CN112962083A - Device and method for coating film on back of seed crystal for growing silicon carbide single crystal - Google Patents
Device and method for coating film on back of seed crystal for growing silicon carbide single crystal Download PDFInfo
- Publication number
- CN112962083A CN112962083A CN202110148005.9A CN202110148005A CN112962083A CN 112962083 A CN112962083 A CN 112962083A CN 202110148005 A CN202110148005 A CN 202110148005A CN 112962083 A CN112962083 A CN 112962083A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- graphite
- nitrogen
- seed crystal
- coating
- 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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
-
- 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
Abstract
A device and a method for coating the back of a seed crystal for growing a silicon carbide single crystal relate to a device and a method for treating the seed crystal. The method aims to solve the technical problem that the existing seed crystal is easy to have a plane hexagonal cavity defect in the growth process of the SiC crystal. The device comprises a furnace body, a graphite crucible, a graphite bracket, an induction coil, a vacuum pump, a temperature measuring instrument and a bubbler; the upper opening and the lower opening of the graphite crucible are arranged on a lower flange of the furnace body; the graphite support is placed in the graphite crucible. The coating method comprises the following steps: placing the silicon carbide seed wafer on a graphite bracket with the Si surface facing downwards, and then covering a graphite sheet; vacuumizing the furnace body and then filling nitrogen; raising the temperature to make the temperature of the graphite crucible reach 1200-1800 ℃; then titanium tetrachloride and hydrogen are introduced to react, and a TiN film is obtained on the Si surface of the silicon carbide seed crystal. The invention can carry out seed crystal coating in batches only by improving the existing crystal growth furnace without carrying out large equipment modification, and can be used in the field of coating.
Description
Technical Field
The invention relates to a method and a device for seed crystal treatment.
Background
The most effective method for growing silicon carbide (SiC) crystals at present is physical vapor phaseThe transmission Method (Physical Vapor Transport Method) is used for growing the silicon carbide crystal by the following steps: keeping a certain temperature gradient in the growth chamber, keeping the SiC raw material in a high-temperature region and the seed crystal in a low-temperature region, raising the temperature in the crucible to 2200-2500 ℃, so that the SiC raw material is sublimated, and a gas phase substance (Si) generated by sublimation is generated2C、SiC2And Si) is transported from the surface of the raw material to the position of the low-temperature seed crystal under the action of the temperature gradient, and crystals are generated by crystallization. However, during the whole growth process, the temperature gradient is formed only between the raw material and the seed crystal, and a certain temperature gradient exists in the grown crystal and between the back surface of the crystal and the seed crystal holder, and the temperature gradient causes thermal evaporation on the back surface of the crystal. In addition, in the process of adhering or mechanically fixing the seed crystal, due to factors such as poor machining precision of the surface of the seed crystal support, uneven adhesion of the adhesive, air release of the adhesive in the curing process and the like, uneven gaps or some air holes exist between the back surface of the seed crystal and the seed crystal support. These gaps or voids will result in a non-uniform temperature distribution on the backside of the seed crystal, while backside evaporation will preferentially occur in higher temperature regions or in regions with denser defects. The vapor phase species generated by the evaporation first accumulate in the gap or air hole region between the back surface of the seed crystal and the seed crystal holder. Crucible materials for growing SiC crystals are mainly graphite materials. The presence of the pores in the graphite cap will cause the escape of gas phase species accumulated in the gaps or pore regions at the back of the seed crystal, which is a continuous process throughout the growth process. Local areas on the back of the crystal are continuously evaporated, and gas-phase substances generated by evaporation continuously escape from pores of the graphite cover, so that plane hexagonal cavity defects are generated in the grown crystal.
Disclosure of Invention
The invention provides a device and a method for coating a film on the back of a seed crystal for growing a silicon carbide single crystal, aiming at solving the technical problem that the existing seed crystal is easy to have a plane hexagonal cavity defect in the SiC crystal growing process.
The device for coating the back of the seed crystal for growing the silicon carbide single crystal comprises a furnace body 1, a graphite crucible 2, a graphite support 3, an induction coil 4, a vacuum pump 5, a temperature measuring instrument 6 and a bubbler 7;
wherein the furnace body 1 consists of a side wall 1-1, an upper flange 1-2 and a lower flange 1-3; the upper flange 1-2 is provided with a temperature measuring port 1-4 and a vacuum pumping port 1-5; arranging a hydrogen inlet 1-6, a nitrogen inlet 1-7 and a titanium tetrachloride and nitrogen inlet 1-8 under the lower flange 1-3;
the graphite crucible 2 is provided with an upper opening and a lower opening; the graphite crucible 2 is placed on the lower flange 1-3, and the hydrogen inlet 1-6, the nitrogen inlet 1-7, the titanium tetrachloride and nitrogen inlet 1-8 are arranged in the graphite crucible 2; the inner side wall of the graphite crucible 2 is provided with a boss 2-1 for placing a graphite bracket 3;
the induction coil 4 is arranged outside the furnace body 1; the current in the induction coil 4 can directly couple induced current on the graphite crucible 2 and the graphite bracket 3 through a heat insulating material, so that the graphite crucible 2 is heated to the temperature required by the coating of the wafer;
the temperature measuring instrument 6 is arranged at the upper ends of the temperature measuring ports 1-4 and is used for monitoring the temperature in the furnace; the hydrogen inlet 1-6 is connected with a hydrogen device; the nitrogen inlet 1-7 is connected with a nitrogen device; a bubbler 7 is provided on the conduit between the titanium tetrachloride and nitrogen inlets 1-8 and the nitrogen plant.
Furthermore, a heat insulation material layer 8 is arranged outside the graphite crucible 2;
furthermore, 3-6 graphite supports 3 are uniformly distributed along the circumference of the inner wall of the graphite crucible 2, and each graphite support 3 consists of a support table 3-1 and a support column 3-2; the support column 3-2 is fixed on the boss 2-1;
furthermore, the number of the support tables 3-1 of the graphite support 3 is 2-5, and a plurality of seed crystals can be placed on the graphite support according to actual needs.
Furthermore, a valve is arranged on a pipeline connecting the hydrogen inlet 1-6 with the hydrogen device;
furthermore, a valve is arranged on a pipeline connecting the nitrogen inlet 1-7 with the nitrogen device;
further, valves are provided on the pipes between the titanium tetrachloride and nitrogen inlets 1-8 and the nitrogen unit.
The method for coating the back of the seed crystal for growing the silicon carbide single crystal by using the device comprises the following steps:
firstly, a silicon carbide seed wafer 9 is placed on a support table 3-1 of a graphite support 3 with the Si surface facing downwards, and then a graphite sheet 10 with the size exceeding that of the seed wafer is covered on the upper surface of the silicon carbide wafer so as to prevent the C surface of the seed wafer from being polluted;
secondly, starting a vacuum pump 5 to vacuumize until the air pressure in the furnace body 1 is 5 multiplied by 10-4～5×10-6A torr for exhausting air in the furnace, and charging nitrogen into the furnace to 380torr through a nitrogen inlet 1-7;
thirdly, turning on a power supply to heat up, so that the temperature of the graphite crucible 2 placed in the furnace reaches 1200-1800 ℃;
fourthly, titanium tetrachloride is added into a bubbler 7, through titanium tetrachloride and nitrogen inlets 1-8, the vaporized titanium tetrachloride is led into the furnace body 1 through nitrogen at a flow rate of 20-40 mL/min, meanwhile, through hydrogen inlets 1-6, hydrogen is led into the furnace body 1 through hydrogen inlets 1-6 at a flow rate of 60-80 mL/min, nitrogen is led into the furnace body 1 through nitrogen inlets 1-7 at a flow rate of 50-100 mL/min, and the reaction time is 30-90 min; keeping a vacuum pump on in the whole reaction process so as to discharge unreacted gas and generated HCl gas; and after the reaction is finished, cooling to obtain the TiN film on the Si surface of the silicon carbide seed crystal sheet 9.
The invention takes nitrogen as protective gas and titanium tetrachloride TiCl4And H2Is a precursor, wherein nitrogen is used as a protective gas and a reaction gas. Before the deposition reaction, the reaction chamber was repeatedly evacuated and filled with nitrogen gas to remove air in the reaction chamber. Titanium tetrachloride and hydrogen were fed into the reaction chamber, a graphite crucible, through two separate gas paths, with the vaporized titanium tetrachloride being carried into the reaction chamber by nitrogen as a carrier gas through a series of bubblers. Utilizing the reaction: TiCl (titanium dioxide)4(g)+2H2(g)+1/2N2(g) → TiN(s) +4HCl (g) deposit a TiN film on the silicon carbide seed (Si-face). The thickness of the TiN film is 0.1-5 μm. The thickness of a wafer coating layer is adjusted by adjusting the proportion of air inlet flow, the pressure and the coating time; the existing crystal growth furnace is utilized for improvement, and seed crystal coating can be carried out in batches without large equipment transformation. The carbonization of the Si surface coated with TiN filmThe silicon seed crystal sheet is used as the seed crystal for growing the silicon carbide single crystal, so that the plane hexagonal defect in the silicon carbide single crystal can be obviously reduced, and the crystal quality and the yield are improved.
Drawings
FIG. 1 is a schematic structural view of an apparatus for back coating a seed crystal for growing a silicon carbide single crystal according to the present invention;
FIG. 2 is a schematic structural view of two graphite supports 3 opposed to each other in example 1;
FIG. 3 is a schematic view of the apparatus for coating the back of the seed crystal in example 1.
In the figure, 1 is a furnace body 1, 1-1 is a side wall, 1-2 is an upper flange, 1-3 is a lower flange, 1-4 is a temperature measuring port, 1-5 is a vacuumizing port, 1-6 is a hydrogen inlet, 1-7 is a nitrogen inlet, and 1-8 is a titanium tetrachloride and nitrogen inlet; 2 is a graphite crucible, and 2-1 is a boss; 3 is a graphite bracket, 3-1 is a supporting table, and 3-2 is a supporting column; 4 is an induction coil, 5 is a vacuum pump, 6 is a temperature measuring instrument, 7 is a bubbler, and 8 is a heat insulation material layer.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention.
Example 1: the device for coating the back of the seed crystal for growing the silicon carbide single crystal comprises a furnace body 1, a graphite crucible 2, a graphite support 3, an induction coil 4, a vacuum pump 5, a temperature measuring instrument 6, a bubbler 7 and a heat insulation material layer 8;
wherein the furnace body 1 consists of a side wall 1-1, an upper flange 1-2 and a lower flange 1-3; the upper flange 1-2 is provided with a temperature measuring port 1-4 and a vacuum pumping port 1-5; arranging a hydrogen inlet 1-6, a nitrogen inlet 1-7 and a titanium tetrachloride and nitrogen inlet 1-8 under the lower flange 1-3;
the graphite crucible 2 is provided with an upper opening and a lower opening; the graphite crucible 2 is placed on the lower flange 1-3, and the hydrogen inlet 1-6, the nitrogen inlet 1-7, the titanium tetrachloride and nitrogen inlet 1-8 are arranged in the graphite crucible 2; 4 uniformly distributed bosses 2-1 are arranged on the inner side wall of the graphite crucible 2 and used for placing 4 graphite brackets 3; each graphite bracket 3 consists of a support table 3-1 and a support column 3-2; the support column 3-2 is fixed on the boss 2-1; the number of the support tables 3-1 of each graphite support 3 is 3; a heat insulation material layer 8 is also arranged outside the graphite crucible 2; the induction coil 4 is arranged outside the furnace body 1; the current in the induction coil 4 can directly couple induced current on the graphite crucible 2 and the graphite bracket 3 through a heat insulating material, so that the graphite crucible 2 is heated to the temperature required by the coating of the wafer;
the temperature measuring instrument 6 is arranged at the upper ends of the temperature measuring ports 1-4 and is used for monitoring the temperature in the furnace; the hydrogen inlet 1-6 is connected with a hydrogen device; the nitrogen inlet 1-7 is connected with a nitrogen device; a bubbler 7 is provided on the conduit between the titanium tetrachloride and nitrogen inlets 1-8 and the nitrogen plant.
The method for coating the back of the seed crystal for the growth of the silicon carbide single crystal by using the device of the embodiment 1 comprises the following steps:
firstly, a silicon carbide seed crystal 9 is placed on a support table 3-1 of a graphite support 3 with the Si surface facing downwards, and then a graphite sheet 10 with the size exceeding that of the seed crystal is covered on the upper surface of the silicon carbide wafer so as to prevent the C surface of the seed crystal from being polluted; the schematic placement diagram is shown in FIG. 2;
secondly, starting a vacuum pump 5 to vacuumize until the air pressure in the furnace body 1 is 5 multiplied by 10-5Discharging air in the furnace, and filling nitrogen into the furnace to 380torr through a nitrogen inlet 1-7;
thirdly, turning on a power supply to heat up the graphite crucible 2 to enable the temperature of the graphite crucible 2 placed in the furnace to reach 1700 ℃;
fourthly, titanium tetrachloride is added into a bubbler 7, nitrogen is used for introducing the vaporized titanium tetrachloride into the furnace body 1 at the flow rate of 30mL/min through titanium tetrachloride and nitrogen inlets 1-8, hydrogen is simultaneously introduced into the furnace body 1 at the flow rate of 70mL/min through hydrogen inlets 1-6, nitrogen is introduced into the furnace body 1 at the flow rate of 70mL/min through nitrogen inlets 1-7, and the reaction time is 90 min; keeping a vacuum pump on in the whole reaction process so as to discharge unreacted gas and generated HCl gas; after the reaction is finished, the temperature is reduced to room temperature, and a TiN film is obtained on the Si surface of the silicon carbide seed crystal sheet 9.
This example produced a TiN thin film on the Si-face of the silicon carbide seed wafer 9 with a thickness of 0.9 microns. The silicon carbide seed crystal wafer with the TiN film on the Si surface is used as the seed crystal for the growth of the silicon carbide single crystal, so that the planar hexagonal defects in the silicon carbide crystal are obviously reduced, and the crystal quality and the yield are improved.
Example 2: the method for coating the back of the seed crystal for the growth of the silicon carbide single crystal by using the device of the embodiment 1 comprises the following steps:
firstly, putting the Si surfaces of two silicon carbide seed crystal sheets 9 downwards on a support table 3-1 of a graphite support 3, and covering graphite sheets 10 with the size exceeding that of the seed crystal sheets on the upper surface of a silicon carbide wafer so as to prevent the C surface of the seed crystal from being polluted;
secondly, starting a vacuum pump 5 to vacuumize until the air pressure in the furnace body 1 is 5 multiplied by 10-6Discharging air in the furnace, and filling nitrogen into the furnace to 380torr through a nitrogen inlet 1-7;
thirdly, turning on a power supply to heat up, so that the temperature of the graphite crucible 2 placed in the furnace reaches 1400 ℃;
fourthly, titanium tetrachloride is added into a bubbler 7, the titanium tetrachloride after vaporization is led into the furnace body 1 through titanium tetrachloride and nitrogen inlets 1-8, meanwhile, hydrogen is led into the furnace body 1 through hydrogen inlets 1-6 at a flow rate of 60mL/min, nitrogen is led into the furnace body 1 through nitrogen inlets 1-7 at a flow rate of 50mL/min, and the reaction time is 40 min; keeping a vacuum pump on in the whole reaction process so as to discharge unreacted gas and generated HCl gas; after the reaction is finished, the temperature is reduced to room temperature, and a TiN film is obtained on the Si surface of the silicon carbide seed crystal sheet 9.
This example produced a TiN thin film on the Si-face of the silicon carbide seed wafer 9 with a thickness of 0.5 microns. The silicon carbide seed crystal wafer with the TiN film on the Si surface is used as the seed crystal for the growth of the silicon carbide single crystal, so that the planar hexagonal defects in the silicon carbide crystal are obviously reduced, and the crystal quality and the yield are improved.
Example 3: the method for coating the back of the seed crystal for the growth of the silicon carbide single crystal by using the device of the embodiment 1 comprises the following steps:
firstly, placing the Si surfaces of three silicon carbide seed crystal sheets 9 downwards on a support table 3-1 of a graphite support 3, and covering graphite sheets 10 with the size exceeding that of the seed crystal sheets on the upper surface of a silicon carbide wafer so as to prevent the C surfaces of the seed crystals from being polluted; the schematic placement diagram is shown in FIG. 2;
secondly, starting a vacuum pump 5 to vacuumize until the air pressure in the furnace body 1 is 5 multiplied by 10-5Discharging air in the furnace, and filling nitrogen into the furnace to 380torr through a nitrogen inlet 1-7;
thirdly, turning on a power supply to heat up, so that the temperature of the graphite crucible 2 placed in the furnace reaches 1300 ℃;
fourthly, titanium tetrachloride is added into a bubbler 7, the vaporized titanium tetrachloride is led into the furnace body 1 through titanium tetrachloride and nitrogen inlets 1-8 at a flow rate of 40mL/min by nitrogen, meanwhile, hydrogen is led into the furnace body 1 through hydrogen inlets 1-6 at a flow rate of 80mL/min, nitrogen is led into the furnace body 1 through nitrogen inlets 1-7 at a flow rate of 90mL/min, and the reaction time is 80 min; keeping a vacuum pump on in the whole reaction process so as to discharge unreacted gas and generated HCl gas; after the reaction is finished, the temperature is reduced to room temperature, and a TiN film is obtained on the Si surface of the silicon carbide seed crystal sheet 9.
This example produced a TiN thin film on the Si-face of the silicon carbide seed wafer 9 with a thickness of 0.3 microns. The silicon carbide seed crystal wafer with the TiN film on the Si surface is used as the seed crystal for the growth of the silicon carbide single crystal, so that the planar hexagonal defects in the silicon carbide crystal are obviously reduced, and the crystal quality and the yield are improved.
Claims (8)
1. A seed crystal back coating device for silicon carbide single crystal growth is characterized by comprising a furnace body (1), a graphite crucible (2), a graphite support (3), an induction coil (4), a vacuum pump (5), a temperature measuring instrument (6) and a bubbler (7);
wherein the furnace body (1) consists of a side wall (1-1), an upper flange (1-2) and a lower flange (1-3); the upper flange (1-2) is provided with a temperature measuring port (1-4) and a vacuum pumping port (1-5); a hydrogen inlet (1-6), a nitrogen inlet (1-7), a titanium tetrachloride and nitrogen inlet (1-8) are arranged below the lower flange (1-3);
the upper opening and the lower opening of the graphite crucible (2); the graphite crucible (2) is placed on the lower flange (1-3), and the hydrogen inlet (1-6), the nitrogen inlet (1-7), the titanium tetrachloride and the nitrogen inlet (1-8) are arranged in the graphite crucible (2); the inner side wall of the graphite crucible (2) is provided with a boss 2-1 for placing a graphite bracket (3);
the induction coil (4) is arranged outside the furnace body (1);
the temperature measuring instrument (6) is arranged at the upper end of the temperature measuring port (1-4); the hydrogen inlets (1-6) are connected with a hydrogen device; the nitrogen inlet (1-7) is connected with a nitrogen device; the titanium tetrachloride bubbler (7) is located in a conduit between the titanium tetrachloride and nitrogen inlet (1-8) and the nitrogen unit.
2. An apparatus for coating the back of a seed crystal for growing a silicon carbide single crystal according to claim 1, wherein a layer of heat insulating material (8) is further provided outside the graphite crucible (2).
3. A seed crystal back coating device for silicon carbide single crystal growth according to claim 1 or 2, characterized in that 3-6 graphite supports (3) are uniformly distributed along the circumference of the inner wall of the graphite crucible (2), each graphite support (3) is composed of a support platform (3-1) and a support column (3-2); the support column (3-2) is fixed on the boss 2-1.
4. A seed crystal back coating apparatus for silicon carbide single crystal growth according to claim 1 or 2, wherein the number of the supporting stands (3-1) of the graphite jig (3) is 3 to 6.
5. An apparatus for coating a back of a seed crystal for growing a silicon carbide single crystal according to claim 1 or 2, wherein a valve is provided on a pipe connecting the hydrogen gas inlet (1-6) and the hydrogen gas means.
6. An apparatus for coating a back of a seed crystal for growing a silicon carbide single crystal according to claim 1 or 2, wherein a valve is provided on a pipe connecting the nitrogen gas inlet (1-7) and the nitrogen gas means.
7. An apparatus for coating the back of a seed crystal for the growth of a silicon carbide single crystal according to claim 1 or 2, characterized in that a valve is provided on the piping between the titanium tetrachloride and nitrogen gas inlet (1-8) and the nitrogen gas means.
8. A method of coating the back of a seed crystal for the growth of a silicon carbide single crystal using the apparatus of claim 1, characterized in that the method is carried out by the steps of:
firstly, a silicon carbide seed wafer 9 is placed on a support table (3-1) of a graphite support (3) with the Si surface facing downwards, and then a graphite sheet 10 with the size exceeding that of the seed wafer is covered on the upper surface of the silicon carbide wafer so as to prevent the C surface of the seed wafer from being polluted;
secondly, starting a vacuum pump (5) to vacuumize until the air pressure in the furnace body (1) is 5 multiplied by 10-4～5×10-6torr, discharging the air in the furnace, and charging nitrogen into the furnace to 380torr through a nitrogen inlet (1-7);
thirdly, turning on a power supply to heat up, so that the temperature of the graphite crucible (2) placed in the furnace reaches 1200-1800 ℃;
fourthly, titanium tetrachloride is added into a bubbler (7), the vaporized titanium tetrachloride is led into the furnace body (1) through titanium tetrachloride and nitrogen inlets (1-8) at the flow rate of 20-40 mL/min by nitrogen, meanwhile, hydrogen is led into the furnace body (1) through hydrogen inlets (1-6) at the flow rate of 60-80 mL/min, nitrogen is led into the furnace body (1) through nitrogen inlets (1-7) at the flow rate of 50-100 mL/min, and the reaction time is 30-90 min; keeping a vacuum pump on in the whole reaction process so as to discharge unreacted gas and generated HCl gas; and after the reaction is finished, cooling to obtain the TiN film on the Si surface of the silicon carbide seed crystal sheet 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110148005.9A CN112962083A (en) | 2021-02-03 | 2021-02-03 | Device and method for coating film on back of seed crystal for growing silicon carbide single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110148005.9A CN112962083A (en) | 2021-02-03 | 2021-02-03 | Device and method for coating film on back of seed crystal for growing silicon carbide single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112962083A true CN112962083A (en) | 2021-06-15 |
Family
ID=76273917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110148005.9A Pending CN112962083A (en) | 2021-02-03 | 2021-02-03 | Device and method for coating film on back of seed crystal for growing silicon carbide single crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112962083A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546821A (en) * | 2021-07-22 | 2021-10-26 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Coating method of silicon carbide seed crystal |
| CN116516468A (en) * | 2023-07-04 | 2023-08-01 | 苏州优晶光电科技有限公司 | Device and method for simultaneously treating multiple silicon carbide seed crystal coatings |
| WO2024050843A1 (en) * | 2022-09-09 | 2024-03-14 | 眉山博雅新材料股份有限公司 | Crystal growth method and apparatus |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5849360A (en) * | 1996-06-20 | 1998-12-15 | National Science Council | Tube chemical gas deposition method of preparing titanium nitride coated titanium carbide for titanium carbide/silicon nitride composites |
| US5985026A (en) * | 1995-08-16 | 1999-11-16 | Siemens Aktiengesellschaft | Seed crystal for producing monocrystals and method for producing SiC monocrystals or monocrystalline SiC layers |
| JP2010132464A (en) * | 2008-12-02 | 2010-06-17 | Mitsubishi Electric Corp | Method for producing silicon carbide single crystal |
| CN103160928A (en) * | 2011-12-13 | 2013-06-19 | 北京有色金属研究总院 | Seed crystal processing method for growing SiC monocrystal with high quality |
| CN104498901A (en) * | 2015-01-06 | 2015-04-08 | 北京华进创威电子有限公司 | Method and device for plating silicon carbide single crystal |
| US20170191183A1 (en) * | 2014-05-29 | 2017-07-06 | Sumitomo Electric Industries, Ltd. | Method of manufacturing silicon carbide ingot, silicon carbide seed substrate, silicon carbide substrate, semiconductor device and method of manufacturing semiconductor device |
-
2021
- 2021-02-03 CN CN202110148005.9A patent/CN112962083A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5985026A (en) * | 1995-08-16 | 1999-11-16 | Siemens Aktiengesellschaft | Seed crystal for producing monocrystals and method for producing SiC monocrystals or monocrystalline SiC layers |
| US5849360A (en) * | 1996-06-20 | 1998-12-15 | National Science Council | Tube chemical gas deposition method of preparing titanium nitride coated titanium carbide for titanium carbide/silicon nitride composites |
| JP2010132464A (en) * | 2008-12-02 | 2010-06-17 | Mitsubishi Electric Corp | Method for producing silicon carbide single crystal |
| CN103160928A (en) * | 2011-12-13 | 2013-06-19 | 北京有色金属研究总院 | Seed crystal processing method for growing SiC monocrystal with high quality |
| US20170191183A1 (en) * | 2014-05-29 | 2017-07-06 | Sumitomo Electric Industries, Ltd. | Method of manufacturing silicon carbide ingot, silicon carbide seed substrate, silicon carbide substrate, semiconductor device and method of manufacturing semiconductor device |
| CN104498901A (en) * | 2015-01-06 | 2015-04-08 | 北京华进创威电子有限公司 | Method and device for plating silicon carbide single crystal |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546821A (en) * | 2021-07-22 | 2021-10-26 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Coating method of silicon carbide seed crystal |
| WO2024050843A1 (en) * | 2022-09-09 | 2024-03-14 | 眉山博雅新材料股份有限公司 | Crystal growth method and apparatus |
| CN116516468A (en) * | 2023-07-04 | 2023-08-01 | 苏州优晶光电科技有限公司 | Device and method for simultaneously treating multiple silicon carbide seed crystal coatings |
| CN116516468B (en) * | 2023-07-04 | 2023-10-13 | 苏州优晶光电科技有限公司 | Device and method for simultaneously treating multiple silicon carbide seed crystal coatings |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112962083A (en) | Device and method for coating film on back of seed crystal for growing silicon carbide single crystal | |
| CN111621851B (en) | Silicon carbide crystal growth device and method | |
| CN109280976B (en) | Large-size high-purity silicon carbide single crystal, single crystal substrate and preparation method thereof | |
| RU2764040C2 (en) | Growing epitaxial 3c-sic on monocrystalline silicon | |
| WO2010121451A1 (en) | Method and apparatus for deposition-forming semiconductor film on substrate by close-spaced sublimation technology | |
| WO2007072855A1 (en) | Apparatus for manufacturing semiconductor thin film | |
| EP0865518A1 (en) | A device for heat treatment of objects and a method for producing a susceptor | |
| CN102668033A (en) | Semiconductor thin-film manufacturing method, seminconductor thin-film manufacturing apparatus, susceptor, and susceptor holding tool | |
| CN111424319B (en) | Preparation method of large-size kilogram-level silicon carbide single crystal | |
| CN112831840B (en) | Single crystal growing device | |
| CN113026106B (en) | Growth process of silicon carbide crystal | |
| TW201930659A (en) | Tantalum carbide coated carbon material, manufacturing method thereof, and member for apparatus for manufacturing semiconductor single crystal | |
| US5356608A (en) | Preparation of a high purity aluminum nitride antenna window by organometallic pyrolysis | |
| CN111033692A (en) | Vapor phase growth method | |
| JP2016050164A (en) | SiC chemical vapor deposition apparatus | |
| CN109280964B (en) | Thermal field structure for growing silicon carbide single crystal | |
| JP2550024B2 (en) | Low pressure CVD equipment | |
| CN110373714B (en) | Method for rapidly preparing large-size high-quality single-layer graphene at room temperature | |
| JP4309509B2 (en) | Method for producing crucible for single crystal growth comprising pyrolytic graphite | |
| JPH03243776A (en) | Graphite member for cvd | |
| CN112458532A (en) | Device and method for preparing silicon carbide single crystal through high-temperature chemical deposition | |
| JPS6045159B2 (en) | Method for manufacturing silicon carbide crystal layer | |
| JP4222630B2 (en) | Method for epitaxially growing objects and apparatus for performing such growth | |
| CN202039157U (en) | Bell jar type hot-wall silicon carbide high-temperature epitaxial wafer growing device | |
| JPS6115150B2 (en) |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210615 |
|
| WD01 | Invention patent application deemed withdrawn after publication |