CN111087251B - Connecting material for connecting silicon carbide materials and application thereof - Google Patents

Connecting material for connecting silicon carbide materials and application thereof Download PDF

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CN111087251B
CN111087251B CN201811245422.XA CN201811245422A CN111087251B CN 111087251 B CN111087251 B CN 111087251B CN 201811245422 A CN201811245422 A CN 201811245422A CN 111087251 B CN111087251 B CN 111087251B
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silicon carbide
yttrium
materials
interface
composite material
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CN111087251A (en
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黄庆
周小兵
刘俊文
梁佳敏
邵俊琦
常可可
黄峰
何流
黄政仁
柴之芳
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Ningbo Institute of Material Technology and Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts

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Abstract

The invention discloses a connecting material for connecting silicon carbide materials and application thereof. The connecting material comprises any one or the combination of more than two of yttrium, yttrium silicon carbon material and yttrium-coated silicon carbide composite material. The invention also discloses the application of the yttrium and yttrium silicon carbon material or the yttrium-coated silicon carbide composite material in connecting silicon carbide materials. The invention also discloses a method for connecting the silicon carbide materials, which comprises the following steps: and arranging yttrium and yttrium silicon carbon materials or yttrium-coated silicon carbide composite materials at the joint interface of the silicon carbide materials to be connected, and heating to 1300-1900 ℃ to ensure that the silicon carbide materials to be connected are connected in a seamless manner. The silicon carbide connecting structure obtained by the invention has high bending strength and excellent high-temperature resistance, oxidation resistance and corrosion resistance, and can be applied to extreme service environments such as aerospace and nuclear energy systems.

Description

Connecting material for connecting silicon carbide materials and application thereof
Technical Field
The invention relates to the technical field of connection of silicon carbide ceramics and composite materials thereof, in particular to a method for preparing a silicon carbide ceramic by using yttrium or yttrium silicon carbon material (Y)3Si2C2) Or yttrium-coated silicon carbide composite material, or a method for connecting silicon carbide ceramics or the composite material thereof.
Background
Silicon carbide (SiC) has the advantages of low neutron absorption cross section, excellent high-temperature mechanical properties, good high-temperature chemical stability, environmental compatibility and the like, and therefore, Silicon carbide and its composite materials (including Silicon carbide ceramics, Silicon carbide ceramic matrix composite materials, such as Silicon carbide fiber reinforced Silicon carbide composite materials, carbon fiber reinforced Silicon carbide composite materials and the like) are considered as one of the preferred materials for the fourth-generation pressurized water reactor nuclear fuel cladding tube, the nuclear fusion reactor flow channel insert, the aerospace engine blade and the thermal protection structure of the hypersonic aircraft. However, since silicon carbide and its composite material have characteristics such as high hardness, high melting point, and poor conductivity, and are difficult to mold, it is necessary to manufacture a large-sized and complex-shaped silicon carbide and its composite material device by a connecting technique. However, silicon carbide has the characteristics of strong covalent bond structure, low surface diffusion coefficient and the like, and the connection of silicon carbide and the composite material thereof is difficult to realize, so that the connection of silicon carbide and the composite material thereof becomes one of the key technical bottlenecks which restrict the application of the silicon carbide and the composite material thereof.
For the connection of silicon carbide, especially for the application in the fields of nuclear energy and aerospace, the requirements on the material of the connection layer are very high due to the very harsh service environment. Therefore, most of the connection layer materials selected by researchers at present have the properties of high temperature resistance, oxidation resistance, corrosion resistance and the like, such as silicon carbide, titanium silicon carbon, titanium aluminum carbon and the like. And for high-temperature unstable phases, the silicon carbide material is not suitable for being used as a silicon carbide connecting layer material in the fields of nuclear energy and aerospace. Due to this technical prejudice, the choice of materials for the silicon carbide connection layer is limited.
Disclosure of Invention
The main object of the present invention is to provide a bonding material for bonding silicon carbide materials, which overcomes the disadvantages of the prior art.
It is a further object of the invention to provide the use of said joining material for joining silicon carbide materials.
It is a further object of the present invention to provide a method of joining silicon carbide materials.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a connecting material for connecting silicon carbide materials, which comprises any one or a combination of more than two of yttrium, yttrium silicon carbon materials and yttrium-coated silicon carbide composite materials.
The embodiment of the invention also provides the application of the yttrium and yttrium silicon carbon material or yttrium-coated silicon carbide composite material in connecting silicon carbide materials.
Further, the use comprises: and arranging yttrium or yttrium silicon carbon material or yttrium-coated silicon carbide composite material at the joint interface of the silicon carbide materials to be connected, and heating to 1300-1900 ℃, so that the silicon carbide materials to be connected are connected in a seamless manner.
The embodiment of the invention also provides a method for connecting the silicon carbide materials, which comprises the following steps: and arranging yttrium or yttrium silicon carbon material or yttrium-coated silicon carbide composite material at the joint interface of the silicon carbide materials to be connected, and heating to 1300-1900 ℃, so that the silicon carbide materials to be connected are connected in a seamless manner.
The embodiment of the invention also provides a silicon carbide connecting structure prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention can obtain yttrium silicon carbon (Y) in situ at the connecting interface by utilizing the interface reaction between yttrium (Y) and the matrix silicon carbide3Si2C2) Phase of using Y3Si2C2The silicon carbide and the liquid phase Y can be decomposed in situ under the characteristic of instability at high temperature, and the liquid phase Y can be further diffused into a crystal boundary and/or a pore of the silicon carbide at the connecting interface as a sintering aid, so that the connection and densification of the silicon carbide at the interface are promoted, and the local seamless connection can be realized;
2) the obtained silicon carbide connecting structure has high bending strength and excellent high-temperature resistance, oxidation resistance and corrosion resistance, and can be applied to extreme service environments such as aerospace, nuclear energy systems and the like.
Drawings
Fig. 1 is a schematic structural view of a silicon carbide material to be bonded and a bonding layer in embodiment 1 of the present invention.
FIG. 2 shows 500nm Y in example 1 of the present invention3Si2C2And (5) carrying out interface back scattering Scanning Electron Microscope (SEM) picture on the connected silicon carbide ceramic connection structure.
FIG. 3 is an interface back-scattering SEM image of the SiC ceramic bonded structure after Y bonding at 500nm in example 2 of the present invention.
FIG. 4 is an interface back scattering scanning electron micrograph of the SiC ceramic bonded structure after the 500nm Y-coated SiC composite material is bonded in example 3 of the present invention.
FIG. 5 is an SEM image of the interface of the SiC ceramic bonded structure after 100nm Y bonding in example 4 of the present invention.
FIG. 6 is a SEM photograph of the interface of the SiC bonded structure obtained in comparative example 1 of the present invention.
Detailed Description
In order to overcome the problems of the prior art, the inventors of the present invention have surprisingly found that seamless connection of silicon carbide materials can be realized with high efficiency by using a high-temperature unstable phase in the course of long-term research and extensive practice, and based on the unexpected finding, the inventors have proposed the technical solution of the present invention, which will be further explained below.
In one aspect of the present invention, the present invention relates to a bonding material for bonding silicon carbide materials, the bonding material including one or a combination of two or more of yttrium, an yttrium silicon carbon material, and an yttrium-coated silicon carbide composite material.
Further, the yttrium-coated silicon carbide composite material comprises a mixture of yttrium and silicon carbide particles, wherein the yttrium is uniformly coated on the surfaces of the silicon carbide particles.
Further, the yttrium content (mass percentage) in the yttrium-coated silicon carbide composite material is 1-50 wt%.
In one aspect of the invention, the yttrium-based silicon carbon material or yttrium-coated silicon carbide composite material is used for connecting silicon carbide materials.
In some embodiments, the use comprises: and arranging yttrium or yttrium silicon carbon material or yttrium-coated silicon carbide composite material at the joint interface of the silicon carbide materials to be connected, and heating to 1300-1900 ℃, so that the silicon carbide materials to be connected are connected in a seamless manner.
Further, the use comprises: and arranging an yttrium film or an yttrium silicon carbon material or an yttrium-coated silicon carbide composite material at the connecting interface of the silicon carbide materials to be connected.
Further, the thickness of the yttrium film is less than 1 μm, preferably 50-500 nm. The inventor of the invention discovers through a great deal of experiments that when the yttrium film is selected as the connecting material and the thickness of the yttrium film is controlled to be less than 1 mu m, the connected silicon carbide ceramic interface can realize local seamless connection, the interface phase is mainly silicon carbide, the silicon carbide ceramic interface has good high-temperature resistance and oxidation resistance, and the obtained silicon carbide connecting interface has high bending strength.
Further, the thickness of the yttrium silicon carbon or yttrium-coated silicon carbide composite material is less than 1mm, and preferably 1-500 μm.
In some embodiments, the bonding material comprises a yttrium silicon carbon material capable of decomposing to produce silicon carbide and liquid phase yttrium.
In some embodiments of the invention, a yttrium silicon carbon material (Y) is utilized3Si2C2) The phase change at high temperature and the yttrium silicon carbon material can be decomposed at a certain temperature to obtain silicon carbide and liquid phase yttrium (Y), and the formed liquid phase yttrium can be used as a sintering aid and can be easily diffused to a crystal boundary and/or pores of the silicon carbide at the connection interface, so that the diffusion, connection and densification of the silicon carbide at the interface are promoted, and the local seamless connection can be realized. Meanwhile, with the volatilization of Y at high temperature, SiC can be precipitated in situ from the liquid phase in the cooling process, and seamless connection is expected to be realized. Thus, after high temperature bonding, the bonding layer material is free of small amounts of residual Y3Si2C2Or the silicon carbide is added to the Y, and the obtained connecting structure has good performances of high temperature resistance, oxidation resistance, corrosion resistance and the like.
In some embodiments, the silicon carbide material includes, but is not limited to, pure silicon carbide ceramic materials, silicon carbide ceramic matrix composites, and the like.
Further, the silicon carbide ceramic matrix composite includes, but is not limited to, a carbon fiber reinforced silicon carbide composite, a silicon carbide fiber reinforced silicon carbide composite, and the like.
As another aspect of the present invention, it further relates to a method for joining silicon carbide materials, as shown in fig. 1, which includes: and arranging yttrium or yttrium silicon carbon material or yttrium-coated silicon carbide composite material at the joint interface of the silicon carbide materials to be connected, and heating to 1300-1900 ℃, so that the silicon carbide materials to be connected are connected in a seamless manner.
Further, the use comprises: arranging an yttrium film, or an yttrium silicon carbon material, or an yttrium-coated silicon carbide composite material at the connecting interface of the silicon carbide materials to be connected
Further, the thickness of the yttrium film is less than 1 μm, preferably 50-500 nm. The inventor of the invention discovers through a great deal of experiments that when the yttrium film is selected as the connecting material and the thickness of the yttrium film is controlled to be less than 1 mu m, the connected silicon carbide ceramic interface can realize local seamless connection, the interface phase is mainly silicon carbide, the silicon carbide ceramic interface has good high-temperature resistance and oxidation resistance, and the obtained silicon carbide connecting interface has high bending strength.
Further, the thickness of the yttrium silicon carbon or yttrium-coated silicon carbide composite material is less than 1mm, and preferably 1-500 μm.
In some embodiments, the bonding material comprises a yttrium silicon carbon material capable of decomposing to produce silicon carbide and liquid phase yttrium.
In some embodiments of the invention, a yttrium silicon carbon material (Y) is utilized3Si2C2) The phase change at high temperature and the yttrium silicon carbon material can be decomposed at a certain temperature to obtain silicon carbide and liquid phase yttrium (Y), and the formed liquid phase yttrium can be used as a sintering aid and can be easily diffused to a crystal boundary and/or pores of the silicon carbide at the connection interface, so that the diffusion, connection and densification of the silicon carbide at the interface are promoted, and the local seamless connection can be realized. Meanwhile, with the volatilization of Y at high temperature, SiC can be precipitated in situ from the liquid phase in the cooling process, and seamless connection is expected to be realized. Thus, after high temperature bonding, the bonding layer material is free of small amounts of residual Y3Si2C2Or the silicon carbide is added to the Y, and the obtained connecting structure has good performances of high temperature resistance, oxidation resistance, corrosion resistance and the like.
In some embodiments, the silicon carbide material includes, but is not limited to, pure silicon carbide ceramic materials, silicon carbide ceramic matrix composites, and the like.
Further, the silicon carbide ceramic matrix composite includes, but is not limited to, a carbon fiber reinforced silicon carbide composite, a silicon carbide fiber reinforced silicon carbide composite, and the like.
In some embodiments, the method for connecting the silicon carbide ceramic material by using the connecting material of the present invention is not limited, and the heating manner includes a pressureless heating connection, a hot pressing connection, an electric field assisted heating connection, a microwave field assisted connection, and the like, and preferably, the electric field assisted heating connection.
The invention can obtain yttrium silicon carbon (Y) at the interface by utilizing the interface reaction between yttrium and matrix silicon carbide3Si2C2) Phase of using Y3Si2C2The liquid yttrium can be further diffused into silicon carbide crystal boundaries and/or pores, so that the densification of interface silicon carbide is promoted, and local seamless connection can be realized. The realization of the seamless connection layer can further improve the high-temperature resistance, oxidation resistance and corrosion resistance of the silicon carbide connection structure.
Further, the preparation method of the connection material of the present invention is not limited, and the yttrium film can be obtained by depositing an yttrium film on the surface of the substrate by a Physical Vapor Deposition (PVD) method, and finally removing the substrate. Or, carrying out physical vapor deposition on the surface of the silicon carbide ceramic material to be connected to form an yttrium film; the yttrium silicon carbon material (Y)3Si2C2) The material can be obtained by a solid-phase reaction method and is made into a casting film or a pre-sintered ceramic sheet; the yttrium-coated silicon carbide composite material can be obtained by adopting a solid-phase ball milling or high-temperature molten salt method and comprises a mixture of yttrium and silicon carbide, wherein the mass percent of yttrium is 1-50 wt%; the structural characteristics are that yttrium is preferably uniformly coated on the surface of the silicon carbide particles.
Accordingly, another aspect of an embodiment of the present invention also provides a silicon carbide connection structure made by the foregoing method.
Further, the connection layer in the silicon carbide connection structure may disappear, or be mainly a silicon carbide phase.
Furthermore, the strength of the connecting interface and the strength of the connecting layer of the silicon carbide connecting structure are both greater than that of the matrix silicon carbide.
In another aspect of the embodiments of the present invention, an application of the foregoing silicon carbide connection structure in the field of preparation of aerospace materials or nuclear energy systems is also provided.
Furthermore, the obtained silicon carbide connecting structure has high bending strength and excellent high-temperature resistance, oxidation resistance and corrosion resistance, and can be applied to extreme service environments such as aerospace and nuclear energy systems.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are explained in further detail below with reference to the accompanying drawings and several preferred embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
In this example, as shown in FIG. 2, it is 500nm Y3Si2C2And (3) a connection structure schematic diagram for connecting the silicon carbide ceramics. The material to be connected is two pieces of silicon carbide with the diameter of 20 multiplied by 20mm, and the material of the connecting layer is 500nm Y3Si2C2And heating the connecting interface by the aid of an electric field to enable the connecting interface to reach 1500 ℃, so that the SiC materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide to be connected to 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) coating a piece of silicon carbide surface to be connected with 500nm Y by using a spraying method3Si2C2Then, another piece of silicon carbide is butted with the surface of the silicon carbide; and then putting the sample into a graphite mold, then putting the graphite mold into a discharge plasma sintering furnace, electrifying, heating to the furnace temperature of 1500 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 1min, applying the pressure of 30MPa to the connection sample in the heating process, and then cooling to the room temperature at the speed of 100 ℃/min to obtain the silicon carbide connection structure.
The microscopic morphology of the interface of the silicon carbide connecting structure obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron microscope photo is shown in fig. 2, which shows that the connecting interface has no obvious cracks, the connecting layer is compact, and the strength is high.
And cutting and polishing the obtained silicon carbide connecting structure, processing the silicon carbide connecting structure into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip to be about 130Mpa by adopting a four-point bending method, and testing the sample strip to be broken on the matrix silicon carbide, wherein the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 2
In this embodiment, fig. 3 is a schematic view of a connection structure of 500nm Y-connected silicon carbide ceramics. The materials to be connected are two pieces of silicon carbide with phi of 20mm by 20mm, the materials of the connecting layer are 500nm Y films, and the connecting interface is heated by the aid of an electric field to reach 1900 ℃, so that the SiC materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide to be connected to 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) plating a 500nm Y film on the surface of one piece of silicon carbide to be connected by a PVD method, and butting the other piece of silicon carbide with the surface of the other piece of silicon carbide; and then putting the sample into a graphite mold, then putting the graphite mold into a discharge plasma sintering furnace, electrifying, heating to 1900 ℃ at the heating rate of 100 ℃/min, keeping the temperature for 10min, applying 35MPa pressure to the connection sample in the heating process, and then cooling to room temperature at the speed of 50 ℃/min to obtain the silicon carbide connection structure.
The microscopic morphology of the interface of the silicon carbide connection structure obtained in the present example was observed with a scanning electron microscope, and the back-scattering scanning electron micrograph shown in FIG. 3 shows that the connection interface has no significant cracks, since Y is at high temperature3Si2C2Most of Y volatilizes when the silicon carbide is converted into a liquid phase, and Si and C are recrystallized to separate out the silicon carbide in the cooling process, so that most of the connecting layers are connected seamlessly, the connecting layers are difficult to find, and only a small amount of Y residues (the bright spots are Y in figure 3) are high in strength.
And cutting and polishing the obtained silicon carbide connecting structure, processing the silicon carbide connecting structure into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip to be about 146MPa by adopting a four-point bending method, and breaking the sample strip on the matrix silicon carbide, wherein the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 3
In this embodiment, as shown in fig. 4, a schematic connection structure of a 500nm Y-coated silicon carbide composite material connected to a silicon carbide ceramic is shown. The materials to be connected are two pieces of silicon carbide with the phi of 20mm by 20mm, the materials of the connecting layer are 500nm Y-coated silicon carbide composite materials, and the connecting interface is heated by the aid of an electric field to reach 1600 ℃, so that the SiC materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide to be connected to 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing a 500nm Y-coated silicon carbide composite material by a molten salt method, preparing a casting film, clamping the 500nm Y-coated silicon carbide composite material casting film between two pieces of silicon carbide, putting a sample into a graphite die, then putting the graphite die into a discharge plasma sintering furnace, electrifying, heating to the furnace temperature of 1600 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 10min, applying 50MPa pressure to a connection sample in the heating process, and then cooling to the room temperature at the speed of 50 ℃/min to obtain the silicon carbide connection structure.
The microscopic morphology of the interface of the silicon carbide connection structure obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron microscope photo is shown in fig. 4, which shows that the connection interface has no obvious cracks, the connection layer is compact, and the connection strength is high.
And cutting and polishing the obtained silicon carbide connecting structure, processing the silicon carbide connecting structure into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip to be about 130Mpa by adopting a four-point bending method, and testing the sample strip to be broken on the matrix silicon carbide, wherein the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 4
In this embodiment, fig. 5 is a schematic view of a connection structure of 100nm Y-connected silicon carbide ceramics. The materials to be connected are two pieces of silicon carbide with the phi of 20mm by 20mm, the materials of the connecting layer are 100nm Y films, and the connecting interface is heated by the aid of an electric field to reach 1300 ℃, so that the SiC materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) plating a 100nm Y film on the surface of one piece of silicon carbide to be connected by a PVD method, and butting the other piece of silicon carbide with the surface of the other piece of silicon carbide; and then putting the sample into a graphite mold, then putting the graphite mold into a discharge plasma sintering furnace, electrifying, heating to the furnace temperature of 1300 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 10min, applying the pressure of 50MPa to the connection sample in the heating process, and then cooling to the room temperature at the speed of 50 ℃/min to obtain the silicon carbide connection structure.
The microscopic morphology of the interface of the silicon carbide connection structure obtained in the embodiment was observed by a scanning electron microscope, and a back-scattering scanning electron micrograph is shown in fig. 5, which shows that the connection interface has no obvious cracks and high strength.
And cutting and polishing the obtained silicon carbide connecting structure, processing the silicon carbide connecting structure into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip by adopting a four-point bending method to be about 110Mpa, and breaking the sample strip on the matrix silicon carbide, wherein the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 5
In the embodiment, the materials to be connected are two pieces of silicon carbide with the phi of 20 multiplied by 20mm, the material of the connecting layer is a 50nm Y film, and the connecting interface is heated by the aid of a microwave field to reach 1300 ℃, so that the SiC materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) plating a 50nm Y film on the surface of one piece of silicon carbide to be connected by a PVD method, and butting the other piece of silicon carbide with the surface of the other piece of silicon carbide; and then putting the sample into a microwave field auxiliary heating furnace, heating to 1300 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 120min, and then cooling to room temperature at the speed of 5 ℃/min to obtain the silicon carbide connecting structure.
The microscopic morphology of the interface of the silicon carbide connecting structure obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron microscope photo is similar to that in FIG. 5, and shows that the connecting interface has no obvious cracks and high strength.
And cutting and polishing the obtained silicon carbide connecting structure, processing the silicon carbide connecting structure into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip to be about 120Mpa by adopting a four-point bending method, and breaking the sample strip on the matrix silicon carbide, wherein the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 6
In the embodiment, the materials to be connected are two pieces of silicon carbide with the phi of 20 multiplied by 20mm, the material of the connecting layer is a 1 mu m Y film, and the connecting interface reaches 1800 ℃ through hot-pressing the connecting interface, so that the SiC materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) plating a 1 mu m Y film on the surface of one piece of silicon carbide to be connected by a PVD method, and butting the other piece of silicon carbide with the surface of the other piece of silicon carbide; and then putting the sample into a microwave field auxiliary heating furnace, heating to the furnace temperature of 1800 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 120min, and then cooling to the room temperature at the speed of 5 ℃/min to obtain the silicon carbide connecting structure.
The microscopic morphology of the interface of the silicon carbide connecting structure obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron microscope photo is similar to that shown in fig. 3, so that the connecting interface has no obvious cracks and high strength.
And cutting and polishing the obtained silicon carbide connecting structure, processing the silicon carbide connecting structure into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip to be about 150Mpa by adopting a four-point bending method, and breaking the sample strip on the matrix silicon carbide, wherein the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 7
In the embodiment, the materials to be connected are two silicon carbide fiber reinforced silicon carbide composite materials with the phi of 20 multiplied by 20mm, the material of the connecting layer is 1 mu m yttrium silicon carbon, and the connecting interface reaches 1800 ℃ through hot-pressing the connecting interface, so that the silicon carbide fiber reinforced silicon carbide composite materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) plating 1 mu m yttrium silicon carbon on the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected by a thermal spraying method, and then butting the other silicon carbide fiber reinforced silicon carbide composite material with the other silicon carbide fiber reinforced silicon carbide composite material; and then putting the sample into a hot pressing furnace, heating to the furnace temperature of 1700 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 100min, and then cooling to the room temperature at the speed of 5 ℃/min to obtain the silicon carbide fiber reinforced silicon carbide composite material connecting structure.
The microscopic morphology of the interface of the silicon carbide fiber reinforced silicon carbide composite material obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron micrograph is similar to that in FIG. 3, which shows that the connecting interface has no obvious cracks and high strength.
The obtained silicon carbide fiber reinforced silicon carbide composite material connecting structure is cut and polished to be processed into a 4X 3X 40mm sample strip, the four-point bending strength of the sample strip is tested to be about 300Mpa by adopting a four-point bending method, and the sample strip is broken on the matrix silicon carbide, which shows that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 8
In the embodiment, the materials to be connected are two carbon fiber reinforced silicon carbide composite materials with phi of 20 multiplied by 20mm, the material of the connecting layer is 100 mu m yttrium silicon carbon, and the connecting interface reaches 1900 ℃ through a pressureless connecting interface, so that the carbon fiber reinforced silicon carbide composite materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the carbon fiber reinforced silicon carbide composite material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing yttrium silicon carbon into a casting film with the thickness of 100 microns, placing the casting film on the surface of the carbon fiber reinforced silicon carbide composite material to be connected, and then butting the other carbon fiber reinforced silicon carbide composite material with the casting film; and then putting the sample into a vacuum furnace, heating to 1900 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 240min, and then cooling to room temperature at the speed of 5 ℃/min to obtain the carbon fiber reinforced silicon carbide composite material connecting structure.
The microscopic morphology of the interface of the carbon fiber reinforced silicon carbide composite material obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron microscope photo is similar to that shown in FIG. 3, so that the connecting interface has no obvious cracks and high strength.
The obtained silicon carbide fiber reinforced silicon carbide composite material connecting structure is cut and polished to be processed into a 4X 3X 40mm sample strip, the four-point bending strength of the sample strip is tested to be about 160Mpa by adopting a four-point bending method, and the sample strip is broken on the matrix silicon carbide, which shows that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 9
In the embodiment, the materials to be connected are two silicon carbide fiber reinforced silicon carbide composite materials with the phi of 20 multiplied by 20mm, the material of the connecting layer is 1mm yttrium silicon carbon, and the connecting interface reaches 1800 ℃ through hot-pressing the connecting interface, so that the silicon carbide fiber reinforced silicon carbide composite materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing yttrium silicon carbon into a casting film with the thickness of 1mm, placing the casting film on the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected, and then butting the other silicon carbide fiber reinforced silicon carbide composite material with the other silicon carbide fiber reinforced silicon carbide composite material; and then putting the sample into a hot pressing furnace, heating to the furnace temperature of 1800 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 120min, and then cooling to the room temperature at the heating rate of 5 ℃/min to obtain the silicon carbide fiber reinforced silicon carbide composite material connecting structure.
The microscopic morphology of the interface of the silicon carbide fiber reinforced silicon carbide composite material obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron micrograph is similar to that in FIG. 3, which shows that the connecting interface has no obvious cracks and high strength.
The obtained silicon carbide fiber reinforced silicon carbide composite material connecting structure is cut and polished to be processed into a 4X 3X 40mm sample strip, the four-point bending strength of the sample strip is tested to be about 260Mpa by adopting a four-point bending method, and the sample strip is broken on the matrix silicon carbide, which shows that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 10
In the embodiment, the materials to be connected are two silicon carbide fiber reinforced silicon carbide composite materials with the phi of 20 multiplied by 20mm, the material of the connecting layer is 100 mu m yttrium-coated silicon carbide composite material, and the connecting interface is assisted by an electric field to reach 1800 ℃, so that the silicon carbide fiber reinforced silicon carbide composite materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing a casting film with the thickness of 100 microns from the yttrium-coated silicon carbide composite material, placing the casting film on the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected, and then butting the other silicon carbide fiber reinforced silicon carbide composite material with the casting film; and then putting the sample into a discharge plasma sintering furnace, electrifying, applying 10MPa of axial pressure, heating to the furnace temperature of 1800 ℃ at the heating rate of 100 ℃/min, preserving the temperature for 10min, and then cooling to the room temperature at the speed of 50 ℃/min to obtain the silicon carbide fiber reinforced silicon carbide composite material connecting structure.
The microscopic morphology of the interface of the silicon carbide fiber reinforced silicon carbide composite material obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron micrograph is similar to that in FIG. 3, which shows that the connecting interface has no obvious cracks and high strength.
The obtained silicon carbide fiber reinforced silicon carbide composite material connecting structure is cut and polished to be processed into a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, the four-point bending strength of the sample strip is tested to be about 295Mpa by adopting a four-point bending method, and the sample strip is broken on the matrix silicon carbide, which shows that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 11
In the embodiment, the materials to be connected are two silicon carbide fiber reinforced silicon carbide composite materials with the phi of 20 multiplied by 20mm, the material of the connecting layer is a yttrium-coated silicon carbide composite material with the thickness of 10 microns, and the connecting interface is assisted by an electric field to reach 1700 ℃, so that the silicon carbide fiber reinforced silicon carbide composite materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing a yttrium-coated silicon carbide composite material into a casting film with the thickness of 10 microns, placing the casting film on the surface of a silicon carbide fiber reinforced silicon carbide composite material to be connected, and then butting another silicon carbide fiber reinforced silicon carbide composite material with the casting film; and then putting the sample into a discharge plasma sintering furnace, electrifying, applying 30MPa of axial pressure, heating to the furnace temperature of 1700 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 30min, and then cooling to the room temperature at the speed of 50 ℃/min to obtain the silicon carbide fiber reinforced silicon carbide composite material connecting structure.
The microscopic morphology of the interface of the silicon carbide fiber reinforced silicon carbide composite material obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron micrograph is similar to that in FIG. 3, which shows that the connecting interface has no obvious cracks and high strength.
The obtained silicon carbide fiber reinforced silicon carbide composite material connecting structure is cut and polished to be processed into a 4X 3X 40mm sample strip, the four-point bending strength of the sample strip is tested to be about 290Mpa by adopting a four-point bending method, and the sample strip is broken on the matrix silicon carbide, which shows that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 12
In the embodiment, the materials to be connected are two silicon carbide fiber reinforced silicon carbide composite materials with the phi of 20 multiplied by 20mm, the material of the connecting layer is 1 micron yttrium-coated silicon carbide composite material, and the connecting interface is assisted by an electric field to reach 1700 ℃, so that the silicon carbide fiber reinforced silicon carbide composite materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide fiber reinforced silicon carbide composite material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing a yttrium-coated silicon carbide composite film with the thickness of 1 mu m on the surface of the silicon carbide fiber reinforced silicon carbide composite material by a spraying method, and then butting the other silicon carbide fiber reinforced silicon carbide composite material with the yttrium-coated silicon carbide composite film; and then putting the sample into a discharge plasma sintering furnace, electrifying, applying 50MPa axial pressure, heating to the furnace temperature of 1700 ℃ at the heating rate of 30 ℃/min, preserving the temperature for 10min, and then cooling to the room temperature at the speed of 30 ℃/min to obtain the silicon carbide fiber reinforced silicon carbide composite material connecting structure.
The microscopic morphology of the interface of the silicon carbide fiber reinforced silicon carbide composite material obtained in the embodiment is observed by using a scanning electron microscope, and a back scattering scanning electron micrograph is similar to that in FIG. 3, which shows that the connecting interface has no obvious cracks and high strength.
The obtained silicon carbide fiber reinforced silicon carbide composite material connecting structure is cut and polished to be processed into a 4X 3X 40mm sample strip, the four-point bending strength of the sample strip is tested to be about 260Mpa by adopting a four-point bending method, and the sample strip is broken on the matrix silicon carbide, which shows that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Comparative example 1
In the comparison example, the materials to be connected are two silicon carbide materials with phi 20 multiplied by 20mm, the material of the connecting layer is a titanium silicon carbon cast film with the thickness of 60 mu m, and the connecting interface reaches 1500 ℃ through electric field auxiliary connection, so that the silicon carbide materials to be connected are connected together. The method comprises the following specific steps:
(1) polishing the surface of the silicon carbide material to be connected to 0.1 mu m by using diamond polishing solution, and removing defects and impurities on the surface;
(2) placing a 60-micron titanium silicon carbon cast film on the surface of silicon carbide, and butting the other piece of silicon carbide with the silicon carbide; and then putting the sample into a discharge plasma sintering furnace, electrifying, applying 50MPa axial pressure, heating to the furnace temperature of 1500 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 10min, and then cooling to the room temperature at the speed of 50 ℃/min to obtain the silicon carbide connecting structure.
The microscopic morphology of the interface of the silicon carbide connection structure obtained in the comparative example was observed by a scanning electron microscope, and a back-scattering scanning electron micrograph is shown in fig. 6, which shows that the connection interface has obvious cracks due to the large difference in thermal expansion coefficient between the titanium silicon carbon and the silicon carbide at the connection layer.
And cutting and polishing the obtained silicon carbide connecting structure to obtain a sample strip with the thickness of 4 multiplied by 3 multiplied by 40mm, testing the four-point bending strength of the sample strip by adopting a four-point bending method to be about 80Mpa, and breaking the sample strip on the interface titanium silicon carbon to show that the strength of a connecting layer is lower.
Compared with the embodiment of the invention, the titanium silicon carbon is taken as the connecting layer to connect the silicon carbide, and the thermal expansion coefficient (about 9.2 multiplied by 10) of the titanium silicon carbon is the material of the connecting layer-6K-1) Is matrix silicon carbide (4.5 multiplied by 10)-6K-1) 2 times of the connection structure, in the cooling process, the carbon, the silicon and the carbon in the connection layer can receive the action of tensile stress, and cracks are generated in the connection layer, so that on one hand, the connection structure is not beneficial to connection and sealing; on the other hand, the crack may become the weakest link in the connection structure. Meanwhile, the residual thermal stress can greatly reduce the mechanical properties of the silicon carbide connecting structure, such as the bending strength of only 80 MPa. According to the invention, the yttrium silicon carbon connecting layer is obtained through in-situ reaction between yttrium and matrix silicon carbide, so that strong interface chemical bonding is formed, meanwhile, silicon carbide and the liquid phase Y are obtained through in-situ decomposition by utilizing the instability of yttrium silicon carbon at high temperature, on one hand, the liquid phase Y can be further diffused and enter into the grain boundary and/or pores of the silicon carbide at the connecting interface as a sintering aid, so that the connection and densification of the interface silicon carbide are promoted, and local seamless connection can be realized; on the other hand, the precipitated silicon carbide has the same composition as the matrix phase, and there is no difference in thermal expansion coefficient, so that no crack occurs, and the flexural strength, the high temperature resistance, the oxidation resistance, and the corrosion resistance of the connection structure are not affected.
In addition, the inventors of the present invention conducted tests using other materials and conditions listed in the present specification in the manner of examples 1 to 12, and also obtained a silicon carbide bonded structure having high flexural strength and excellent high-temperature oxidation resistance and corrosion resistance.
It should be understood that the above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.

Claims (6)

1. A method of joining silicon carbide materials, comprising: an yttrium film with the thickness of 50-500 nm, or an yttrium silicon carbon material with the thickness of 1-500 mu m, or an yttrium-coated silicon carbide composite material is arranged at the joint interface of two silicon carbide materials to be connected, the materials are heated to 1300-1900 ℃, and simultaneously pressurized, and the decomposed yttrium is further diffused into the crystal boundary and/or the pore of the silicon carbide at the joint interface as a sintering aid, so that the connection and densification of the interface silicon carbide are promoted, and the two silicon carbide materials to be connected are connected seamlessly, wherein the yttrium-coated silicon carbide composite material comprises a mixture of yttrium and silicon carbide particles, the yttrium is uniformly coated on the surfaces of the silicon carbide particles, the content of the yttrium in the yttrium-coated silicon carbide composite material is 1-50 wt%, and the joint interface strength and the joint layer strength of the silicon carbide joint structure are both greater than the strength of the matrix silicon carbide.
2. The connecting method according to claim 1, characterized in that: the silicon carbide material is selected from pure silicon carbide ceramic materials and/or silicon carbide ceramic matrix composite materials.
3. The connecting method according to claim 2, characterized in that: the silicon carbide ceramic matrix composite is selected from a carbon fiber reinforced silicon carbide composite and/or a silicon carbide fiber reinforced silicon carbide composite.
4. The connecting method according to claim 1, characterized in that: the heating mode is selected from hot-pressing connection, electric field auxiliary heating connection or microwave field auxiliary heating connection.
5. The connecting method according to claim 4, characterized in that: the heating mode is electric field auxiliary heating connection.
6. A silicon carbide interconnect structure made by the method of any of claims 1-5 in which the interconnect layer is absent.
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