CN115852477A - Method and device for manufacturing high-quality silicon carbide single crystal layer - Google Patents
Method and device for manufacturing high-quality silicon carbide single crystal layer Download PDFInfo
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Abstract
The invention provides a method and a device for manufacturing a high-quality silicon carbide single crystal layer, wherein the method for manufacturing the high-quality silicon carbide single crystal layer comprises the following steps: providing a growth cavity, and arranging a first heating module and a second heating module on the periphery of the growth cavity; (II) providing a silicon carbide raw material and at least one target substrate, and placing the target substrate in the growth chamber; and (III) independently heating different areas in the growth cavity by adopting the first heating module and the second heating module to form a temperature difference between the silicon carbide raw material and the target substrate, generating an atmosphere containing silicon and carbon in the growth cavity, and depositing the silicon carbide raw material on the surface of the target substrate to grow and obtain the silicon carbide single crystal layer. The invention does not need to use silicon source gases such as poisonous and harmful silane and the like, has high growth speed which can reach tens of microns to hundreds of microns per hour, improves the growth quality, and ensures that the BPD density of the grown silicon carbide single crystal layer is lower than 0.1.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and relates to a method and a device for manufacturing a high-quality silicon carbide single crystal layer.
Background
Silicon carbide is a wide bandgap semiconductor material, and devices manufactured by using a silicon carbide single crystal substrate have the advantages of high temperature resistance, high pressure resistance, high frequency, high power, radiation resistance, high efficiency and the like, and have important application values in the fields of radio frequency, new energy and the like.
One of the necessary processes for manufacturing a semiconductor device using silicon carbide is: a high-quality single-crystal layer is formed on a silicon carbide single-crystal substrate. At present, the method for forming a high quality single crystal layer is mainly Chemical Vapor Deposition (CVD), and the working principle thereof is: and under a high-temperature environment, filling mixed gas comprising silicon source gas and carbon source gas into the reaction chamber, so that the silicon source gas and the carbon source gas are subjected to chemical reaction to form a silicon carbide single crystal thin layer on the silicon carbide single crystal substrate. However, the growth rate of chemical vapor deposition is slow, only several microns per hour, which reduces the working efficiency, and in addition, the commonly used silicon source gas silane has pungent odor and toxicity, which has potential safety hazard.
Therefore, it is important to provide a method for manufacturing a single crystal layer having a high growth rate and high safety.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method and a device for manufacturing a high-quality silicon carbide single crystal layer, which do not need to use toxic and harmful silicon source gases such as silane and the like, have high growth speed which can reach tens of microns to hundreds of microns per hour, improve the growth efficiency and have higher safety.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for producing a high-quality silicon carbide single crystal layer, the method comprising:
providing a growth cavity, and arranging a first heating module and a second heating module on the periphery of the growth cavity;
(II) providing a silicon carbide raw material and at least one target substrate, and placing the target substrate in the growth chamber;
and (III) independently heating different areas in the growth cavity by adopting the first heating module and the second heating module to form a temperature difference between the silicon carbide raw material and the target substrate, generating an atmosphere containing silicon and carbon in the growth cavity, and depositing the silicon carbide raw material on the surface of the target substrate to grow and obtain the silicon carbide single crystal layer.
According to the invention, the first heating module and the second heating module are adopted to respectively heat different areas in the growth cavity, the first heating module is used for heating the silicon carbide raw material, the second heating module is used for heating the target substrate, so that the heating temperature is controllable, the silicon carbide raw material and the target substrate form a temperature difference, the silicon carbide raw material is conveyed to the surface of the target substrate, and the silicon carbide single crystal layer is obtained by growth.
As a preferred technical scheme of the invention, the material of the growth cavity is any one of high-purity graphite, silicon carbide, tantalum, tungsten, molybdenum, tantalum carbide, tungsten carbide and molybdenum carbide.
When the material of the growth chamber is silicon carbide, the growth of the silicon carbide single crystal layer can be directly carried out by taking the growth chamber as the silicon carbide raw material without adding extra silicon carbide raw material.
The target substrate is single crystal silicon carbide.
The target substrate has a crystal form of 4H, 6H or 3C.
And the growth surface of the target substrate is a Si surface or a C surface.
The included angle between the (0001) surface of the target substrate single crystal and the growth surface of the target substrate is less than or equal to 8 degrees.
The temperature in the growth chamber is 1500 to 2300 ℃, and may be, for example, 1500 ℃, 1550 ℃, 1600 ℃, 1700 ℃, 1800 ℃, 1900 ℃, 2000 ℃, 2100 ℃, 2200 ℃ or 2300 ℃, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
The air pressure in the growth chamber is 10 to 5000Pa, and may be, for example, 10Pa, 100Pa, 200Pa, 500Pa, 1000Pa, 1500Pa, 2000Pa, 2500Pa, 3000Pa, 3500Pa, 4000Pa, 4500Pa or 5000Pa, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
The temperature difference is 1 to 50 ℃, and may be, for example, 1 ℃, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 48 ℃ or 50 ℃, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
The growth rate is 1 to 200. Mu.m/h, and may be, for example, 1 μm/h, 5 μm/h, 10 μm/h, 15 μm/h, 20 μm/h, 30 μm/h, 50 μm/h, 60 μm/h, 80 μm/h, 100 μm/h, 120 μm/h, 150 μm/h, 160 μm/h, 180 μm/h or 200 μm/h, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
The thickness of the silicon carbide single crystal layer is 1 to 100. Mu.m, and may be, for example, 1 μm, 5 μm, 10 μm, 20 μm, 30 μm, 50 μm, 60 μm, 80 μm, 90 μm or 100 μm, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
The basal plane dislocation density BPD of the silicon carbide single crystal layer is less than 0.1/cm -2 。
As a preferred embodiment of the present invention, the growing of the silicon carbide single crystal layer specifically includes:
the first heating module and the second heating module are adopted to respectively heat the growth cavity and the target substrate, so that the temperature of the inner cavity wall of the growth cavity is higher than that of the target substrate, silicon carbide raw materials of the inner cavity wall of the growth cavity are sublimated and deposited on the surface of the target substrate, the silicon carbide single crystal layer grows and is formed, and the growth cavity is made of silicon carbide.
When the growth cavity is made of silicon carbide materials, the growth cavity is used as a silicon carbide raw material to provide materials required by growth of a silicon carbide single crystal layer for a target substrate, the growth cavity is heated by a first heating module, the target substrate is heated by a second heating module, and the first heating module and the second heating module are respectively regulated and controlled to enable the growth cavity and the target substrate to form a temperature difference, so that the silicon carbide raw material on the inner cavity wall of the growth cavity is sublimated and moves to the surface of the target substrate to realize growth of the silicon carbide single crystal layer; when the material of the growth cavity is not silicon carbide, other silicon carbide raw materials are introduced into the growth cavity to provide the target substrate with the material required for growing the silicon carbide single crystal layer.
As a preferred embodiment of the present invention, the growing of the silicon carbide single crystal layer specifically includes:
providing at least one source substrate, and placing the source substrate in the growth cavity;
respectively heating the source substrate and the target substrate by using the first heating module and the second heating module to enable the temperature of the source substrate to be higher than that of the target substrate, so as to sublimate the source substrate, deposit the source substrate on the surface of the target substrate and grow to form the silicon carbide single crystal layer;
the source substrate is single crystal silicon carbide or polycrystalline silicon carbide.
According to the invention, other source substrates are introduced into a growth cavity, materials required for growing the silicon carbide single crystal layer are provided for a target substrate, the source substrate is heated by a first heating module, the target substrate is heated by a second heating module, the source substrate and the target substrate are respectively corresponding to different heating modules to regulate and control the temperature, so that a temperature difference is formed between the source substrate and the target substrate, the source substrate is sublimated and moves to the surface of the target substrate, and the growth of the silicon carbide single crystal layer is realized.
As a preferable embodiment of the present invention, the growing of the silicon carbide single crystal layer further includes:
providing at least one silicon source, and placing the silicon source in the growth chamber;
and adjusting the heating temperature of the first heating module and the second heating module to evaporate the silicon source so as to regulate and control the content of silicon and carbon in the growth cavity.
According to the invention, the silicon source is arranged and evaporated to change the atomic number ratio of silicon and carbon in the atmosphere in the growth cavity, so that the growth rate is improved. Because the evaporation temperature of silicon is lower than carborundum, accessible heat conduction, heat radiation obtain the heat and heat up to evaporation temperature, consequently, need not to set up corresponding heating element for the silicon source, at the in-process of carborundum raw materials, carborundum substrate or the target substrate of heating growth chamber inner chamber wall, can realize the evaporation of silicon source.
The method for producing a high-quality silicon carbide single crystal layer further comprises:
providing a vacuum chamber, and placing the growth chamber in an inner cavity of the vacuum chamber;
and pumping the vacuum chamber while filling the process gas into the vacuum chamber.
The process gas comprises any one or a combination of at least two of argon, nitrogen or helium.
As a preferred embodiment of the present invention, the method for producing a high-quality silicon carbide single crystal layer further includes: before the growth, etching the surface of the target substrate;
the specific way of the etching treatment is as follows:
and adjusting the heating temperature of the first heating module and the second heating module to enable the temperature of the target substrate to be higher than the temperature of the inner cavity wall of the growth cavity part, so that the surface raw material of the target substrate is sublimated and deposited on the inner cavity wall of the growth cavity, and scratches, scratches or damages on the surface of the target substrate are removed.
Or, the specific way of the etching treatment is as follows:
and adjusting the heating temperature of the first heating module and the second heating module to enable the temperature of the target substrate to be higher than that of the source substrate, so that the surface raw material of the target substrate is sublimated and deposited on the source substrate, and scratches, scratches or damages on the surface of the target substrate are removed.
The invention firstly carries out etching treatment on the target substrate and then carries out the growth of the single crystal layer. The surface of the etched target substrate is free of scratches, scratches or damaged layers, on the basis of which the single crystal layer produced has a higher quality with a lower dislocation density.
In the etching treatment process, the temperature in a growth cavity is 1500-2300 ℃, the air pressure in the growth cavity is 10-5000 Pa, the temperature difference is 1-50 ℃, the etching speed is 1-200 mu m/h, and the etching thickness is 1-100 mu m.
In a second aspect, the present invention provides an apparatus for manufacturing a high-quality silicon carbide single crystal layer, which is used in the method for manufacturing a high-quality silicon carbide single crystal layer according to the first aspect, and which comprises a growth chamber in which at least one target substrate is disposed, and a first heating module and a second heating module which are disposed on the periphery of the growth chamber and are used for heating different regions in the growth chamber, respectively.
As a preferred technical solution of the present invention, at least one source substrate is further disposed in the growth chamber.
The invention does not have specific limitation or special requirements on the structure and the size thickness of the source substrate and the target substrate, and exemplarily, the source substrate with a square, circular, prismatic or circular cross section structure can be adopted; the target substrate can be in a disc shape, the diameter is 1~8 inches, the thickness is 300 to 1000 mu m, and the target substrate can be adjusted by a person skilled in the art according to actual conditions.
The first heating module is arranged corresponding to the source substrate and used for heating the source substrate.
The second heating module is arranged corresponding to the target substrate and used for heating the target substrate.
The first heating module includes at least one first heating assembly located above and/or below the source substrate.
The second heating module includes at least one second heating assembly located above and/or below the target substrate.
The cross section of the growth cavity is rectangular.
The first heating assembly and the second heating assembly are positioned on at least one side of the long edge of the growth cavity.
Short edges on two sides of the growth cavity are respectively provided with air vents which penetrate through the cavity wall of the growth cavity.
The growth cavity has a flat internal space, the internal height is narrow (namely the short side of the growth cavity), and the short sides at two sides of the growth cavity are provided with vent holes within the range of 0.5-5 mm, so that the interior of the growth cavity is communicated with the external atmosphere. In addition, a first heating assembly is arranged above and/or below the corresponding source substrate and a second heating assembly is arranged above and below the corresponding target substrate outside the long edge of the growth cavity, the temperature of the source substrate and the temperature of the target substrate are controlled by respectively adjusting the power of the first heating assembly and the power of the second heating assembly, and a temperature difference is formed between the source substrate and the target substrate. The first heating assembly and the second heating assembly in the invention are independently selected from any one of a graphite heater, an infrared radiation heater or an induction coil heater.
As a preferred technical solution of the present invention, at least one silicon source is further disposed in the growth chamber, and the at least one silicon source is located between the source substrate and the target substrate.
The silicon source is blocky, granular or powdery.
The silicon source is high-purity silicon.
In the present invention, the number and the corresponding position of the silicon source are adjusted according to the relationship between the shape, the number and the position of the source substrate and the target substrate, and in order to help those skilled in the art to better understand the overall technical scheme and the working process of the present invention, the present invention exemplarily provides the following layout forms of the source substrate, the target substrate and the silicon source:
(1) The source substrate and the target substrate are arranged side by side, and the silicon source is respectively arranged on two sides of a central line connecting line of the source substrate and the target substrate.
(2) The source substrate surrounds the periphery of the target substrate and is concentrically arranged with the target substrate, and the silicon source is distributed in an annular space formed by the source substrate and the target substrate.
(3) The source substrates are arranged around the periphery of the target substrate and are uniformly distributed, and the silicon sources are arranged between the adjacent source substrates in an inserting mode.
It should be noted that the source substrate, the target substrate and the silicon source in the present invention are not limited to the layout forms described above, and any layout forms that can achieve the same or similar functions may be arbitrarily replaced, and the technical solutions obtained after the replacement also fall within the protection scope and the disclosure scope of the present invention.
As a preferred technical solution of the present invention, a vacuum chamber is arranged around the growth chamber, the vacuum chamber is provided with an air inlet and an air outlet, the air inlet is used for being communicated with an air source, and the air outlet is used for being communicated with an air exhaust assembly.
And a cooling water flow channel is also arranged in the cavity wall of the vacuum cavity.
The vacuum chamber is internally provided with a heat insulation cover body, the heat insulation cover body covers at least part of the surface of the growth chamber, and the first heating module and the second heating module are arranged in the heat insulation cover body.
A vacuum chamber is arranged outside the growth chamber, an atmosphere containing silicon and carbon is arranged inside the growth chamber, and process gas is filled in the vacuum chamber. The air vent of growth chamber both sides can run through the chamber wall in growth chamber, with the inside intercommunication of vacuum chamber, also can set up airflow channel in air vent department, and airflow channel extends and runs through the chamber wall of vacuum chamber, with the outside intercommunication of vacuum chamber. When the inside of the growth chamber is communicated with the outside of the vacuum chamber, the atmosphere in the growth chamber can be prevented from entering the vacuum chamber to pollute the heat insulation cover body, the heating assembly and the like in the growth chamber.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method and a device for manufacturing a high-quality silicon carbide single crystal layer, wherein a first heating module and a second heating module are adopted to respectively heat different areas in a growth cavity, the first heating module is used for heating a silicon carbide raw material, the second heating module is used for heating a target substrate, the heating temperature is controllable, the silicon carbide raw material and the target substrate form a temperature difference, the silicon carbide raw material is conveyed to the surface of the target substrate to grow and obtain the silicon carbide single crystal layer, the growth speed is high and reaches 10 to 200 mu m/h, the growth efficiency is improved, the single crystal layer has higher quality, the base plane dislocation density BPD of the single crystal layer is less than 0.1/cm -2 And does not need to use toxic and harmful silicon source gases such as silane and the like, thereby having higher safety.
Drawings
FIG. 1 is a schematic structural view of an apparatus for producing a high-quality silicon carbide single crystal layer according to example 1 of the present invention;
FIG. 2 is a schematic structural view of an apparatus for producing a high-quality silicon carbide single crystal layer according to example 2 of the present invention;
FIG. 3 is a schematic configuration view of an apparatus for producing a high-quality silicon carbide single crystal layer according to example 3 of the present invention;
fig. 4 is a schematic layout diagram of a source substrate, a target substrate and a silicon source according to embodiment 3 of the present invention;
FIG. 5 is a schematic structural view of an apparatus for producing a high-quality silicon carbide single crystal layer according to example 4 of the present invention;
fig. 6 is a schematic layout diagram of a source substrate, a target substrate and a silicon source according to embodiment 5 of the present invention;
fig. 7 is a schematic layout diagram of a source substrate, a target substrate and a silicon source according to embodiment 6 of the present invention;
fig. 8 is a layout diagram of a source substrate, a target substrate and a silicon source according to embodiment 7 of the present invention.
Wherein, 1-growth chamber; 101-a vent; 102-an airflow channel; 2-a vacuum chamber; 201-air inlet; 202-gas outlet; 3-a source substrate; 301-a first heating assembly; 4-a target substrate; 401-a second heating assembly; 5-a silicon source; 6-heat insulation cover body.
Detailed Description
It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be taken as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
It should be noted that, unless explicitly stated or limited otherwise, the terms "disposed," "connected" and "connected" in the description of the present invention are to be construed broadly and may include, for example, a fixed connection, a detachable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
In one embodiment, the present invention provides a method for producing a high-quality silicon carbide single crystal layer, the method comprising:
(1) Providing a growth cavity 1, and arranging a first heating module and a second heating module on the periphery of the growth cavity 1;
(2) Providing a silicon carbide raw material and at least one target substrate 4, and placing the target substrate 4 in the growth cavity 1;
(3) And independently heating different areas in the growth cavity 1 by adopting the first heating module and the second heating module to form a temperature difference between the silicon carbide raw material and the target substrate 4, generating an atmosphere containing silicon and carbon in the growth cavity 1, and depositing the silicon carbide raw material on the surface of the target substrate 4 to grow and obtain a silicon carbide single crystal layer.
According to the invention, different areas in the growth cavity 1 are respectively heated by the first heating module and the second heating module, the first heating module is used for heating the silicon carbide raw material, the second heating module is used for heating the target substrate 4, so that the heating temperature is controllable, the silicon carbide raw material and the target substrate 4 form a temperature difference, the silicon carbide raw material is conveyed to the surface of the target substrate 4 to grow and obtain the silicon carbide single crystal layer, the growth speed is high, toxic and harmful silicon source gases such as silane are not required to be used, and the safety is high.
In some embodiments, the material of the growth chamber 1 is any one of high-purity graphite, silicon carbide, tantalum, tungsten, molybdenum, tantalum carbide, tungsten carbide, and molybdenum carbide. When the material of the growth cavity 1 is silicon carbide, the growth of the silicon carbide single crystal layer can be directly carried out by taking the growth cavity 1 as the silicon carbide raw material without adding extra silicon carbide raw material.
In some embodiments, the target substrate 4 is single crystal silicon carbide. The target substrate 4 has a crystal form of 4H, 6H or 3C. The growth surface of the target substrate 4 is a Si surface or a C surface. The included angle between the (0001) surface of the target substrate 4 single crystal and the growth surface of the target substrate 4 is less than or equal to 8 degrees.
In some embodiments, the temperature in the growth cavity 1 is 1500-2300 ℃, the air pressure in the growth cavity 1 is 10-5000 Pa, the temperature difference is 1-50 ℃, and the growth speed is 1-200 μm/h.
In some embodiments, the thickness of the silicon carbide single crystal layer is 1 to 100 μm, and the base plane dislocation density BPD of the silicon carbide single crystal layer is less than 0.1/cm -2 。
In some embodiments, the growing of the silicon carbide single crystal layer specifically includes:
the first heating module and the second heating module are adopted to respectively heat the growth cavity 1 and the target substrate 4, so that the temperature of the inner cavity wall of part of the growth cavity 1 is higher than that of the target substrate 4, silicon carbide raw materials on the inner cavity wall of the growth cavity 1 are sublimated and deposited on the surface of the target substrate 4, and the silicon carbide single crystal layer is grown and formed, wherein the growth cavity 1 is made of silicon carbide.
When the growth cavity 1 is made of silicon carbide materials, the growth cavity 1 is used as a silicon carbide raw material to provide materials required for growing a silicon carbide single crystal layer for the target substrate 4, the growth cavity 1 is heated by the first heating module, the target substrate 4 is heated by the second heating module, and the first heating module and the second heating module are respectively regulated and controlled to enable the growth cavity 1 and the target substrate 4 to form a temperature difference, so that the silicon carbide raw material on the inner cavity wall of the growth cavity 1 is sublimated and moved to the surface of the target substrate 4 to realize the growth of the silicon carbide single crystal layer; when the material of the growth chamber 1 is not silicon carbide, other silicon carbide raw materials should be introduced into the growth chamber 1 to provide the target substrate 4 with the material required for growing a silicon carbide single crystal layer.
In some embodiments, the growing of the silicon carbide single crystal layer specifically includes:
providing at least one source substrate 3, and placing the source substrate 3 in the growth cavity 1;
respectively heating the source substrate 3 and the target substrate 4 by using the first heating module and the second heating module to ensure that the temperature of the source substrate 3 is higher than that of the target substrate 4, so as to sublimate the source substrate 3, deposit the sublimated source substrate 3 on the surface of the target substrate 4, and grow to form the silicon carbide single crystal layer;
the source substrate 3 is single crystal silicon carbide or polycrystalline silicon carbide.
According to the invention, other source substrates 3 are introduced into a growth cavity 1, materials required for growing the silicon carbide single crystal layer are provided for a target substrate 4, the source substrate 3 is heated by a first heating module, the target substrate 4 is heated by a second heating module, the source substrate 3 and the target substrate 4 are respectively corresponding to different heating modules to regulate and control the temperature, so that a temperature difference is formed between the source substrate 3 and the target substrate 4, the source substrate 3 is sublimated and moves to the surface of the target substrate 4, and the growth of the silicon carbide single crystal layer is realized.
In some embodiments, the growing of the silicon carbide single crystal layer further comprises:
providing at least one silicon source 5, and placing the silicon source 5 in the growth chamber 1;
and adjusting the heating temperature of the first heating module and the second heating module to evaporate the silicon source 5 so as to regulate and control the content of silicon and carbon in the growth cavity 1.
In the present invention, the silicon source 5 is provided and evaporated to change the atomic number ratio of silicon to carbon in the atmosphere in the growth chamber 1. Because the evaporation temperature of silicon is lower than carborundum, accessible heat conduction, heat radiation obtain the heat and heat up to evaporation temperature, consequently, need not to set up corresponding heating element for silicon source 5, at the carborundum raw materials of heating growth chamber 1 inner chamber wall, carborundum substrate or the in-process of target substrate 4, can realize the evaporation of silicon source 5.
In some embodiments, the method of manufacturing a high quality silicon carbide single crystal layer further comprises:
providing a vacuum chamber 2, and placing the growth chamber 1 in the inner cavity of the vacuum chamber 2;
the vacuum chamber 2 is evacuated while the process gas is charged into the vacuum chamber 2.
The process gas comprises any one or a combination of at least two of argon, nitrogen or helium.
In some embodiments, the method of manufacturing a high quality silicon carbide single crystal layer further comprises: before the growth, the surface of the target substrate 4 is subjected to etching treatment.
In some embodiments, the specific manner of the etching treatment is:
and adjusting the heating temperature of the first heating module and the second heating module to enable the temperature of the target substrate 4 to be higher than the temperature of part of the inner cavity wall of the growth cavity 1, so that the surface raw material of the target substrate 4 is sublimated and deposited on the inner cavity wall of the growth cavity 1, and scratches, scratches or damages on the surface of the target substrate 4 are removed.
In some embodiments, the etching treatment is performed in a specific manner:
and adjusting the heating temperature of the first heating module and the second heating module to enable the temperature of the target substrate 4 to be higher than that of the source substrate 3, so that the surface raw material of the target substrate 4 is sublimated and deposited on the source substrate 3, and scratches, scratches or damages on the surface of the target substrate 4 are removed.
The invention first carries out etching treatment on the target substrate 4 and then carries out growth of a single crystal layer. The surface of the etched target substrate 4 is free of scratches, scratches or damaged layers, on the basis of which the produced monocrystalline layer is of higher quality, with a lower dislocation density.
In the etching process, the temperature in the growth cavity 1 is 1500-2300 ℃, the air pressure in the growth cavity 1 is 10-5000 Pa, the temperature difference is 1-50 ℃, the etching speed is 1-200 mu m/h, and the etching thickness is 1-100 mu m.
In another embodiment, the present invention provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is used in the method for producing a high-quality silicon carbide single crystal layer described in one embodiment;
the device for manufacturing the high-quality silicon carbide single crystal layer comprises a growth cavity 1, wherein at least one target substrate 4 is arranged in the growth cavity 1, a first heating module and a second heating module are arranged on the periphery of the growth cavity 1, and the first heating module and the second heating module are used for heating different areas in the growth cavity 1 respectively.
In some embodiments, at least one source substrate 3 is also disposed within the growth chamber 1.
The present invention does not specifically limit or require any particular structure or dimension thickness of the source substrate 3 and the target substrate 4, and for example, the source substrate 3 having a cross section of a square, circular, prismatic, or circular structure; the target substrate 4 can be disc-shaped, with a diameter of 1~8 inches and a thickness of 300 to 1000 μm, and can be adjusted by those skilled in the art according to actual conditions.
In some embodiments, the first heating module is disposed in correspondence with the source substrate 3 for heating the source substrate 3. The second heating module is disposed corresponding to the target substrate 4, and is configured to heat the target substrate 4.
In some embodiments, the first heating module comprises at least one first heating assembly 301, the first heating assembly 301 being located above and/or below the source substrate 3. The second heating module comprises at least one second heating assembly 401, the second heating assembly 401 being located above and/or below the target substrate 4.
In some embodiments, the growth chamber 1 is rectangular in cross-section. The first heating assembly 301 and the second heating assembly 401 are positioned on at least one side of the long side of the growth chamber 1. Short edges on two sides of the growth cavity 1 are respectively provided with air vents 101 which penetrate through the cavity wall of the growth cavity 1.
The growth cavity 1 has a flat internal space, the internal height is narrow (namely the short side of the growth cavity 1), and vent holes are formed in the short sides at two sides of the growth cavity within the range of 0.5-5 mm, so that the interior of the growth cavity 1 is communicated with the external atmosphere. In addition, a first heating unit 301 is provided above and/or below the source substrate 3 and a second heating unit 401 is provided above and below the target substrate 4 outside the long sides of the growth chamber 1, and the temperatures of the source substrate 3 and the target substrate 4 are controlled by adjusting the powers of the first heating unit 301 and the second heating unit 401, respectively, thereby forming a temperature difference between the source substrate 3 and the target substrate 4. The first heating element 301 and the second heating element 401 are independently selected from any one of a graphite heater, an infrared radiation heater, or an induction coil heater in the present invention.
According to the present invention, the structures and the number of the first heating assembly 301 and the second heating assembly 401 are adjusted according to the shapes and the numbers of the target substrate 4 and the source substrate 3, so that the heating regions thereof substantially cover the source substrate 3 and the target substrate 4.
In some embodiments, at least one silicon source 5 is also disposed within growth chamber 1, and the at least one silicon source 5 is located between source substrate 3 and target substrate 4. The silicon source 5 is in the form of block, granule or powder. The silicon source 5 is high-purity silicon.
In the present invention, the number and the corresponding position of the silicon source 5 are adjusted according to the relationship between the shape, the number and the position of the source substrate 3 and the target substrate 4, and in order to help those skilled in the art to better understand the overall technical solution and the working process of the present invention, the present invention exemplarily provides the following layout forms of the source substrate 3, the target substrate 4 and the silicon source 5:
(1) The source substrate 3 and the target substrate 4 are arranged side by side, and the silicon source 5 is respectively arranged at two sides of a central line connecting line of the source substrate 3 and the target substrate 4.
(2) The source substrate 3 surrounds the periphery of the target substrate 4 and is concentrically arranged with the target substrate 4, and the silicon source 5 is distributed in an annular space formed by the source substrate 3 and the target substrate 4.
(3) The source substrates 3 are arranged around the periphery of the target substrate 4 and are uniformly distributed, and the silicon sources 5 are arranged between the adjacent source substrates 3 in an inserting mode.
When 1 target substrate 4, x source substrates 3 and y silicon sources 5 are arranged in growth cavity 1, x + y areas surround target substrate 4 and are uniformly distributed on the outer circumference of target substrate 4. The y silicon sources 5 are positioned so as to avoid concentration and to penetrate as uniformly as possible through the middle of the source substrate 3. Efficiency is improved when the number of target substrates 4 is greater than 1, with x source substrates 3 and y silicon sources 5 surrounding any one target substrate 4. The x + y areas surround the target substrate 4 and are uniformly distributed on the outer circumference of the target substrate 4. The y silicon sources 5 are positioned so as to avoid concentration and to penetrate as uniformly as possible through the middle of the source substrate 3. The silicon source 5 may not be provided, that is, y =0.
In some embodiments, the outer periphery of the growth chamber 1 is provided with a vacuum chamber 2, the vacuum chamber 2 is provided with a gas inlet 201 and a gas outlet 202, the gas inlet 201 is used for communicating with a gas source, and the gas outlet 202 is used for communicating with a gas exhaust assembly. And a cooling water flow channel is also arranged in the cavity wall of the vacuum cavity 2.
In some embodiments, a heat insulating cover 6 is disposed inside the vacuum chamber 2, the heat insulating cover 6 covers at least part of the surface of the growth chamber 1, and the first and second heating modules are disposed inside the heat insulating cover 6.
In the invention, a vacuum chamber 2 is arranged outside a growth chamber 1, an atmosphere containing silicon and carbon is arranged inside the growth chamber 1, and a process gas is filled in the vacuum chamber 2. The ventilation ports 101 at both sides of the growth chamber 1 may penetrate through the chamber wall of the growth chamber 1 to communicate with the inside of the vacuum chamber 2, or the ventilation ports 101 may be provided with airflow passages 102, and the airflow passages 102 extend through the chamber wall of the vacuum chamber 2 to communicate with the outside of the vacuum chamber 2. When the inside of the growth chamber 1 and the outside of the vacuum chamber 2 communicate with each other, it is possible to prevent the atmosphere in the growth chamber 1 from entering into the vacuum chamber 2, contaminating the heat insulating cover body 6 and the heating member etc. inside thereof.
Example 1
The embodiment provides a device for manufacturing a high-quality silicon carbide single crystal layer, which specifically comprises a vacuum chamber 2 as shown in figure 1, wherein a growth chamber 1 is arranged in the vacuum chamber 2. Vacuum chamber 2 is made by the stainless steel, and the both sides of vacuum chamber 2 are provided with air inlet 201 and gas outlet 202 respectively, and the external evacuation subassembly of gas outlet 202, the external nitrogen gas source of air inlet 201, the inside in the chamber wall of vacuum chamber 2 has the cooling water runner.
Example 2
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 1 in that: as shown in fig. 2, the short sides of the growth chamber 1 are provided with air flow passages 102 at the air vents 101, the air flow passages 102 extend through the vacuum chamber 2, so that the interior of the growth chamber 1 is communicated with the exterior of the vacuum chamber 2, thereby preventing the steam in the growth chamber 1 from entering the vacuum chamber 2 and polluting the heat insulating cover 6 and the heating assembly therein, and the rest of the component structures and process parameters are the same as those of embodiment 1.
Example 3
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 1 in that: as shown in fig. 3 and 4, two block-shaped silicon sources 5 are further disposed inside the growth chamber 1, the two silicon sources 5 are respectively disposed on two sides of a central line connecting line between the source substrate 3 and the target substrate 4, the silicon sources 5 are made of high-purity silicon, and the structure and process parameters of the rest of the components are the same as those in embodiment 1.
Example 4
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 2 in that: as shown in fig. 5, two block-shaped silicon sources 5 are further disposed inside the growth chamber 1, the two silicon sources 5 are respectively disposed on two sides of a central line connecting line between the source substrate 3 and the target substrate 4, the silicon source 5 is made of high-purity silicon, and the structure and process parameters of the rest of the components are the same as those in embodiment 2.
Example 5
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 3 in that: as shown in fig. 6, the source substrate 3 has a ring-shaped structure, surrounds the outer periphery of the target substrate 4, and is disposed concentrically with the target substrate 4. The number of the silicon sources 5 is four, the silicon sources 5 are uniformly distributed in an annular space formed by the source substrate 3 and the target substrate 4, so that the deposition layers at all positions of the target substrate 4 are more uniform, and the structures and the process parameters of other components are the same as those of the embodiment 3.
Example 6
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 3 in that: as shown in fig. 7, the diameter of the source substrate 3 is 1 inch, the number of the source substrates 3 is six, the source substrates 3 are uniformly distributed around the periphery of the target substrate 4, two silicon sources 5 are oppositely arranged, the silicon sources 5 are alternately arranged between the adjacent source substrates 3, and the structures and process parameters of the rest of the components are the same as those in embodiment 3.
Example 7
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 3 in that: as shown in fig. 8, the number of the target substrates 4 is four, and the target substrates are distributed on the bottom surface of the growth chamber 1 in a 2 × 2 matrix, six source substrates 3 and two silicon sources 5 are surrounded around each target substrate 4, the diameters of the source substrates 3 and the silicon sources 5 are both 1 inch, and the positions of the silicon sources 5 are prevented from being concentrated and uniformly penetrate through the middle of the source substrates 3. The source substrate 3 and the silicon source 5 surround the target substrate 4 and are uniformly distributed over the outer circumference of the target substrate 4. Two adjacent target substrates 4 share one silicon source 5 and one source substrate 3, or share two source substrates 3, and the rest of the component structures and process parameters are the same as those of embodiment 3.
Example 8
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 1 in that: the material of the growth chamber 1 is silicon carbide, the source substrate 3 is not disposed in the growth chamber 1, and the structure and process parameters of the remaining components are the same as those of embodiment 1.
This embodiment regards growth chamber 1 as the carborundum raw materials, provides the required material of growth carborundum single crystal layer for target substrate 4, utilizes first heating module heating growth chamber 1, utilizes second heating module heating target substrate 4, regulates and control first heating module and second heating module respectively for growth chamber 1 and target substrate 4 form the temperature difference, and the carborundum raw materials on the inner chamber wall of growth chamber 1 sublimes, and removes the surface to target substrate 4, realizes the growth on carborundum single crystal layer.
Example 9
This example provides an apparatus for producing a high-quality silicon carbide single crystal layer, which is different from example 3 in that: the material of the growth chamber 1 is silicon carbide, the source substrate 3 is not disposed in the growth chamber 1, and the structure and process parameters of the remaining components are the same as those of embodiment 3.
This embodiment regards growth chamber 1 as the carborundum raw materials, provides the required material of growth carborundum single crystal layer for target substrate 4, utilizes first heating module heating growth chamber 1, utilizes second heating module heating target substrate 4, regulates and control first heating module and second heating module respectively for growth chamber 1 and target substrate 4 form the temperature difference, and the carborundum raw materials on the inner chamber wall of growth chamber 1 sublimes, and removes the surface to target substrate 4, realizes the growth on carborundum single crystal layer. The present embodiment changes the atomic number ratio of silicon to carbon in the atmosphere in growth chamber 1 by providing silicon source 5 to evaporate during heating.
Example 10
This example provides a method for producing a high-quality silicon carbide single crystal layer using the apparatus provided in example 1, including:
the first heating assembly 301 is adopted to heat the source substrate 3, and the second heating assembly 401 is adopted to heat the target substrate 4, so that the temperature of the source substrate 3 is higher than that of the target substrate 4, the temperature difference is 30 ℃, so as to sublimate the source substrate 3, and the sublimated source substrate is deposited on the surface of the target substrate 4, and a silicon carbide single crystal layer is grown. The temperature in the growth chamber 1 is 1800 ℃ and the air pressure in the growth chamber 1 is 2000Pa.
In this example, the growth rate of the silicon carbide single crystal layer was 60 μm/h, the thickness of the obtained silicon carbide single crystal layer was 70 μm, and the basal plane dislocation density BPD of the silicon carbide single crystal layer was 0.05/cm -2 。
Example 11
The present embodiment provides a method for producing a high-quality silicon carbide single crystal layer, using the apparatus provided in embodiment 3 to produce a high-quality silicon carbide single crystal, specifically including:
(1) Etching treatment of the target substrate 4:
heating the source substrate 3 by using a first heating component 301, heating the target substrate 4 by using a second heating component 401, so that the temperature of the target substrate 4 is higher than that of the source substrate 3, the temperature difference is 40 ℃, a silicon source 5 is evaporated to regulate the atomic number ratio of silicon to carbon in a growth cavity 1 to be more than 1, the surface raw material of the target substrate 4 is sublimated and deposited on the source substrate 3 to remove scratches, scratches or damages on the surface of the target substrate 4, the temperature in the growth cavity 1 is 1800 ℃, the air pressure in the growth cavity 1 is 2000Pa, the etching speed is 60 mu m/h, and the etching thickness is 10 mu m;
(2) Growing to form a silicon carbide single crystal layer:
the first heating assembly 301 is adopted to heat the source substrate 3, the second heating assembly 401 is adopted to heat the target substrate 4, the temperature of the source substrate 3 is higher than that of the target substrate 4, the temperature difference is 30 ℃, the source substrate 3 is sublimated and is deposited on the surface of the target substrate 4, a silicon carbide single crystal layer is grown and formed, the silicon source 5 is evaporated, the atomic number ratio of silicon to carbon in the growth cavity 1 is regulated and controlled to be larger than 1, the temperature in the growth cavity 1 is 1800 ℃, and the air pressure in the growth cavity 1 is 2000Pa.
In this example, the growth rate of the silicon carbide single crystal layer was 80 μm/h, the thickness of the silicon carbide single crystal layer obtained was 100 μm, and the basal plane dislocation density BPD of the silicon carbide single crystal layer was 0.02/cm -2 。
Example 12
The present embodiment provides a method for producing a high-quality silicon carbide single crystal layer by using the apparatus provided in embodiment 7, comprising:
the first heating assembly 301 is adopted to heat the growth cavity 1, the second heating assembly 401 is adopted to heat the target substrate 4, the temperature of part of the inner cavity wall of the growth cavity 1 is higher than that of the target substrate 4, the temperature difference is 60 ℃, so that the source substrate 3 is sublimated and deposited on the surface of the target substrate 4, and a silicon carbide single crystal layer is grown and formed. The temperature in the growth chamber 1 was 2000 ℃ and the air pressure in the growth chamber 1 was 2100Pa.
In this example, the growth rate of the silicon carbide single crystal layer was 55 μm/h, the thickness of the silicon carbide single crystal layer obtained was 40 μm, and the basal plane dislocation density BPD of the silicon carbide single crystal layer was 0.07/cm -2 。
Example 13
The present embodiment provides a method for producing a high-quality silicon carbide single crystal layer by using the apparatus provided in embodiment 8, comprising:
(1) Etching treatment of the target substrate 4:
heating the growth cavity 1 by using a first heating assembly 301, heating the target substrate 4 by using a second heating assembly 401, so that the temperature of the target substrate 4 is higher than that of the growth cavity 1, the temperature difference is 20 ℃, the surface raw material of the target substrate 4 is sublimated and deposited on the inner cavity wall of the growth cavity 1, and scratches, scratches or damages on the surface of the target substrate 4 are removed, the temperature in the growth cavity 1 is 2000 ℃, the air pressure in the growth cavity 1 is 1500Pa, the etching speed is 60 mu m/h, and the etching thickness is 15 mu m;
(2) Growing to form a silicon carbide single crystal layer:
the first heating assembly 301 is adopted to heat the growth cavity 1, the second heating assembly 401 is adopted to heat the target substrate 4, the temperature of the partial inner cavity wall of the growth cavity 1 is higher than that of the target substrate 4, the temperature difference is 30 ℃, so that raw materials on the inner cavity wall of the growth cavity 1 are sublimated and deposited on the surface of the target substrate 4, and a silicon carbide single crystal layer is grown and formed. The temperature in the growth chamber 1 is 1800 ℃ and the air pressure in the growth chamber 1 is 2000Pa.
In this example, the growth rate of the silicon carbide single crystal layer was 70 μm/h, the thickness of the obtained silicon carbide single crystal layer was 60 μm, and the BPD of the basal plane dislocation density of the silicon carbide single crystal layer was 0.04/cm -2 。
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (9)
1. A method for producing a high-quality silicon carbide single crystal layer, comprising:
providing a growth cavity, and arranging a first heating module and a second heating module on the periphery of the growth cavity;
(II) providing a silicon carbide raw material and at least one target substrate, and placing the target substrate in the growth chamber;
and (III) independently heating different areas in the growth cavity by adopting the first heating module and the second heating module to form a temperature difference between the silicon carbide raw material and the target substrate, generating an atmosphere containing silicon and carbon in the growth cavity, and depositing the silicon carbide raw material on the surface of the target substrate to grow and obtain the silicon carbide single crystal layer.
2. The method for producing a high-quality silicon carbide single crystal layer according to claim 1, wherein the growth chamber is made of any one of high-purity graphite, silicon carbide, tantalum, tungsten, molybdenum, tantalum carbide, tungsten carbide, and molybdenum carbide;
the target substrate is single crystal silicon carbide;
the growth surface of the target substrate is a Si surface or a C surface;
an included angle between the (0001) surface of the target substrate single crystal and the growth surface of the target substrate is less than or equal to 8 degrees;
the temperature in the growth cavity is 1500 to 2300 ℃;
the air pressure in the growth cavity is 10-5000 Pa;
the temperature difference is 1 to 50 ℃;
the growth speed is 1 to 200 mu m/h;
the thickness of the silicon carbide single crystal layer is 1 to 100 mu m;
the basal plane dislocation density BPD of the silicon carbide single crystal layer is less than 0.1/cm -2 。
3. The method for producing a high-quality silicon carbide single crystal layer according to claim 2, wherein the growing of the silicon carbide single crystal layer specifically includes:
respectively heating the growth cavity and the target substrate by using the first heating module and the second heating module to enable the temperature of part of the inner cavity wall of the growth cavity to be higher than that of the target substrate, so as to sublimate the silicon carbide raw material of the inner cavity wall of the growth cavity, deposit the silicon carbide raw material on the surface of the target substrate, and grow to form the silicon carbide single crystal layer;
the growth cavity is made of silicon carbide;
or, the growing of the silicon carbide single crystal layer specifically includes:
providing at least one source substrate, and placing the source substrate in the growth chamber;
respectively heating the source substrate and the target substrate by using the first heating module and the second heating module to enable the temperature of the source substrate to be higher than that of the target substrate, so as to sublimate the source substrate, deposit the source substrate on the surface of the target substrate and grow to form the silicon carbide single crystal layer;
the source substrate is single crystal silicon carbide or polycrystalline silicon carbide.
4. The method for producing a high-quality silicon carbide single crystal layer according to claim 1, wherein the growing of the silicon carbide single crystal layer further comprises:
providing at least one silicon source, and placing the silicon source in the growth chamber;
adjusting the heating temperature of the first heating module and the second heating module to evaporate the silicon source so as to regulate and control the content of silicon and carbon in the growth cavity;
the method for producing a high-quality silicon carbide single crystal layer further comprises:
providing a vacuum chamber, and placing the growth chamber in an inner cavity of the vacuum chamber;
and pumping the vacuum chamber while filling the process gas into the vacuum chamber.
5. The method for producing a high-quality silicon carbide single crystal layer according to claim 3, wherein the method for producing a high-quality silicon carbide single crystal layer further comprises: before the growth, etching the surface of the target substrate; the specific way of the etching treatment is as follows:
adjusting the heating temperature of the first heating module and the second heating module to enable the temperature of the target substrate to be higher than the temperature of the inner cavity wall of the growth cavity part, so that the surface raw material of the target substrate is sublimated and deposited on the inner cavity wall of the growth cavity, and scratches, scratches or damages on the surface of the target substrate are removed;
or, the specific way of the etching treatment is as follows:
and adjusting the heating temperature of the first heating module and the second heating module to enable the temperature of the target substrate to be higher than that of the source substrate, so that the surface raw material of the target substrate is sublimated and deposited on the source substrate, and scratches, scratches or damages on the surface of the target substrate are removed.
6. An apparatus for manufacturing a high-quality silicon carbide single crystal layer, which is used in the method for manufacturing a high-quality silicon carbide single crystal layer according to any one of claims 1 to 5, comprising a growth chamber in which at least one target substrate is disposed, and a first heating module and a second heating module disposed on the outer periphery of the growth chamber and configured to heat different regions in the growth chamber, respectively.
7. The apparatus for producing a high-quality silicon carbide single crystal layer according to claim 6, wherein at least one source substrate is further provided in said growth chamber;
the first heating module is arranged corresponding to the source substrate and used for heating the source substrate;
the second heating module is arranged corresponding to the target substrate and is used for heating the target substrate;
the first heating module comprises at least one first heating assembly located above and/or below the source substrate;
the second heating module comprises at least one second heating assembly located above and/or below the target substrate;
the cross section of the growth cavity is rectangular;
the first heating assembly and the second heating assembly are positioned on at least one side of the long edge of the growth cavity;
short edges on two sides of the growth cavity are respectively provided with air vents which penetrate through the cavity wall of the growth cavity.
8. The apparatus for producing a high quality silicon carbide single crystal layer according to claim 7 wherein at least one silicon source is further provided in said growth chamber, said at least one silicon source being located between said source substrate and a target substrate;
the silicon source is in a block shape, a granular shape or a powder shape.
9. The apparatus for manufacturing a high-quality silicon carbide single crystal layer according to claim 6, wherein a vacuum chamber is provided around the growth chamber, and a gas inlet and a gas outlet are provided on the vacuum chamber, the gas inlet is used for communicating with a gas source, and the gas outlet is used for communicating with a gas exhaust assembly;
a heat insulation cover body is arranged in the vacuum chamber, the heat insulation cover body covers at least part of the surface of the growth chamber, and the first heating module and the second heating module are arranged in the heat insulation cover body;
and a cooling water flow channel is also arranged in the cavity wall of the vacuum cavity.
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CN111118598A (en) * | 2019-12-26 | 2020-05-08 | 山东天岳先进材料科技有限公司 | High-quality silicon carbide single crystal, substrate and efficient preparation method thereof |
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JP2006021954A (en) * | 2004-07-08 | 2006-01-26 | Fuji Electric Holdings Co Ltd | Method and apparatus for manufacturing silicon carbide single crystal film |
US20160060789A1 (en) * | 2014-09-03 | 2016-03-03 | Ii-Vi Incorporated | Silicon Carbide Crystal Growth by Silicon Chemical Vapor Transport |
CN111018535A (en) * | 2019-12-26 | 2020-04-17 | 湖南德智新材料有限公司 | Method for preparing silicon carbide ceramic by CVD |
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