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Example 13
The embodiment provides a method for improving the growth rate of silicon carbide crystals prepared by a PVT method.
The silicon carbide powder is prepared by mixing silicon carbide powder with the particle size of 100 mu m and silicon carbide powder with the particle size of 200 mu m, wherein the silicon carbide powder with the particle size of 100 mu m in the silicon carbide powder accounts for 55 percent of the total weight of the powder.
And placing the obtained silicon carbide powder into a graphite crucible, wherein the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 150 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG- 4And (3) torr, heating to 800 ℃ at the heating rate of 700 ℃/h, keeping for 2h, filling argon to the pressure of 1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2300 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Comparative example 1
According to the comparative example, silicon carbide crystals grow only by taking silicon carbide powder with the particle size of 100 microns as a raw material, silicon carbide powder with a single particle size is placed into a graphite crucible, and the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of graphite crucible to obtain graphiteThe crucible is put into a crystal growth furnace and is vacuumized to 10 DEG-4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
Comparative example 2
According to the comparative example, silicon carbide crystals grow only by taking silicon carbide powder with the particle size of 50 microns as a raw material, silicon carbide powder with a single particle size is placed into a graphite crucible, and the paving thickness of the silicon carbide powder at the bottom of the graphite crucible is 100 mm. Adhering silicon carbide seed crystal to the cover of a graphite crucible, putting the graphite crucible into a crystal growth furnace, and vacuumizing to 10 DEG-4And torr, heating to 700 ℃ at the heating rate of 800 ℃/h, keeping for 2h, filling argon to the air pressure of 0.1atm, continuing to heat until the central temperature of the upper cover of the crucible is 2200 ℃ to start crystal growth, naturally cooling to 500 ℃ after the crystal growth is finished for 20h, filling argon to normal pressure, and continuing to naturally cool to obtain the silicon carbide crystal.
It was measured that, for the same growth time, silicon carbide crystals grown from the silicon carbide powders of different particle sizes of example 3 in which the silicon carbide powder having a particle size of 50 μm was 10% by weight of the total powder had a thickness of 2.1cm, whereas silicon carbide crystals grown from comparative examples 1 and 2 had thicknesses of only 1.6cm and 1.4 cm. By comparison, the silicon carbide crystal prepared by the PVT method with the silicon carbide powder with different particle sizes as the raw material can obviously improve the crystal growth rate.
Claims (9)
1. A method for improving growth rate of silicon carbide crystals prepared by a PVT method is characterized in that silicon carbide powder with different particle sizes is mixed to prepare the silicon carbide powder, the silicon carbide powder is placed into a graphite crucible, silicon carbide seed crystals are adhered to a graphite crucible cover, the graphite crucible is placed into a crystal growth furnace, the silicon carbide powder is heated to 400-800 ℃ under a vacuum condition and is kept for 2 hours, argon gas is filled into the graphite crucible, the graphite crucible is continuously heated to a crystal growth temperature to start crystal growth, the natural cooling is carried out to 500 ℃ after the crystal growth is completed, the argon gas is filled into the graphite crucible to normal pressure, and the natural cooling is continuously carried out to obtain the silicon carbide.
2. The method for improving the growth rate of silicon carbide crystals prepared by the PVT method according to claim 1, wherein the silicon carbide powder with different particle sizes is prepared by mixing silicon carbide powder with the particle size of 10-200 μm and silicon carbide powder with the particle size of 50-500 μm.
3. The method for improving the growth rate of the silicon carbide crystal prepared by the PVT method according to claim 1 or 2, wherein the silicon carbide powder with the particle size of 10-200 μm accounts for 5-60% of the total weight of the silicon carbide powder.
4. The method for increasing the growth rate of silicon carbide crystals prepared by the PVT method according to claim 3, wherein the silicon carbide powder with the particle size of 10-200 μm accounts for 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55% or 60% of the total weight of the silicon carbide powder.
5. The method for improving the growth rate of silicon carbide crystals prepared by the PVT method according to claim 4, wherein the silicon carbide powder is spread at the bottom of the graphite crucible to a thickness of 50-150 mm.
6. The method for increasing the growth rate of silicon carbide crystals prepared by the PVT method according to claim 5, wherein the vacuum condition is that the inside of a graphite crucible is vacuumized to 10 degrees-4torr。
7. The method for increasing the growth rate of silicon carbide crystals prepared by the PVT method according to claim 6, wherein the pressure of the argon gas is 0.1-1 atm.
8. The method for increasing the growth rate of the silicon carbide crystal prepared by the PVT method according to claim 7, wherein the heating rate is 200-800 ℃/h.
9. The method for increasing the growth rate of the silicon carbide crystal prepared by the PVT method according to claim 8, wherein the crystal growth temperature is 1800-2300 ℃ at the center of the upper cover of the crucible.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110276280.9A CN113026095A (en) | 2021-03-15 | 2021-03-15 | Method for improving growth rate of silicon carbide crystal prepared by PVT method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110276280.9A CN113026095A (en) | 2021-03-15 | 2021-03-15 | Method for improving growth rate of silicon carbide crystal prepared by PVT method |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113026095A true CN113026095A (en) | 2021-06-25 |
Family
ID=76469197
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110276280.9A Pending CN113026095A (en) | 2021-03-15 | 2021-03-15 | Method for improving growth rate of silicon carbide crystal prepared by PVT method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113026095A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115573030A (en) * | 2022-10-25 | 2023-01-06 | 山东大学 | Silicon carbide single crystal growth method and silicon carbide single crystal |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000007492A (en) * | 1998-06-25 | 2000-01-11 | Denso Corp | Production of single crystal |
JP2009051702A (en) * | 2007-08-28 | 2009-03-12 | Denso Corp | Method for producing silicon carbide single crystal |
CN102912431A (en) * | 2012-10-25 | 2013-02-06 | 西安理工大学 | Silicon carbide crystal growth method for increasing primary feeding ingot thickness |
CN103209923A (en) * | 2010-11-15 | 2013-07-17 | 独立行政法人产业技术综合研究所 | Silicon carbide powder for production of silicon carbide single crystal, and method for producing same |
CN103757703A (en) * | 2014-01-24 | 2014-04-30 | 汪长安 | High-purity large-size silicon carbide single crystal and preparation process thereof |
CN105603530A (en) * | 2016-01-12 | 2016-05-25 | 台州市一能科技有限公司 | Raw material for high-speed growth of silicon carbide crystals and silicon carbide crystal growing method |
CN107955970A (en) * | 2017-12-29 | 2018-04-24 | 北京华进创威电子有限公司 | A kind of growing method of high quality aluminum-nitride single crystal |
JP2018118866A (en) * | 2017-01-24 | 2018-08-02 | 太平洋セメント株式会社 | Silicon carbide powders |
CN108624963A (en) * | 2018-05-16 | 2018-10-09 | 福建北电新材料科技有限公司 | A kind of raw material sintering process of carborundum crystals for the growth of PVT methods |
CN112226815A (en) * | 2020-11-16 | 2021-01-15 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Pretreatment method of silicon carbide powder for growing silicon carbide single crystal by PVT (physical vapor transport) method |
-
2021
- 2021-03-15 CN CN202110276280.9A patent/CN113026095A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000007492A (en) * | 1998-06-25 | 2000-01-11 | Denso Corp | Production of single crystal |
JP2009051702A (en) * | 2007-08-28 | 2009-03-12 | Denso Corp | Method for producing silicon carbide single crystal |
CN103209923A (en) * | 2010-11-15 | 2013-07-17 | 独立行政法人产业技术综合研究所 | Silicon carbide powder for production of silicon carbide single crystal, and method for producing same |
CN102912431A (en) * | 2012-10-25 | 2013-02-06 | 西安理工大学 | Silicon carbide crystal growth method for increasing primary feeding ingot thickness |
CN103757703A (en) * | 2014-01-24 | 2014-04-30 | 汪长安 | High-purity large-size silicon carbide single crystal and preparation process thereof |
CN105603530A (en) * | 2016-01-12 | 2016-05-25 | 台州市一能科技有限公司 | Raw material for high-speed growth of silicon carbide crystals and silicon carbide crystal growing method |
JP2018118866A (en) * | 2017-01-24 | 2018-08-02 | 太平洋セメント株式会社 | Silicon carbide powders |
CN107955970A (en) * | 2017-12-29 | 2018-04-24 | 北京华进创威电子有限公司 | A kind of growing method of high quality aluminum-nitride single crystal |
CN108624963A (en) * | 2018-05-16 | 2018-10-09 | 福建北电新材料科技有限公司 | A kind of raw material sintering process of carborundum crystals for the growth of PVT methods |
CN112226815A (en) * | 2020-11-16 | 2021-01-15 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Pretreatment method of silicon carbide powder for growing silicon carbide single crystal by PVT (physical vapor transport) method |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115573030A (en) * | 2022-10-25 | 2023-01-06 | 山东大学 | Silicon carbide single crystal growth method and silicon carbide single crystal |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104805504B (en) | A kind of method of fast-growth large size silicon-carbide monocrystalline | |
CN109234798B (en) | The continuous long crystal method of single-crystal silicon carbide | |
CN110055587B (en) | High-purity graphite crucible and preparation method of high-quality silicon carbide single crystal | |
CN108946735B (en) | Synthesis method of large-particle-size silicon carbide powder for silicon carbide crystal growth | |
CN113061985B (en) | Method for improving crystal quality by adjusting carbon-silicon ratio distribution | |
US20240183063A1 (en) | Method for sic step flow growth by regulating growth monmoers using chemical potential under non-equilibrium condition | |
CN104828825A (en) | Low-cost method for synthesizing silicon carbide powder at low temperature | |
CN102021653B (en) | Method for growing silicon carbide single crystal by using high-density material block | |
CN108624963A (en) | A kind of raw material sintering process of carborundum crystals for the growth of PVT methods | |
CN111962152A (en) | Preparation method of silicon carbide single crystal for reducing crystal defects | |
CN110306239A (en) | A kind of silicon carbide material seed crystal support | |
CN113026095A (en) | Method for improving growth rate of silicon carbide crystal prepared by PVT method | |
CN209144310U (en) | A kind of device for silicon carbide monocrystal growth | |
CN109629003B (en) | Preparation method of low-concentration P-type indium phosphide single crystal | |
JP2024508945A (en) | How to grow high quality single crystal silicon carbide | |
CN112010311B (en) | Method for treating prefabricated material for high-purity silicon carbide powder | |
CN106591952A (en) | Preparation method of SiC wafer | |
CN115478324A (en) | Method for growing single crystal or polycrystalline SiC crystal by cosolvent method | |
CN111575801B (en) | Preparation method and wafer growth raw material | |
CN113788480B (en) | Preparation method of high-purity silicon carbide and corresponding high-purity silicon carbide | |
CN115124040A (en) | Solid-phase synthesis method for improving material ratio of large-particle-size silicon carbide powder | |
CN113355743A (en) | Method for recycling residual sintering raw material after silicon carbide crystal growth | |
CN113403681B (en) | Method for adding powder of additional carbon source in growth of PVT method silicon carbide crystals | |
CN103757703B (en) | A kind of High-purity large-size silicon carbide single crystal and preparation technology thereof | |
CN107059124A (en) | A kind of method that utilization microwave synthesizes zinc oxide in large size crystal |
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 | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210625 |