CN115849933B - Silicon carbide ceramic connecting piece and preparation method and application thereof - Google Patents
Silicon carbide ceramic connecting piece and preparation method and application thereof Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 84
- 239000000919 ceramic Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 229910000679 solder Inorganic materials 0.000 claims abstract description 20
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 18
- 238000003466 welding Methods 0.000 claims abstract description 17
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 13
- 229920001709 polysilazane Polymers 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000007650 screen-printing Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 229910004140 HfO Inorganic materials 0.000 description 13
- 239000000463 material Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of ceramic welding, and discloses a silicon carbide ceramic connecting piece, a preparation method and application thereof, wherein polysilazane, carbon powder, silicon powder and hafnium oxide powder are used as raw materials, a solvent is added, and the raw materials are mixed by roller ball milling to prepare solder; heating silicon carbide ceramics by using mixed liquid of hydrofluoric acid and nitric acid in water bath at 90-95 ℃, coating solder on areas to be welded of the two silicon carbide ceramics, and then placing the two silicon carbide ceramics according to the structure of a product to be formed to obtain a component to be connected; and (3) placing the part to be welded of the component to be connected into a heating furnace, performing welding treatment in a nitrogen atmosphere, and cooling to obtain the silicon carbide ceramic connecting piece. The thickness of the connecting layer of the silicon carbide ceramic connecting piece is 5-50 mu m, and the silicon carbide ceramic connecting piece can be applied to the fields of high-temperature heat exchange and space.
Description
Technical Field
The invention relates to the technical field of ceramic connection, in particular to a silicon carbide ceramic connecting piece and a preparation method and application thereof.
Background
The silicon carbide ceramic has the excellent characteristics of high strength, excellent high-temperature performance, oxidation resistance, wear resistance, high thermal conductivity and the like, and is widely applied to the fields of aerospace, metallurgy, nuclear energy, high-temperature heat exchange and the like. With the rapid development of industry, the structure and the size of the silicon carbide ceramic component have higher and higher requirements, however, under the existing industrial development level, the preparation difficulty of large and complex silicon carbide components is high, the production cost is high, and the development of the silicon carbide ceramic welding technology is an effective method for solving the problems. The development of the welding technology of silicon carbide ceramics has great significance for the development of the national industry.
Currently, the solders used for silicon carbide ceramic connection mainly comprise active metals, refractory metals, glass, ceramics and the like. The welding mechanism of different solders is different, and the welding process requirement and the performance of the welding piece are also different. In practical applications, a suitable solder is usually selected in a targeted manner according to the structure and application conditions of the solder. In the extreme application fields of high temperature (more than or equal to 1000 ℃) and the like, the silicon carbide connecting piece which takes high temperature resistant ceramics as the connecting layer material generally has larger application potential.
The Si 3N4/SiC composite ceramic is a ceramic material with high strength, excellent high temperature resistance, creep resistance and high temperature oxidation resistance, has more excellent comprehensive performance compared with single-phase Si 3N4 or single-phase SiC ceramic, and the Si 3N4/SiC composite ceramic has a thermal expansion coefficient close to that of the SiC ceramic. The Si 3N4/SiC complex phase ceramic is used as a connecting layer material, so that the SiC connecting piece with excellent connecting strength and high temperature resistance can be obtained. Since Si 3N4/SiC is a difficult-to-sinter material, the sintering temperature is usually high, and a low-temperature liquid phase sintering aid needs to be introduced to promote densification of Si 3N4/SiC, however, the performance of the SiC ceramic joint taking Si 3N4/SiC as a connecting layer at high temperature is reduced; in addition, in order to obtain a compact Si 3N4/SiC multiphase ceramic connecting layer and realize compact high-strength connection between the connecting layer and a base material, high connecting pressure (more than or equal to 10 MPa) is usually required to be applied to a connecting piece in the connecting process, so that the application of the connecting technology in the field of SiC ceramic welding is severely limited.
Disclosure of Invention
In order to solve the problems that the Si 3N4/SiC ceramic is used as a connecting layer material, and the densification of the Si 3N4/SiC connecting layer and the effective connection with a SiC base material are difficult to realize under the conditions of no addition of a low-temperature liquid phase sintering aid and low-pressure or even no-pressure connection, the invention aims at providing a preparation method of a silicon carbide ceramic connecting piece.
It is another object of the present invention to provide a silicon carbide ceramic joint prepared by the above method.
It is a further object of the present invention to provide the use of the silicon carbide ceramic joint described above.
The aim of the invention is achieved by the following technical scheme:
The preparation method of the silicon carbide ceramic connecting piece comprises the following specific steps:
S1, taking polysilazane, carbon powder, silicon powder and hafnium oxide powder as raw materials, adding a solvent, and carrying out roller ball milling and mixing to prepare solder;
S2, heating the silicon carbide ceramic in a water bath at 90-95 ℃ by using mixed solution of hydrofluoric acid and nitric acid;
S3, coating solder on the areas to be welded of the two silicon carbide ceramics treated in the step S2, and then placing the two silicon carbide ceramics according to the structure of the product to be formed to obtain a component to be connected;
s4, placing the components to be connected into a heating furnace, applying a connecting pressure of 0.05-0.5 MPa to the components to be connected in a nitrogen atmosphere, heating to 1450-1600 ℃ for welding treatment, and cooling to below 200 ℃ in the furnace to obtain the silicon carbide ceramic connecting piece.
Preferably, in the step S1, the mass ratio of the polysilazane to the carbon powder to the silicon powder to the hafnium oxide powder is (70-85): (0.5-4.9): (10-29): (0.1-0.5); the purities of the carbon powder, the silicon powder and the hafnium oxide powder are all more than 95 percent.
Preferably, the particle size of the carbon powder in the step S1 is 200-500 nm, the particle size of the silicon powder is 500-1000 nm, and the particle size of the HfO 2 powder is 100-200 nm;
preferably, the solvent in step S1 is xylene or di-n-butyl ether.
Preferably, the coating in step S3 is screen printing, spraying or dipping.
Preferably, the specific parameters of the welding process in step S4 are: heating to 200 ℃ at a speed of 1-2 ℃/min, preserving heat for 5-30 min, heating to 900 ℃ at 1-5 ℃/min, preserving heat for 5-30 min at 1150-1350 ℃ at 1-10 ℃/min, preserving heat for 5-60 min at 1450-1600 ℃ at 1-10 ℃/min, cooling to 800 ℃ at 1-10 ℃/min, and finally cooling along with the furnace.
A silicon carbide ceramic connector is prepared by the method.
Preferably, the thickness of the connecting layer in the silicon carbide ceramic connecting piece is 5-50 mu m, the room temperature shear strength of the joint is 70-90 MPa at room temperature, the helium leakage rate of the joint is 1.0X10 -8～1.0×10-10Pa·m3/s, and the shear strength of the joint under the flowing protective atmosphere at 800 ℃ and 1300 ℃ is 75-95 MPa and 60-85 MPa respectively;
the silicon carbide ceramic connecting piece is applied to the field of high-temperature heat exchange or the field of space.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the nitriding auxiliary HfO 2 is introduced to promote the rapid nitridation of Si powder, and silicon nitride formed by the volume expansion of the Si powder can effectively fill the pores formed by Polysilazane (PSZ) at high temperature, so that the air tightness of the joint is obviously improved.
2. According to the invention, through introducing the C powder, oxygen impurities on the surface of the Si powder are removed, the nitriding process of the Si powder is promoted, the C powder further reacts with residual non-nitrided Si to generate a SiC reinforcing phase, and a silicon carbide ceramic connecting piece is obtained through subsequent heat treatment, wherein a connecting layer is Si 3N4/SiC complex-phase ceramic, and only a small amount of Si, C and HfO 2 are left at a ceramic grain boundary in the connecting layer finally, and compared with pure Si serving as a grain boundary, the grain boundary has more excellent high temperature resistance and corrosion resistance.
3. The invention realizes the densification by taking Si 3N4/SiC complex phase ceramic as an intermediate layer and the connection of the base material SiC ceramic under the assistance of low pressure and even no pressure without introducing low-temperature liquid phase sintering auxiliary agent.
Detailed Description
The present invention is further illustrated below in conjunction with specific examples, but should not be construed as limiting the invention. The technical means used in the examples are conventional means well known to those skilled in the art unless otherwise indicated. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Example 1
1. According to the mass ratio of PSZ to C to Si to HfO 2 of 75:2.9:22:0.1, using dimethylbenzene as a solvent, and ball-milling and mixing for 6 hours in a roller ball mill with the ball-milling rotating speed of 100rpm to prepare the solder. Wherein the purity of the C powder, the Si powder and the HfO 2 powder is more than 99.5 percent.
2. Immersing the part to be welded of the silicon carbide ceramic into a mixed solution of nitric acid and hydrofluoric acid with the volume ratio of 1:2 at 90 ℃ for 10min, cleaning with deionized water and absolute ethyl alcohol, and drying in a vacuum oven.
3. Coating solder on the areas to be welded of the two silicon carbide ceramics, and then placing the two silicon carbide ceramics according to the structure of a product to be formed to obtain a component to be connected;
4. And (3) placing the part to be welded of the component to be connected into a heating furnace, applying a connecting pressure of 0.2MPa to the component to be connected under the nitrogen atmosphere of 0.1MPa, and performing welding treatment, wherein the heat treatment process parameters are that the temperature is raised to 200 ℃ at1 ℃/min and kept for 20min, then the temperature is raised to 900 ℃ at 3 ℃/min and kept for 20min at 1300 ℃ at 5 ℃/min, then the temperature is raised to 1550 ℃ at 5 ℃/min and kept for 30min, then the temperature is lowered to 800 ℃ at 5 ℃/min, and finally the silicon carbide ceramic connecting piece is obtained after furnace cooling.
The thickness of the connecting layer (composition Si 3N4/SiC complex phase) in the silicon carbide ceramic connecting piece of this example was 10 μm, the room temperature shear strength of the joint was 90MPa at room temperature, the helium leakage rate at the joint part of the connecting piece was 1.0X10 -10Pa·m3/s, and the shear strengths of the joint under nitrogen atmosphere at 800℃and 1300℃were 95MPa and 85MPa, respectively.
Example 2
1. According to the mass ratio of PSZ to C to Si to HfO 2 of 70:2.9:27:0.1, xylene is used as a solvent, and the solder is prepared by ball milling and mixing for 6 hours in a roller ball mill with the ball milling rotating speed of 100 rpm. Wherein the purity of the C powder, the Si powder and the HfO 2 powder is more than 99.5 percent.
2. Immersing the part to be welded of the silicon carbide ceramic part in a mixed solution of nitric acid and hydrofluoric acid with the volume ratio of 1:2 at 90 ℃ for 10min, cleaning with deionized water and absolute ethyl alcohol, and drying in a vacuum oven.
3. Coating solder on the areas to be welded of the two silicon carbide ceramics, and then placing the two silicon carbide ceramics according to the structure of a product to be formed to obtain a component to be connected;
4. And (3) placing the part to be welded of the component to be connected into a heating furnace, applying a connecting pressure of 0.1MPa to the component to be connected under the nitrogen atmosphere of 0.2MPa, and performing welding treatment, wherein the heat treatment process parameters are that the temperature is raised to 200 ℃ at 2 ℃/min for 30min, then the temperature is raised to 900 ℃ at 5 ℃/min, then the temperature is raised to 1350 ℃ at 10 ℃/min for 30min, then the temperature is raised to 1600 ℃ at 10 ℃/min for 30min, then the temperature is lowered to 800 ℃ at 10 ℃/min, and finally the silicon carbide ceramic connecting piece is obtained after furnace cooling.
The thickness of the joint connection layer in the silicon carbide ceramic joint of this example was 30 μm, the room temperature shear strength of the joint was 75MPa at room temperature, the helium leakage rate at the joint portion of the joint was 5.0x10 -9Pa·m3/s, and the shear strengths of the joint at 800 ℃ and 1300 ℃ under nitrogen atmosphere were 80MPa and 65MPa, respectively.
Example 3
1. According to the mass ratio of PSZ to C to Si to HfO 2 of 85:4.9:10:0.1, xylene is used as a solvent, and the solder is prepared by ball milling and mixing for 6 hours in a roller ball mill with the ball milling rotating speed of 100 rpm. Wherein the purity of the C powder, the Si powder and the HfO 2 powder is more than 99.5 percent.
2. Immersing the part to be welded of the silicon carbide ceramic part in a mixed solution of nitric acid and hydrofluoric acid with the volume ratio of 1:2 at 90 ℃ for 10min, cleaning with deionized water and absolute ethyl alcohol, and drying in a vacuum oven.
3. Coating solder on the areas to be welded of the two silicon carbide ceramic parts, and then placing the two silicon carbide ceramic parts according to the structure of the product to be formed to obtain a component to be connected;
4. And (3) placing the part to be welded of the component to be connected into a heating furnace, applying a connecting pressure of 0.1MPa to the component to be connected under the nitrogen atmosphere of 0.2MPa, and performing welding treatment, wherein the heat treatment process parameters are that the temperature is raised to 200 ℃ at 1 ℃/min, the temperature is kept at 200 ℃ for 5min, then the temperature is raised to 900 ℃ at 1 ℃/min, the temperature is kept at 1150 ℃ for 30min at 2 ℃/min, the temperature is kept at 1600 ℃ for 5min at 2 ℃/min, the temperature is lowered to 800 ℃ at 2 ℃/min, and finally the silicon carbide ceramic connecting piece is obtained along with furnace cooling.
The thickness of the joint connection layer in the silicon carbide ceramic connector of the embodiment is 30 μm, the room temperature shear strength of the joint is 85MPa at room temperature, the helium leakage rate of the joint part of the connector is 6.0X10 -10Pa·m3/s, and the high temperature shear strengths of the joint at 800 ℃ and 1300 ℃ under nitrogen atmosphere are 95MPa and 80MPa respectively.
Example 4
1. According to the mass ratio of PSZ to C to Si to HfO 2 of 80:4.5:15:0.5, di-n-butyl ether is taken as a solvent, and ball milling and mixing are carried out for 6 hours in a roller ball mill with the ball milling rotating speed of 100rpm, so that the solder is prepared. Wherein the purity of the C powder, the Si powder and the HfO 2 powder is more than 99.5 percent.
2. Immersing the part to be welded of the silicon carbide ceramic part in a mixed solution of nitric acid and hydrofluoric acid with the volume ratio of 1:2 at 90 ℃ for 10min, cleaning with deionized water and absolute ethyl alcohol, and drying in a vacuum oven.
3. Coating solder on the areas to be welded of the two silicon carbide ceramic parts, and then placing the two silicon carbide ceramic parts according to the structure of the product to be formed to obtain a component to be connected;
4. And (3) placing the part to be welded of the component to be connected into a heating furnace, welding the part to be connected under the nitrogen atmosphere of 0.1MPa without applying additional connecting pressure, wherein the heat treatment process parameters are that the temperature is raised to 200 ℃ at 2 ℃/min for 15min, then the temperature is raised to 900 ℃ at 3 ℃/min, then the temperature is raised to 1150 ℃ at 10 ℃/min for 15min, then the temperature is raised to 1500 ℃ at 10 ℃/min for 20min, then the temperature is lowered to 800 ℃ at 8 ℃/min, and finally the part to be connected is cooled along with the furnace, thus obtaining the silicon carbide ceramic connecting piece.
The thickness of the joint connection layer in the silicon carbide ceramic connecting piece of the embodiment is 50 μm, the room temperature shear strength of the joint is 75MPa at room temperature, the helium leakage rate of the joint part of the connecting piece is 2.0X10 -9Pa·m3/s, and the high temperature shear strengths of the joint at 800 ℃ and 1300 ℃ under nitrogen atmosphere are 75MPa and 60MPa respectively.
Example 5
1. According to the mass ratio of PSZ to C to Si to HfO 2 of 70:4.7:25:0.3, di-n-butyl ether is taken as a solvent, and ball milling and mixing are carried out for 6 hours in a roller ball mill with the ball milling rotating speed of 100rpm, so that the solder is prepared. Wherein the purity of the C powder, the Si powder and the HfO 2 powder is more than 99.5 percent.
2. Immersing the part to be welded of the silicon carbide ceramic part in a mixed solution of nitric acid and hydrofluoric acid with the volume ratio of 1:2 at 95 ℃ for 10min, cleaning with deionized water and absolute ethyl alcohol, and drying in a vacuum oven.
3. Coating solder on the areas to be welded of the two silicon carbide ceramic parts, and then placing the two silicon carbide ceramic parts according to the structure of the product to be formed to obtain a component to be connected;
4. And (3) placing the part to be welded of the component to be connected into a heating furnace, applying a connecting pressure of 0.5MPa to the component to be connected under the nitrogen atmosphere of 0.5MPa, and performing welding treatment, wherein the heat treatment process parameters are that the temperature is raised to 200 ℃ at 2 ℃/min for 30min, then the temperature is raised to 900 ℃ at 5 ℃/min, then the temperature is raised to 1150 ℃ at 10 ℃/min for 30min, then the temperature is raised to 1450 ℃ at 10 ℃/min for 60min, then the temperature is lowered to 800 ℃ at 10 ℃/min, and finally the silicon carbide ceramic connecting piece is obtained after furnace cooling.
The thickness of the joint connection layer in the silicon carbide ceramic joint of this example was 5 μm, the room temperature shear strength of the joint was 85MPa at room temperature, the helium leakage rate at the joint portion of the joint was 8.0x10 -9Pa·m3/s, and the high temperature shear strengths of the joint at 800 ℃ and 1300 ℃ under nitrogen atmosphere were 80MPa and 65MPa, respectively.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the silicon carbide ceramic connecting piece is characterized by comprising the following specific steps:
S1, taking polysilazane, carbon powder, silicon powder and hafnium oxide powder as raw materials, adding a solvent, and carrying out roller ball milling and mixing to prepare solder; the mass ratio of the polysilazane to the carbon powder to the silicon powder to the hafnium oxide powder is (70-85): (0.5-4.9): (10-29): (0.1-0.5); the purities of the carbon powder, the silicon powder and the hafnium oxide powder are all more than 95 percent; the particle size of the carbon powder is 200-500 nm, the particle size of the silicon powder is 500-1000 nm, and the particle size of the HfO 2 powder is 100-200 nm; the solvent is dimethylbenzene or di-n-butyl ether;
S2, heating the silicon carbide ceramic in a water bath at 90-95 ℃ by using mixed liquid of hydrofluoric acid and nitric acid;
s3, coating solder on the areas to be welded of the two silicon carbide ceramics treated in the step S2, and then placing the two silicon carbide ceramics according to the structure of the product to be formed to obtain a component to be connected;
S4, placing the components to be connected into a heating furnace, applying a connecting pressure of 0.05-0.5 MPa to the components to be connected in a nitrogen atmosphere, heating to 1450-1600 ℃ for welding treatment, and cooling to below 200 ℃ in the furnace to obtain the silicon carbide ceramic connecting piece; the specific parameters of the welding treatment are as follows: heating to 200 ℃ at a speed of 1-2 ℃/min, preserving heat for 5-30 min, heating to 900 ℃ at 1-5 ℃/min, preserving heat for 5-30 min at 1150-1350 ℃ at 1-10 ℃/min, preserving heat for 5-60 min at 1450-1600 ℃ at 1-10 ℃/min, cooling to 800 ℃ at 1-10 ℃/min, and cooling with a furnace; the silicon carbide ceramic connecting piece is characterized in that a connecting layer is Si 3N4/SiC complex phase ceramic, the thickness of the connecting layer is 5-50 mu m, the room temperature shear strength of the joint is 70-90 MPa at room temperature, the helium leakage rate of the joint is 1.0X10 -8~1.0×10-10 Pa·m3/s, and the shear strength of the joint under the flowing protective atmosphere at 800 ℃ and 1300 ℃ is 75-95 MPa and 60-85 MPa respectively.
2. The method of producing a silicon carbide ceramic joint according to claim 1, wherein the coating in step S3 is screen printing, spraying or dipping.
3. A silicon carbide ceramic joint, characterized in that it is produced by the method of claim 1 or 2.
4. Use of the silicon carbide ceramic joint according to claim 3 in the field of high temperature heat exchange or in the field of space.
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| CN109400167A (en) * | 2018-10-15 | 2019-03-01 | 广东工业大学 | A kind of SiC ceramic and its preparation method and application with fine and close articulamentum |
| CN109516828A (en) * | 2018-10-15 | 2019-03-26 | 广东工业大学 | The silicon carbide ceramics of a kind of connection method and its preparation of nucleus silicon carbide ceramics and application |
| CN109942310A (en) * | 2019-03-19 | 2019-06-28 | 广东工业大学 | A kind of preparation method of high-performance porous SiN ceramic |
| CN113429215A (en) * | 2021-07-30 | 2021-09-24 | 广东工业大学 | Method for connecting polysilazane with silicon carbide |
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