CN113136622A - PVT method airflow-oriented silicon carbide single crystal growth device and using method - Google Patents
PVT method airflow-oriented silicon carbide single crystal growth device and using method Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 78
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 43
- 239000010439 graphite Substances 0.000 claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 25
- 239000011261 inert gas Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000012495 reaction gas Substances 0.000 claims abstract description 10
- 239000007770 graphite material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 8
- 238000000859 sublimation Methods 0.000 claims description 6
- 230000008022 sublimation Effects 0.000 claims description 6
- 230000007547 defect Effects 0.000 claims description 4
- 238000003795 desorption Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000011810 insulating material Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000009529 body temperature measurement Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- Chemical & Material Sciences (AREA)
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- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a PVT method gas flow guide silicon carbide single crystal growth device and a using method thereof. The device comprises a bonded graphite seed crystal support, seed crystals, a crucible upper part, a graphite connecting ring, a crucible lower part, a shell box body, an upper temperature measuring rod and a lower temperature measuring rod, wherein the graphite connecting ring is made of a porous graphite material different from the material of the crucible upper part and the material of the crucible lower part, the aperture is 1-100 mu m, and the porosity and the aperture are different from those of the crucible upper part and the crucible lower part. The method comprises the following steps: charging, heating, vacuumizing, filling inert gas, heating and maintaining pressure, reducing pressure and cooling. The invention ensures that gas in the reaction system overflows at a designated position by utilizing the pore difference of graphite, achieves high growth quality by controlling the detention time and the flow direction of the reaction gas on the surface and the edge of the seed crystal and the pressure difference of the gas inside and outside the crucible, particularly can inhibit the generation of small cracks and polycrystal at the edge, and can reduce the impurity content in the crystal growth process.
Description
Technical Field
The invention relates to the technical field of single crystal growth, in particular to a PVT method airflow-oriented silicon carbide single crystal growth device and a using method thereof.
Background
Silicon carbide is a typical wide bandgap semiconductor material, and is a third generation semiconductor material following silicon, gallium arsenide. Compared with silicon and gallium arsenide, the silicon carbide material has excellent performances of high thermal conductivity, high breakdown field strength, high saturated electron drift rate and the like, and has huge application prospects in the aspects of high-temperature, high-frequency, high-power and anti-radiation devices. The gallium nitride radio frequency device with the high-purity semi-insulating silicon carbide as the substrate is mainly applied to the field of 5G communication; the high-voltage large-current power electronic device with the conductive silicon carbide as the substrate can be applied to the fields of large-scale power transformation systems, electric automobiles, charging piles and the like.
The current commercial silicon carbide substrate growth method is Physical Vapor Transport (PVT). Namely, silicon carbide powder is put in a closed graphite crucible, and silicon carbide seed crystals are placed on the top of the crucible. The heating of a resistance furnace or an induction furnace is adopted, the thermal field distribution of the single crystal furnace is reasonably designed, the temperature of the powder source area is higher than that of the seed crystal area, and the powder source area reaches the sublimation temperature point of the silicon carbide powder source. Si, C, Si2C, SiC2 and SiC molecules generated by sublimation of the silicon carbide powder source are transported to the vicinity of the seed crystal region through diffusion or convection effect. Because the temperature of the seed crystal region is lower, the atmosphere forms a certain supercooling degree and is crystallized into SiC crystals on the surface of the seed crystals.
The silicon carbide single crystal growth uses a graphite crucible processed by isostatic pressing graphite, and the whole system is in a closed or semi-closed state. The growth of the silicon carbide is carried out under the conditions of high temperature and low pressure, the growth pressure kept outside the crucible is 0.1-20mbar, and the growth rate is increased along with the reduction of the pressure; in the crucible, the silicon carbide powder forms a mixed gas containing Si, C, Si2C, SiC2 and SiC during sublimation, and the pressure inside the crucible is higher than the external pressure.
Gas components in the crucible can leak through unsealed graphite interfaces or graphite pores, and the mass loss before and after growth is 10-1000 mg and is uncontrollable; in addition, as the reaction gas etches the graphite material, the occurrence of macroscopic defects such as cracks or polycrystals at the edge of the crystal is caused; in a general growth device, reaction gas is vertically conveyed upwards and overflows from the edge of a seed crystal, so that the temperature and the gas components of the central part and the edge part of the seed crystal are different. The uncontrollable nature of gas evolution during crystal growth, including the amount and path of the overflow, directly affects the quality of the single crystal growth and the consistency of the batch production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a PVT method gas flow guide silicon carbide single crystal growth device, which guides gas overflow to the direction by changing the material of a crucible connecting piece, and simultaneously changes the overflow rate of the gas by controlling the selection of the pore size of the crucible connecting piece, namely graphite, so as to control the growth rate of the crystal and the content of impurities in the crystal.
The technical scheme of the invention is as follows: the utility model provides a carborundum single crystal growth device of PVT method air current direction, includes that the bonding graphite seed crystal holds in the palm, the seed crystal, on the crucible, under graphite go-between, the crucible, the shell box, goes up temperature measurement pole and lower temperature measurement pole, the shell comprises insulation material, it passes the up end setting on the upper portion of shell box to go up the temperature measurement pole, the bottom surface that the temperature measurement pole passed the shell box down sets up the lower part at the shell box, set up the top at temperature measurement pole down under the crucible, set up the below of temperature measurement pole on the crucible, the bonding graphite seed crystal holds in the palm the upper end of setting on the crucible, the seed crystal sets up the lower extreme that holds in the palm at the graphite seed crystal, the crucible subassembly sets up on the crucible and under the crucible between its characterized in that: the graphite connecting ring is made of porous graphite material different from the material on the crucible and the material under the crucible, the aperture is 1-100 μm, and the porosity and the aperture are different from those on the crucible and under the crucible.
The use method of the PVT method gas flow guide silicon carbide single crystal growth device is characterized in that: the method comprises the following specific steps:
the first step is as follows: loading a SiC powder source for growing silicon carbide into the lower part of a crucible, assembling SiC seed crystals and a bonded graphite seed crystal support on the upper end of the crucible, and fixedly connecting the upper part of the crucible and the lower part of the crucible by a graphite connecting ring;
the second step is that: after the furnace is charged, carrying out vacuum pumping and temperature rise treatment on the single crystal growth furnace, setting the temperature of a temperature measuring point at the top of the crucible to be 1000-;
the third step: when the vacuum degree of the furnace body is lower than 5 multiplied by 10-5Stopping vacuumizing when the pressure is mbar; at the moment, the air molecules adsorbed on the surface of the SiC powder source in the graphite crucible complete desorption and are arranged in a growth system;
at the moment, the material of the graphite connecting ring is different from the material of the upper crucible and the lower crucible, so that the porosity and the aperture are different from those of the upper crucible and the lower crucible, and meanwhile, the gas overflows from the position of the graphite connecting ring due to the porosity of the graphite connecting ring;
the fourth step: filling inert gas into the single crystal growth furnace, wherein the flow rate of the inert gas is 1-5L/min, and the pressure of the furnace body is increased to 700-1000 mbar;
the fifth step: raising the temperature to the temperature of 2000-; during the temperature rise, the flow rate of inert gas is 10-1000mL/min, the gas is discharged out of the single crystal growth furnace through a vacuum pump, and the pressure in the furnace is kept constant;
and a sixth step: when the temperature reaches the growth temperature of the single crystal, gradually reducing the air pressure to 0.1-20mbar, keeping the flow of inert gas constant at 10-1000mL/min, and setting the growth time;
at the moment, residual impurities in the growth system are reduced from entering the silicon carbide crystal through the control of non-participating reaction gas outside the crucible; the phenomenon that the reaction gas etches the graphite material of the crucible to cause cracks at the edge of the crystal or macro defects of polycrystal is avoided; due to the pressure difference between the inside and the outside of the crucible, the vapor pressure at the upper part of the silicon carbide powder in the crucible is reduced, the sublimation rate of the silicon carbide powder is increased, and the growth rate of single crystals is increased;
the seventh step: and (4) cooling under the gas pressure of 400-960 mbar for 5 hours to 1000 ℃, then cooling to room temperature along with the furnace, and finishing the growth.
The beneficial effects produced by the invention are as follows: the method controls the residence time and the flow direction of the reaction gas on the surface and the edge of a seed crystal and controls the pressure difference of the gas inside and outside a crucible to achieve high growth quality, particularly can inhibit small cracks at the edge and polycrystal generation, and can reduce the impurity content in the crystal growth process. The invention has the two characteristics of high efficiency and simple equipment. Can be popularized and used in most of the silicon carbide single crystal furnace systems in the field at present.
Drawings
FIG. 1 is a schematic diagram of the structure of the apparatus of the present invention.
Detailed Description
As shown in figure 1, a PVT method airflow-oriented silicon carbide single crystal growth device comprises a bonded graphite seed crystal support 1, seed crystals 2, an upper crucible 4, a graphite connecting ring 5, a lower crucible 6, a shell box body 8, an upper temperature measuring rod 9 and a lower temperature measuring rod 10, wherein the shell 8 is made of heat-insulating materials, the upper temperature measuring rod 9 penetrates through the upper end face of the shell box body 8 and is arranged at the upper part of the shell box body 8, the lower temperature measuring rod 10 penetrates through the bottom face of the shell box body 8 and is arranged at the lower part of the shell box body 8, the lower crucible 6 is arranged above the lower temperature measuring rod 10, the upper crucible 4 is arranged below the upper temperature measuring rod 9, the bonded graphite seed crystal support 1 is arranged at the upper end of the upper crucible 4, the seed crystals 2 are arranged at the lower end of the graphite seed crystal support 1, a crucible assembly 5 is arranged between the upper crucible 4 and the lower crucible 6, the graphite connecting ring 5 is made of porous graphite materials different from the upper crucible 4 and the lower crucible 6, the aperture is 1-100 μm, and the porosity and aperture are different from the upper crucible 4 and the lower crucible 6.
A use method of a PVT method gas flow guide silicon carbide single crystal growth device comprises the following specific steps:
the first step is as follows: loading a SiC powder source 7 for growing silicon carbide into a crucible lower part 6, assembling a SiC seed crystal 2 and an adhesive graphite seed crystal holder 1 on the upper end of a crucible upper part 4, and fixedly connecting the crucible upper part 4 and the crucible lower part 6 by a graphite connecting ring 5;
the second step is that: after the furnace is charged, carrying out vacuum pumping and temperature rise treatment on the single crystal growth furnace, setting the temperature of a temperature measuring point at the top of the crucible to be 1000-;
the third step: when the vacuum degree of the furnace body is lower than 5 multiplied by 10-5Stopping vacuumizing when the pressure is mbar; at the moment, the air molecules adsorbed on the surface of the SiC powder source in the graphite crucible complete desorption and are arranged in a growth system;
at the moment, because the material of the graphite connecting ring 5 is different from the material of the upper crucible 4 and the lower crucible 6, the porosity and the aperture are different from the material of the upper crucible 4 and the lower crucible 6, and simultaneously, because the graphite connecting ring 5 is porous, the gas overflows from the position of the graphite connecting ring 5;
the fourth step: filling inert gas into the single crystal growth furnace, wherein the flow rate of the inert gas is 1-5L/min, and the pressure of the furnace body is increased to 700-1000 mbar;
the fifth step: raising the temperature to the temperature of 2000-; during the temperature rise, the flow rate of inert gas is 10-1000mL/min, hydrogen or nitrogen can be introduced according to the requirement of the electrical property of the silicon carbide single crystal to be grown, the flow rate of gas is 1-100 mL/min, the gas is discharged out of the single crystal growth furnace through a vacuum pump, the pressure in the furnace is kept constant, and the growth time is set;
and a sixth step: when the temperature reaches the growth temperature of the single crystal, gradually reducing the air pressure to 0.1-20mbar, keeping the flow of inert gas constant at 10-1000mL/min, and setting the growth time; introducing hydrogen or nitrogen according to the electrical property requirement of the silicon carbide single crystal to be grown, wherein the gas flow is 1-100 mL/min;
at the moment, the residual impurities in the growth system are reduced from entering the silicon carbide crystal 3 by controlling the flow of non-participating reaction gas, namely inert gas, outside the crucible; the phenomenon that the reaction gas etches the graphite material of the crucible to cause cracks at the edge of the crystal or macro defects of polycrystal is avoided; due to the pressure difference between the inside and the outside of the crucible, the vapor pressure at the upper part of the silicon carbide powder in the crucible is reduced, the sublimation rate of the silicon carbide powder is increased, and the growth rate of single crystals is increased;
the seventh step: and (4) cooling under the gas pressure of 400-960 mbar for 5 hours to 1000 ℃, then cooling to room temperature along with the furnace, and finishing the growth.
Claims (2)
1. A PVT method airflow-oriented silicon carbide single crystal growth device comprises a bonded graphite seed crystal support (1), seed crystals (2), an upper crucible (4), a graphite connecting ring (5), a lower crucible (6), a shell box body (8), an upper temperature measuring rod (9) and a lower temperature measuring rod (10), wherein the shell (8) is made of heat-insulating materials, the upper temperature measuring rod (9) penetrates through the upper end face of the shell box body (8) and is arranged at the upper part of the shell box body (8), the lower temperature measuring rod (10) penetrates through the bottom face of the shell box body (8) and is arranged at the lower part of the shell box body (8), the lower crucible (6) is arranged above the lower temperature measuring rod (10), the upper crucible (4) is arranged below the upper temperature measuring rod (9), the bonded graphite seed crystal support (1) is arranged at the upper end of the upper crucible (4), and the seed crystals (2) are arranged at the lower end of the graphite seed crystal support (1), the crucible assembly (5) is arranged between the upper crucible (4) and the lower crucible (6), and is characterized in that:
the graphite connecting ring (5) is made of porous graphite material which is different from the material of the upper crucible (4) and the lower crucible (6), the aperture is 1-100 mu m, and the porosity and the aperture are different from those of the upper crucible (4) and the lower crucible (6).
2. A method of using a silicon carbide single crystal growth apparatus using PVT process gas flow guide according to claim 1, characterized in that: the method comprises the following specific steps:
the first step is as follows: loading a SiC powder source (7) for growing silicon carbide into a crucible lower part (6), assembling a SiC seed crystal (2) and a bonded graphite seed crystal holder (1) on the upper end of a crucible upper part (4), and fixedly connecting the crucible upper part (4) and the crucible lower part (6) by a graphite connecting ring (5);
the second step is that: after the furnace is charged, carrying out vacuum pumping and temperature rise treatment on the single crystal growth furnace, setting the temperature of a temperature measuring point at the top of the crucible (4) to be 1000-;
the third step: when the vacuum degree of the furnace body is lower than 5 multiplied by 10-5Stopping vacuumizing when the pressure is mbar; at the moment, the air molecules adsorbed on the surface of the SiC powder source (7) in the graphite crucible complete desorption and are arranged in a growth system;
at the moment, because the graphite connecting ring (5) is made of different materials from the upper crucible (4) and the lower crucible (6), the porosity and the aperture are different from the upper crucible (4) and the lower crucible (6), and simultaneously, because of the porosity of the graphite connecting ring (5), gas overflows from the position of the graphite connecting ring (5);
the fourth step: filling inert gas into the single crystal growth furnace, wherein the flow rate of the inert gas is 1-5L/min, and the pressure of the furnace body is increased to 700-1000 mbar;
the fifth step: raising the temperature to the temperature of 2000-; during the temperature rise, the flow rate of inert gas is 10-1000mL/min, the gas is discharged out of the single crystal growth furnace through a vacuum pump, and the pressure in the furnace is kept constant;
and a sixth step: when the temperature reaches the growth temperature of the single crystal, gradually reducing the air pressure to 0.1-20mbar, keeping the flow of inert gas constant at 10-1000mL/min, and setting the growth time;
at the moment, the residual impurities in the growth system are reduced from entering the silicon carbide crystal (3) through the control of the flow of non-participating reaction gas, namely inert gas, outside the crucible; the phenomenon that the reaction gas etches the graphite material of the crucible to cause cracks at the edge of the crystal or macro defects of polycrystal is avoided; due to the pressure difference between the inside and the outside of the crucible, the vapor pressure at the upper part of the silicon carbide powder in the crucible is reduced, the sublimation rate of the silicon carbide powder is increased, and the growth rate of single crystals is increased;
the seventh step: and (4) cooling under the gas pressure of 400-960 mbar for 5 hours to 1000 ℃, then cooling to room temperature along with the furnace, and finishing the growth.
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Cited By (3)
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CN114657632A (en) * | 2022-02-24 | 2022-06-24 | 国宏中宇科技发展有限公司 | Tantalum structure, temperature measuring hole structure, crucible assembly and temperature measuring hole anti-blocking method |
CN116695089A (en) * | 2023-08-09 | 2023-09-05 | 通威微电子有限公司 | Relay ring tantalum carbide coating device and method |
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CN114182357A (en) * | 2021-12-10 | 2022-03-15 | 中国电子科技集团公司第四十六研究所 | Method for regrowing silicon carbide single crystal by using broken crystal grains of silicon carbide crystal |
CN114657632A (en) * | 2022-02-24 | 2022-06-24 | 国宏中宇科技发展有限公司 | Tantalum structure, temperature measuring hole structure, crucible assembly and temperature measuring hole anti-blocking method |
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