Method for determining the silicon and carbon faces of 3c-sic single crystal wafers
By performing molten alkaline etching on 3C-SiC single crystal wafers and observing the surface morphology, the problem of not being able to distinguish between the (111)Si plane and the ()C plane in the existing technology was solved, realizing simple and accurate crystal plane identification and supporting the industrialization process of 3C-SiC single crystals.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-14
- Publication Date
- 2026-03-24
AI Technical Summary
Existing technologies fail to effectively distinguish between the (111)Si plane and the ()C plane of a 3C-SiC single crystal wafer, affecting its accurate selection in seed crystal growth and epitaxial processes.
By immersing 3C-SiC single crystal wafers in molten alkali for etching treatment, observing the surface morphology after etching, and using the difference between stacking faults and dislocation corrosion pits to distinguish between (111)Si plane and ()C plane.
This provides a simple and reliable method that can quickly and accurately distinguish the two crystal planes of 3C-SiC single crystal wafers. It is applicable to wafers and epitaxial wafers at different processing stages and supports industrial applications.
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Figure CN121207971B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of semiconductor materials. Specifically, this invention relates to a method for determining the silicon and carbon surfaces of a 3C-SiC (cubic silicon carbide) single-crystal wafer. Background Technology
[0002] Silicon carbide (SiC) is widely used in new energy vehicles, photovoltaics and 5G communications due to its excellent properties such as wide bandgap, high breakdown field strength, high saturated electron drift velocity and high thermal conductivity.
[0003] SiC crystal structures are diverse, with over 250 types discovered to date. Among them, the hexagonal crystal systems (such as 4H-SiC and 6H-SiC), the cubic crystal system (3C-SiC), and the rhombic crystal system (15R-SiC) are the most common. Compared to 4H-SiC, 3C-SiC exhibits higher carrier mobility (approximately 2-4 times) and lower interface state defect density (approximately one order of magnitude lower). Therefore, fabricating metal-oxide-semiconductor field-effect transistors (MOSFETs) based on 3C-SiC holds promise for solving the device reliability problem caused by gate oxide interface defects in 4H-SiC MOSFETs.
[0004] Recent studies have shown that 2- to 6-inch 3C-SiC single crystals can be successfully epitaxially grown on 4H-SiC seed crystals using the high-temperature solution growth method (HTSG) and by controlling the solid-liquid interface energy between the cosolvent and the crystal (see Energy Environ. Mater., 2024, 7(4): e12678; Crystal Growth and Design, 2025, 25, 1211-1216). Since this process is typically performed on 4H-SiC (000... The process is carried out on a seed crystal, and the resulting 3C-SiC single crystal is obtained along the surface. <111> Crystalline growth, with the two surfaces of the wafer being (111) plane and (...). ) face. In 3C-SiC, the (111) face is terminated by silicon atoms [i.e., the (111)Si face], while ( The surface terminates at a carbon atom [i.e. ( (Side C)
[0005] These two crystal planes have vastly different physicochemical properties, therefore, they must be accurately distinguished when used as seed crystals for crystal growth or in homoepitaxial growth or heteroepitaxial growth during subsequent device fabrication. However, existing technologies do not provide an effective method for distinguishing between the two crystal planes.
[0006] In summary, there is an urgent need to develop a method that can accurately distinguish between the (111)Si plane and (...) of 3C-SiC. The C-plane method will provide a key basis for selecting 3C-SiC as the seed crystal for single crystal growth and for the selection of crystal planes in subsequent epitaxial processes, thereby accelerating the industrialization process of large-size 3C-SiC single wafers. Summary of the Invention
[0007] The purpose of this invention is to provide a method for determining the silicon and carbon faces of a 3C-SiC single crystal wafer. This method can clearly distinguish the (111)Si face and (111)C face of a 3C-SiC single crystal by the difference in characteristic corrosion morphology (stacking faults and dislocation pits). The method of this invention is simple to operate and easy to implement, and can achieve the processing of 3C-SiC substrate wafers, polished wafers, grinding wafers and diced wafers (111) Si surface and ( The distinction between the (111) Si plane and the ( ) C plane of the 3C-SiC epitaxial wafer can also be used to differentiate between them. The C-side is differentiated for industrial applications.
[0008] The above-mentioned objective of the present invention is achieved through the following technical solution.
[0009] This invention provides a method for determining the silicon and carbon faces of a 3C-SiC single crystal wafer, comprising the following steps:
[0010] (1) Immerse the 3C-SiC single crystal wafer in molten alkali for etching treatment;
[0011] (2) Remove the etched 3C-SiC single crystal wafer and observe its surface morphology:
[0012] - If the surface only exhibits stacking fault characteristics, then the surface is determined to be ( C side;
[0013] - If the surface has both stacking faults and dislocation corrosion pits, then the surface is determined to be the (111)Si surface.
[0014] The inventors of this application unexpectedly discovered that by immersing a 3C-SiC single crystal wafer in molten alkali for etching, the morphology of the etched 3C-SiC single crystal wafer can be observed to accurately determine the (111) Si plane and (… Side C.
[0015] Preferably, in the method described in this invention, the temperature of the molten alkali is 450-550°C.
[0016] Preferably, in the method described in this invention, the molten alkali is selected from one or more of KOH, NaOH, and Na2O2. For example, the molten alkali can be a mixed alkali of KOH and Na2O2, wherein the mass fraction of Na2O2 in the mixed alkali is less than or equal to 16%.
[0017] Preferably, in the method of the present invention, the corrosion treatment is performed for 1-60 minutes. More preferably, in the method of the present invention, the corrosion treatment is performed for 1-10 minutes.
[0018] Preferably, in the method described in this invention, the method further includes the following step prior to step (1): cleaning the surface of the 3C-SiC single crystal wafer.
[0019] Preferably, in the method described in this invention, the cleaning process is performed by cleaning the wafer using an acidic solution and / or an alkaline solution.
[0020] Preferably, in the method described in this invention, the method further includes the following step after removing the etched 3C-SiC single crystal wafer in step (2): placing the etched 3C-SiC single crystal wafer in an organic solvent for ultrasonic cleaning.
[0021] Preferably, in the method described in this invention, the organic solvent is ethanol and / or acetone, and the ultrasonic cleaning is performed for 1-30 minutes.
[0022] Preferably, in the method described in this invention, the method further includes the following step after ultrasonic cleaning: drying the ultrasonically cleaned wafer with high-purity inert gas.
[0023] Preferably, in the method described in this invention, the high-purity inert gas is high-purity argon and / or high-purity nitrogen.
[0024] Preferably, in the method described in this invention, the purity of the high-purity nitrogen gas is greater than or equal to 99.999%, and the purity of the high-purity argon gas is greater than or equal to 99.999%.
[0025] Preferably, in the method described in this invention, the observation in step (2) is performed using an optical microscope.
[0026] Preferably, in the method described in this invention, the 3C-SiC single crystal wafer is n-type, p-type, or semi-insulating.
[0027] Preferably, in the method described in this invention, the surface orientation of the 3C-SiC single crystal wafer is (111) crystal axis direction.
[0028] Preferably, in the method described in this invention, the 3C-SiC single crystal wafer is a diced wafer, a grinding wafer, a polished wafer, or a substrate wafer.
[0029] Preferably, in the method described in this invention, the dicing wafer is a wafer obtained by dicing a 3C-SiC ingot using a single-wire dicing machine or a multi-wire dicing machine, with a surface roughness of 0.2-2 μm.
[0030] Preferably, in the method described in this invention, the grinding wafer is a wafer obtained by thinning a 3C-SiC diced wafer using a single-sided grinder, a double-sided grinder, or a thinning machine, with a surface roughness of 20-80 nm.
[0031] Preferably, in the method described in this invention, the polishing wafer is a wafer obtained by polishing a 3C-SiC grinding wafer with a mechanical polishing machine, and the surface roughness is 1-5 nm.
[0032] Preferably, in the method described in this invention, the substrate is a 3C-SiC polished wafer that has undergone chemical mechanical polishing and cleaning, and has a surface roughness of less than 0.5 nm.
[0033] Preferably, in the method described in this invention, the molten alkali in step (1) is melted in a crucible.
[0034] Preferably, in the method described in this invention, the crucible is a nickel crucible, a silver crucible, a high-nickel alloy crucible, or a graphite crucible.
[0035] Preferably, in the method described in this invention, the molten alkali in step (1) is heated by a corrosion furnace.
[0036] Preferably, in the method described in this invention, the corrosion furnace is a muffle furnace or a tubular furnace.
[0037] In some specific embodiments of the present invention, the method of the present invention includes the following steps:
[0038] (1) Clean the surface of the 3C-SiC wafer;
[0039] (2) Place the alkali in a crucible;
[0040] (3) Set the temperature of the corrosion furnace to 450-550°C;
[0041] (4) After the temperature of the corrosion furnace reaches the set temperature, put the crucible containing alkali into the corrosion furnace;
[0042] (5) After the alkali melts, the 3C-SiC single crystal wafer is immersed in the molten alkali for etching;
[0043] (6) After etching at a set temperature of 450-550°C for 1-60 minutes, the 3C-SiC single crystal wafer is removed from the molten alkali;
[0044] (7) Place the etched 3C-SiC single crystal wafer in ethanol and sonicate for 1-30 min;
[0045] (8) Remove the 3C-SiC single crystal wafer and dry it with high-purity inert gas;
[0046] (9) Observe the surface morphology of the wafer using an optical microscope: If only stacking fault features appear on the surface, then the surface is ( ) C surface; if stacking faults and dislocation corrosion pits exist on the surface at the same time, then the surface is (111) Si surface.
[0047] In some specific embodiments of the present invention, cleaning the 3C-SiC wafer surface in step (1) is achieved by a method comprising the following steps:
[0048] The 3C-SiC wafer was boiled in a solution of sulfuric acid and hydrogen peroxide with a volume ratio of 4:1 for 10-20 minutes at a temperature of 75-85℃; then rinsed with deionized water for 5 minutes; then boiled in a mixed solution of ammonia, hydrogen peroxide and deionized water with a volume ratio of 0.5:1:5 for 5 minutes at a temperature of 85℃; then rinsed with deionized water for 5 minutes; finally, the 3C-SiC wafer was dried with high-purity inert gas.
[0049] The present invention has the following beneficial effects:
[0050] (1) This invention provides a clear and reliable method for distinguishing crystal planes for the first time. This invention is the first to discover and utilize molten alkali to distinguish the (111)Si plane and (…) of a 3C-SiC single crystal. The inherent differences in corrosion morphology of the C-plane: (111) The Si-plane will simultaneously exhibit stacking faults and dislocation corrosion pits, while ( The C-plane shows only stacking faults. By observing this significant morphological contrast, the two crystal planes can be quickly and accurately distinguished.
[0051] (2) It has excellent universality and wide applicability. This method is not only applicable to the final substrate wafer, but can also effectively distinguish wafers at different processing stages (such as cutting, grinding, and polishing), and can identify epitaxial wafers. This wide applicability allows it to be seamlessly integrated into existing wafer fabrication and device manufacturing processes.
[0052] (3) Simple operation and easy to industrialize. The method has a simple process, requires conventional equipment, does not require high operator skills, and has good process repeatability and low cost. These characteristics make it very suitable for large-scale industrial production, providing key and practical technical support for the industrialization of 3C-SiC single crystal materials. Attached Figure Description
[0053] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings, wherein:
[0054] Figure 1 The image shows an optical photograph of the (111) Si surface obtained by etching a 3C-SiC single crystal wafer using Example 1. The long strips in the image represent stacking fault corrosion morphology, and the irregular and regular triangles represent dislocation corrosion pits.
[0055] Figure 2 The method used in Example 1 to etch a 3C-SiC single crystal wafer ( Optical photograph of surface C, where the long strips represent stacking fault corrosion morphology;
[0056] Figure 3 The image shows an optical photograph of the (111) Si surface obtained by etching a 3C-SiC single crystal wafer using Example 2. The long strips in the image represent stacking fault corrosion morphology, and the irregular and regular triangles represent dislocation corrosion pits.
[0057] Figure 4 The 3C-SiC single crystal obtained by etching in Example 2 ( Optical photograph of surface C, where the long strips represent stacking fault corrosion morphology;
[0058] Figure 5 The image shows an optical photograph of the (111) Si surface obtained by etching a 3C-SiC single crystal wafer using Example 3. The long strips in the image represent stacking fault corrosion morphology, and the irregular and regular triangles represent dislocation corrosion pits.
[0059] Figure 6 The method used in Example 3 to etch a 3C-SiC single crystal wafer ( The image shows an optical photograph of surface C, where the long strips represent stacking fault corrosion morphology.
[0060] Figure 7 To obtain by etching a 3C-SiC single crystal using Comparative Example 1 ( The optical photograph of side C shows no corrosion defects.
[0061] Figure 8 The image shows an optical photograph of the (111) Si surface obtained by etching a 3C-SiC single crystal using Comparative Example 1. No etching defects were found. Detailed Implementation
[0062] The present invention will be further described in detail below with reference to specific embodiments. The embodiments given are only for illustrating the present invention and are not intended to limit the scope of the present invention.
[0063] Example 1
[0064] (1) The known (111)Si surface with a surface roughness of 0.2 nm is compared with ( The 3C-SiC single crystal substrate on the C-side was boiled in a solution of sulfuric acid and hydrogen peroxide with a volume ratio of 4:1 for 10 minutes at a temperature of 80°C; then rinsed with deionized water for 5 minutes; then boiled in a mixed solution of ammonia, hydrogen peroxide and deionized water with a volume ratio of 0.5:1:5 for 5 minutes at a temperature of 85°C; then rinsed with deionized water for 5 minutes; finally, the 3C-SiC wafer was dried with high-purity N2.
[0065] (2) Put potassium hydroxide (KOH) and sodium peroxide (Na2O2) into a nickel (Ni) crucible, wherein the weight ratio of KOH to Na2O2 is 4:1; then, set the temperature of the muffle furnace to 550°C, and after the temperature of the corrosion furnace reaches the set temperature, put the Ni crucible containing KOH and Na2O2 into the muffle furnace.
[0066] (3) After KOH and Na2O2 are melted, the 3C-SiC single crystal wafer is immersed in the molten KOH and Na2O2 and etched at 550℃ for 30 min.
[0067] (4) Take out the 3C-SiC single crystal wafer, then clean it with ethanol for 10 minutes by ultrasonic cleaning, and then dry the wafer with high-purity N2.
[0068] (5) Observe the surface morphology of the wafer using an optical microscope, such as Figure 1 and Figure 2 As shown, ( The C-surface shows only stacking fault corrosion morphology, while the Si-surface shows both stacking fault and dislocation corrosion pit morphology.
[0069] It can be seen that the (111)Si plane of the 3C-SiC single crystal wafer, as determined by the testing method of the present invention, is different from the (111)Si plane. The C-plane is accurate and conforms to the (111) Si plane of the 3C-SiC single crystal wafer that was determined before conducting the test method of this invention. The fact of side C.
[0070] Example 2
[0071] (1) The known (111)Si surface with a surface roughness of 2 μm is compared with ( The 3C-SiC wafers on the C-side were boiled in a solution of sulfuric acid and hydrogen peroxide with a volume ratio of 4:1 for 10 minutes at 80°C; then rinsed with deionized water for 5 minutes; subsequently boiled in a mixed solution of ammonia, hydrogen peroxide, and deionized water with a volume ratio of 0.5:1:5 for 5 minutes at 85°C; then rinsed with deionized water for 5 minutes; and finally dried with high-purity N2.
[0072] (2) Put potassium hydroxide (KOH) into a nickel (Ni) crucible, and then set the temperature of the muffle furnace to 550°C. After the temperature of the corrosion furnace reaches the set temperature, put the Ni crucible containing KOH into the muffle furnace.
[0073] (3) After KOH is melted, the 3C-SiC single crystal wafer is immersed in the molten KOH and etched at 550°C for 30 min.
[0074] (4) Take out the 3C-SiC single crystal wafer, then clean it with acetone for 30 minutes by ultrasonic cleaning, and then dry the wafer with high-purity N2.
[0075] (5) Observe the surface morphology of the wafer using an optical microscope, such as Figure 3 and Figure 4 As shown, ( The C-surface shows only stacking fault corrosion morphology, while the Si-surface shows both stacking fault and dislocation corrosion pit morphology.
[0076] It can be seen that the (111)Si plane of the 3C-SiC single crystal wafer, as determined by the testing method of the present invention, is different from the (111)Si plane. The C-plane is accurate and conforms to the (111) Si plane of the 3C-SiC single crystal wafer that was determined before conducting the test method of this invention. The fact of side C.
[0077] Example 3
[0078] (1) The known (111)Si surface with a surface roughness of 2 μm is compared with ( The 3C-SiC wafers on the C-side were boiled in a solution of sulfuric acid and hydrogen peroxide with a volume ratio of 4:1 for 10 minutes at 80°C; then rinsed with deionized water for 5 minutes; subsequently boiled in a mixed solution of ammonia, hydrogen peroxide, and deionized water with a volume ratio of 0.5:1:5 for 5 minutes at 85°C; then rinsed with deionized water for 5 minutes; finally, the 3C-SiC wafers were dried using high-purity N2.
[0079] (2) Put potassium hydroxide (KOH) into a nickel (Ni) crucible, and then set the temperature of the muffle furnace to 450°C. After the temperature of the corrosion furnace reaches the set temperature, put the Ni crucible containing KOH into the muffle furnace.
[0080] (3) After KOH is melted, the 3C-SiC single crystal wafer is immersed in KOH alkali and etched at 450℃ for 10 min.
[0081] (4) Take out the 3C-SiC single crystal wafer, then clean it with acetone for 5 minutes by ultrasonic cleaning, and then dry the wafer with high-purity N2.
[0082] (5) Observe the surface morphology of the wafer using an optical microscope, such as Figure 5 and Figure 6 As shown, ( The C-surface shows only stacking fault corrosion morphology, while the Si-surface shows both stacking fault and dislocation corrosion pit morphology.
[0083] It can be seen that the (111)Si plane of the 3C-SiC single crystal wafer, as determined by the testing method of the present invention, is different from the (111)Si plane. The C-plane is accurate and conforms to the (111) Si plane of the 3C-SiC single crystal wafer that was determined before conducting the test method of this invention. The fact of side C.
[0084] Example 4
[0085] (1) The known (111)Si surface with a surface roughness of 2 μm is compared with ( The 3C-SiC wafers on the C-side were boiled in a solution of sulfuric acid and hydrogen peroxide with a volume ratio of 4:1 for 10 minutes at 80°C; then rinsed with deionized water for 5 minutes; subsequently boiled in a mixed solution of ammonia, hydrogen peroxide, and deionized water with a volume ratio of 0.5:1:5 for 5 minutes at 85°C; then rinsed with deionized water for 5 minutes; and finally dried with high-purity N2.
[0086] (2) Put potassium hydroxide (KOH) into a nickel (Ni) crucible, and then set the temperature of the muffle furnace to 500°C. After the temperature of the corrosion furnace reaches the set temperature, put the Ni crucible containing KOH into the muffle furnace.
[0087] (3) After KOH is melted, the 3C-SiC single crystal wafer is immersed in the molten KOH and etched at 500℃ for 5 min.
[0088] (4) Take out the 3C-SiC single crystal wafer, then clean it with ethanol for 10 minutes by ultrasonic cleaning, and then dry the wafer with high-purity N2.
[0089] (5) Observe the surface morphology of the wafer using an optical microscope. The C-surface shows only stacking fault corrosion morphology, while the Si-surface shows both stacking fault and dislocation corrosion pit morphology.
[0090] It can be seen that the (111)Si plane of the 3C-SiC single crystal wafer, as determined by the testing method of the present invention, is different from the (111)Si plane. The C-plane is accurate and conforms to the (111) Si plane of the 3C-SiC single crystal wafer that was determined before conducting the test method of this invention. The fact of side C.
[0091] Comparative Example 1
[0092] (1) The known (111)Si surface with a surface roughness of 0.2 nm is compared with ( The 3C-SiC single crystal substrate on the C-side was boiled in a solution of sulfuric acid and hydrogen peroxide with a volume ratio of 4:1 for 10 minutes at a temperature of 80°C; then rinsed with deionized water for 5 minutes; then boiled in a mixed solution of ammonia, hydrogen peroxide and deionized water with a volume ratio of 0.5:1:5 for 5 minutes at a temperature of 85°C; then rinsed with deionized water for 5 minutes; finally, the 3C-SiC wafer was dried with high-purity N2.
[0093] (2) Put potassium hydroxide (KOH) and sodium peroxide (Na2O2) into a nickel (Ni) crucible, wherein the weight ratio of KOH to Na2O2 is 4:1; then, set the temperature of the muffle furnace to 440°C, and after the temperature of the corrosion furnace reaches the set temperature, put the Ni crucible containing KOH and Na2O2 into the muffle furnace.
[0094] (3) After KOH and Na2O2 are melted, the 3C-SiC single crystal wafer is immersed in the molten KOH and Na2O2 and etched at 440℃ for 30 min.
[0095] (4) Take out the 3C-SiC single crystal wafer, then clean it with ethanol for 10 minutes by ultrasonic cleaning, and then dry the wafer with high-purity N2.
[0096] (5) Observe the surface morphology of the wafer using an optical microscope, such as Figure 7 and Figure 8 As shown, due to insufficient etching temperature, the (111)Si plane of the 3C-SiC single crystal wafer and ( No etched dislocations or stacking faults were found on the (111) Si plane of the 3C-SiC single crystal wafer, making it impossible to compare the (111) Si plane with the ( (C) side is used for differentiation.
Claims
1. A method for determining the silicon and carbon faces of a 3C-SiC single crystal wafer, comprising the following steps: (1) Immerse the 3C-SiC single crystal wafer in molten alkali for etching treatment; (2) Remove the etched 3C-SiC single crystal wafer and observe its surface morphology: - If the surface only exhibits stacking fault characteristics, then the surface is determined to be ( C side; - If the surface has both stacking faults and dislocation corrosion pits, then the surface is determined to be (111)Si surface; The temperature of the molten alkali is 450-550℃; The molten alkali is selected from one or more of KOH, NaOH and Na2O2; The corrosion treatment is performed for 5-30 minutes.
2. The method according to claim 1, wherein, The method also includes the following steps prior to step (1): cleaning the surface of the 3C-SiC single crystal wafer.
3. The method according to claim 2, wherein, The cleaning process is performed by cleaning the wafer using an acidic solution and / or an alkaline solution.
4. The method according to claim 1, wherein, The method further includes the following steps after removing the etched 3C-SiC single crystal wafer in step (2): placing the etched 3C-SiC single crystal wafer in an organic solvent for ultrasonic cleaning.
5. The method according to claim 4, wherein, The organic solvent is ethanol and / or acetone, and the ultrasonic cleaning is performed for 1-30 minutes.
6. The method according to claim 4, wherein, The method also includes the following step after ultrasonic cleaning: drying the ultrasonically cleaned wafer with high-purity inert gas.
7. The method according to claim 6, wherein, The high-purity inert gas is high-purity argon and / or high-purity nitrogen.
8. The method according to claim 7, wherein, The purity of the high-purity nitrogen gas is greater than or equal to 99.999%, and the purity of the high-purity argon gas is greater than or equal to 99.999%.
9. The method according to claim 1, wherein, The observation in step (2) is performed using an optical microscope.
10. The method according to claim 1, wherein, The 3C-SiC single crystal wafer is n-type, p-type, or semi-insulating.
11. The method according to claim 1, wherein, The surface orientation of the 3C-SiC single crystal wafer is (111) crystal axis direction.
12. The method according to claim 1, wherein, The 3C-SiC single crystal wafer is a diced wafer, a grinding wafer, a polished wafer, or a substrate wafer.
13. The method according to claim 12, wherein, The dicing wafer is a wafer obtained by cutting a 3C-SiC ingot using a single-wire dicing machine or a multi-wire dicing machine, with a surface roughness of 0.2-2 μm.
14. The method according to claim 12, wherein, The grinding wafer is a wafer obtained by thinning a 3C-SiC diced wafer using a single-sided grinding machine, a double-sided grinding machine, or a thinning machine, with a surface roughness of 20-80 nm.
15. The method according to claim 12, wherein, The polishing wafer is a wafer obtained by polishing a 3C-SiC grinding wafer with a mechanical polishing machine, and the surface roughness is 1-5 nm.
16. The method according to claim 12, wherein, The substrate is a 3C-SiC polished wafer that has undergone chemical mechanical polishing and cleaning, with a surface roughness of less than 0.5 nm.
17. The method according to claim 1, wherein, The molten alkali in step (1) is molten in a crucible.
18. The method according to claim 17, wherein, The crucible is a nickel crucible, a silver crucible, a high-nickel alloy crucible, or a graphite crucible.
19. The method according to claim 1, wherein, The molten alkali in step (1) is heated by a corrosion furnace.
20. The method according to claim 19, wherein, The corrosion furnace is a muffle furnace or a tube furnace.
Citation Information
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