CN112851388A - Silicon carbide ceramic connecting piece and connecting method and application thereof - Google Patents
Silicon carbide ceramic connecting piece and connecting method and application thereof Download PDFInfo
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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
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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
- 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
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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
- 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
- C04B2237/365—Silicon carbide
Abstract
The invention belongs to the technical field of ceramic connection and discloses a silicon carbide ceramic connecting piece and a connection method and application thereof, wherein the method comprises the steps of mixing mixed powder of SiC nano powder and a liquid-phase sintering aid with an organic solvent to obtain a connection brazing filler metal, and uniformly coating the connection brazing filler metal on a silicon carbide base metal for connection to prepare a preliminary connecting piece; and coating or immersing the precursor slurry in a connecting area of the primary connecting piece, curing at 100-300 ℃ in Ar or vacuum atmosphere, and cracking at 1000-1500 ℃ and 0.01-1 MPa to obtain the silicon carbide ceramic connecting piece. The joint thickness of the obtained connecting piece is 20-100 mu m, the room-temperature shear strength is 40-100 MPa, the shear strength at 1200 ℃ is 45-120 MPa, and the leakage rate is 1 multiplied by 10‑13～1×10～9Pa·m3And s. The silicon carbide ceramic connecting piece can be applied to the fields of nuclear energy, aviation, aerospace, military industry and the like.
Description
Technical Field
The invention belongs to the technical field of non-oxide ceramic materials, and particularly relates to a silicon carbide ceramic connecting piece and a connecting method and application thereof.
Background
Silicon carbide (SiC) ceramics have the characteristics of high strength, high hardness, low density, oxidation resistance, corrosion resistance and the like, and also have excellent properties of small thermal expansion coefficient, high thermal conductivity, good high-temperature performance, low neutron absorption cross section and the like, so that the SiC ceramics are widely used in the fields of aviation, aerospace and nuclear energy. However, SiC, a strongly covalent bonding compound, has a high melting point and a small self-diffusion coefficient, making direct bonding difficult, and therefore a bonding solder and a method that can adapt to the above-mentioned environmental conditions are required. At present, the silicon carbide connection method mainly comprises a nanometer transient eutectic connection method, a precursor method, a glass ceramic brazing method, a maximum phase brazing method, a reaction connection method, a direct connection method and the like.
The above methods each have advantages and disadvantages. The joint obtained by connecting the nanometer transient eutectic phase has high strength, good high-temperature performance, good radiation resistance and hydrothermal corrosion resistance, but higher connection temperature and connection pressure are required in the connection process; the precursor method has the advantages of small connecting pressure, low connecting temperature, small thermal stress at the joint and good irradiation resistance, but a large amount of gas can be released in the cracking process of the precursor to cause volume shrinkage to form air holes, so that the connecting strength is reduced, and the air tightness of the joint is difficult to ensure; the glass ceramic brazing method can prepare a joint with good sealing performance, heat resistance and thermal shock resistance, but crystalline phase and amorphous phase of the glass ceramic have different irradiation behaviors under irradiation conditions and have poor resistance to hot corrosion; the maximum phase is connected with better thermal shock resistance and oxidation resistance, but is easy to decompose at high temperature and has poorer radiation resistance; the connection process of the reaction connection is mild, but residual silicon is difficult to avoid in the joint of the connecting piece, which is unfavorable for the high-temperature performance of the joint; the direct connection can obtain a joint having more excellent properties than the parent material, but the matching degree and surface roughness of the parent material are required to be high, and a high connection temperature and connection pressure are required, so that the application range of the direct connection method is severely limited.
Based on the advantages of the connection of the nano transient eutectic phase, particularly the connection piece has higher strength and high temperature performance, the temperature and pressure of the connection of the nano transient eutectic phase need to be reduced, and the advantages of the connection strength and the high temperature performance of the connection of the nano transient eutectic phase are kept as much as possible.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide a connection method of a silicon carbide ceramic connecting piece.
The invention also aims to provide a silicon carbide ceramic connecting piece prepared by the silicon carbide ceramic connecting method.
It is a further object of the present invention to provide the use of the above silicon carbide ceramic connector.
The purpose of the invention is realized by the following technical scheme:
a connecting method of a silicon carbide ceramic connecting piece comprises the following steps:
s1, carrying out planetary ball milling and mixing on SiC nano powder and a liquid-phase sintering aid, and drying to obtain mixed powder;
s2, mixing the mixed powder with an organic solvent to obtain a connecting brazing filler metal, uniformly coating the connecting brazing filler metal between silicon carbide base metals, and connecting at 1500-1700 ℃ and 0.01-5 MPa to realize primary connection of a nanometer transient eutectic phase of silicon carbide ceramics to prepare a primary connecting piece;
and S3, mixing the precursor powder with an organic solvent to form slurry, coating the slurry on a connection area of the preliminary connecting piece, or immersing the connection area of the preliminary connecting piece in a liquid precursor, curing at 100-300 ℃ in Ar or vacuum atmosphere, and cracking at 1000-1500 ℃ and 0.01-1 MPa to obtain the silicon carbide ceramic connecting piece.
Preferably, the liquid-phase sintering aid in step S1 is X — Re, where X is Al2O3、MgO、CaO、SiO2More than one of them, Re is Y2O3、Nd2O3、La2O3、Gd2O3、CeO2、Eu2O3Or Ho2O3。
Preferably, the mass ratio of the SiC nano powder to the liquid-phase sintering aid in step S1 is (80-99): (1-20); the grain size of the SiC nano powder is 30-80 nm.
Preferably, the ball-milling medium in step S1 is Si3N4The ball milling time of the ball or the SiC ball is 8-24 h, and the ball milling speed is 200-400 r/min.
Preferably, the mass ratio of the mixed powder to the organic solvent in the step S2 is 1 (1-4); the organic solvent is more than one of absolute ethyl alcohol, acetone, normal hexane or cyclohexane.
Preferably, the precursor powder in step S3 is one or more of polycarbosilane, hydrogenated polycarbosilane, and polyallyl hydroxyl carbosilane; the liquid precursor is vinyl-containing liquid hyperbranched polycarbosilane; the organic solvent is more than one of absolute ethyl alcohol, acetone, normal hexane or cyclohexane.
Preferably, in the step S2, the temperature is raised to 1200 ℃ at the speed of 5-20 ℃/min, and then raised to 1500-1700 ℃ at the speed of 10-20 ℃/min, and the temperature is kept for 0.5-2 h; in step S3, the temperature is raised to 100-300 ℃ at a rate of 2 ℃/min and is kept for 0.5-2 h, and the temperature is raised to 1000-1500 ℃ at a rate of 5-20 ℃/min and is kept for 0.5-2 h.
A ceramic connecting piece is prepared by the method.
Preferably, the thickness of the joint of the obtained silicon carbide ceramic connecting piece is 50-100 mu m, the room-temperature shear strength is 40-100 MPa, the high-temperature shear strength at 1200 ℃ is 45-120 MPa, and the leakage rate is 1 multiplied by 10-13～1×10～9Pa·m3/s。
The silicon carbide ceramic connecting piece is applied to the fields of nuclear energy, aviation, aerospace or military industry.
The method adopts silicon carbide nano powder and a liquid phase sintering aid which are uniformly mixed as a connecting material, and the connecting material is mixed with absolute ethyl alcohol to form a connecting brazing filler metal; uniformly coating a connecting brazing filler metal between two pieces of silicon carbide base materials to obtain a pre-connecting piece, and carrying out heat treatment on the pre-connecting piece at the temperature of 1500-1700 ℃ and the pressure of 0.01-5 MPa to realize primary connection of the nanometer transient eutectic phase of the silicon carbide ceramic; and mixing the precursor powder with dimethylbenzene or directly coating the liquid precursor in a connecting area of the primary connecting piece, then solidifying the precursor at 100-300 ℃, then pyrolyzing the precursor at 1000-1500 ℃, and finally connecting the SiC ceramics after the precursor impregnation pyrolysis process is circulated for 1-5 times.
Compared with the prior art, the invention has the following beneficial effects:
1. compared with the common process of connecting the nanometer transient eutectic phase at the temperature higher than 1750 ℃ and higher than 5MPa, the method can realize the primary connection of the silicon carbide ceramics at the lower temperature of 1500-1700 ℃ and the lower pressure of 0.01-5 MPa.
2. According to the invention, a connection layer obtained after the connection of the nanometer transient eutectic phase is a porous silicon carbide framework; the shape of the nanometer transient eutectic phase connection layer framework can be regulated, controlled and optimized through the type and content of the sintering aid and the heat treatment temperature and pressure, and the next step of precursor impregnation pyrolysis is facilitated.
3. According to the invention, the precursor is subjected to dipping and cracking on the primary connecting piece after the nanometer transient eutectic connection, so that the strength of the primary connecting piece is improved, meanwhile, the air tightness of the primary connecting piece is improved, and finally, the connecting piece with higher strength, good air tightness and good high-temperature performance is obtained.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
1. The nano transient eutectic phase is connected: mixing 30nm SiC powder with Al2O3-Y2O3Mixing the powder according to the mass ratio of 90:10, wherein Al is contained in the powder2O3And Y2O3In a mass ratio of 4:6, absolute ethyl alcohol is used as a solvent, and Si is used as3N4Grinding ball as ball grinding medium, mixing SiC with Al2O3-Y2O3Ball milling is carried out for 24 hours in a planetary ball mill with the rotating speed of 400rpm, and then rotary evaporation is carried out to obtain the connecting solder. And mixing the connecting solder with absolute ethyl alcohol, uniformly coating the mixture on the polished surfaces of the two pieces of SiC ceramics, and then bonding the surfaces of the two pieces of SiC ceramics coated with the connecting solder to obtain the pre-connecting piece. And (3) placing the pre-connecting piece in a vacuum environment, heating to 1500 ℃ at the speed of 10 ℃/min, then heating to 1700 ℃ at the speed of 5 ℃/min, preserving heat for 1h, and pressurizing at 5MPa in the heat treatment process to obtain a primary connecting piece.
2. Dipping and cracking a precursor: immersing a connecting area of the preliminary connecting piece in liquid hyperbranched polycarbosilane containing vinyl, then placing the preliminary connecting piece in a vacuum environment, heating to 300 ℃ at the speed of 5 ℃/min, preserving heat for 2h, then heating to 1000 ℃ at the speed of 10 ℃/min, heating to 1500 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and pressurizing to 0.01MPa in the heat treatment process.
3. The precursor impregnation cracking process is circulated for 5 times, specifically, the primary impregnation cracking process is to immerse the connection region of the primary connecting piece in liquid hyperbranched polycarbosilane containing vinyl, then heat the connection region to 1500 ℃ for cracking, and then cool the connection region to room temperature. And (5) dipping and cracking the precursor for 5 times to obtain the silicon carbide ceramic connecting piece.
And (3) performance testing: the obtained silicon carbide ceramic connecting piece has a joint thickness of 90 μm, a room-temperature shear strength of 90MPa, a high-temperature shear strength of 110MPa at 1200 ℃, and a leakage rate of 0.5 × 10～9Pa·m3/s。
Example 2
1. The nano transient eutectic phase is connected: mixing 30nm SiC powder with Al2O3-MgO-SiO2-CaO-Y2O3Mixing the powder according to the mass ratio of 90:10, wherein Al is contained in the powder2O3-MgO-SiO2-CaO-Y2O3The mass ratio of (A) to (B) is 5.0:0.7:1.0:0.5:2.8, absolute ethyl alcohol is used as a solvent, and Si is used as a solvent3N4Grinding ball as ball grinding medium, mixing SiC with Al2O3-MgO～SiO2-CaO-Y2O3After mixing, ball milling is carried out for 24 hours in a planetary ball mill with the rotating speed of 400rpm, and then rotary evaporation is carried out to obtain the connecting solder. And mixing the connecting solder with absolute ethyl alcohol, uniformly coating the mixture on the polished surfaces of the two pieces of SiC ceramics, and then bonding the surfaces of the two pieces of SiC ceramics coated with the connecting solder to obtain the pre-connecting piece. And (3) placing the pre-connecting piece in an Ar atmosphere environment, heating to 1200 ℃ at the speed of 20 ℃/min, then heating to 1700 ℃ at the speed of 10 ℃/min, preserving heat for 2h, and pressurizing at 5MPa in the heat treatment process to obtain the primary connecting piece.
2. Dipping and cracking a precursor: mixing polyallyloxycarbonyl silane and xylene, coating the mixture on a connection area of a primary connecting piece, then placing the primary connecting piece in a vacuum environment, heating to 250 ℃ at the speed of 2 ℃/min, preserving heat for 2h, heating to 1000 ℃ at the speed of 5 ℃/min, heating to 1500 ℃ at the speed of 10 ℃/min, preserving heat for 2h, and pressurizing to 1MPa in the heat treatment process.
3. The precursor impregnation cracking process is circulated for 3 times, specifically, the impregnation cracking process is to mix the polyallyloxycarbonyl silane and the xylene, coat the mixture on the connecting area of the primary connecting piece, then heat the mixture to 1500 ℃ for cracking, and then cool the mixture to room temperature. And (3) dipping and cracking the precursor for 3 times to obtain the silicon carbide ceramic connecting piece.
And (3) performance testing: the obtained silicon carbide ceramic connector has a joint thickness of 70 μm, a shear strength at room temperature of 100MPa, a shear strength at high temperature of 1200 ℃ of 115MPa, and a leakage rate of 1 × 10～9Pa·m3/s。
Example 3
1. The nano transient eutectic phase is connected: mixing 100nm SiC powder with Al2O3-Y2O3-CeO2Mixing the powder according to the mass ratio of 85:15, wherein Al is contained in the powder2O3-Y2O3-CeO2In the mass ratio of 1:1:1, absolute ethyl alcohol is taken as a solvent, and Si is taken as3N4Grinding ball as ball grinding medium, mixing SiC with Al2O3-Y2O3-CeO2After mixing, ball milling is carried out for 24 hours in a planetary ball mill with the rotating speed of 400rpm, and then rotary evaporation is carried out to obtain the connecting solder. And mixing the connecting solder with absolute ethyl alcohol, uniformly coating the mixture on the polished surfaces of the two pieces of SiC ceramics, and then bonding the surfaces of the two pieces of SiC ceramics coated with the connecting solder to obtain the pre-connecting piece. And (3) placing the pre-connecting piece in a vacuum environment, heating to 1500 ℃ at the speed of 10 ℃/min, then heating to 1600 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and pressurizing to 2MPa in the heat treatment process to obtain the primary connecting piece.
2. Dipping and cracking a precursor: immersing a connection region of the preliminary connecting piece in liquid hyperbranched polycarbosilane containing vinyl, then placing the preliminary connecting piece in a vacuum environment, heating to 300 ℃ at the speed of 5 ℃/min, preserving heat for 1h, then heating to 1000 ℃ at the speed of 10 ℃/min, heating to 1450 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and pressurizing to 0.1MPa in the heat treatment process.
3. The precursor dipping and cracking process is circulated for 5 times, specifically, the process of one dipping and cracking is that the connection area of the primary connecting piece is immersed in liquid hyperbranched polycarbosilane containing vinyl, then the temperature is raised to 1450 ℃ for cracking, and then the temperature is lowered to the room temperature. And (5) dipping and cracking the precursor for 5 times to obtain the silicon carbide ceramic connecting piece.
And (3) performance testing: the joint thickness of the obtained connecting piece is 60 mu m, the room-temperature shear strength is 75MPa, the high-temperature shear strength at 1200 ℃ is 100MPa, and the leakage rate is 0.8 multiplied by 10～9Pa·m3/s。
Example 4
1. The nano transient eutectic phase is connected: mixing 30nm SiC powder with Al2O3-CaO-Y2O3Mixing the powder according to the mass ratio of 91:9, wherein Al is contained in the powder2O3-CaO-Y2O3The mass ratio of (A) to (B) is 6:1.5:1.5, absolute ethyl alcohol is used as a solvent, and Si is used as3N4Grinding balls are used as ball milling media, SiC and CaO-Y are mixed2O3And ball-milling the mixture for 8 hours in a planetary ball mill with the rotating speed of 400rpm, and then performing rotary evaporation to obtain the connecting solder. And mixing the connecting solder with absolute ethyl alcohol, uniformly coating the mixture on the polished surfaces of the two pieces of SiC ceramics, and then bonding the surfaces of the two pieces of SiC ceramics coated with the connecting solder to obtain the pre-connecting piece. And (3) placing the pre-connecting piece in a vacuum environment, heating to 1500 ℃ at the speed of 10 ℃/min, then heating to 1700 ℃ at the speed of 5 ℃/min, preserving heat for 1h, and pressurizing to 3MPa in the heat treatment process to obtain the primary connecting piece.
2. Dipping and cracking a precursor: mixing polyallyloxycarbonyl silane and xylene to form slurry, coating the slurry on a connection area of a primary connecting piece, then placing the primary connecting piece in a vacuum environment, heating to 250 ℃ at the speed of 3 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the speed of 5 ℃/min, heating to 1400 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and pressurizing to 1MPa in the heat treatment process.
3. The precursor impregnation cracking process is circulated for 3 times, and specifically, the impregnation cracking process for one time is to mix the polyallyloxycarbonyl silane and the xylene to form slurry, coat the slurry on a connecting area of a primary connecting piece, then heat the slurry to 1400 ℃ for cracking, and then cool the slurry to room temperature. And (3) dipping and cracking the precursor for 3 times to obtain the silicon carbide ceramic connecting piece.
And (3) performance testing: the joint thickness of the obtained connecting piece is 50 μm, the room-temperature shear strength is 80MPa, the high-temperature shear strength at 1200 ℃ is 110MPa, and the leakage rate is 0.8 multiplied by 10～9Pa·m3/s。
Example 5
1. The nano transient eutectic phase is connected: mixing 50nm SiC powder with Al2O3-SiO2-Ho2O3Mixing the powder according to the mass ratio of 90:10, wherein Al is contained in the powder2O3-SiO2-Ho2O3In the mass ratio of 1:1:3, absolute ethyl alcohol is used as a solvent, and Si is used as3N4Grinding ball as ball grinding medium, mixing SiC with Al2O3-SiO2-Ho2O3After mixing, ball milling is carried out for 16h in a planetary ball mill with the rotating speed of 400rpm, and then rotary evaporation is carried out to obtain the connecting solder. And mixing the connecting solder with absolute ethyl alcohol, uniformly coating the mixture on the polished surfaces of the two pieces of SiC ceramics, and then bonding the surfaces of the two pieces of SiC ceramics coated with the connecting solder to obtain the pre-connecting piece. And (3) placing the pre-connecting piece in an Ar atmosphere environment, heating to 1200 ℃ at the speed of 10 ℃/min, then heating to 1550 ℃ at the speed of 5 ℃/min, preserving heat for 1.5h, and pressurizing at 1MPa in the heat treatment process to obtain the primary connecting piece.
2. Dipping and cracking a precursor: mixing polycarbosilane and acetone to form slurry, coating the slurry on a connection area of a primary connecting piece, then placing the primary connecting piece in a vacuum environment, heating to 300 ℃ at the speed of 1 ℃/min, preserving heat for 1h, then heating to 800 ℃ at the speed of 3 ℃/min, heating to 1450 ℃ at the speed of 5 ℃/min, preserving heat for 2h, and pressurizing to 0.1MPa in the heat treatment process.
3. The precursor impregnation cracking process is circulated for 5 times, and specifically, the impregnation cracking process for one time is to mix polycarbosilane and acetone to form slurry, coat the slurry on a connection area of the primary connecting piece, then heat the slurry to 1450 ℃ for cracking, and then cool the slurry to room temperature. And (5) dipping and cracking the precursor for 5 times to obtain the silicon carbide ceramic connecting piece.
And (3) performance testing: the joint thickness of the obtained connecting piece is 40 μm, the room-temperature shear strength is 50MPa, the high-temperature shear strength at 1200 ℃ is 60MPa, and the leakage rate is 1 multiplied by 10～9Pa·m3/s。
The silicon carbide ceramic connecting piece obtained by the invention has the joint thickness of 50-100 mu m, the room-temperature shear strength of 40-100 MPa, the high-temperature shear strength of 45-120 MPa at 1200 ℃, and the leakage rate of 1 multiplied by 10-13～1×10～9Pa·m3And s. The silicon carbide ceramic connecting piece can be applied to the fields of nuclear energy, aviation, aerospace, military industry and the like.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for connecting silicon carbide ceramic connectors, comprising the steps of:
s1, carrying out planetary ball milling and mixing on SiC nano powder and a liquid-phase sintering aid, and drying to obtain mixed powder;
s2, mixing the mixed powder with an organic solvent to obtain a connecting brazing filler metal, uniformly coating the connecting brazing filler metal between silicon carbide base metals, and connecting at 1500-1700 ℃ and 0.01-5 MPa to realize primary connection of a nanometer transient eutectic phase of silicon carbide ceramics to prepare a primary connecting piece;
and S3, mixing the precursor powder with an organic solvent to form slurry, coating the slurry on a connection area of the preliminary connecting piece, or immersing the connection area of the preliminary connecting piece in a liquid precursor, curing at 100-300 ℃ in Ar or vacuum atmosphere, and cracking at 1000-1500 ℃ and 0.01-1 MPa to obtain the silicon carbide ceramic connecting piece.
2. The method of joining silicon carbide ceramic joining members according to claim 1, wherein the step of joining comprisesThe liquid phase sintering aid in S1 is X-Re, wherein X is Al2O3、MgO、CaO、SiO2More than one of them, Re is Y2O3、Nd2O3、La2O3、Gd2O3、CeO2、Eu2O3Or Ho2O3。
3. The method for connecting the silicon carbide ceramic connecting pieces according to claim 1, wherein the mass ratio of the SiC nanopowder to the liquid phase sintering aid in step S1 is (80-99): (1-20); the grain size of the SiC nano powder is 30-80 nm.
4. The method for connecting silicon carbide ceramic connectors according to claim 1, wherein the ball-milled medium in step S1 is Si3N4The ball milling time of the ball or the SiC ball is 8-24 h, and the ball milling speed is 200-400 r/min.
5. The method for connecting the silicon carbide ceramic connecting pieces according to claim 1, wherein the mass ratio of the mixed powder to the organic solvent in step S2 is 1 (1-4); the organic solvent is more than one of absolute ethyl alcohol, acetone, normal hexane or cyclohexane.
6. The method for connecting silicon carbide ceramic connectors according to claim 1, wherein the precursor powder in step S3 is one or more of polycarbosilane, hydrogenated polycarbosilane, and polyallyloxycarbonylsilane; the liquid precursor is vinyl-containing liquid hyperbranched polycarbosilane; the organic solvent is more than one of absolute ethyl alcohol, acetone, normal hexane or cyclohexane.
7. The method for connecting the silicon carbide ceramic connecting pieces according to claim 1, wherein the temperature is raised to 1200 ℃ at 5-20 ℃/min in step S2, and then raised to 1500-1700 ℃ at 10-20 ℃/min and kept for 0.5-2 h; in step S3, the temperature is raised to 100-300 ℃ at a rate of 2 ℃/min and is kept for 0.5-2 h, and the temperature is raised to 1000-1500 ℃ at a rate of 5-20 ℃/min and is kept for 0.5-2 h.
8. A ceramic connecting member, characterized in that it is produced by the method of any one of claims 1 to 7.
9. The silicon carbide ceramic connector according to claim 8, wherein the resulting silicon carbide ceramic connector has a joint thickness of 50 to 100 μm, a room-temperature shear strength of 40 to 100MPa, a high-temperature shear strength at 1200 ℃ of 45 to 120MPa, and a leak rate of 1X 10-13～1×10～9Pa·m3/s。
10. Use of a silicon carbide ceramic joint according to claim 8 or 9 in the nuclear, aeronautical, aerospace or military fields.
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| CN114478043A (en) * | 2022-01-12 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | Connection method of silicon carbide ceramic based on liquid phase sintering |
| CN114920575A (en) * | 2022-04-21 | 2022-08-19 | 广东工业大学 | High-performance ceramic connecting piece and preparation method and application thereof |
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| CN115403387A (en) * | 2022-09-22 | 2022-11-29 | 岭东核电有限公司 | Low-temperature connection method of silicon carbide for nucleus |
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| CN115806443A (en) * | 2023-02-06 | 2023-03-17 | 成都超纯应用材料有限责任公司 | Connecting material of silicon carbide substrate, preparation method and application |
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| CN114478043A (en) * | 2022-01-12 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | Connection method of silicon carbide ceramic based on liquid phase sintering |
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| CN115849932A (en) * | 2022-11-30 | 2023-03-28 | 广东工业大学 | Method for preparing SiC ceramic connecting piece under ultralow temperature condition and application |
| CN115849932B (en) * | 2022-11-30 | 2024-01-02 | 广东工业大学 | Method for preparing SiC ceramic connecting piece under ultralow temperature condition and application thereof |
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