CN112759410A - Silicon carbide ceramic connection method and silicon carbide cladding - Google Patents
Silicon carbide ceramic connection method and silicon carbide cladding Download PDFInfo
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
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Abstract
The invention discloses a silicon carbide ceramic connecting method and a silicon carbide cladding, wherein the silicon carbide ceramic connecting method comprises the following steps: s1, adding a curing agent into liquid polycarbosilane serving as a precursor for curing; s2, heating and pretreating the solidified polycarbosilane to form precursor powder; s3, mixing the precursor powder and an organic solvent to prepare slurry; s4, smearing the slurry between the SiC cladding tube and the end plug which are matched with each other to form a sandwich connection structure; and S5, carrying out high-temperature curing and cracking treatment on the sandwich connection structure to enable the slurry to form a connection layer tightly connected between the SiC cladding tube and the end plug. The silicon carbide ceramic connection method of the invention realizes the high-strength connection of the SiC cladding and the end plug at low temperature (less than or equal to 1500 ℃) and no pressure, does not need to add filler, reduces the defect of air holes of the middle connection layer, and improves the air tightness of the formed joint; the connection process is simple, the requirement on equipment is low, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of nuclear energy materials, in particular to a silicon carbide ceramic connecting method and a silicon carbide cladding.
Background
Silicon carbide (SiC) as a structural ceramic material has good mechanical properties, high temperature resistance, corrosion resistance and other properties, and simultaneously has a low neutron absorption cross section and good neutron irradiation resistance, so that SiC has a very wide application prospect in the field of nuclear energy and is particularly prominent in the application of a cladding material in a nuclear reactor. However, to realize the application of the SiC cladding material in the extremely harsh high-temperature and high-irradiation working environment, it is necessary to ensure that the junction of the SiC cladding and the end plug can withstand the above influence of the extreme working environment.
In the existing SiC joining technology, the commonly used joining methods mainly include precursor joining, nano instantaneous liquid phase joining, brazing joining, solid phase diffusion joining, MAX joining, glass joining, reaction joining, and the like. In the above connection method, a large residual stress is generated at the joint due to the introduction of the dissimilar connection material, and the high temperature resistance, the radiation resistance, the corrosion resistance and the like of the joint may be affected. For example, the metal phase has a large difference in thermal expansion coefficient from SiC, which may generate joint residual stress due to mismatch of thermal expansion coefficients; moreover, the reaction by-products of the metal with the SiC may affect the overall performance of the joint.
Analysis shows that in the connection method, only the precursor connection, the nano transient liquid phase connection and the reaction connection do not have the connection of dissimilar materials. However, the nano transient liquid phase connection requires extremely high connection temperature (1800 ℃ C.) and extremely high connection pressure (10 MPa) and is difficult to be directly applied to SiC cladding connection. The reactive connection greatly reduces the high temperature resistance, corrosion resistance and other properties of the joint because 8-10% of residual silicon exists in the joint after connection. Only the precursor connection can realize connection under the conditions of low temperature (less than 1500 ℃) and low pressure (less than 1MPa), can ensure that the joint has good performances of high temperature resistance, corrosion resistance, neutron irradiation resistance and the like after connection, and is very expected to be applied to SiC cladding connection. In the prior art, although the shrinkage rate in the connection process can be inhibited and the connection strength can be improved by adding the filler into the precursor, the introduction of the filler can reduce the performances of high temperature resistance, radiation resistance and the like of the joint and reduce the reliability of the joint.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silicon carbide ceramic connection method with high connection strength and simple process and a silicon carbide cladding formed by connection by adopting the method aiming at the defects in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the silicon carbide ceramic connection method comprises the following steps:
s1, adding a curing agent into liquid polycarbosilane serving as a precursor for curing;
s2, heating and pretreating the solidified polycarbosilane to form precursor powder;
s3, mixing the precursor powder and an organic solvent to prepare slurry;
s4, smearing the slurry between the SiC cladding tube and the end plug which are matched with each other to form a sandwich connection structure;
and S5, carrying out high-temperature curing and cracking treatment on the sandwich connection structure to enable the slurry to form a connection layer tightly connected between the SiC cladding tube and the end plug.
Preferably, in step S1, the polycarbosilane has a molecular formula of (-SiHCH)3-CH2-) n, n is 10-40;
the ceramic yield of the polycarbosilane is 60-80%.
Preferably, in step S1, the curing agent includes at least one of dicumyl peroxide and platinum metal.
Preferably, in step S1, during the curing process: heating to 100-130 ℃ at the speed of 1-5 ℃/min under the inert atmosphere, and preserving heat for 1-3 h; then heating to 140-160 ℃ at the speed of 0.5-2 ℃/min, and preserving heat for 1-3 h; and (6) cooling.
Preferably, in step S2, in the heating pretreatment: heating to 500-800 deg.C at a rate of 5-10 deg.C/min under inert gas or vacuum atmosphere, and maintaining for 1-4 h.
Preferably, in step S3, the mass percentages of the precursor powder and the organic solvent are 25% -35% and 65% -75%, respectively;
the organic solvent is at least one of absolute ethyl alcohol, acetone, xylene and polyethylene glycol.
Preferably, in step S4, the slurry is applied to a thickness of 50 μm to 200 μm.
Preferably, in step S5, during the high temperature curing and cracking treatment, the temperature is raised to 1000-1500 ℃ at 5-20 ℃/min, and the temperature is maintained for 0.5-2 h.
Preferably, in step S5, the atmosphere of the high-temperature curing and cracking process is air, argon, nitrogen, or vacuum atmosphere.
The invention also provides a silicon carbide cladding which comprises a SiC cladding tube and an end plug which are matched with each other; the SiC cladding tube and the end plug are connected into a whole by adopting the silicon carbide ceramic connecting method.
The silicon carbide ceramic connection method of the invention realizes the high-strength connection of the SiC cladding and the end plug at low temperature (less than or equal to 1500 ℃) and no pressure, does not need to add filler, reduces the defect of air holes of the middle connection layer, and improves the air tightness of the formed joint; the connection process is simple, the requirement on equipment is low, and the cost is reduced.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is an electron micrograph of a silicon carbide cladding made in accordance with the present invention.
Detailed Description
In the heating wire winding device according to an embodiment of the present invention,
the invention relates to a silicon carbide ceramic connection method for realizing high-strength connection of two adaptive silicon carbide structural members, which comprises the following steps:
and S1, adding a curing agent into liquid polycarbosilane serving as a precursor for curing.
In the precursor and the curing agent, the curing agent accounts for 0.3 to 0.5 percent by mass.
The molecular formula of the polycarbosilane is (-SiHCH)3-CH2-) n, n is 10-40; the porcelain yield of the polycarbosilane is 60-80%. The curing agent comprises at least one of dicumyl peroxide and metal platinum. The curing agent and the polycarbosilane are mixed for curing treatment, so that the ceramic yield is improved.
During curing treatment: heating to 100-130 ℃ at the speed of 1-5 ℃/min under inert atmosphere (preferably nitrogen or argon), and preserving heat for 1-3 h; then heating to 140-160 ℃ at the speed of 0.5-2 ℃/min, and preserving heat for 1-3 h; and (6) cooling.
And S2, heating and pretreating the solidified polycarbosilane to form precursor powder.
Through the heating pretreatment in the step, the solidified polycarbosilane is subjected to primary cracking, and the volume shrinkage degree caused by subsequent cracking treatment is reduced.
During heating pretreatment: heating to 500-800 deg.C at the rate of 5-10 deg.C/min under inert gas (preferably nitrogen or argon) or vacuum atmosphere, and maintaining for 1-4 h.
And S3, mixing the precursor powder and the organic solvent to prepare slurry.
The mass percentages of the precursor powder and the organic solvent are respectively 25-35% and 65-75%.
The organic solvent is at least one of absolute ethyl alcohol, acetone, xylene and polyethylene glycol.
And S4, smearing the slurry between the SiC cladding tube and the end plug which are matched with each other to form a sandwich connection structure.
Wherein the thickness of the slurry coating is 50-200 μm.
And S5, carrying out high-temperature curing and cracking treatment on the sandwich connection structure to enable the slurry to form a connection layer tightly connected between the SiC cladding tube and the end plug.
The coating thickness of the corresponding slurry is 50-200 μm, and the thickness of the connecting layer formed after curing and cracking is 2-10 μm.
During high-temperature curing and cracking treatment, the temperature is raised to 1000-1500 ℃ at the speed of 5-20 ℃/min, and the temperature is kept for 0.5-2 h. The atmosphere of the high-temperature curing and cracking treatment is air, argon, nitrogen or vacuum atmosphere.
The silicon carbide ceramic connection method can be applied to the connection of the silicon carbide cladding in nuclear power, and the SiC cladding tube and the end plug which are matched are connected into a whole to form the silicon carbide cladding.
The electron microstructure of the silicon carbide cladding is shown in figure 1, in figure 1(a), base materials connected through a middle connecting layer are a SiC cladding tube and an end plug respectively, and the thickness of the connecting layer is uniformly distributed; as can be seen from fig. 1(b), the connection layer has no pore defects, and the silicon carbide cladding has good densification.
The shear strength of the silicon carbide cladding is 60-110MPa, the thickness of the connecting layer is 2-10 μm, the high-temperature shear strength at 1200 ℃ is 80-120MPa, and the air tightness is 10-13Pa·m3/s-10-9Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is not higher than 5% of that of the parent metal (the SiC cladding tube and the end plug).
It will be appreciated that the joining method of the present invention is not limited to joining of cladding tubes and end plugs, but may be applied to joining of other silicon carbide parent materials to form joints and the like.
The present invention is further illustrated by the following specific examples.
Example 1
With a molecular formula of (-SiHCH)3-CH2-) n polycarbosilane as precursor, n ═ 17, ceramic yield 60 wt%; using 0.3 wt% dicumyl peroxide as curing agent, heating to 120 deg.C at 3 deg.C/min under argon atmosphere, holding for 2h, heating to 150 deg.C at 1 deg.C/min, holding for 2h, and furnace cooling. And continuously heating the cured precursor to 500 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere, and preserving the heat for 2h for pretreatment to prepare the powder. Taking absolute ethyl alcohol as an organic solvent, and mixing the powder and the absolute ethyl alcohol according to the weight ratio of 25 percent: and mixing at a ratio of 75 wt% to obtain a slurry. After a sandwich structure is formed by silicon carbide, slurry and silicon carbide, the sandwich structure is firstly placed in an oven at 80 ℃ for drying for 2h, then placed in a tube furnace, heated to 1500 ℃ at a speed of 10 ℃/min for heat preservation for 2h for cracking, and the cracking is carried out in a nitrogen atmosphere. The thickness of the connecting layer after cracking is distributed uniformly, the thickness is only 2 mu m, and the connecting layer is distributed compactly and has no hole defect.
The SiC ceramic joint prepared in this example 1 had a room-temperature shear strength of 110MPa, a high-temperature shear strength of 120MPa at 1200 ℃ and a joint airtightness of 10-13Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is consistent with that of the parent metal.
Example 2
With a molecular formula of (-SiHCH)3-CH2-) n polycarbosilane as a precursor, n ═ 10, the ceramic yield was 70 wt%; 0.5 wt% of dicumyl peroxide is used as a curing agent, xylene is used as an organic solvent, and the volume ratio of the cured and pretreated precursor to the organic solvent is 30 wt%: 70 wt%; the end plugs were coated with a 100 μm thick slurry layer on the surface and attached as in example 1, with a curing temperature of 160 ℃, a pre-treatment temperature of 800 ℃ and a cracking temperature of 1200 ℃.
The fruitThe SiC ceramic connecting piece prepared in the embodiment 2 has a connecting layer with the thickness of 5 μm; the room temperature shear strength of the SiC ceramic connecting piece is 80MPa, the high temperature shear strength at 1200 ℃ is 100MPa, and the air tightness of the joint is 10-10Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is 5% higher than that of the parent metal.
Example 3
With a molecular formula of (-SiHCH)3-CH2-) n polycarbosilane as a precursor, n ═ 40, the ceramic yield was 80 wt%; taking 0.5 wt% of metal platinum as a curing agent, taking dimethylbenzene as an organic solvent, and setting the volume ratio of the cured and pretreated precursor to the organic solvent to be 35 wt%: 65 wt%; the end plugs were coated with a 50 μm thick slurry layer on the surface and attached as in example 1, with a cure temperature of 140 ℃, a pre-treatment temperature of 700 ℃ and a cleavage temperature of 1500 ℃.
The thickness of the connecting layer of the SiC ceramic connecting piece prepared in the embodiment 3 is 4 μm; the room temperature shear strength of the SiC ceramic connecting piece is 90MPa, the high temperature shear strength at 1200 ℃ is 100MPa, and the air tightness of the joint is 10-11Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is 2% higher than that of the parent metal.
Example 4
With a molecular formula of (-SiHCH)3-CH2-) n polycarbosilane as a precursor, n ═ 20, the ceramic yield was 60 wt%; 0.3 wt% of dicumyl peroxide is used as a curing agent, xylene is used as an organic solvent, and the volume ratio of the cured and pretreated precursor to the organic solvent is 35 wt%: 65 wt%; the end plugs were coated with a 200 μm thick slurry layer on the surface and attached as in example 1, with a curing temperature of 150 ℃, a pre-treatment temperature of 500 ℃ and a cracking temperature of 1000 ℃.
In the SiC ceramic connector prepared in this example 4, the thickness of the connecting layer is 2 μm; the room temperature shear strength of the SiC ceramic connecting piece is 100MPa, the high temperature shear strength at 1200 ℃ is 105MPa, and the air tightness of the joint is 10-10Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is 5% higher than that of the parent metal.
Example 5
With the molecular formula (-Si)HCH3-CH2-) n polycarbosilane as a precursor, n ═ 30, the ceramic yield was 70 wt%; 0.5 wt% of dicumyl peroxide is used as a curing agent, xylene is used as an organic solvent, and the volume ratio of the cured and pretreated precursor to the organic solvent is 35 wt%: 65 wt%; the end plugs were coated with a 100 μm thick slurry layer on the surface and attached as in example 1, with a curing temperature of 150 ℃, a pre-treatment temperature of 750 ℃ and a cracking temperature of 1400 ℃.
The thickness of the connecting layer of the SiC ceramic connecting piece prepared in the embodiment 5 is 5 μm; the room temperature shear strength of the SiC ceramic connecting piece is 80MPa, the high temperature shear strength at 1200 ℃ is 100MPa, and the air tightness of the joint is 10-10Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is 5% higher than that of the parent metal.
Example 6
With a molecular formula of (-SiHCH)3-CH2-) n polycarbosilane as a precursor, n is 25, the ceramic yield is 80 wt%, 0.5 wt% dicumyl peroxide is used as a curing agent, xylene is used as an organic solvent, and the volume ratio of the cured and pretreated precursor to the organic solvent is 35 wt%: 65 wt%, the surface of the end plug was coated with a 100 μm thick slurry layer and the connection was made by the method shown in example 1, where the curing temperature was 160 ℃, the pretreatment temperature was 800 ℃ and the cleavage temperature was 1450 ℃.
The thickness of the connecting layer of the SiC ceramic connector prepared in this example 6 is 5 μm; the room temperature shear strength of the SiC ceramic connecting piece is 80MPa, the high temperature shear strength at 1200 ℃ is 100MPa, and the air tightness of the joint is 10-10Pa·m3And/s, the corrosion rate of the connecting layer after hydrothermal corrosion is 5% higher than that of the parent metal.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for connecting silicon carbide ceramics is characterized by comprising the following steps:
s1, adding a curing agent into liquid polycarbosilane serving as a precursor for curing;
s2, heating and pretreating the solidified polycarbosilane to form precursor powder;
s3, mixing the precursor powder and an organic solvent to prepare slurry;
s4, smearing the slurry between the SiC cladding tube and the end plug which are matched with each other to form a sandwich connection structure;
and S5, carrying out high-temperature curing and cracking treatment on the sandwich connection structure to enable the slurry to form a connection layer tightly connected between the SiC cladding tube and the end plug.
2. The method of claim 1, wherein the polycarbosilane has a formula of (-SiHCH) in step S13-CH2-) n, n is 10-40;
the ceramic yield of the polycarbosilane is 60-80%.
3. The silicon carbide ceramic joining method according to claim 1, wherein in step S1, the curing agent includes at least one of dicumyl peroxide and platinum metal.
4. The method for joining silicon carbide ceramics according to claim 1, wherein in the step S1, in the curing treatment: heating to 100-130 ℃ at the speed of 1-5 ℃/min under the inert atmosphere, and preserving heat for 1-3 h; then heating to 140-160 ℃ at the speed of 0.5-2 ℃/min, and preserving heat for 1-3 h; and (6) cooling.
5. The method for joining silicon carbide ceramics according to claim 1, wherein in the step S2, in the heat pretreatment: heating to 500-800 deg.C at a rate of 5-10 deg.C/min under inert gas or vacuum atmosphere, and maintaining for 1-4 h.
6. The silicon carbide ceramic connection method according to claim 1, wherein in step S3, the mass percentages of the precursor powder and the organic solvent are 25% -35% and 65% -75%, respectively;
the organic solvent is at least one of absolute ethyl alcohol, acetone, xylene and polyethylene glycol.
7. The method for joining silicon carbide ceramics according to claim 1, wherein the slurry is applied to a thickness of 50 μm to 200 μm in step S4.
8. The method for connecting silicon carbide ceramics according to claim 1, wherein in step S5, the temperature is raised to 1000 ℃ to 1500 ℃ at a rate of 5 ℃/min to 20 ℃/min during the high temperature curing and cracking treatment, and the temperature is maintained for 0.5 to 2 hours.
9. The method for joining silicon carbide ceramics according to claim 8, wherein in step S5, the atmosphere of the high-temperature curing/cracking treatment is air, argon, nitrogen, or a vacuum atmosphere.
10. A silicon carbide cladding comprising a fitted SiC cladding tube and end plugs; the SiC cladding tube and end plug are joined together using the silicon carbide ceramic joining method of any one of claims 1 to 9.
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| CN113402289A (en) * | 2021-05-08 | 2021-09-17 | 中广核研究院有限公司 | Silicon carbide cladding induction heating connection method and silicon carbide cladding |
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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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| 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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| CN113402289A (en) * | 2021-05-08 | 2021-09-17 | 中广核研究院有限公司 | Silicon carbide cladding induction heating connection method and silicon carbide cladding |
| CN113698224A (en) * | 2021-07-22 | 2021-11-26 | 中广核研究院有限公司 | Resistance welding connection device and silicon carbide connection method |
| CN113698224B (en) * | 2021-07-22 | 2023-03-03 | 中广核研究院有限公司 | Resistance welding connection device and silicon carbide connection method |
| WO2023070889A1 (en) * | 2021-10-29 | 2023-05-04 | 中广核研究院有限公司 | Silicon carbide joint and metal penetration connection method therefor |
| CN116408252A (en) * | 2021-12-29 | 2023-07-11 | 南昌中微半导体设备有限公司 | Workpiece processing method, workpiece and plasma processing apparatus |
| 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 |
| 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 |
| CN115806443B (en) * | 2023-02-06 | 2023-07-14 | 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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