CN113441803A - Method for brazing C/C composite material and niobium alloy - Google Patents

Method for brazing C/C composite material and niobium alloy Download PDF

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CN113441803A
CN113441803A CN202110798057.0A CN202110798057A CN113441803A CN 113441803 A CN113441803 A CN 113441803A CN 202110798057 A CN202110798057 A CN 202110798057A CN 113441803 A CN113441803 A CN 113441803A
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brazing
composite material
niobium alloy
induction heating
vacuum induction
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CN113441803B (en
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章强
张艺凡
贾德浩
刘梦如
付茂青
姚丽媛
杜玉祥
张洁
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Linyi University
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Linyi University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/008—Soldering within a furnace
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/002—Soldering by means of induction heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B23K1/206—Cleaning
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/08—Non-ferrous metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/16—Composite materials, e.g. fibre reinforced

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Ceramic Products (AREA)

Abstract

A method for brazing C/C composite materials and niobium alloys relates to a brazing method. The invention aims to solve the problems of poor room temperature mechanical property and overlarge thermal stress of a soldered joint obtained by the existing solder for connecting C/C composite materials and niobium alloys and the soldering connection method. The method comprises the following steps: firstly, polishing; secondly, ultrasonic cleaning; thirdly, assembling; fourthly, brazing. The invention utilizes CoCrFeNiCuTi0.25 high-entropy alloy solder to carry out pressureless soldering connection on the C/C composite material and the niobium alloy, the shear strength of the joint at room temperature reaches 47.44MPa to the maximum, and the strength of the joint is in the leading position in the same type of joints. The brazing seam structure of the brazing joint obtained by the method is mainly a solid solution phase, has good plasticity, and can better relieve the residual stress of the joint through plastic deformation. The invention can obtain a method for brazing C/C composite materials and niobium alloys.

Description

Method for brazing C/C composite material and niobium alloy
Technical Field
The present invention relates to a brazing method.
Background
The carbon fiber reinforced carbon-based composite material (C/C composite material) has the advantages of both carbon fiber and graphite, and has the characteristics of smaller specific gravity, higher room temperature and high temperature strength, lower thermal expansion coefficient, better heat conduction performance, wear resistance, ablation resistance, excellent impact resistance and the like compared with the graphite. Due to its excellent characteristics, the C/C composite material has been used in key thermal protection systems of aerospace vehicles in various countries, parts of rocket engine throat liners, nozzles, heat exchangers and the like, and thermal protection layers in the nuclear energy field and the like. However, it is difficult to process the composite material into a complicated shape or a large-sized member, so that the C/C composite material is often connected. The niobium alloy has higher melting point, better thermal stability and relatively lower density in high-temperature resistant metal, and is a good alternative material for hot-end components. Therefore, the research on the reliable connection of the C/C composite material has important significance.
For joining of C/C composite materials, active brazing is currently more effective. However, the difference between the thermal physical properties of the solder alloy and the metal base material and the C/C composite material is large, which often causes large residual thermal stress in a soldered connection joint, and the residual thermal stress is also the largest factor restricting the improvement of the performance of the soldered joint of the C/C composite material at present. The internal structure of the material determines the performance, and the excessive residual thermal stress of the joint is relieved by regulating and controlling the structure of the brazing seam structure, so that the mechanical property of the joint is improved, which is a hot spot in the research of the welding joint of the carbon fiber reinforced carbon-based composite material at present.
Aiming at the problem of large residual stress of a C/C composite material soldered joint, two solutions are mainly provided at present. One method is to add an intermediate layer in a brazing seam, adjust the tissue structure of the brazing seam, improve the plasticity and toughness of the brazing seam and relieve the residual thermal stress of a welded joint in a plastic deformation mode; one method is to introduce a reinforcing phase with low expansion coefficient into a brazing seam, optimize the brazing seam performance, reduce the thermal expansion coefficient of a brazing seam area and achieve the purpose of relieving the residual stress of a joint.
However, the introduction of an intermediate layer, particularly a composite intermediate layer, into the brazing seam increases the difficulty of sample assembly and also tends to increase excessive interface layers in the brazing seam; on the other hand, the introduction of the intermediate layer in the brazing seam is generally implemented on the basis of the AgCuTi brazing filler metal, and the high-temperature performance of the obtained joint is poor. The addition of the reinforcing phase with a low coefficient of expansion is generally less, so that the difference of the reduced coefficients of thermal expansion is limited. One principle of the two methods is to increase the plasticity of the brazing seam structure and relieve the stress through plastic deformation; the other is to reduce the thermal mismatch between the base material and the brazing seam structure, thereby reducing the thermal stress.
Disclosure of Invention
The invention aims to solve the problems of poor room-temperature mechanical property and overlarge thermal stress of a brazed joint obtained by the existing brazing filler metal for connecting the C/C composite material and the niobium alloy and the brazing connection method, and provides a method for brazing the C/C composite material and the niobium alloy.
A method for brazing C/C composite materials and niobium alloys is completed according to the following steps:
firstly, polishing:
firstly, polishing the C/C composite material to obtain a polished C/C composite material;
secondly, polishing the niobium alloy until the surface is bright to obtain the polished niobium alloy;
secondly, ultrasonic cleaning:
firstly, immersing a polished C/C composite material and a polished niobium alloy into acetone, then ultrasonically cleaning, washing with absolute ethyl alcohol, and blow-drying to obtain a cleaned C/C composite material and a cleaned niobium alloy;
thirdly, assembling:
adhering a brazing sheet between the cleaned C/C composite material and the cleaned niobium alloy by using glue to assemble a C/C composite material/brazing sheet/niobium alloy structural member;
fourthly, brazing:
putting a C/C composite material/brazing filler metal sheet/niobium alloy structural part into a graphite mold, and then putting the graphite mold into a vacuum induction heating furnace;
secondly, vacuumizing the vacuum induction heating furnace, introducing inert gas into the furnace chamber to a normal pressure state, and vacuumizing again;
and thirdly, circulating the step IV for 2-4 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40-60 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1150-1275 ℃ at the heating rate of 20-30 ℃/min, preserving heat at 1150-1275 ℃, turning off the power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy.
The principle and the advantages of the invention are as follows:
in the high-temperature brazing filler metal, compared with expensive noble metal-based brazing filler metal, the metals of Co, Cr, Fe, Ni, Cu and Ti are relatively cheap, CoCrFeNiCu is a high-entropy alloy with very good plasticity, the internal structure of the CoCrFeNiCu is mainly fcc phase solid solution, Ti is the most common active element, and certain Ti is added into the brazing filler metal alloy, so that the wetting of the brazing filler metal and a C/C composite material base metal can be ensured; therefore, the invention designs and prepares the CoCrFeNiCuTi0.25The high-entropy alloy is used as brazing filler metal, can wet C/C composite materials, can generate brazing seam tissues with good plasticity, and relieves the stress of brazed joints through plastic deformation; the brazing joint has better thermal stability due to the thermal stability of the high-entropy alloy;
secondly, the joint structure obtained by using the method for brazing the C/C composite material and the niobium alloy is basically complete, the phases in the brazing seam are mainly fcc phase and bcc phase solid solutions, and the overall plasticity of the brazing seam is good. And because the brazing seam is mainly a high-entropy alloy solid solution phase and has a high melting point, the high-temperature stability of the brazing joint is presumed to be good; the highest shearing strength of the soldered joint can reach 47.44MPa, and the strength of the soldered joint is in the leading position in the same type of joints. The brazing seam structure of the brazing joint obtained by the method is mainly a solid solution phase, has good plasticity, and can better relieve the residual stress of the joint through plastic deformation.
The invention can obtain a method for brazing C/C composite materials and niobium alloys.
Drawings
FIG. 1 is a schematic representation of a process using CoCrFeNiCuTi0.25The joint structure obtained by brazing the C/C composite material and the niobium alloy by using the high-entropy alloy as brazing filler metal is shown in the figure, wherein a) is example 1, b) is example 2, and C) is example 3;
FIG. 2 is a schematic representation of a process using CoCrFeNiCuTi0.25The joint structure obtained by brazing a C/C composite material and a niobium alloy with a high-entropy alloy as a brazing material is shown in the figure, wherein a) is example 1, b) is example 4, C) is example 5, and d) is example 6.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
The first embodiment is as follows: the method for brazing the C/C composite material and the niobium alloy comprises the following steps:
firstly, polishing:
firstly, polishing the C/C composite material to obtain a polished C/C composite material;
secondly, polishing the niobium alloy until the surface is bright to obtain the polished niobium alloy;
secondly, ultrasonic cleaning:
firstly, immersing a polished C/C composite material and a polished niobium alloy into acetone, then ultrasonically cleaning, washing with absolute ethyl alcohol, and blow-drying to obtain a cleaned C/C composite material and a cleaned niobium alloy;
thirdly, assembling:
adhering a brazing sheet between the cleaned C/C composite material and the cleaned niobium alloy by using glue to assemble a C/C composite material/brazing sheet/niobium alloy structural member;
fourthly, brazing:
putting a C/C composite material/brazing filler metal sheet/niobium alloy structural part into a graphite mold, and then putting the graphite mold into a vacuum induction heating furnace;
secondly, vacuumizing the vacuum induction heating furnace, introducing inert gas into the furnace chamber to a normal pressure state, and vacuumizing again;
and thirdly, circulating the step IV for 2-4 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40-60 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1150-1275 ℃ at the heating rate of 20-30 ℃/min, preserving heat at 1150-1275 ℃, turning off the power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: and in the first step, 180#, 400#, 600# and 800# metallographic abrasive paper is used for polishing the C/C composite material in sequence to obtain the polished C/C composite material. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and step one, sequentially using No. 400, No. 600 and No. 1000 metallographic abrasive paper to polish the niobium alloy until the surface is bright, thereby obtaining the polished niobium alloy. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the ultrasonic cleaning time in the step two is 5min to 10min, and the ultrasonic cleaning power is 100W to 1500W. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the glue in the third step is 502 glue, and the brazing filler metal sheet is CoCrFeNiCuTi0.25The thickness of the high-entropy alloy is 400-800 mu m. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: and fourthly, keeping the temperature for 5-40 min. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the CoCrFeNiCuTi0.25The preparation method of the high-entropy alloy is completed according to the following steps:
firstly, weighing raw materials;
respectively weighing Co powder, Cr powder, Fe powder, Ni powder, Cu powder and Ti powder according to a molar ratio of 1:1:1:1: 0.25;
secondly, vacuum arc melting:
adding the Co, Cr, Fe, Ni, Cu and Ti powder weighed in the step one into a vacuum arc melting furnace for arc melting to obtain CoCrFeNiCuTi0.25A high temperature brazing filler metal;
the current of the electric arc melting in the step two is 180-220A, the time of each melting is 30-50 s, and the melting times are 3-5. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the current of the arc melting in the second step is 200A, the time of each melting is 40s, and the melting times are 5 times. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and step IV, circulating the step IV for 2-4 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of argon, heating the vacuum induction heating furnace to 1175 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving the heat at 1175 ℃, turning off the power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: and step four, circulating the step four, namely 2-4 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of argon, heating the vacuum induction heating furnace to 1200-1250 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving heat at the temperature of 1200-1250 ℃, turning off a power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps are the same as those in the first to ninth embodiments.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Example (b): CoCrFeNiCuTi0.25The preparation method of the high-entropy alloy is completed according to the following steps:
firstly, weighing raw materials;
respectively weighing Co powder, Cr powder, Fe powder, Ni powder, Cu powder and Ti powder according to a molar ratio of 1:1:1:1: 0.25;
secondly, vacuum arc melting:
adding the Co, Cr, Fe, Ni, Cu and Ti powder weighed in the step one into a vacuum arc melting furnace for arc melting to obtain CoCrFeNiCuTi0.25A high temperature brazing filler metal;
the current of the arc melting in the second step is 200A, the time of each melting is 40s, and the melting times are 5 times.
Example 1: a method for brazing C/C composite materials and niobium alloys is completed according to the following steps:
firstly, polishing:
firstly, grinding the C/C composite material by using 180#, 400#, 600# and 800# metallographic abrasive paper in sequence to obtain a ground C/C composite material;
secondly, sequentially using 400#, 600# and 1000# metallographic abrasive paper to polish the niobium alloy until the surface is bright, so as to obtain the polished niobium alloy;
secondly, ultrasonic cleaning:
firstly, immersing a polished C/C composite material and a polished C/C composite material into acetone, then ultrasonically cleaning, washing with absolute ethyl alcohol, and blow-drying to obtain a cleaned C/C composite material and a cleaned niobium alloy;
the ultrasonic cleaning time in the step two is 10min, and the ultrasonic cleaning power is 1000W;
thirdly, cementing a brazing sheet between the cleaned C/C composite material and the cleaned niobium alloy by using glue to assemble a C/C composite material/brazing sheet/niobium alloy structural member;
the glue in the third step is 502 glue, and the brazing filler metal sheet is CoCrFeNiCuTi prepared in the example0.25High-entropy alloy with the thickness of 600 mu m;
fourthly, brazing:
putting a C/C composite material/brazing filler metal sheet/niobium alloy structural part into a graphite mold, and then putting the graphite mold into a vacuum induction heating furnace;
secondly, vacuumizing the vacuum induction heating furnace, introducing inert gas into the furnace chamber to a normal pressure state, and vacuumizing again;
and thirdly, circulating the step IV for 3 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1175 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving the heat for 10min at the temperature of 1175 ℃, turning off the power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to the room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy.
The C/C composite material and the niobium alloy obtained in example 1 after brazing had a brazed joint shear strength of 47.44 MPa.
Example 2: the present embodiment is different from embodiment 1 in that: and step four, circulating the step four and the step three for 3 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1200 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving the heat for 10min at 1200 ℃, turning off a power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps and parameters were the same as in example 1.
The shear strength of the brazed joint between the C/C composite material and the niobium alloy obtained in example 2 was 33.4 MPa.
Example 3: the present embodiment is different from embodiment 1 in that: and step four, circulating the step four and the step three for 3 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1250 ℃ at the heating rate of 20 ℃/min, preserving the heat for 10min at 1250 ℃, turning off a power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps and parameters were the same as in example 1.
The shear strength of the brazed joint between the C/C composite material and the niobium alloy obtained in example 3 was 17.1 MPa.
Example 4: the present embodiment is different from embodiment 1 in that: and fourthly, circulating the step IV for 3 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1175 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving the heat for 20min at the temperature of 1175 ℃, turning off a power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to the room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps and parameters were the same as in example 1.
The shear strength of the brazed joint between the C/C composite material and the niobium alloy obtained in example 4 was 40.5 MPa.
Example 5: the present embodiment is different from embodiment 1 in that: and fourthly, circulating the step IV for 3 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1175 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving the heat for 30min at the temperature of 1175 ℃, turning off a power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to the room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps and parameters were the same as in example 1.
The shear strength of the brazed joint between the C/C composite material and the niobium alloy obtained in example 5 was 40.4 MPa.
Example 6: the present embodiment is different from embodiment 1 in that: and fourthly, circulating the step IV for 3 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1175 ℃ from 1000 ℃ at the heating rate of 20 ℃/min, preserving the heat for 40min at the temperature of 1175 ℃, turning off a power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to the room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy. The other steps and parameters were the same as in example 1.
The shear strength of the brazed joint between the C/C composite material and the niobium alloy obtained in example 6 was 35.2 MPa.
FIG. 1 is a schematic representation of a process using CoCrFeNiCuTi0.25The joint structure obtained by brazing the C/C composite material and the niobium alloy by using the high-entropy alloy as brazing filler metal is shown in the figure, wherein a) is example 1, b) is example 2, and C) is example 3;
FIG. 2 is a schematic representation of a process using CoCrFeNiCuTi0.25The joint structure obtained by brazing a C/C composite material and a niobium alloy with a high-entropy alloy as a brazing material is shown in the figure, wherein a) is example 1, b) is example 4, C) is example 5, and d) is example 6.
As can be seen from FIGS. 1 and 2, the joint structure is basically complete, the solid solution of fcc phase and bcc phase is mainly in the brazing seam, and the overall plasticity of the brazing seam is better. And the brazing seam is mainly a high-entropy alloy solid solution phase and has a high melting point, so that the high-temperature stability of the brazing joint is presumed to be good.
The shear strength of the soldered joint is better when the temperature is kept for 10-30min at 1175 ℃, the highest 47.44MPa is reached when the temperature is kept for 10min (example 1), and the strength is still kept above 40MPa when the temperature is kept for 20min and 30 min.

Claims (10)

1. A method for brazing C/C composite materials and niobium alloys is characterized in that the method for brazing C/C composite materials and niobium alloys is completed according to the following steps:
firstly, polishing:
firstly, polishing the C/C composite material to obtain a polished C/C composite material;
secondly, polishing the niobium alloy until the surface is bright to obtain the polished niobium alloy;
secondly, ultrasonic cleaning:
firstly, immersing a polished C/C composite material and a polished niobium alloy into acetone, then ultrasonically cleaning, washing with absolute ethyl alcohol, and blow-drying to obtain a cleaned C/C composite material and a cleaned niobium alloy;
thirdly, assembling:
adhering a brazing sheet between the cleaned C/C composite material and the cleaned niobium alloy by using glue to assemble a C/C composite material/brazing sheet/niobium alloy structural member;
fourthly, brazing:
putting a C/C composite material/brazing filler metal sheet/niobium alloy structural part into a graphite mold, and then putting the graphite mold into a vacuum induction heating furnace;
secondly, vacuumizing the vacuum induction heating furnace, introducing inert gas into the furnace chamber to a normal pressure state, and vacuumizing again;
and thirdly, circulating the step IV for 2-4 times, introducing argon, heating the vacuum induction heating furnace to 1000 ℃ at the heating rate of 40-60 ℃/min under the protection of the argon, heating the vacuum induction heating furnace to 1150-1275 ℃ at the heating rate of 20-30 ℃/min, preserving heat at 1150-1275 ℃, turning off the power supply of the vacuum induction heating furnace after the protection is finished, and cooling the vacuum induction heating furnace to room temperature along with the furnace to obtain the brazed C/C composite material and niobium alloy.
2. The method for brazing the C/C composite material and the niobium alloy as claimed in claim 1, wherein in the step one (r), 180#, 400#, 600# and 800# metallographic sandpaper is used for grinding the C/C composite material in sequence to obtain the ground C/C composite material.
3. The method for brazing the C/C composite material and the niobium alloy as claimed in claim 1, wherein in the first step, the niobium alloy is polished to be bright surface by using 400#, 600# and 1000# metallographic abrasive paper in sequence, so as to obtain polished niobium alloy.
4. The method for brazing C/C composite material and niobium alloy as claimed in claim 1, wherein said ultrasonic cleaning in step two is performed for a time period of 5min to 10min at a power of 100W to 1500W.
5. The method of claim 1, wherein said glue in step three is 502 glue, and said brazing sheet is CoCrFeNiCuTi0.25The thickness of the high-entropy alloy is 400-800 mu m.
6. The method for brazing a C/C composite material and a niobium alloy as claimed in claim 1 or 5, wherein said holding time in step IV is 5-40 min.
7. The method of brazing C/C composite and niobium alloy of claim 6, wherein said CoCrFeNiCuTi0.25The preparation method of the high-entropy alloy is completed according to the following steps:
firstly, weighing raw materials;
respectively weighing Co powder, Cr powder, Fe powder, Ni powder, Cu powder and Ti powder according to a molar ratio of 1:1:1:1: 0.25;
secondly, vacuum arc melting:
adding the Co, Cr, Fe, Ni, Cu and Ti powder weighed in the step one into a vacuum arc melting furnace for arc melting to obtain CoCrFeNiCuTi0.25A high temperature brazing filler metal;
the current of the electric arc melting in the step two is 180-220A, the time of each melting is 30-50 s, and the melting times are 3-5.
8. The method of claim 7, wherein the arc melting in step two is performed at a current of 200A for 40s for 5 times.
9. The method of claim 1, wherein the step four is repeated 2-4 times, argon is introduced, the vacuum induction heating furnace is heated to 1000 ℃ at a heating rate of 40 ℃/min under the protection of argon, the temperature is raised from 1000 ℃ to 1175 ℃ at a heating rate of 20 ℃/min, the temperature is maintained at 1175 ℃, the power supply of the vacuum induction heating furnace is turned off after the protection is finished, and the furnace is cooled to room temperature, so that the brazed C/C composite material and niobium alloy are obtained.
10. The method of claim 1, wherein the step four is repeated 2 to 4 times, argon is introduced, the temperature of the vacuum induction heating furnace is raised to 1000 ℃ at a temperature raising rate of 40 ℃/min under the protection of argon, the temperature is raised from 1000 ℃ to 1200 ℃ to 1250 ℃ at a temperature raising rate of 20 ℃/min, the temperature is maintained at 1200 ℃ to 1250 ℃, the power supply of the vacuum induction heating furnace is turned off after the protection is finished, and the furnace is cooled to room temperature, thereby obtaining the brazed C/C composite material and niobium alloy.
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