CN111960844A - Ceramic connecting piece and preparation method and application thereof - Google Patents
Ceramic connecting piece and preparation method and application thereof Download PDFInfo
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/001—Joining burned ceramic articles with other burned ceramic articles or other articles by heating directly with other burned ceramic articles
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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- 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
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- 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
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- C04B2237/368—Silicon nitride
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
- C04B2237/525—Pre-treatment of the joining surfaces, e.g. cleaning, machining by heating
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/54—Oxidising the surface before joining
Abstract
The invention belongs to the technical field of ceramic connection and discloses a ceramic connecting piece and a preparation method and application thereof, wherein the ceramic connecting piece is prepared by polishing the surface of the connecting end face of a ceramic base material and then carrying out pre-oxidation treatment at 800-1200 ℃ to prepare the ceramic base material with an oxide layer; and (3) placing the two ceramic base materials with the oxide layers in a butt joint mode according to the oxide layers, and reacting at 1300-1500 ℃ in a reaction atmosphere to connect to obtain the ceramic connecting piece. The ceramic connection prepared by the method under the non-pressure condition has good corrosion resistance, the shear strength of the joint at room temperature is 80-150 MPa, the shear strength at 1200 ℃ is 100-200 MPa, and the residual stress is 50-100 MPa.
Description
Technical Field
The invention belongs to the technical field of ceramic connection, and particularly relates to a ceramic connecting piece and a preparation method and application thereof.
Background
Si3N4And Si-based structural ceramics such as SiC and the like generally have the excellent characteristics of high melting point, corrosion resistance, high strength, high hardness, high temperature resistance and the like, and have wide application in the high-temperature and high-corrosion application fields of war industry, ocean, aerospace and the like. However, since the above materials have excellent mechanical properties, their difficult processability also limits their application in the field of complex structural members. Therefore, it is necessary to form parts having complicated shapes by a joining technique between ceramics. For the currently mature NITE connection, solid phase diffusion connection and MAX connection, although high-strength connection can be realized, large connection pressure is usually required, and connection of parts with complex shapes is not facilitated. Moreover, other phases are often introduced into the middle connection layer during the ceramic connection, which may greatly reduce the high temperature and corrosion resistance; meanwhile, the thermal expansion coefficient between the intermediate layer and the base material is not matched, so that the joint generates thermal stress, and the reliability of the joint is further reduced; for example, although the glass ceramic can be connected under a pressureless condition, the joint has poor high-temperature resistance and corrosion resistance; for the braze welding connection realized under the conditions of low temperature and no pressure, the joint quality is greatly reduced by the larger residual stress between the metal and the ceramic at the joint; based on the above research background, it is urgently needed to develop a connection technology, so that the joint has high strength, high temperature resistance and corrosion resistance, and simultaneously, the residual stress of the joint can be reduced.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, a preparation method of a ceramic connecting piece is provided. According to the method, through pre-oxidation of the ceramic material, the oxide layer reacts in a reaction atmosphere to generate a material with the same components as the base material, so that the residual stress of a joint between the ceramics is reduced while the connection performance is ensured, and traceless connection of the ceramics under a non-pressure condition is realized.
It is another object of the present invention to provide a ceramic connecting member prepared by the above method, which has a reliable connection strength.
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:
s1, polishing the surface of the connecting end face of the ceramic base material, and then carrying out pre-oxidation treatment at 800-1200 ℃ to obtain the ceramic base material with an oxide layer;
s2, placing the oxide layers of the two pre-oxidized ceramic base materials in a butt joint mode, and reacting at 1300-1500 ℃ in a reaction atmosphere to connect to obtain the ceramic connecting piece.
Preferably, in step S1, the ceramic base material is silicon nitride or silicon carbide.
Preferably, the purity of the ceramic base material is 99-99.999%.
Preferably, the time of the pre-oxidation treatment in the step S1 is 1-2 h.
Preferably, the reaction atmosphere in step S2 is carbon gas or nitrogen gas.
Preferably, the connection time in the step S2 is 1-4 h.
A ceramic connecting piece is prepared by the method.
Preferably, the shear strength of the joint in the ceramic connecting piece at room temperature is 80-150 MPa, the shear strength at 1200 ℃ is 100-200 MPa, and the residual stress of the joint is 50-100 MPa.
The ceramic connecting piece is applied to the fields of oceans, aerospace or nuclear energy in a high-temperature environment or a corrosive environment.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, through pre-oxidation of the ceramic material, the oxide layer reacts in a reaction atmosphere to generate a material with the same composition as the base material, so that the residual stress of the joint between the ceramics is reduced while the connection performance is ensured, traceless connection of the ceramics under a non-pressure condition is realized, the thermal stress caused by mismatching of the thermal expansion coefficients of the intermediate layer and the base material is greatly reduced, and the reliability of the ceramic connecting piece is improved.
2. The ceramic base material is connected through the preoxidation on the surface of the ceramic base material, and a connecting material is not needed in the connecting process, so that the cost is greatly saved; meanwhile, the method can be carried out under the conditions of low temperature and no pressure, and the connection of complex structural parts can be met.
3. The material at the connecting layer is consistent with the composition of the parent metal, and has good high-temperature resistance and corrosion resistance. The shear strength of the joint at room temperature is 80-150 MPa, the shear strength at 1200 ℃ is 100-200 MPa, and the residual stress of the joint is 50-100 MPa.
Drawings
FIG. 1 is a schematic view of a SiC ceramic joint according to the invention before and after joining.
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. SiC ceramic with the purity of 99.99 percent is taken as a connecting parent metal; polishing the SiC ceramic by using diamond grinding paste until the surface roughness is 0.1 mu m, cleaning and drying the connecting surface of the SiC ceramic, and then carrying out preoxidation treatment on the connecting surface in a muffle furnace at 1200 ℃ for 1h to prepare an oxide layer/SiC ceramic;
2. stacking SiC ceramic/oxide layer/SiC ceramic into a sandwich structure, heating to 1450 ℃ in a carbon atmosphere of 1atm, and preserving heat for 2h, thereby realizing seamless connection of SiC under a non-pressure condition, wherein the connection process is shown in figure 1.
FIG. 1 is a schematic view of a SiC ceramic joint according to the invention before and after joining. (a) Before connection, and (b) after connection. The light gray portion indicated by the black arrow in fig. 1 (a) indicates an oxide layer of the SiC surface, and the dotted line indicates an interface where the oxide layer/the oxide layer of the SiC ceramic contact; under the carbon atmosphere, an oxide layer on the surface of the SiC reacts with carbon to generate SiC, namely, after connection, as shown in (b) in FIG. 1, an interface is formed at a dotted line of a black arrow in (b) in FIG. 1, so that traceless connection of ceramics is realized.
The connecting layer at the joint of the SiC ceramic connecting piece prepared by the embodiment has no pore defects, the shear strength of the joint of the SiC ceramic connecting piece at room temperature is 150MPa, the shear strength at 1200 ℃ is 180MPa, and the residual stress of the joint is 70 MPa.
Example 2
1. Si with a purity of 99.99%3N4Polishing the ceramic serving as a base material by using diamond grinding paste until the surface roughness is 0.1 mu m, cleaning and drying the connecting surface, and then carrying out pre-oxidation treatment on the connecting surface in a muffle furnace at 1000 ℃ for 2 h;
2. the connection is carried out by adopting the method of the embodiment 1, the connection atmosphere is a nitrogen atmosphere of 1atm in the connection process, the connection temperature is 1400 ℃, the heat preservation is carried out for 4h, and the Si is realized3N4Traceless connection of ceramic materials, Si produced3N4The joint connecting layer has no pore defect.
Si prepared in this example3N4The joint of the ceramic connecting piece has the shear strength of 100MPa at room temperature, the shear strength of 110MPa at high temperature of 1200 ℃ and the residual stress of 50 MPa.
Example 3
1. Si with a purity of 99.9%3N4Polishing the ceramic serving as a base material by using diamond grinding paste until the surface roughness is 0.1 mu m, cleaning and drying the connecting surface, and then carrying out preoxidation treatment on the connecting surface in a muffle furnace at 800 ℃ for 1 h;
2. the connection is carried out by adopting the method of the embodiment 1, the connection atmosphere is a nitrogen atmosphere of 1atm in the connection process, the connection temperature is 1300 ℃, the heat preservation is carried out for 1h, and the Si is realized3N4Traceless connection of ceramic materials, Si produced3N4The joint connecting layer has no pore defect.
Si prepared in this example3N4The shear strength of the ceramic connector joint at room temperature is 80MPa, the shear strength at high temperature of 1200 ℃ is 100MPa, and the residual stress of the joint is 50 MPa.
Example 4
1. Taking SiC ceramic with the purity of 99.99 percent as a base material, polishing the SiC ceramic by adopting diamond grinding paste until the surface roughness is 0.1 mu m, cleaning and drying the connecting surface, and then carrying out pre-oxidation treatment on the connecting surface in a muffle furnace at the temperature of 1000 ℃ for 1 h;
2. the connection is carried out by adopting the method of the embodiment 1, the connection atmosphere is carbon gas atmosphere of 1atm in the connection process, the connection temperature is 1450 ℃, the temperature is kept for 1h, the traceless connection of the SiC ceramic material is realized, and the prepared SiC joint connection layer has no air hole defect.
The joint of the SiC ceramic connector prepared in this example had a shear strength of 110MPa at room temperature, a shear strength of 130MPa at a high temperature of 1200 ℃, and a residual stress of 60 MPa.
Example 5
1. Taking SiC ceramic with the purity of 99.999 percent as a base material, polishing the SiC ceramic by adopting diamond grinding paste until the surface roughness is 0.1 mu m, cleaning and drying the connecting surface, and then carrying out preoxidation treatment on the connecting surface in a muffle furnace at 1200 ℃ for 2 h;
2. the connection is carried out by adopting the method of the embodiment 1, the connection atmosphere is 1atm of nitrogen atmosphere in the connection process, the connection temperature is 1350 ℃, the heat preservation is carried out for 2h, the traceless connection of the SiC ceramic material is realized, and the prepared SiC joint connection layer has no air hole defects.
The joint of the SiC ceramic connecting piece prepared by the embodiment has the shear strength of 120MPa at room temperature, the shear strength of 140MPa at the high temperature of 1200 ℃, and the residual stress of 90 MPa.
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. The preparation method of the ceramic connecting piece is characterized by comprising the following specific steps of:
s1, polishing the surface of the connecting end face of the ceramic base material, and then carrying out pre-oxidation treatment at 800-1200 ℃ to obtain the ceramic base material with an oxide layer;
s2, placing the oxide layers of the two pre-oxidized ceramic base materials in a butt joint mode, and reacting at 1300-1500 ℃ in a reaction atmosphere to connect to obtain the ceramic connecting piece.
2. The method according to claim 1, wherein the ceramic base material is silicon nitride or silicon carbide in step S1.
3. The method of manufacturing a ceramic connection member according to claim 1, wherein the purity of the ceramic base material is 99 to 99.999%.
4. The method for preparing a ceramic connecting member according to claim 1, wherein the time of the pre-oxidation treatment in step S1 is 1-2 hours.
5. The method of manufacturing a ceramic connecting member as recited in claim 1, wherein the reaction atmosphere in step S2 is carbon gas or nitrogen gas.
6. The method for preparing a ceramic connecting member according to claim 1, wherein the connecting time in step S2 is 1-4 h.
7. A ceramic joining member, characterized in that it is produced by the method according to any one of claims 1 to 6.
8. The ceramic connecting member according to claim 7, wherein the joint in the ceramic connecting member has a shear strength of 80 to 150MPa at room temperature and a shear strength of 100 to 200MPa at 1200 ℃; the residual stress of the joint is 50-100 MPa.
9. Use of the ceramic connection according to claim 7 or 8 in the field of marine, aerospace or nuclear energy in high temperature environments or corrosive environments.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115611651A (en) * | 2022-11-02 | 2023-01-17 | 哈尔滨工业大学 | Low-temperature connection method for silicon carbide ceramic oxidation assisted by electric field |
| CN115724678A (en) * | 2022-11-16 | 2023-03-03 | 广东工业大学 | Method for preparing ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation and application |
| CN116354738A (en) * | 2022-11-24 | 2023-06-30 | 广东工业大学 | Ceramic connecting piece with high temperature resistance and irradiation resistance, and preparation method and application thereof |
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| 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 |
| CN115611651A (en) * | 2022-11-02 | 2023-01-17 | 哈尔滨工业大学 | Low-temperature connection method for silicon carbide ceramic oxidation assisted by electric field |
| CN115611651B (en) * | 2022-11-02 | 2023-10-20 | 哈尔滨工业大学 | Low-temperature connection method for electric field assisted silicon carbide ceramic oxidation |
| CN115724678A (en) * | 2022-11-16 | 2023-03-03 | 广东工业大学 | Method for preparing ceramic connecting piece by combining nano transient eutectic liquid with surface oxidation and application |
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| CN111960844B (en) | 2022-08-02 |
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