CN111018555A - Connecting material for connecting silicon carbide with crack self-healing characteristic and application thereof - Google Patents

Connecting material for connecting silicon carbide with crack self-healing characteristic and application thereof Download PDF

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CN111018555A
CN111018555A CN202010000804.7A CN202010000804A CN111018555A CN 111018555 A CN111018555 A CN 111018555A CN 202010000804 A CN202010000804 A CN 202010000804A CN 111018555 A CN111018555 A CN 111018555A
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silicon carbide
sic
mixture
connection
film
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CN111018555B (en
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周小兵
刘俊文
黄政仁
黄庆
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Ningbo Institute of Material Technology and Engineering of CAS
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
    • C04B2237/04—Ceramic interlayers
    • C04B2237/08—Non-oxidic interlayers
    • C04B2237/083—Carbide interlayers, e.g. silicon carbide interlayers
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/36—Non-oxidic
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining

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  • Organic Chemistry (AREA)

Abstract

The invention discloses a connecting material for connecting silicon carbide and having the characteristic of crack self-healing and application thereof. The connecting material comprises Al4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4Mixtures with SiC, and the like. The invention also discloses the application of the connecting material in connecting silicon carbide materials. The invention also discloses a method for connecting the silicon carbide materials, which comprises the following steps: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And mixing the silicon carbide and SiC, and heating to realize high-strength connection between the silicon carbide materials to be connected. The silicon carbide connecting structure obtained by the invention has high bending strength, excellent high-temperature resistance, oxidation resistance and corrosion resistance, has the function of crack self-healing at high temperature, and can be applied to extreme service environments such as aerospace, nuclear energy systems and the like。

Description

Connecting material for connecting silicon carbide with crack self-healing characteristic 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 Al4C3、Al4SiC4、Al4C3With SiC mixture and Al4SiC4A connecting material and a connecting method for connecting silicon carbide with crack self-healing characteristics such as SiC mixture and the like, and application thereof in a connecting layer of silicon carbide and a composite material thereof.
Background
Silicon carbide (SiC) has become one of the key structural materials in the nuclear industry and aerospace field due to its excellent characteristics of high strength, good corrosion resistance, high temperature stability, and low induced radioactivity. However, SiC has a strong covalent bond characteristic and a low surface self-diffusion coefficient, which makes it difficult to machine and form large-sized and complex-shaped silicon carbide materials. The preparation of the large-size and complex-shape silicon carbide component by the connection technology is one of the more effective technical schemes at present.
Generally, the direct connection of SiC is achieved at higher connection temperatures, requiring temperatures of 1900 ℃ or even higher, and requiring the application of greater axial pressure to assist the connection. By selecting a suitable material for the connection layer, the SiC connection process can be improved. Therefore, the selection of the material of the connection layer is crucial in order to avoid failure of the connection layer during service of the SiC connection. Over the past several decades, a number of interlayer materials have been used to join SiC, including metals, ceramics, cermets, and glass-ceramics (Al)2O3-Y2O3-SiO2) And the like. However, under the action of high temperature or water vapor corrosion, the SiC connector fails at the interface layer due to cracks at the connection interface or residual stress caused by thermal mismatch, which is difficult to meet the actual use requirements.
Disclosure of Invention
The invention mainly aims to provide a connecting material for connecting silicon carbide, which has the characteristic of crack self-healing, so as to overcome the defects 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, which has the characteristic of crack self-healing, wherein the connecting material comprises Al4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And any one or a combination of two or more of the above and SiC, wherein the connecting material has a high-temperature crack self-healing function.
The embodiment of the invention also provides Al4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4Use of a mixture with SiC for bonding silicon carbide materials.
Further, the use comprises: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And heating the mixture with SiC to 1000-2000 ℃ to realize high-strength connection between the silicon carbide materials to be connected.
The embodiment of the invention also provides a method for connecting the silicon carbide materials, which comprises the following steps: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And one or more than two of the SiC mixtures are combined and heated to 1000-2000 ℃, so that the silicon carbide materials to be connected are connected with each other in a high-strength manner.
The embodiment of the invention also provides the silicon carbide connecting structure prepared by the method, and the silicon carbide connecting structure has a crack self-healing function at high temperature.
The embodiment of the invention also provides a self-healing method of the silicon carbide connection structure, which comprises the following steps: and carrying out high-temperature oxidation treatment on the silicon carbide connecting structure to enable the cracks in the silicon carbide connecting structure to be self-healed.
Further, the embodiment of the invention also provides the application of the silicon carbide connecting structure in the field of aerospace or nuclear energy systems.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention utilizes Al4C3The interface reaction between the three-element layered ceramic carbon silicide (Al) and the matrix silicon carbide can be obtained in situ at the connecting interface4SiC4) Phase of using Al4SiC4The characteristic of strength rise at high temperature can realize high-strength connection, the connection strength can reach 200MPa, is higher than that of a silicon carbide substrate, and is broken on the silicon carbide substrate;
2) realization of the high-strength connecting layer of the invention, the obtained silicon carbide connecting structure and Al in the connecting layer4SiC4The thermal expansion coefficient of the phase is similar to that of the matrix silicon carbide, the bending strength is high, the high-temperature resistance, the oxidation resistance and the corrosion resistance are excellent, the failure caused by the difference of the heat, the force, the environmental compatibility and the like of the connecting layer material and the matrix silicon carbide in the prior art can be effectively solved, and the phase-change material can be applied to the extreme service environment of aerospace, nuclear energy systems and the like;
3) realization of the high-strength connecting layer of the invention, the obtained silicon carbide connecting structure and Al in the connecting layer4SiC4The phase has the self-healing and self-healing capabilities of cracks under the high-temperature steam oxidation condition, and can prolong the service life in the extreme service process of aerospace, nuclear energy systems and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic view of a silicon carbide connection structure in example 1 of the present invention.
FIGS. 2a and 2b are 100 μm Al in example 1 of the present invention4SiC4And (4) comparing the secondary electron scanning electron microscope photographs of the connecting layer of the connected silicon carbide ceramic connecting piece before and after high-temperature steam corrosion.
FIGS. 3a and 3b are 100 μm Al in example 2 of the present invention4C3And (3) a comparison picture of secondary electron scanning electron micrographs of the connecting layer of the silicon carbide ceramic connecting piece before and after high-temperature air oxidation after membrane connection.
FIGS. 4a and 4b are the comparison of scanning electron micrographs of the connecting layer before and after high temperature water vapor corrosion of the silicon carbide ceramic connecting piece after the 50 μm titanium silicon carbon cast film is connected as the connecting layer in comparative example 1.
Detailed Description
Aluminum silicon carbon (Al)4SiC4) The ceramic material has good high-temperature mechanical property, and the high-temperature bending strength of the ceramic material is 50% higher than that of the ceramic material at room temperature. And the high-temperature oxidation performance is excellent, a compact alumina and mullite protective film can be formed on the surface during high-temperature oxidation, further oxidation in the alumina and mullite protective film is inhibited, and the aluminum silicon carbon can still be stably used in a high-temperature oxidation environment at 1800 ℃. In addition, the aluminum silicon carbon also has stronger corrosion resistance and radiation resistance, which are similar to the silicon carbide. In addition, the unique laminated structure of the material ensures that the material has good thermal shock resistance and certain damage tolerance, and the thermal expansion coefficient is about 6 to 10-6K-1Coefficient of thermal expansion with SiC 4.4 x 10-6K-1Therefore, the aluminum silicon carbon ceramic material has wide application prospect as the connecting layer material of the silicon carbide ceramic material.
In order to overcome the problems of the prior art, the inventor of the present invention found ternary layered Al in the course of long-term research and extensive practice4SiC4The material has the characteristic of self-healing of cracks in a high-temperature air and water vapor corrosion environment, and can realize the connection structure of the silicon carbide material in the high-temperature air and water vapor environmentBased on the unexpected finding, the present inventors have proposed the technical solution of the present invention, and further explain the technical solution, the implementation process and the principle thereof as follows.
In one aspect, the present invention is directed to a connecting material for connecting silicon carbide having crack self-healing characteristics, the connecting material comprising Al4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And a mixture with SiC, or the like, the connecting material having a high-temperature crack self-healing function.
In some embodiments, the connecting material comprises Al4C3Film, Al4SiC4Film, Al4C3Mixture with SiC and Al4SiC4And a mixture of SiC and one or a combination of two or more thereof, and the thickness is 1000 μm or less, preferably 0.1 to 100 μm.
As one aspect of the invention, Al-based material is provided4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4Use of a mixture with SiC for bonding silicon carbide materials.
In some embodiments, the use comprises: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And heating the mixture with SiC to 1000-2000 ℃ to realize high-strength connection between the silicon carbide materials to be connected.
Further, the use comprises: providing Al at the joint interface of the silicon carbide materials to be joined4C3Film, Al4SiC4Film, Al4C3With SiC mixture and Al4SiC4And one or a combination of two or more of the above SiC mixtures.
Further, the Al4C3Film, Al4SiC4Film, Al4C3Film of a mixture with SiC or Al4SiC4The thickness of the mixture film with SiC is 1000 μm or less, preferably 0.1 to 100 μm.
The inventor discovers through a large amount of experiments that Al is selected4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4A silicon carbide connecting structure obtained by using any one or a combination of two or more of the above materials as a connecting material in a mixture with SiC, and Al in a connecting layer thereof4SiC4The phase has the self-healing capability of cracks under the conditions of high-temperature air and high-temperature steam oxidation.
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 material includes, but is not limited to, a carbon fiber reinforced silicon carbide composite material, a silicon carbide fiber reinforced ternary layered ceramic material, 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: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And any one or the combination of two or more of the SiC and the mixture of the SiC are heated to 1000-2000 ℃, so that the silicon carbide materials to be connected are connected with each other in a high-strength manner. Resulting silicon carbide connection structure, Al in the connection layer thereof4SiC4The phase has the self-healing capability of cracks under the conditions of high-temperature air and high-temperature steam oxidation.
In some embodiments, the connection method comprises: providing Al at the joint interface of the silicon carbide materials to be joined4C3Film, Al4SiC4Film, Al4C3Mixture with SiC and Al4SiC4And one or a combination of two or more of the above compounds with SiC.
Further, the Al4C3Film, Al4SiC4Film, Al4C3Film of a mixture with SiC or Al4SiC4The thickness of the mixture film with SiC is 1000 μm or less, preferably 0.1 to 100 μm.
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 material includes, but is not limited to, a carbon fiber reinforced silicon carbide composite material, a silicon carbide fiber reinforced ternary layered ceramic material, 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 pressureless heating connection, hot pressing connection, electric field assisted heating connection, microwave field assisted connection, laser assisted connection, and the like, and preferably, the electric field assisted heating connection.
The invention utilizes Al4C3The interface reaction between the Al and the matrix silicon carbide can obtain ternary layered Al at the interface4SiC4And high-strength connection can be realized. Therefore, after high-temperature connection, the connection layer is made of ternary layered ceramic aluminum silicon carbon or aluminum silicon carbon silicon carbide ceramic complex phase, and the obtained connection structure has high strength which can reach 200MPa and is higher than a silicon carbide substrate and is fractured on the silicon carbide substrate.
Further, the preparation method of the connecting material of the present invention is not limited, and the Al is4C3The material can be obtained by a solid-phase reaction method to obtain powder for connection or prepare a casting film; the Al is4C3The SiC mixture material can be obtained by a solid-phase reaction method, and powder which can be used for connection in different proportions is obtained; the Al is4SiC4Can be obtained by a solid-phase reaction method and is made into a casting film or a pre-sintered ceramic sheet; the above-mentionedAl4SiC4The mixture with SiC can use Al4C3Obtained by in-situ reaction with SiC mixture material or by using Al4SiC4Mixed with SiC powder, or made into cast films or pre-sintered ceramic sheets.
Accordingly, another aspect of the embodiments of the present invention also provides a silicon carbide connection structure manufactured by the foregoing method, which has a function of crack self-healing at high temperature.
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.
Further, the silicon carbide connection structure has a connection interface strength of 200MPa or more.
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, due to the implementation of the high-strength connecting layer, the obtained silicon carbide connecting structure is high in bending strength, has the capability of self-healing cracks in high-temperature air and high-temperature water vapor environments, and can be applied to extreme service environments such as aerospace and nuclear energy systems.
Correspondingly, another aspect of the embodiments of the present invention further provides a self-healing method of a silicon carbide connection structure, including: and carrying out high-temperature oxidation treatment on the silicon carbide connecting structure to enable cracks in the silicon carbide connecting structure to be self-healed.
Further, the high temperature oxidation treatment includes, but is not limited to, a high temperature water vapor oxidation corrosion treatment or a high temperature air oxidation corrosion treatment, and the like.
Further, the temperature of the high-temperature oxidation treatment is 1000-1500 ℃, and the time is 0.1-100 h.
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. 1, it is 100 μm Al4SiC4And (3) a connection structure schematic diagram for connecting the silicon carbide ceramics. The material to be connected is two pieces of silicon carbide with phi of 20 multiplied by 20mm, and the material of the connecting layer is 100 mu m Al4SiC4And heating the connecting interface by the aid of an electric field to enable the connecting interface to reach 1700 ℃, 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) by placing 100 μm Al on a silicon carbide surface to be joined4SiC4Casting a film, and butting the other piece of silicon carbide with the surface of the film; 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 1700 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 10min, 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 connection structure obtained in this example was observed with a scanning electron microscope, and a back-scattered scanning electron micrograph shown in fig. 2a shows that the connection interface had an obvious crack, the connection layer was dense, and the strength was high.
(3) And (3) putting the silicon carbide connecting piece into the center of a furnace tube of the tube furnace, raising the temperature to 1200 ℃, continuously introducing water vapor at a constant speed during the period, corroding for 2 hours and taking out.
(4) Observing the microstructure of the interface of the connecting layer of the silicon carbide connecting piece after the water vapor oxidation corrosion by using a scanning electron microscope; showing cracks in the connecting layer of the connector, which healed automatically after 2h of water corrosion, as shown in fig. 2 b.
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 210Mpa, 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 2
In this embodiment, the material to be connected is two pieces of silicon carbide with a diameter of 20X 20mm, and the material of the connecting layer is 100 μm Al4C3And the film heats the connecting interface under the assistance of an electric field to enable the connecting interface to reach 1800 ℃, so that 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) preparation of 100 μm Al on a silicon carbide surface to be bonded by spraying4C3Film, then butt-jointing another piece of silicon carbide with its surface; 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 1800 ℃ at the heating rate of 100 ℃/min, preserving the temperature for 10min, applying 35MPa pressure 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 this example was observed with a scanning electron microscope, and as shown in fig. 3a, it was shown that the connection interface had an obvious crack, the connection layer was dense, and the strength was high.
(3) And (3) putting the silicon carbide connecting piece into the center of a furnace tube of the tube furnace, raising the temperature to 1300 ℃, oxidizing and corroding the silicon carbide connecting piece in the air for 1h, and taking out the silicon carbide connecting piece.
(4) The microscopic morphology of the connecting layer of the silicon carbide connecting piece corroded in the air is observed by a scanning electron microscope, and the fact that the cracks in the connecting layer of the original connecting piece are automatically healed due to the aluminum-silicon-glass phase generated on the surface after the cracks are oxidized and corroded for 1 hour is shown in figure 3 b.
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 196Mpa 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 3
In this embodiment, the material to be connected is two pieces of silicon carbide with a diameter of 20X 20mm, and the material of the connecting layer is 100 μm Al4C3And casting the film and the SiC mixture, and heating the connection interface under the assistance of an electric field to enable the connection interface to reach 1400 ℃, 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) a10 μm Al layer was deposited on a silicon carbide surface to be bonded4C3Casting a film with the SiC mixture, 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 1400 ℃ at the heating rate of 100 ℃/min, preserving the temperature for 10min, applying 100MPa pressure 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 connecting structure obtained in the embodiment is observed by a scanning electron microscope, and the connecting interface is shown to have 2 obvious cracks, a connecting layer is compact, and the strength is high.
(3) And placing the obtained silicon carbide connecting piece into the center of a furnace tube of a tubular furnace, raising the temperature to 1300 ℃, oxidizing and corroding the silicon carbide connecting piece in the air for 2 hours, and then taking out the silicon carbide connecting piece.
(4) The microscopic morphology of the connecting layer of the silicon carbide connecting piece corroded in the air is observed by a scanning electron microscope, and the fact that the cracks in the connecting layer of the original connecting piece are automatically healed due to the aluminum-silicon-glass phase generated on the surface after 2 hours of oxidation corrosion is shown, and the structure is similar to that shown in figure 3 b.
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 205Mpa 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, the material to be connected is two silicon carbide fiber reinforced silicon carbide composite materials with phi 10 multiplied by 10mm, and the material of the connecting layer is 50 μm Al4SiC4And heating the connection interface of the/SiC mixed material by a hot pressing method to ensure that the connection interface reaches 1900 ℃, thereby connecting the silicon carbide fiber reinforced silicon carbide composite materials to be 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 50 mu m Al by a spraying method4SiC4The SiC/silicon carbide composite material is prepared by butt-jointing the other silicon carbide fiber reinforced silicon carbide composite material with the surface of the SiC/silicon carbide composite material; and then putting the sample into a graphite mold, then putting the graphite mold into a hot-pressing sintering furnace, heating to 1900 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 60min, applying 10MPa pressure to the connection sample in the heating process, and then cooling to room temperature at the speed of 50 ℃/min to obtain the connection structure of the silicon carbide fiber reinforced silicon carbide composite material.
The microscopic morphology of the interface of the silicon carbide fiber reinforced silicon carbide composite material connecting structure obtained in the embodiment is observed by using a scanning electron microscope, and the result is similar to that shown in fig. 2, and shows that the connecting interface has obvious cracks, a connecting layer is compact, and the strength is high.
(3) And (3) putting the silicon carbide connecting piece into the center of a furnace tube of the tube furnace, raising the temperature to 1000 ℃, continuously introducing water vapor at a constant speed during the period, corroding for 100 hours and taking out.
(4) Observing the microscopic appearance of the interface of the connecting layer of the silicon carbide fiber reinforced silicon carbide composite connecting piece after the water vapor oxidation corrosion by using a scanning electron microscope; it shows cracks in the connecting layer of the connector, which healed automatically after 3h of water corrosion, with results similar to those shown in fig. 2 b.
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 218Mpa 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 5
In the embodiment, the materials to be connected are two pieces of silicon carbide with the phi of 20 multiplied by 20mm, and the material of the connecting layer is 500nm Al4C3And the film is used for heating the connecting interface under the assistance of an electric field to enable the connecting interface to reach 1000 ℃, 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 500nm Al on a silicon carbide surface to be connected by PVD method4C3Film, then butt-jointing another piece of silicon carbide with its surface; 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 1000 ℃ at the heating rate of 100 ℃/min, preserving the temperature for 10min, applying the pressure of 100MPa 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 connecting structure obtained in the embodiment is observed by a scanning electron microscope, and the connecting interface has no obvious cracks, a compact connecting layer 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 199Mpa by adopting a four-point bending method, and breaking the sample strip on the matrix silicon carbide, thereby showing that the strength of a connecting layer and an interface is higher than that of the matrix silicon carbide.
Example 6
In this embodiment, the material to be connected is two pieces of silicon carbide with a diameter of 20X 20mm, and the material of the connecting layer is 50 μm Al4C3And heating the connection interface with the SiC mixture film by microwave to enable the connection interface to reach 1600 ℃, thereby connecting the SiC materials to be 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) 50 mu m Al is coated on a silicon carbide surface to be connected by a spin coating method4C3And the SiC mixture film, and then another piece of silicon carbide is butted with the surface of the SiC mixture film; and then putting the sample into a graphite mold, then putting the graphite mold into a microwave sintering furnace, electrifying, heating to the furnace temperature of 1600 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 10min, 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 the connecting interface has 1 obvious crack, a compact connecting layer and high strength.
(3) And (3) putting the silicon carbide connecting piece into the center of a furnace tube of the tube furnace, raising the temperature to 1500 ℃, continuously introducing water vapor at a constant speed during the period, corroding for 0.1h, and taking out.
(4) Observing the microscopic appearance of the interface of the connecting layer of the silicon carbide fiber reinforced silicon carbide composite connecting piece after the water vapor oxidation corrosion by using a scanning electron microscope; it shows cracks in the connecting layer of the connector, which healed automatically after 2h of water corrosion, with results similar to those shown in fig. 2 b.
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 186Mpa 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 20 mu m aluminum silicon carbon, and the connecting interface is sintered under no pressure to reach 2000 ℃, 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 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) plating 20 mu m of aluminum 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 high-temperature vacuum furnace, heating to the furnace temperature of 2000 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 200min, 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 microscope photo is similar to that shown in fig. 3a, and shows that the connecting interface has a plurality of microcracks and high strength.
(3) And (3) putting the obtained connecting piece into the center of a tube furnace tube of a tube furnace, heating to 1300 ℃, and oxidizing in air for 2h and taking out.
(4) Observing the microscopic appearance of the interface of the connecting layer of the silicon carbide fiber reinforced silicon carbide composite connecting piece after oxidation corrosion in the air by using a scanning electron microscope; it is shown that cracks in the connecting layer of the connector, which healed automatically after 2h of oxidative corrosion in air, result similarly as shown in fig. 3 b.
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 aluminum 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 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing aluminum silicon carbon into a casting film with the thickness of 100 mu m, 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 2 ℃/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. 2a, and shows that the connecting interface has a plurality of microcracks 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 of aluminum 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 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) preparing aluminum 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 casting film; 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 shown in fig. 2a, and shows that the connecting interface has a plurality of microcracks and high strength.
(3) And putting the obtained connecting piece into the center of a tube furnace, raising the temperature to 1200 ℃, continuously introducing steam at a constant speed during the period, corroding for 2 hours and taking out.
(4) Observing the microscopic appearance of the interface of the connecting layer of the silicon carbide fiber reinforced silicon carbide composite connecting piece after the water vapor oxidation corrosion by using a scanning electron microscope; it shows cracks in the connecting layer of the connector, which healed automatically after 2h of water corrosion, with results similar to those shown in fig. 2 b.
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 50 μm, and the connecting interface reaches 1400 ℃ 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 1 micron by using diamond polishing solution, and removing defects and impurities on the surface;
(2) placing a 50-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 1400 ℃ 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 this comparative example was observed with a scanning electron microscope, and the photograph of the back-scattering scanning electron microscope is shown in fig. 4 a. There were many cracks evident at the interface.
(3) And (3) putting the silicon carbide connecting piece into the center of a furnace tube of the tube furnace, raising the temperature to 1200 ℃, continuously introducing water vapor at a constant speed during the period, corroding for 2 hours and taking out.
(4) Observing the microstructure of the interface of the connecting layer of the silicon carbide connecting piece after the water vapor oxidation corrosion by using a scanning electron microscope; it is shown that cracks in the connecting layer of the connector still exist, as shown in fig. 4 b.
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 155Mpa, 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 of the titanium silicon carbon (about 9.2 multiplied by 10) is increased by the material of the connecting layer-6K-1) Is matrix silicon carbide (about 4.5X 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 155 MPa. In the present invention, Al is added4C3The Al-Si-C connecting layer is obtained by in-situ reaction with the matrix silicon carbide, so that stronger interface chemical bonding is formed, and meanwhile, ternary layered carbon silicide Al is utilized4SiC4The thermal expansion coefficient is similar to that of the matrix silicon carbide, and the high strength and the steam corrosion oxidation resistance performance under high temperature are achieved, the obtained silicon carbide connecting structure and the Al in the connecting layer are obtained4SiC4The phase has the self-healing and self-healing capabilities of cracks under the high-temperature steam oxidation condition, and can prolong the service life in the extreme service process of aerospace, nuclear energy systems and the like.
In addition, the inventors of the present invention also conducted experiments using other materials and conditions listed in the present specification in the manner of examples 1 to 9, and also produced a silicon carbide connection structure having high bending strength and high-temperature oxidative water vapor corrosion crack self-healing capability.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (10)

1. A connecting material for connecting silicon carbide with the characteristic of crack self-healing is characterized in that: the connecting material comprises Al4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4The connecting material has the function of high-temperature crack self-healing; preferably, the connecting material includes Al4C3Film, Al4SiC4Film, Al4C3Mixture with SiC and Al4SiC4The thickness of the mixture of SiC and one or more of the above compounds is 1000 μm or less, preferably 0.1 to 100 μm.
2.Al4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4Use of a mixture with SiC for bonding silicon carbide materials.
3. Use according to claim 2, characterized in that it comprises: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And heating the mixture with SiC to 1000-2000 ℃ to realize high-strength connection between the silicon carbide materials to be connected.
4. Use according to claim 2 or 3, characterized in that it comprises: providing Al at the joint interface of the silicon carbide materials to be joined4C3Film, Al4SiC4Film, Al4C3With SiC mixture and Al4SiC4And one or a combination of two or more of SiC mixtures; preferably, the Al is4C3Film, Al4SiC4Film, Al4C3Mixtures with SiC or Al4SiC4The thickness of the mixture of the SiC and the SiC is less than 1000 μm, and preferably 0.1-100 μm;
and/or the silicon carbide material comprises a pure silicon carbide ceramic material and/or a silicon carbide ceramic matrix composite material; preferably, the silicon carbide ceramic matrix composite comprises any one or a combination of more than two of carbon fiber reinforced silicon carbide composite, silicon carbide fiber reinforced silicon carbide composite and silicon carbide fiber reinforced ternary layered ceramic material.
5. A method of joining silicon carbide materials, comprising: providing Al at the joint interface of the silicon carbide materials to be joined4C3、Al4SiC4、Al4C3Mixture with SiC and Al4SiC4And one or more than two of the SiC mixtures are combined and heated to 1000-2000 ℃, so that the silicon carbide materials to be connected are connected with each other in a high-strength manner.
6. The connecting method according to claim 5, characterized by comprising: providing Al at the joint interface of the silicon carbide materials to be joined4C3Film, Al4SiC4Film, Al4C3Mixture with SiC and Al4SiC4One or a combination of two or more of the above compounds with SiC; preferably, the Al is4C3Film, Al4SiC4Film, Al4C3Mixtures with SiC or Al4SiC4The thickness of the mixture with SiC is less than 1000 μm, preferably 0.1 to 100 μm.
7. The connecting method according to claim 5, characterized in that: the silicon carbide material comprises a pure silicon carbide ceramic material and/or a silicon carbide ceramic matrix composite material; preferably, the silicon carbide ceramic matrix composite comprises any one or a combination of more than two of carbon fiber reinforced silicon carbide composite, silicon carbide fiber reinforced silicon carbide composite and silicon carbide fiber reinforced ternary layered ceramic material;
and/or the heating mode comprises pressureless heating connection, hot pressing connection, electric field auxiliary heating connection, microwave field auxiliary heating connection or laser auxiliary connection, and preferably the electric field auxiliary heating connection.
8. A silicon carbide connection made by the method of any one of claims 5-7, the silicon carbide connection having a crack self-healing function at high temperatures; preferably, the connecting layer in the silicon carbide connecting structure is an aluminum-silicon-carbon phase; preferably, the connecting layer in the silicon carbide connecting structure is mainly an aluminum-silicon-carbon-silicon carbide composite phase; preferably, the strength of the connecting interface of the silicon carbide connecting structure is greater than that of the matrix silicon carbide, and the bonding strength of the connecting interface is more than 200 MPa.
9. A self-healing method of a silicon carbide connection structure is characterized by comprising the following steps:
subjecting the silicon carbide interconnect structure of claim 8 to a high temperature oxidation process to self-heal cracks in the silicon carbide interconnect structure;
preferably, the high-temperature oxidation treatment comprises high-temperature steam oxidation corrosion treatment or high-temperature air oxidation corrosion treatment;
preferably, the temperature of the high-temperature oxidation treatment is 1000-1500 ℃, and the time is 0.1-100 h.
10. Use of the silicon carbide connecting structure according to claim 8 for the preparation of aerospace materials or nuclear energy systems.
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