CN111892418A - Connecting material for connecting silicon carbide ceramics and application method thereof - Google Patents
Connecting material for connecting silicon carbide ceramics and application method thereof Download PDFInfo
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- CN111892418A CN111892418A CN202010646284.7A CN202010646284A CN111892418A CN 111892418 A CN111892418 A CN 111892418A CN 202010646284 A CN202010646284 A CN 202010646284A CN 111892418 A CN111892418 A CN 111892418A
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/12—Metallic interlayers
- C04B2237/122—Metallic interlayers based on refractory metals
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/12—Metallic interlayers
- C04B2237/123—Metallic interlayers based on iron group metals, e.g. steel
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/12—Metallic interlayers
- C04B2237/124—Metallic interlayers based on copper
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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
Abstract
The invention discloses a method for connecting silicon carbide ceramics with the aid of an electric field and a connecting material adopted by the method, and belongs to the field of silicon carbide ceramic materials, wherein the method comprises the steps of clamping a connecting layer between the silicon carbide ceramic materials to be connected, and connecting the SiC materials to be connected together by heating a connecting interface with the aid of an external electric field to a connecting temperature of more than 1000 ℃; the connecting layer is a high-entropy alloy sheet with the thickness of less than 1 mm; the material used for the connecting layer is CoFeCrNiCuTixHigh entropy alloy. The invention has lower requirement on external heat source, high connection speed and better mechanical strength property of the connected silicon carbide ceramic material, is favorable for saving cost, reduces the difficulty of industrial production and realizes quick and high-quality connection.
Description
Technical Field
The invention relates to the field of silicon carbide ceramic materials, in particular to a connecting material for connecting silicon carbide ceramics and an application method thereof.
Background
With the rapid development of scientific and technical and industrial demands, there is an increasing demand for new materials that can be used in extremely harsh high temperature environments. The silicon carbide (SiC) ceramic material has good wear resistance, stability, thermal conductivity, oxidation resistance and excellent high-temperature mechanical property, and can be widely applied to the fields of optical systems, space technology, thermal protection, vehicles, energy technology and the like. However, the high brittleness and low ductility of silicon carbide ceramics and their composites make it difficult to manufacture complex parts, often in combination with other parts to form a composite structure for use. Therefore, the strengthening of the research on the connection problem of the silicon carbide ceramic and the composite material thereof has important significance for expanding the engineering application thereof.
However, SiC has some properties, such as covalent bond, small diffusion coefficient, inertness, etc., so that its connection is also difficult. Currently, the SiC connection method uses a connection layer, which is sandwiched between SiC materials to be connected, and the SiC materials to be connected are connected together by heating a connection interface to a certain temperature (i.e., a connection temperature) by an external heat source. The connection method of the silicon carbide ceramic and the composite material thereof comprises mechanical connection, friction welding, high-energy beam welding, microwave connection, glass connection, reaction connection, active brazing, diffusion connection, transient liquid phase connection, partial transient liquid phase connection and the like. Wherein, mechanical connection, active brazing, diffusion connection, transient liquid phase connection and partial transient liquid phase connection are the main methods for connecting the silicon carbide ceramics and the composite materials thereof at present.
A suitable solder and its good wettability are a prerequisite for achieving a good joint. The high-entropy alloy is used as a novel alloy system, the high entropy of thermodynamics can promote the mixing of elements, and a body-centered cubic or face-centered cubic solid solution structure is easy to form, so that the formation of brittle metal compounds is inhibited. In the process of solidification of the kinetic high-entropy alloy, the separation and diffusion processes of elements are very slow, so that nucleation and growth are delayed, and the microstructure is prone to nanocrystallization and amorphization. If the brazing filler metal is used as the brazing filler metal, the unique thermodynamic and kinetic properties of the brazing filler metal have positive effects on the aspects of inhibiting excessive dissolution of base metal and brazing filler metal elements in the brazing process, reducing the generation of harmful substances at an interface, improving the solid solution strengthening capacity of a joint and the like.
The required connection temperature of the connecting material is generally higher and at least higher than 1000 ℃, while the existing connecting material completely depends on an external heat source to provide heat, and the heat required by the external heat source is higher; and the connecting layer formed by the existing connecting material is thick, and when an external heat source supplies heat to improve the connecting temperature, the heat required to be supplied by the external heat source is increased, so that the requirement on the external heat source is high, the cost is increased, and the industrial production difficulty is high. In addition, because the connecting layer formed by the existing connecting material is thick, the concentration of silicon atoms and carbon atoms diffused from the silicon carbide and the composite material thereof in the connecting layer is low, the element distribution range is large, the reaction is insufficient, and other brittle phases are easily generated, so that the mechanical strength performance of the connected silicon carbide ceramic material is influenced.
Disclosure of Invention
1. Technical problem to be solved
The technical problem to be solved by the invention is to provide a method for connecting silicon carbide ceramic by electric field assistance and a connecting material adopted by the method, the requirement on an external heat source is lower, the connecting speed is high, the mechanical strength performance of the connected silicon carbide ceramic material is better, the cost is saved, the industrial production difficulty is reduced, and the quick and high-quality connection is realized.
2. Technical scheme
In order to solve the problems, the invention adopts the following technical scheme:
a method for electric field auxiliary connection of silicon carbide ceramics comprises the following steps: clamping the connecting layer between two silicon carbide ceramic materials to be connected, and then rapidly heating a connecting interface to a connecting temperature in an electric field auxiliary heating connection mode so as to connect the silicon carbide ceramic materials to be connected together through the connecting material;
the connecting layer is CoFeCrNiCuTixA high entropy alloy sheet, and the CoFeCrNiCuTixThe thickness of the high-entropy alloy sheet is less than 1 mm.
Further, the CoFeCrNiCuTixThe thickness of the high-entropy alloy sheet is 100-400 mu m.
Further, the connection temperature is 1000-1150 ℃.
Further, the silicon carbide ceramic material is a pure silicon carbide ceramic material or a composite material taking the pure silicon carbide ceramic material as a matrix.
Furthermore, the composite material is a carbon fiber reinforced silicon carbide composite material or a silicon carbide fiber reinforced silicon carbide composite material.
Further, the surface roughness Ra of the silicon carbide ceramic material is less than 0.1 μm.
Furthermore, an electric field-assisted hot-pressing connection mode is adopted, so that the connection interface is quickly heated to the connection temperature.
The invention also provides a connecting material applied to the method, wherein the connecting material is CoFeCrNiCuTixHigh entropy alloy.
Further, the CoFeCrNiCuTixThe preparation method of the high-entropy alloy comprises the following steps: firstly, preparing CoFeCrNiCu quinary alloy according to equal atomic ratio to obtain high-entropy alloy with single FCC structure, and then adding Ti element to form CoFeCrNiCuTixThe high-entropy alloy is characterized in that x is 0, 0.5, 1 or 2.
3. Advantageous effects
(1) The invention uses CoFeCrNiCuTixThe high-entropy alloy is used as an intermediate connecting material of the silicon carbide ceramic material, the high-entropy alloy element has the problems of slow diffusion and slow reaction, Ti is added as an active element, the high activity of the titanium element can improve the interface surface energy of the silicon carbide ceramic material, increase the reaction activity of the silicon carbide ceramic material, is beneficial to the sintering densification between the material to be connected and a connecting layer, can improve the wetting of the brazing filler metal on a ceramic interface, and is beneficial to the metallurgical reaction of a joint.
(2) In the method provided by the invention, when the electric field is used for auxiliary heating, the Ti active element can perform exothermic reaction with silicon atoms and carbon atoms diffused into the connecting layer from the matrix silicon carbide ceramic material at a certain connecting temperature, so that the connecting layer between the two silicon carbide ceramic materials can release a part of heat, thereby reducing the external energy supply, lowering the requirement on an external heat source, reducing the cost and ensuring less industrial production difficulty.
(3) In the method provided by the invention, the thickness of the connecting layer is thinner, so that the concentration of atoms diffused from the matrix silicon carbide ceramic material in the connecting layer is improved, the full reaction of three elements of Ti, Si and C is facilitated, and the heat released by the connecting layer can be further increased, so that the connecting temperature required by the silicon carbide ceramic material is further reduced, the requirement on an external heat source can be promoted to be reduced, the cost is reduced, and the industrial production difficulty is lower.
(4) In the method provided by the invention, the thickness of the connecting layer is thinner, so that the concentration of silicon atoms and carbon atoms diffused from the matrix silicon carbide ceramic material in the connecting layer is higher, the element distribution range is large, the reaction can be promoted fully, the quantity of generated brittle phases is reduced, the mechanical strength of a connecting interface is favorably improved, and the influence on the mechanical strength performance of the connected silicon carbide ceramic material can be avoided.
In conclusion, the invention has lower requirement on external heat source, high connection speed and better mechanical strength property of the connected silicon carbide ceramic material, is favorable for saving cost, reduces the difficulty of industrial production and realizes quick and high-quality connection.
Drawings
FIG. 1 is a schematic structural view of the present invention;
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
Connecting the silicon carbide ceramic materials to be connected by adopting a connecting layer as shown in figure 1, wherein the silicon carbide ceramic materials to be connected are two cylindrical pure silicon carbide ceramic materials with the diameter and the height of 20 mm; the connecting layer is a CoFeCrNiCu high-entropy alloy sheet, the thickness of the CoFeCrNiCu high-entropy alloy sheet is 100 mu m, the material used by the connecting layer is CoFeCrNiCu high-entropy alloy, and the preparation method of the material comprises the following steps: the CoFeCrNiCu quinary alloy is prepared according to the equal atomic ratio to obtain the high-entropy alloy with a single FCC structure, so that the CoFeCrNiCu high-entropy alloy is formed.
And adopting an external heat source heating connection method, connecting the silicon carbide materials to be connected together through the connecting layer, wherein the external heat source heating connection method is electric field assisted hot-pressing connection. The connection method comprises the following specific steps:
(1) grinding the surface of the silicon carbide ceramic material to be connected by using sand paper, and then polishing by using 0.25 micron diamond polishing solution to remove larger defects and impurities on the surface so as to ensure that the surface roughness Ra of the silicon carbide ceramic material is less than 0.1 mu m;
(2) grinding the surface of a high-entropy alloy sheet to be used by using abrasive paper, and then polishing by using 0.25 micron diamond polishing solution to remove larger defects and impurities on the surface;
(3) soaking the polished silicon carbide ceramic material and the high-entropy alloy sheet in alcohol, putting the soaked silicon carbide ceramic material and the high-entropy alloy sheet into an ultrasonic cleaning machine for cleaning, and then putting the silicon carbide ceramic material and the high-entropy alloy sheet into a drying box for drying;
(4) connecting surfaces of the two dried silicon carbide ceramic materials are opposite, a high-entropy alloy sheet is clamped between the two silicon carbide ceramic materials to form a connecting sample, and meanwhile, two pieces of graphite paper are respectively placed on one side (namely between the silicon carbide ceramic material and a pressing tool on the corresponding side) of the two silicon carbide ceramic materials, which is back to the connecting surfaces, so that the silicon carbide ceramic materials and the pressing tool are prevented from being adhered; placing graphite paper, a silicon carbide ceramic material and a high-entropy alloy sheet into a mould one by one according to the structure (namely placing two graphite paper, one silicon carbide ceramic material, the high-entropy alloy sheet, the other silicon carbide ceramic material and the other two graphite paper into the mould in sequence), then placing the mould into a discharge plasma sintering furnace (SPS furnace), connecting by adopting a SiC/high-entropy alloy sheet/SiC superposition mode, so as to analyze the influence of voltage polarity on diffusion connection, wherein the SiC/high-entropy alloy sheet interface is defined as a voltage positive electrode interface and the high-entropy alloy sheet/SiC interface is defined as a voltage negative electrode interface from SiC to the high-entropy alloy sheet along the electric field direction;
(5) and measuring the temperature by an upper pressure head, electrifying a discharge plasma sintering furnace (SPS furnace), heating up at a heating rate of 100 ℃/min, applying a pressure of 19MPa to a connected sample in the heating process, heating to the furnace temperature of 1000 ℃ (namely the connection temperature is 1000 ℃), keeping the temperature for 10min, and then cooling to the room temperature at the rate of 100 ℃/min to obtain the silicon carbide ceramic material with the cylindrical structure, wherein the diameter of the silicon carbide ceramic material is 20mm, and the height of the silicon carbide ceramic material is approximately 40 mm.
Example 2
The present embodiment is different from embodiment 1 in that:
the silicon carbide ceramic materials to be connected are two composite materials which take pure silicon carbide ceramic materials as matrixes, in particular carbon fiber reinforced silicon carbide composite materials; the connecting layer is CoFeCrNiCuTi0.5High entropy alloy sheet, and CoFeCrNiCuTi0.5The thickness of the high-entropy alloy sheet is 400 mu m, and the material used for the connecting layer is CoFeCrNiCuTi0.5The preparation method of the high-entropy alloy comprises the following steps: firstly, preparing CoFeCrNiCu quinary alloy according to equal atomic ratio to obtain high-entropy alloy with single FCC structure, and then adding Ti element to form CoFeCrNiCuTi0.5High entropy alloy.
In step (5), the temperature is raised to 1075 ℃ (i.e. the link temperature is 1075 ℃).
Otherwise, the same procedure as in example 1 was repeated.
Example 3
The present embodiment is different from embodiment 1 in that:
the silicon carbide ceramic materials to be connected are two composite materials which take pure silicon carbide ceramic materials as matrixes, in particular to silicon carbide fiber reinforced silicon carbide composite materials; the connecting layer is a CoFeCrNiCuTi high-entropy alloy sheet, the thickness of the CoFeCrNiCuTi high-entropy alloy sheet is 300 mu m, the material used by the connecting layer is CoFeCrNiCuTi high-entropy alloy, and the preparation method of the material comprises the following steps: firstly, preparing the CoFeCrNiCu quinary alloy according to an equal atomic ratio to obtain the high-entropy alloy with a single FCC structure, and then adding Ti element to form the CoFeCrNiCuTi high-entropy alloy.
In step (5), the temperature is raised to 1100 ℃ (i.e., the junction temperature is 1100 ℃).
Otherwise, the same procedure as in example 1 was repeated.
Example 4
The present embodiment is different from embodiment 1 in that:
the connecting layer is CoFeCrNiCuTi2High entropy alloy sheet, and CoFeCrNiCuTi2The thickness of the high-entropy alloy sheet is 400 mu m, and the material used for the connecting layer is CoFeCrNiCuTi2High-entropy alloy and preparation method of high-entropy alloyThe method comprises the following steps: firstly, preparing CoFeCrNiCu quinary alloy according to equal atomic ratio to obtain high-entropy alloy with single FCC structure, and then adding Ti element to form CoFeCrNiCuTi2High entropy alloy.
In step (5), the temperature is raised to 1150 ℃ (i.e., the junction temperature is 1150 ℃).
Otherwise, the same procedure as in example 1 was repeated.
Cutting the silicon carbide ceramic material (the diameter is 20mm, the height is approximately 40mm) subjected to the connection treatment by a diamond wire cutting machine, polishing, processing into a sample strip of 4 multiplied by 40mm, and testing the three-point bending strength of the sample strip by a three-point bending method. The results show that the compressive capacity of the tie layer is better.
And observing the microscopic interface morphology of the intermediate connection layer of the silicon carbide ceramic material after the connection treatment by using a scanning electron microscope. The result shows that the connecting interface has no obvious crack parallel to the interface, the connecting layer is compact, the strength is high, and the interface has no obvious phase contrast.
From the above, the requirements on an external heat source are low, the connection speed is high, the mechanical strength performance of the connected silicon carbide ceramic material is good, the cost is saved, the industrial production difficulty is reduced, and the quick and high-quality connection is realized.
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as a limitation of the present invention, and that changes and modifications to the above embodiments are within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (9)
1. A method for connecting silicon carbide ceramics in an electric field auxiliary manner is characterized in that a connecting layer is clamped between two silicon carbide ceramic materials to be connected, then the connecting interface is quickly heated to the connecting temperature in an electric field auxiliary heating connection manner, and the silicon carbide ceramic materials to be connected are connected together through a connecting material;
the connecting layer is CoFeCrNiCuTixA high entropy alloy sheet, and the CoFeCrNiCuTixThe thickness of the high-entropy alloy sheet is less than 1 mm.
2. The method of claim 1, wherein the CoFeCrNiCuTi is used for electric field assisted bonding of silicon carbide ceramicxThe thickness of the high-entropy alloy sheet is 100-400 mu m.
3. The method of claim 1, wherein the joining temperature is 1000 ℃ to 1150 ℃.
4. The method of claim 1, wherein the silicon carbide ceramic material is a pure silicon carbide ceramic material or a composite material with a matrix of a pure silicon carbide ceramic material.
5. The method of claim 4, wherein the composite material is a carbon fiber reinforced silicon carbide composite material or a silicon carbide fiber reinforced silicon carbide composite material.
6. An electric field assisted method of joining silicon carbide ceramic according to claim 1 wherein the silicon carbide ceramic material has a joint surface roughness Ra of less than 0.1 μm.
7. The method of claim 1, wherein the electric field assisted hot pressing is used to rapidly raise the temperature of the bonding interface to the bonding temperature.
8. A connecting material applied to the method of any one of claims 1 to 7, wherein the connecting material is CoFeCrNiCuTixHigh entropy alloy.
9. A joining material according to claim 8, wherein said CoFeCrNiCuTixThe preparation method of the high-entropy alloy comprises the following steps: firstly, preparing CoFeCrNiCu quinary alloy according to equal atomic ratio to obtain high-entropy alloy with single FCC structure, and then adding Ti element to form CoFeCrNiCuTixThe high-entropy alloy is characterized in that x is 0, 0.5, 1 or 2.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN113828880A (en) * | 2021-10-09 | 2021-12-24 | 浙江工业大学 | Method for connecting silicon carbide ceramic by adopting refractory high-entropy alloy interlayer discharge plasma diffusion |
| CN114133263A (en) * | 2021-10-29 | 2022-03-04 | 中广核研究院有限公司 | High-entropy alloy connection method of silicon carbide and silicon carbide connecting piece |
| CN114133264A (en) * | 2021-12-24 | 2022-03-04 | 哈尔滨工业大学 | Method for connecting silicon carbide ceramic composite material and nickel-based high-temperature alloy and joint |
| CN115196968A (en) * | 2022-06-10 | 2022-10-18 | 华南理工大学 | High-entropy boride ceramic powder and preparation method and application thereof |
| CN115477545A (en) * | 2022-07-26 | 2022-12-16 | 华东交通大学 | Continuous carbon fiber reinforced high-entropy ceramic composite material and preparation method thereof |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| CN113828880A (en) * | 2021-10-09 | 2021-12-24 | 浙江工业大学 | Method for connecting silicon carbide ceramic by adopting refractory high-entropy alloy interlayer discharge plasma diffusion |
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| CN115477545A (en) * | 2022-07-26 | 2022-12-16 | 华东交通大学 | Continuous carbon fiber reinforced high-entropy ceramic composite material and preparation method thereof |
| 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 |
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