CN115724678A - Method for preparing ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation and application - Google Patents
Method for preparing ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation and application Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 123
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000010301 surface-oxidation reaction Methods 0.000 title claims abstract description 22
- 230000005496 eutectics Effects 0.000 title claims abstract description 14
- 230000001052 transient effect Effects 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 title claims abstract description 13
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- 229910004298 SiO 2 Inorganic materials 0.000 claims description 30
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 21
- 239000011521 glass Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
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- 238000000576 coating method Methods 0.000 claims description 7
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
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- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004806 packaging method and process Methods 0.000 abstract description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 57
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the technical field of ceramic connection, and discloses a method for preparing a ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation and application. Weighing oxide powder, ball-milling, mixing and drying to obtain powder, keeping the temperature of the powder at 1200-1500 ℃ for 1-6 hours, performing water quenching to obtain a sintering aid, grinding and sieving the sintering aid, weighing the sintering aid and nano ceramic powder to obtain NITE phase powder, attaching the NITE phase powder and surface oxidized SiC ceramic to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure, and connecting the NITE phase powder and the surface oxidized SiC ceramic under the conditions of keeping the temperature at 1200-1500 ℃ and 0-10 MPa for 10-60 minutes. The obtained ceramic connecting piece has high shear strength and good resistance to hydrothermal corrosion, and can be widely applied to the fields of heat exchange tubes, hot end parts of aircraft engines, thermal protection structures of aerospace vehicles or the packaging of cladding tubes of nuclear power plants.
Description
Technical Field
The invention belongs to the technical field of ceramic connection, and particularly relates to a method for preparing a ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation and application.
Background
The SiC ceramic has good properties of corrosion resistance, thermal shock resistance, high hardness, high-temperature strength and the like, and is widely applied to the fields of heat exchange tubes, hot end parts of aircraft engines, heat protection structures of aerospace vehicles or nuclear cladding tubes and the like. However, since SiC ceramics are brittle, it is difficult to manufacture components having large sizes and complicated shapes. Therefore, it is necessary to form parts having complicated shapes by a joining technique between ceramics. In order to avoid the thermal stress at the joint after connection due to the material difference between the intermediate layer and the ceramic base material, the nano SiC ceramic consistent with the SiC ceramic base material is widely adopted and a small amount of oxide sintering aid is combined to be used as a connection layer material, namely a nano transient eutectic liquid phase (NITE phase) material, the room temperature shear strength of the ceramic connection piece prepared by the NITE connection process is as high as more than 100MPa, however, the NITE connection process needs to be carried out under the conditions of high temperature (> 1500 ℃) and high pressure (> 20 MPa), the SiC ceramic is easily thermally damaged due to high temperature, the performance of the matrix is reduced, and the NITE connection is difficult to realize engineering application. Therefore, it is highly desirable to reduce the NITE bonding process conditions to achieve high strength bonding of SiC ceramics at low temperature and low pressure.
Disclosure of Invention
In order to solve the defects of the prior art, the invention mainly aims to provide a method for preparing a ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation; the method can connect SiC ceramics at low temperature and low pressure to obtain the ceramic connecting piece with high strength at room temperature and high temperature and good resistance to hydrothermal corrosion.
The invention also aims to provide a ceramic connecting piece prepared by the method.
It is a further object of the present invention to provide a use of the above ceramic connecting member.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a ceramic connecting piece comprises the following specific steps:
a method for preparing a ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation comprises the following operation steps:
s1, weighing Al 2 O 3 -SiO 2 Ball-milling, mixing and drying the oxide powder, the solvent and the grinding balls to obtain mixed powder, heating the mixed powder to 1200-1500 ℃, preserving the temperature for 1-6 h, and performing water quenching to obtain a glass sintering aid;
s2, grinding and sieving the glass sintering aid, then ball-milling, mixing, drying and sieving the glass sintering aid, the nano SiC ceramic powder, a grinding ball and a solvent to obtain NITE phase powder;
s3, carrying out surface oxidation on the SiC ceramic, coating the NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; and (3) placing the prefabricated connecting piece in connecting equipment, heating to 1200-1500 ℃ in a vacuum atmosphere or an inert atmosphere, and connecting under the condition that the temperature is kept for 10-60 min at the pressure of 0-10 MPa to obtain the ceramic connecting piece.
Al in step S1 2 O 3 -SiO 2 Medium Al 2 O 3 With SiO 2 The mass ratio of (A) to (B) is 60-80; the oxide powder comprises TiO 2 、CaO、MgO、ZrO 2 、Y 2 O 3 、Nd 2 O 3 、Dy 2 O 3 、Lu 2 O 3 、Sc 2 O 3 、Yb 2 O 3 、Ho 2 O 3 、Dy 2 O 3 、Ba 2 O 3 And B 2 O 3 One or more of (a); the Al is 2 O 3 -SiO 2 The mass ratio of the oxide powder to the oxide powder is 30-50; the solvent is absolute ethyl alcohol; the Al is 2 O 3 -SiO 2 And the mass ratio of the oxide powder to the solvent and the grinding ball is 1:2-10: 10 to 20; the grinding ball is Si 3 N 4 And one or more of SiC and WC, wherein the ball milling mode is roller ball milling or planetary ball milling.
The temperature rising rate of the step S1 is 5-10 ℃/min; the water quenching adopts deionized water or ultrapure water with the purity of more than 99.99 percent.
S2, grinding the glass sintering aid, and then sieving the ground glass sintering aid with a 200-300-mesh sieve; the grain diameter of the nano SiC ceramic powder is 20-100 nm; the mass ratio of the glass sintering aid after grinding and sieving to the nano SiC ceramic powder is 5-20; the grinding ball is Si 3 N 4 (ii) a The solvent is absolute ethyl alcohol, acetone or tetrahydrofuran; the mass ratio of the sum of the glass sintering aid after grinding and sieving and the nano SiC ceramic powder to the solvent and the grinding ball is 1:2-5: 20 to 30 percent; the ball milling mode is planetary ball milling; and the dried powder passes through a 200-300-mesh screen.
The surface oxidation in the step S3 is carried out in air or gas with 20-25 vol% oxygen content, at the temperature of 1000-1400 ℃ and the heat preservation time of 0.5-4 h.
S3, the connecting equipment is a discharge plasma sintering furnace, a microwave sintering furnace, a vacuum sintering furnace or a non-pressure sintering furnace, wherein the heating rate of the discharge plasma sintering furnace and the microwave sintering furnace is 50-300 ℃/min, and the heating rate of the vacuum sintering furnace and the non-pressure sintering furnace is 5-20 ℃/min; the vacuum degree of the vacuum atmosphere is 10 -4 ～10 -2 Pa, and the inert atmosphere is nitrogen, argon or helium.
A ceramic connecting piece is prepared by the method.
The shear strength of the ceramic connecting piece at room temperature is 110-160 MPa, the shear strength at 800-1200 ℃ is 70-100 MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion of heating for 72 hours at 20MPa and 400 ℃ is 5-20 mg/dm 2 Has good resistance to hydrothermal corrosion.
The ceramic connecting piece is applied to heat exchange tubes, hot end parts of aero-engines, heat protection structures of aerospace vehicles and encapsulation of cladding tubes of nuclear power stations.
The principle schematic of the invention is shown in fig. 1.
As shown in (a) of fig. 1, the silicon carbide ceramic is oxidized to form an oxide layer, the connection layer powder is nano silicon carbide powder (black) and a small amount of glass sintering aid (white), the structure of the prefabricated ceramic connecting piece at this time is "silicon carbide ceramic-oxide layer-connection layer powder-oxide layer-silicon carbide ceramic", when the prefabricated ceramic connecting piece is subjected to heat treatment conditions of 1200-1500 ℃ and 0-10 MPa for 10-60 min of heat preservation, the glass aid forms a liquid phase to wet the nano silicon carbide ceramic powder and promote sintering of the connection layer material, and the oxide layer forms a liquid phase to wet the surface of the silicon carbide ceramic and the connection layer material and promote element diffusion between the connection layer and the substrate to form a firm joint, as shown in (b) of fig. 1, the main phase of the connection layer of the joint is silicon carbide, but a gradient structure exists mainly because the content of silicon carbide in the middle of the connection layer is high and the content of silicon carbide on both sides of the connection layer is relatively low. Through the double wetting action of the sintering aid and the oxide layer, the connection layer is tightly combined with the ceramic matrix, and meanwhile, the formed liquid phase can effectively reduce the residual stress of the joint and improve the compactness, so that the mechanical properties of the joint at room temperature and high temperature are good.
Compared with the prior art, the invention has the following advantages and effects:
(1) According to the invention, the ceramic connecting piece is prepared at relatively low temperature and pressure by double wetting effects of the sintering aid and the oxide layer, so that the ceramic matrix is prevented from being damaged by high temperature.
(2) The main phase of the connecting layer of the ceramic connecting piece prepared by the invention is consistent with that of the ceramic substrate, almost no residual stress exists, and the ceramic connecting piece has good hydrothermal corrosion resistance and high temperature performance.
Drawings
FIG. 1 is a schematic diagram of the present invention for preparing a ceramic connector by combining the surface oxidation of a nano transient eutectic liquid.
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. The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated.
Example 1
1. Mixing Al 2 O 3 :SiO 2 Weighing and mixing the components according to the mass ratio of 60wt% to 40wt% to obtain Al 2 O 3 -SiO 2 Then adding Al 2 O 3 -SiO 2 : caO is weighed according to the mass ratio of 40wt% to 60wt%, and is weighed according to Al 2 O 3 -SiO 2 And the total mass of the oxide powder is as follows: the SiC grinding balls are subjected to ball milling mixing and drying according to the mass ratio of 1.
2. And (3) sieving the glass sintering aid: weighing 50nm nano SiC ceramic powder according to the mass ratio of 7wt% to 93wt%, and mixing the weighed powder in parts by weight: anhydrous ethanol: si 3 N 4 And (3) weighing grinding balls according to the mass ratio of 1.
3. Preserving the temperature of SiC ceramic at 1200 ℃ for 2h in air atmosphere for surface oxidation, uniformly coating NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; and (3) placing the prefabricated ceramic connecting piece in a microwave sintering furnace, heating to 1400 ℃ at the speed of 100 ℃/min in flowing nitrogen, pressurizing to 0.5MPa, and preserving heat for 10min to obtain the SiC ceramic connecting piece.
The shear strength of the SiC ceramic connecting piece at room temperature is 130MPa, the shear strength at 1000 ℃ is 80MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion for 360 ℃/18.6MPa/72h is 10mg/dm 2 The ceramic connecting piece has good resistance to hydrothermal corrosion, and can be widely applied to the fields of heat exchange tubes, hot end parts of aircraft engines, thermal protection structures of aerospace vehicles or cladding tube packaging of nuclear power plants.
Example 2
1. Mixing Al 2 O 3 :SiO 2 Weighing and mixing according to the mass ratio of 70wt% to 30wt% to obtain Al 2 O 3 -SiO 2 Then adding Al 2 O 3 -SiO 2 ：Y 2 O 3 Weighing 50wt% to 50wt% of Al 2 O 3 -SiO 2 And the total mass of the oxide powder is as follows: the SiC grinding balls are subjected to ball milling mixing and drying according to the mass ratio of 1.
2. And (3) sieving the glass sintering aid: weighing 40nm nano SiC ceramic powder according to the mass ratio of 7wt% to 93wt%, and mixing the weighed powder: absolute ethanol: si 3 N 4 And (3) weighing grinding balls according to the mass ratio of 1.
Preserving the heat of the SiC ceramic at 1200 ℃ for 2h in air atmosphere for surface oxidation, uniformly coating the NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding the two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; and (3) placing the prefabricated ceramic connecting piece in a microwave sintering furnace, heating to 1400 ℃ at the speed of 100 ℃/min in flowing nitrogen, pressurizing to 0.5MPa, and preserving heat for 20min to obtain the SiC ceramic connecting piece.
The shear strength of the SiC ceramic connecting piece at room temperature is 152MPa, the shear strength at 1000 ℃ is 90MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion for 360 ℃/18.6MPa/72h is 11mg/dm 2 The ceramic connecting piece has good resistance to hydrothermal corrosion, and can be widely applied to the fields of heat exchange tubes, hot end parts of aircraft engines and thermal protection structures of aerospace vehicles.
Example 3
1. Mixing Al 2 O 3 :SiO 2 Weighing and mixing the components according to the mass ratio of 60wt% to 40wt% to obtain Al 2 O 3 -SiO 2 Then Al is added 2 O 3 -SiO 2 ：Ba 2 O 3 Weighing 40wt% to 60wt% of Al 2 O 3 -SiO 2 And the total mass of the oxide powder is as follows: the SiC grinding balls are subjected to ball milling mixing and drying according to the mass ratio of 1.
2. Weighing the sieved glass sintering aid 100nm nano SiC ceramic powder according to the mass ratio of 20wt% to 80wt%, and mixing the weighed powder: anhydrous ethanol: si 3 N 4 And (2) weighing grinding balls according to the mass ratio of 1.
Preserving the heat of the SiC ceramic at 1200 ℃ for 2h in air atmosphere for surface oxidation, uniformly coating the NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding the two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; and (3) placing the prefabricated ceramic connecting piece in a discharge plasma sintering furnace, heating to 1500 ℃ at the speed of 200 ℃/min in flowing nitrogen, pressurizing to 5MPa, and preserving heat for 30min to obtain the SiC ceramic connecting piece.
The shear strength of the SiC ceramic connecting piece at room temperature is 140MPa, the shear strength at 1000 ℃ is 95MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion for 360 ℃/18.6MPa/72h is 5mg/dm 2 The ceramic connecting piece has good resistance to hydrothermal corrosion, and can be widely applied to the fields of heat exchange tubes, hot end parts of aircraft engines, thermal protection structures of aerospace vehicles or cladding tube packaging of nuclear power plants.
Example 4
1. Mixing Al 2 O 3 :SiO 2 Weighing and mixing the components according to the mass ratio of 50wt% to obtain Al 2 O 3 -SiO 2 Then Al is added 2 O 3 -SiO 2 ：ZrO 2 Weighing 50wt% to 50wt% of Al 2 O 3 -SiO 2 And the total mass of the oxide powder is as follows: ball-milling, mixing and drying the WC grinding balls according to the mass ratio of 1.
2. Weighing the sieved glass sintering aid 80nm nano SiC ceramic powder according to the mass ratio of 10wt% to 90wt%, and mixing the weighed powder: tetrahydrofuran: si 3 N 4 And (3) weighing grinding balls according to the mass ratio of 1.
Preserving the heat of the SiC ceramic at 1400 ℃ for 4h in air atmosphere for surface oxidation, uniformly coating the NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding the two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; placing the prefabricated ceramic connector in a vacuum sintering furnace at 10 -3 And (3) heating the Pa vacuum degree to 1450 ℃ at the speed of 10 ℃/min, keeping the temperature for 10min without pressure, and thus obtaining the SiC ceramic connecting piece.
The shear strength of the SiC ceramic connecting piece at room temperature is 110MPa, the shear strength at 1000 ℃ is 70MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion for 360 ℃/18.6MPa/72h is 18mg/dm 2 The ceramic connecting piece has good resistance to hydrothermal corrosion, and can be widely applied to the field of heat exchange tubes, hot end parts of aircraft engines or thermal protection structure packaging of aircraft spacecraft.
Example 5
1. Mixing Al 2 O 3 :SiO 2 Weighing and mixing the components according to the mass ratio of 60wt% to 40wt% to obtain Al 2 O 3 -SiO 2 Then Al is added 2 O 3 -SiO 2 : mgO is weighed according to the mass ratio of 40wt% to 60wt%, and is weighed according to Al 2 O 3 -SiO 2 And the quality of the oxide powderThe total amount of the components is absolute ethyl alcohol: the SiC grinding balls are subjected to ball milling mixing and drying according to the mass ratio of 1.
2. And (3) sieving the glass sintering aid: weighing 50nm nanometer SiC ceramic powder according to a mass ratio of 15wt% to 85wt%, and mixing the weighed powder: acetone: si 3 N 4 And (3) weighing grinding balls according to the mass ratio of 1.
Preserving the heat of the SiC ceramic at 1200 ℃ for 2h in air atmosphere for surface oxidation, uniformly coating the NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding the two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; and (3) placing the prefabricated ceramic connecting piece in a pressureless sintering furnace, heating to 1500 ℃ at the speed of 10 ℃/min in flowing argon, keeping the temperature for 60min without pressure, and obtaining the SiC ceramic connecting piece.
The measured shearing strength of the SiC ceramic connecting piece at room temperature is 120MPa, the shearing strength at 1000 ℃ is 90MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion for 360 ℃/18.6MPa/72h is 16mg/dm 2 The ceramic connecting piece has good resistance to hydrothermal corrosion, and can be widely applied to the fields of heat exchange tubes, thermal protection structures of aerospace vehicles or encapsulation tubes of nuclear power plants.
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 (9)
1. A method for preparing a ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation is characterized by comprising the following operation steps:
s1, weighing Al 2 O 3 -SiO 2 The oxide powder, the solvent and the grinding balls are ball-milled, mixed and dried to obtain mixed powder, the mixed powder is heated to 1200-1500 ℃ and is kept warm for 1-6 h, and the glass sintering aid is prepared after water quenching;
s2, grinding and sieving the glass sintering aid, ball-milling, mixing, drying and sieving the glass sintering aid, the nano SiC ceramic powder, a grinding ball and a solvent to obtain NITE phase powder;
s3, carrying out surface oxidation on the SiC ceramic, coating the NITE phase powder on the oxidized surface of the SiC ceramic, and then bonding two SiC ceramics coated with the NITE phase powder together to form a prefabricated connecting piece of a ceramic-connecting powder-ceramic sandwich structure; and (3) placing the prefabricated connecting piece in connecting equipment, heating to 1200-1500 ℃ in a vacuum atmosphere or an inert atmosphere, and connecting under the condition that the temperature is kept for 10-60 min at the pressure of 0-10 MPa to obtain the ceramic connecting piece.
2. The method for preparing the ceramic connecting piece by combining the nano transient eutectic liquid with the surface oxidation according to claim 1, wherein the method comprises the following steps: al in step S1 2 O 3 -SiO 2 Middle Al 2 O 3 With SiO 2 The mass ratio of (A) to (B) is 60-80; the oxide powder comprises TiO 2 、CaO、MgO、ZrO 2 、Y 2 O 3 、Nd 2 O 3 、Dy 2 O 3 、Lu 2 O 3 、Sc 2 O 3 、Yb 2 O 3 、Ho 2 O 3 、Dy 2 O 3 、Ba 2 O 3 And B 2 O 3 One or more of (a); the Al is 2 O 3 -SiO 2 The mass ratio of the oxide powder to the oxide powder is 30-50; the solvent is absolute ethyl alcohol; the Al is 2 O 3 -SiO 2 And the mass ratio of the oxide powder to the solvent and the grinding ball is 1:2-10: 10 to 20; the grinding ball is Si 3 N 4 And one or more of SiC and WC, wherein the ball milling mode is roller ball milling or planetary ball milling.
3. The method for preparing the ceramic connecting piece by combining the nano transient eutectic liquid with the surface oxidation according to claim 1, wherein the method comprises the following steps: the temperature rising rate of the step S1 is 5-10 ℃/min; the water quenching adopts deionized water or ultrapure water with the purity of more than 99.99 percent.
4. The method for preparing the ceramic connecting piece by combining the nano transient eutectic liquid with the surface oxidation according to claim 1, wherein the method comprises the following steps: s2, grinding the glass sintering aid, and then sieving the ground glass sintering aid with a 200-300-mesh sieve; the grain diameter of the nano SiC ceramic powder is 20-100 nm; the mass ratio of the glass sintering aid after grinding and sieving to the nano SiC ceramic powder is 5-20; the grinding ball is Si 3 N 4 (ii) a The solvent is absolute ethyl alcohol, acetone or tetrahydrofuran; the mass ratio of the sum of the glass sintering aid after grinding and sieving and the nano SiC ceramic powder to the solvent and the grinding ball is 1:2-5: 20 to 30 percent; the ball milling mode is planetary ball milling; and the dried powder passes through a 200-300-mesh screen.
5. The method for preparing the ceramic connecting piece by combining the nano transient eutectic liquid with the surface oxidation according to claim 1, wherein the method comprises the following steps: the surface oxidation in the step S3 is carried out in air or gas with 20-25 vol% oxygen content, at the temperature of 1000-1400 ℃ and the heat preservation time of 0.5-4 h.
6. The method for preparing the ceramic connecting piece by combining the nano transient eutectic liquid with the surface oxidation according to claim 1, wherein the method comprises the following steps: s3, the connecting equipment is a discharge plasma sintering furnace, a microwave sintering furnace, a vacuum sintering furnace or a non-pressure sintering furnace, wherein the heating rate of the discharge plasma sintering furnace and the microwave sintering furnace is 50-300 ℃/min, and the heating rate of the vacuum sintering furnace and the non-pressure sintering furnace is 5-20 ℃/min; the vacuum degree of the vacuum atmosphere is 10 -4 ～10 -2 Pa, the inert atmosphere is nitrogen, argon or helium。
7. A ceramic joining member produced by the method according to any one of claims 1 to 6.
8. The ceramic connection according to claim 7, wherein: the shear strength of the ceramic connecting piece at room temperature is 110-160 MPa, the shear strength at 800-1200 ℃ is 70-100 MPa, and the weight loss rate of the ceramic joint after hydrothermal corrosion of heating for 72 hours at 20MPa and 400 ℃ is 5-20 mg/dm 2 。
9. Use of a ceramic connector according to claim 7 or 8 in heat exchange tubes, hot end parts of aircraft engines, thermal protection structures of aerospace vehicles and cladding tube encapsulation for nuclear power plants.
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| 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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