Supporting ring, single crystal furnace and manufacturing method of supporting ring

Abstract

The invention provides a supporting ring, a single crystal furnace and a manufacturing method of the supporting ring, and relates to the technical field of monocrystalline silicon production. The supporting ring is used for the single crystal furnace and comprises a base body and a protective layer, the base body comprises a reinforcing framework and filler filled in the reinforcing framework, the reinforcing framework is made of a carbon-carbon composite material, and the filler is graphite; the protective layer comprises an anti-oxidation layer and a sealing layer, the anti-oxidation layer wraps the base body, the sealing layer wraps the anti-oxidation layer, the anti-oxidation layer is made of a nanoscale silicon carbide-silicon boride composite material, and the sealing layer is made of ceramic glaze. The invention provides a supporting ring, a single crystal furnace and a manufacturing method of the supporting ring. The supporting ring is high in impact resistance and oxidation resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of single crystal silicon production, and in particular to a support ring, a single crystal furnace and a method for manufacturing the support ring. Background Art

[0002] The support ring in a single crystal furnace is generally used to carry components such as heat shields and guide tubes to ensure the integrity of the structure; or it relies on thermal insulation performance to maintain a uniform thermal field, guide heat flow, and create a thermal environment suitable for crystal growth; or it participates in gas management, guides gas flow through specific shapes, cooperates with sealing, stabilizes the gas environment in the furnace, and meets crystal growth requirements.

[0003] Existing support rings are generally formed in one piece from graphite material. However, on the one hand, support rings made of graphite have poor toughness and are easily broken when impacted. On the other hand, in the high temperature environment of a single crystal furnace, graphite is easily oxidized, which not only causes its own structural loss, but also produces oxides that contaminate single crystal silicon. Summary of the invention

[0004] In order to solve at least one of the problems mentioned in the background technology, the present invention provides a support ring, a single crystal furnace and a method for manufacturing the support ring, which have strong impact resistance and oxidation resistance.

[0005] In order to achieve the above object, the present invention provides the following technical solutions:

[0006] In a first aspect, the present invention provides a support ring for a single crystal furnace, comprising a substrate and a protective layer, wherein the substrate comprises a reinforcement frame and a filler filled in the reinforcement frame, the reinforcement frame is made of a carbon-carbon composite material, and the filler is graphite;

[0007] The protective layer comprises an anti-oxidation layer and a sealing layer. The anti-oxidation layer is wrapped outside the substrate, and the sealing layer is wrapped outside the anti-oxidation layer. The anti-oxidation layer is a nano-scale silicon carbide-silicon boride composite material, and the sealing layer is a ceramic glaze.

[0008] As an optional implementation, the thickness of the anti-oxidation layer is 50 μm-100 μm.

[0009] As an optional implementation, the thickness of the sealing layer is 30 μm-50 μm.

[0010] As an optional implementation, the mass ratio of silicon carbide to silicon boride in the anti-oxidation layer is 3:1-5:1.

[0011] As an optional implementation, the reinforcement skeleton has a heat-conducting channel extending radially along the support ring, and the heat-conducting channel is filled with graphite.

[0012] In a second aspect, the present invention further provides a single crystal furnace, comprising the support ring in the first aspect.

[0013] In a third aspect, the present invention further provides a method for manufacturing a support ring, which is used to manufacture the support ring in the first aspect, comprising the following steps:

[0014] The carbon fibers are woven into a carbon fiber skeleton by a three-dimensional weaving process, and then the carbon fiber skeleton is placed in a chemical vapor deposition furnace to be converted into a reinforcement skeleton, and graphite is filled into the reinforcement skeleton during the conversion process to form a matrix;

[0015] Depositing nano-scale silicon carbide-silicon boride composite material on the substrate surface by chemical vapor deposition process to form an anti-oxidation layer;

[0016] A sealing layer composed of ceramic glaze is formed on the surface of the anti-oxidation layer by means of immersion coating and high-temperature sintering.

[0017] As an optional implementation, in the three-dimensional weaving process, the weaving density of the carbon fiber is 60%-85%.

[0018] As an optional implementation, the reaction temperature of the chemical vapor deposition process is 1200°C-1400°C.

[0019] As an optional implementation, the high temperature sintering temperature is 1600°C-1800°C.

[0020] The support ring provided by the present invention is used for a single crystal furnace, and includes a support ring body, a first positioning block and a second positioning block. The support ring body is provided with a first slot and a second slot, the first positioning block is clamped in the first slot, the second positioning block is clamped in the second slot, the first positioning block has a first positioning hole, the second positioning block has a second positioning hole, the first positioning hole and the second positioning hole are symmetrically distributed on both sides of the central axis of the support ring body, so as to position the support ring through the first positioning hole and the second positioning hole.

[0021] The support ring provided by the present invention is used for a single crystal furnace, and comprises a substrate and a protective layer, wherein the substrate comprises a reinforcement skeleton and a filler filled in the reinforcement skeleton, the reinforcement skeleton is made of a carbon-carbon composite material, and the filler is graphite; the protective layer comprises an anti-oxidation layer and a sealing layer, the anti-oxidation layer is wrapped outside the substrate, and the sealing layer is wrapped outside the anti-oxidation layer, the anti-oxidation layer is a nano-scale silicon carbide-silicon boride composite material, and the sealing layer is a ceramic glaze.

[0022] The support ring provided by the present invention uses a carbon-carbon composite material as a reinforcement skeleton and graphite as a filler to form a matrix of the support ring. Compared with the existing pure graphite matrix, the entire matrix can be reinforced by a high-strength and high-toughness carbon-carbon composite material, thereby improving the overall toughness and impact resistance of the matrix and greatly reducing the risk of the support ring breaking during use. By wrapping an anti-oxidation layer made of a nano-scale silicon carbide-silicon boride composite material on the surface of the matrix, the matrix can be protected and the risk of the matrix material being oxidized can be reduced. Specifically, the silicon carbide in the anti-oxidation layer can react with oxygen at high temperature to generate a dense silicon dioxide oxide film, which can prevent oxygen from contacting and reacting with the matrix. At the same time, silicon boride can also react with oxygen, and the generated liquid oxidation product can further fill the pores that may exist on the silicon dioxide oxide film, so that the effect of the anti-oxidation layer isolating oxygen is further improved. By forming a sealing layer composed of ceramic glaze on the surface of the antioxidant layer, not only can the tiny pores that may exist in the antioxidant layer be sealed to further prevent oxygen penetration, but also the antioxidant layer can be prevented from volatilizing or falling off at high temperatures, thereby ensuring the durability of the antioxidant effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0024] Figure 1 A schematic diagram of the overall structure of a support ring provided in an embodiment of the present invention;

[0025] Figure 2 for Figure 1 A top view of

[0026] Figure 3 for Figure 2 A cross-sectional view at AA;

[0027] Figure 4 for Figure 3 Enlarged view of point A in the middle.

[0028] Description of reference numerals:

[0029] 100-support ring;

[0030] 110-matrix;

[0031] 111-Reinforced skeleton;

[0032] 112-filler;

[0033] 120-antioxidation layer;

[0034] 130-Sealing layer. DETAILED DESCRIPTION

[0035] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0036] In the application, the terms "upper", "lower", "left", "right", "front", "back", "top", "bottom", "inner", "outer", "vertical", "horizontal", "lateral", "longitudinal" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings. These terms are mainly used to better describe the present invention and its embodiments, and are not used to limit the indicated devices, elements or components to have a specific orientation, or to be constructed and operated in a specific orientation.

[0037] In addition, some of the above terms may be used to express other meanings in addition to indicating orientation or positional relationship. For example, the term "on" may also be used to express a certain dependency or connection relationship in some cases. For those skilled in the art, the specific meanings of these terms in the present invention can be understood according to specific circumstances.

[0038] In addition, the terms "installed", "set", "provided with", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral structure; it can be a mechanical connection, or an electrical connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be an internal connection between two devices, elements, or components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0039] In addition, the terms "first", "second", etc. are mainly used to distinguish different devices, elements or components (the specific types and structures may be the same or different), and are not used to indicate or imply the relative importance and quantity of the indicated devices, elements or components. Unless otherwise specified, "plurality" means two or more.

[0040] The support rings in a single crystal furnace are generally used to carry components such as heat shields and guide tubes to ensure structural integrity; or to rely on thermal insulation performance to maintain uniform thermal fields, guide heat flow, and create a thermal environment suitable for crystal growth; or to participate in gas management, guide gas flow through specific shapes, cooperate with seals, stabilize the gas environment in the furnace, and meet the needs of crystal growth. Existing support rings are generally formed in one piece from graphite material. However, on the one hand, support rings made of graphite have poor toughness and are prone to breakage after high-temperature thermal expansion or when impacted. On the other hand, in the high-temperature environment of a single crystal furnace, graphite is easily oxidized, which not only causes its own structural loss, but also produces oxides that contaminate single crystal silicon.

[0041] In view of this, the present invention provides a support ring, including a substrate and a protective layer, the substrate includes a reinforcement skeleton and a filler filled in the reinforcement skeleton, the reinforcement skeleton is made of a carbon-carbon composite material, and the filler is graphite; the protective layer includes an anti-oxidation layer and a sealing layer, the anti-oxidation layer is wrapped outside the substrate, the sealing layer is wrapped outside the anti-oxidation layer, the anti-oxidation layer is a nano-scale silicon carbide-silicon boride composite material, and the sealing layer is a ceramic glaze. The support ring provided by the present invention uses a carbon-carbon composite material as a reinforcement skeleton and graphite as a filler to form a substrate of the support ring. Compared with the existing pure graphite substrate, the entire substrate can be reinforced by a high-strength and high-toughness carbon-carbon composite material, the overall toughness and impact resistance of the substrate are improved, and the risk of the support ring breaking during use is greatly reduced. By wrapping an anti-oxidation layer made of a nano-scale silicon carbide-silicon boride composite material on the surface of the substrate, the substrate can be protected and the risk of oxidation of the substrate material can be reduced. By forming a sealing layer composed of ceramic glaze on the surface of the antioxidant layer, not only can the tiny pores that may exist in the antioxidant layer be sealed to further prevent oxygen penetration, but also the antioxidant layer can be prevented from volatilizing or falling off at high temperatures, thereby ensuring the durability of the antioxidant effect.

[0042] Figure 1 A schematic diagram of the overall structure of a support ring provided in an embodiment of the present invention; Figure 2 for Figure 1 A top view of Figure 3 for Figure 2 A cross-sectional view at AA; Figure 4 for Figure 3 Enlarged view of point A in the middle.

[0043] You can refer to Figures 1 to 4An embodiment of the present invention provides a support ring for a single crystal furnace, including a substrate 110 and a protective layer, the substrate 110 includes a reinforcement skeleton 111 and a filler 112 filled in the reinforcement skeleton 111, the reinforcement skeleton 111 is made of a carbon-carbon composite material, and the filler 112 is graphite; the protective layer includes an anti-oxidation layer 120 and a sealing layer 130, the anti-oxidation layer 120 is wrapped around the outside of the substrate 110, and the sealing layer 130 is wrapped around the outside of the anti-oxidation layer 120, the anti-oxidation layer 120 is a nano-scale silicon carbide-silicon boride composite material, and the sealing layer 130 is a ceramic glaze.

[0044] The support ring 100 provided in the embodiment of the present invention uses a carbon-carbon composite material as a reinforcement skeleton 111 and graphite as a filler 112 to form a matrix 110 of the support ring 100. Compared with the existing pure graphite matrix 110, the entire matrix 110 can be reinforced by a high-strength and high-toughness carbon-carbon composite material, thereby improving the overall toughness and impact resistance of the matrix 110, and greatly reducing the risk of the support ring 100 breaking during use. By wrapping the anti-oxidation layer 120 made of nano-scale silicon carbide-silicon boride composite material on the surface of the substrate 110, the substrate 110 can be protected and the risk of oxidation of the substrate 110 material can be reduced. Specifically, the silicon carbide in the anti-oxidation layer 120 can react with oxygen at high temperature to generate a dense silicon dioxide oxide film, which can prevent oxygen from contacting and reacting with the substrate 110. At the same time, silicon boride can also react with oxygen, and the generated liquid oxidation product can further fill the pores that may exist on the silicon dioxide oxide film, so that the effect of the anti-oxidation layer 120 is further improved. By forming a sealing layer 130 composed of ceramic glaze on the surface of the anti-oxidation layer, not only can the tiny pores that may exist in the anti-oxidation layer 120 be closed, further preventing oxygen penetration, but also preventing the anti-oxidation layer 120 from volatilizing or falling off at high temperatures, ensuring the durability of the anti-oxidation effect.

[0045] In the above embodiment, the thickness of the anti-oxidation layer 120 can be 50μm-100μm. Among them, when the thickness of the anti-oxidation layer 120 is within the range of 50μm-100μm, it can not only generate a dense silicon dioxide oxide film that effectively blocks oxygen penetration through the reaction of silicon carbide and oxygen, but also can fully fill the pores of the film layer with the help of liquid boron oxide produced by silicon boride oxidation, so as to achieve a more ideal protective effect. When the thickness of the anti-oxidation layer 120 is less than 50μm, it may cause the local area of ​​the substrate 110 to be unable to form a continuous and complete silicon dioxide oxide film, causing oxygen to easily penetrate through the pores to the surface of the substrate 110, causing the substrate 110 to oxidize. When the thickness of the anti-oxidation layer 120 exceeds 100μm, the thickness of the silicon dioxide oxide film is too thick, which is easy to cause cracking and peeling of the coating under high temperature environment. At the same time, the liquid boron oxide generated by excessive silicon boride oxidation is also easy to be unable to effectively fill the pores due to excessive fluidity, but reduces the ability of the silicon dioxide oxide film to block oxygen.

[0046] In the above embodiment, the thickness of the sealing layer 130 can be 30μm-50μm. The thickness of the sealing layer 130 needs to be designed within the range of 30μm-50μm to achieve performance balance. This thickness can not only completely cover the micropores on the surface of the anti-oxidation layer 120 through the melt flow characteristics of the ceramic glaze to form a continuous glass-state sealing structure, but also avoid the concentration of thermal stress caused by excessive thickness of the coating. When the thickness is less than 30μm, the glaze layer cannot completely seal the pores of the anti-oxidation layer 120, and oxygen can still penetrate through the pores to the interface of the substrate 110; and when the thickness exceeds 50μm, the glaze layer is prone to radial cracks due to cooling shrinkage, and at the same time, the alkali metal components in the glaze at high temperature may diffuse to the anti-oxidation layer 120, destroying the interface bonding strength. The optimized thickness range can ensure that the sealing layer 130 remains stable in the single crystal furnace environment while maintaining good adhesion to the anti-oxidation layer 120.

[0047] In the above embodiment, the mass ratio of silicon carbide to silicon boride in the anti-oxidation layer 120 can be 3:1-5:1, so that a silicon dioxide film of sufficient thickness can be generated by oxidation of silicon carbide to form a main protective barrier, and the filling efficiency of the liquid boron oxide generated by oxidation of silicon boride to the pores of the film layer can be optimized, so that the anti-oxidation layer 120 maintains a stable oxygen permeability in the single crystal furnace environment, while maintaining the interface bonding strength between the film layer and the substrate 110. When the mass ratio is lower than 3:1, excessive boron content of silicon will lead to excessive generation of liquid boron oxide, which cannot be stably attached to the pores of the film layer due to excessive fluidity at high temperature, but reduces the overall sealing performance; and when the mass ratio exceeds 5:1, excessive proportion of silicon carbide will make the silicon dioxide crystal structure in the oxide film tend to be densified, resulting in increased brittleness of the film layer, and easy to generate microcracks during thermal cycling.

[0048] In the above embodiment, the reinforcement skeleton 111 may have a heat conduction channel extending radially along the support ring 100, and the heat conduction channel is filled with graphite. It can be understood that the fiber braided structure of the carbon-carbon composite skeleton has directional heat conduction characteristics, and the radially distributed graphite filling channel can significantly improve the radial heat conduction capacity of the support ring 100. The high thermal conductivity of graphite complements the high strength of the carbon-carbon skeleton. While maintaining the structural rigidity, the circumferential temperature difference of the support ring 100 is reduced to a reasonable range, effectively alleviating the problem of thermal stress concentration. This composite heat conduction structure exhibits dual advantages in a high temperature environment: on the one hand, the graphite filling channel can quickly balance the radial temperature gradient and avoid local overheating; on the other hand, the fiber network of the carbon-carbon skeleton can constrain the thermal expansion of graphite and reduce the risk of interface debonding caused by temperature fluctuations. Through this design, the support ring 100 can achieve a more uniform thermal field distribution during the operation of the single crystal furnace, provide a stable thermodynamic environment for crystal growth, extend the service life of components, and improve the production quality of single crystals.

[0049] In addition, an embodiment of the present invention further provides a single crystal furnace, comprising the support ring 100 in the above embodiment. The support ring 100 uses a carbon-carbon composite material as a reinforcement skeleton 111 and graphite as a filler 112 to form a matrix 110 of the support ring 100. Compared with the existing pure graphite matrix 110, the entire matrix 110 can be reinforced by a high-strength and high-toughness carbon-carbon composite material, thereby improving the overall toughness and impact resistance of the matrix 110, and greatly reducing the risk of the support ring 100 breaking during use. By wrapping the anti-oxidation layer 120 made of nano-scale silicon carbide-silicon boride composite material on the surface of the substrate 110, the substrate 110 can be protected and the risk of oxidation of the substrate 110 material can be reduced. Specifically, the silicon carbide in the anti-oxidation layer 120 can react with oxygen at high temperature to generate a dense silicon dioxide oxide film, which can prevent oxygen from contacting and reacting with the substrate 110. At the same time, silicon boride can also react with oxygen, and the generated liquid oxidation product can further fill the pores that may exist on the silicon dioxide oxide film, so that the effect of the anti-oxidation layer 120 is further improved. By forming a sealing layer 130 composed of ceramic glaze on the surface of the anti-oxidation layer, not only can the tiny pores that may exist in the anti-oxidation layer 120 be closed, further preventing oxygen penetration, but also preventing the anti-oxidation layer 120 from volatilizing or falling off at high temperature, ensuring the durability of the anti-oxidation effect, thereby reducing the failure rate and use cost of the single crystal furnace.

[0050] In addition, an embodiment of the present invention further provides a method for manufacturing a support ring 100, which is used to manufacture the support ring 100 in the above embodiment, and includes the following steps:

[0051] Step 1: Use a three-dimensional weaving process to weave carbon fiber into a carbon fiber skeleton, then put the carbon fiber skeleton into a chemical vapor deposition furnace to transform it into a reinforcement skeleton 111, and fill graphite into the reinforcement skeleton 111 during the transformation process of the reinforcement skeleton 111, thereby forming a matrix 110.

[0052] In the above embodiment, in the three-dimensional weaving process, the weaving density of the carbon fiber can be designed to be 60%-85%. In this way, the structural strength and weight can be balanced, so that the support ring 100 has sufficient strength while reducing the weight of the support ring 100 as much as possible; if the weaving density is too low, the skeleton structure is loose, the support ring 100 is insufficient in strength, and it is easy to deform or crack at high temperature; if the weaving density is too high,

[0053] If there are too few voids in the skeleton, the graphite filler 112 is difficult to be evenly distributed, and the heat transfer efficiency is reduced.

[0054] Step 2: depositing a nano-scale silicon carbide-silicon boride composite material on the surface of the substrate 110 by a chemical vapor deposition process to form an anti-oxidation layer 120 .

[0055] In the above embodiment, the reaction temperature of the chemical vapor deposition process can be set to 1200°C-1400°C. If the reaction temperature is too low, the process of silicon carbide reacting with oxygen to form a silicon dioxide protective film will be affected, the reaction will be incomplete, and the formed silicon dioxide protective film will not be dense enough, and the effect of preventing oxygen from entering the body interface will decrease. If the reaction temperature is too high, on the one hand, silicon boride and silicon carbide will react to form a low melting point phase, causing the film layer to soften, and on the other hand, the film layer structure may change, the pores will increase, and oxygen will be easier to pass through.

[0056] Step 3: Forming a sealing layer 130 composed of ceramic glaze on the surface of the anti-oxidation layer 120 by means of immersion coating and high-temperature sintering.

[0057] In the above embodiment, the temperature of high temperature sintering can be 1600°C-1800°C. In this temperature range, the ceramic glaze can be fully melted and react well with the anti-oxidation layer 120, and the components in the ceramic glaze can be fully diffused and migrated to form a uniform and dense glass structure, which can well seal the tiny pores that may exist in the anti-oxidation layer 120, and further prevent oxygen from penetrating into the substrate 110. In addition, this temperature range helps to improve the bonding strength between the sealing layer 130 and the anti-oxidation layer 120. Specifically, high temperature sintering forms a strong chemical bond between the sealing layer 130 and the anti-oxidation layer 120, ensuring the stability and durability of the sealing layer 130 in a high temperature environment, preventing the anti-oxidation layer 120 from volatilizing or falling off at high temperatures, and ensuring that the anti-oxidation effect can continue to play a role. When the temperature is lower than 1600°C, the ceramic glaze may not be completely melted, resulting in insufficient compactness of the sealing layer 130, the presence of more pores and defects, and oxygen may still penetrate into the substrate 110 through these channels, reducing the protective effect. Moreover, the sealing layer 130 and the anti-oxidation layer 120 are not tightly bonded, and peeling is likely to occur during the thermal cycle. When the temperature is higher than 1800°C, the excessively high temperature may cause certain components in the ceramic glaze to volatilize or decompose excessively, destroying the structural integrity of the sealing layer 130, generating cracks or holes, and also making it easier for oxygen to enter, weakening the protective function of the sealing layer 130. In addition, the excessively high temperature may also damage the substrate 110 and the anti-oxidation layer 120, affecting the overall performance and service life of the support ring 100.

[0058] In order to facilitate those skilled in the art to further understand the manufacturing method of the support ring 100 in this embodiment, several specific implementation cases are listed below for reference:

[0059] Embodiment 1:

[0060] A fiber skeleton with a weaving density of 60% is prepared by using a polyacrylonitrile-based carbon fiber with a diameter of 7 microns through a three-dimensional weaving process. The prepared carbon fiber skeleton is placed in a chemical vapor deposition furnace and treated at 1200°C and 50 kPa for 200 hours to be converted into a carbon-carbon composite skeleton. Graphite is simultaneously filled by an asphalt impregnation-carbonization process. Subsequently, a nano-scale silicon carbide-silicon boride composite material (silicon carbide to boride carbon mass ratio 3:1) is deposited on the surface of the substrate 110 by a chemical vapor deposition process, and deposited at 1500°C and 10 kPa for 4 hours to form a 75-micron thick anti-oxidation layer 120. Finally, a silicon dioxide-alumina-boric oxide ceramic glaze is used for impregnation coating, and sintered at 1600°C for 2 hours to form a 40-micron thick glass sealing layer 130.

[0061] Embodiment 2:

[0062] A fiber skeleton with a braiding density of 70% is prepared by using a polyacrylonitrile-based carbon fiber with a diameter of 5 microns through a three-dimensional braiding process. The prepared carbon fiber skeleton is placed in a chemical vapor deposition furnace and treated at 1300°C and 40 kPa for 180 hours to be converted into a carbon-carbon composite skeleton. Graphite is simultaneously filled by an asphalt impregnation-carbonization process. Subsequently, a nano-scale silicon carbide-silicon boride composite material (silicon carbide to boride carbon mass ratio 3:1) is deposited on the surface of the substrate 110 by a chemical vapor deposition process, and deposited at 1600°C and 8 kPa for 3.5 hours to form an 85-micron thick anti-oxidation layer 120. Finally, a silicon dioxide-zirconia-boric oxide ceramic glaze is used for impregnation coating, and sintered at 1700°C for 1.5 hours to form a 40-micron thick glass sealing layer 130.

[0063] Embodiment 3:

[0064] A fiber skeleton with a braiding density of 85% is prepared by using a pitch-based carbon fiber with a diameter of 10 microns through a three-dimensional braiding process. The prepared carbon fiber skeleton is placed in a chemical vapor deposition furnace and treated at 1400°C and 60 kPa for 220 hours to be converted into a carbon-carbon composite skeleton. Graphite is simultaneously filled by a pitch impregnation-carbonization process. Subsequently, a nano-scale silicon carbide-silicon boride composite material (silicon carbide to boride carbon mass ratio of 5:1) is deposited on the surface of the substrate 110 by a chemical vapor deposition process, and deposited at 1700°C and 12 kPa for 5 hours to form a 100-micron thick anti-oxidation layer 120. Finally, a silicon dioxide-alumina-sodium oxide ceramic glaze is used for impregnation coating, and sintered at 1800°C for 1 hour to form a 50-micron thick glass sealing layer 130.

[0065] The manufacturing method of the support ring 100 provided in the embodiment of the present invention includes the following key steps: first, a three-dimensional weaving process is used to make a skeleton with a specific structure of carbon fiber, and then it is placed in a chemical vapor deposition furnace for carbonization treatment, and the carbon fiber is converted into a high-strength carbon-carbon composite skeleton by vapor deposition technology, and graphite is simultaneously filled into the skeleton pores in the process to form a composite matrix 110 with high toughness and thermal conductivity. Then, a nano-scale silicon carbide-silicon boride composite material is uniformly deposited on the surface of the matrix 110 by a chemical vapor deposition process to form an anti-oxidation protective layer. Finally, a dip coating process is used to uniformly cover the surface of the anti-oxidation layer 120 with ceramic glaze, and the glaze is melted by high-temperature sintering and reacts with the anti-oxidation layer 120 to form a glassy dense sealing layer 130 on the surface, so as to achieve double protection for the matrix 110. The manufacturing method of the support ring 100 is simple and practical, and is suitable for industrial large-scale production.

[0066] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments can still be modified, or some or all of the technical features therein can be replaced by equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A support ring, characterized in that: Used in a single crystal furnace, comprising a substrate and a protective layer, wherein the substrate comprises a reinforcement skeleton and a filler filled in the reinforcement skeleton, wherein the reinforcement skeleton is made of a carbon-carbon composite material, and the filler is graphite; The protective layer comprises an anti-oxidation layer and a sealing layer, wherein the anti-oxidation layer is wrapped outside the substrate, and the sealing layer is wrapped outside the anti-oxidation layer, the anti-oxidation layer is a nano-scale silicon carbide-silicon boride composite material, and the sealing layer is a ceramic glaze.

2. The support ring according to claim 1, characterized in that: The thickness of the anti-oxidation layer is 50 μm-100 μm.

3. The support ring according to claim 2, characterized in that: The sealing layer has a thickness of 30 μm-50 μm.

4. The support ring according to claim 3, characterized in that: The mass ratio of silicon carbide to silicon boride in the anti-oxidation layer is 3:1-5:

1.

5. The support ring according to claim 4, characterized in that: The reinforcement skeleton has a heat conduction channel extending radially along the support ring, and the heat conduction channel is filled with the graphite.

6. A single crystal furnace, characterized in that: The invention comprises the support ring as described in any one of claims 1 to 5.

7. A method for manufacturing a support ring, characterized in that: The method for manufacturing the support ring according to any one of claims 1 to 5 comprises the following steps: Weaving carbon fibers into a carbon fiber skeleton using a three-dimensional weaving process, then placing the carbon fiber skeleton into a chemical vapor deposition furnace to transform it into the reinforcement skeleton, and filling the graphite into the reinforcement skeleton during the transformation of the reinforcement skeleton, thereby forming the matrix; Depositing a nano-scale silicon carbide-silicon boride composite material on the surface of the substrate by a chemical vapor deposition process to form the anti-oxidation layer; The sealing layer composed of ceramic glaze is formed on the surface of the anti-oxidation layer by means of immersion coating and high-temperature sintering.

8. The method for manufacturing a support ring according to claim 7, characterized in that: In the three-dimensional weaving process, the weaving density of the carbon fiber is 60%-85%.

9. The method for manufacturing a support ring according to claim 8, characterized in that: The reaction temperature of the chemical vapor deposition process is 1200°C-1400°C.

10. The method for manufacturing a support ring according to claim 9, characterized in that: The high temperature sintering temperature is 1600°C-1800°C.

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