CN114749743B - High-temperature connection method for soldering C/C composite material and Ni-based alloy by adopting pure Cu - Google Patents

High-temperature connection method for soldering C/C composite material and Ni-based alloy by adopting pure Cu Download PDF

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CN114749743B
CN114749743B CN202210439214.3A CN202210439214A CN114749743B CN 114749743 B CN114749743 B CN 114749743B CN 202210439214 A CN202210439214 A CN 202210439214A CN 114749743 B CN114749743 B CN 114749743B
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composite material
based alloy
brazing
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temperature
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CN114749743A (en
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曹健
郭夏君
司晓庆
薛鹏鹏
赵文迪
李淳
冯吉才
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Harbin Institute of Technology
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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
    • B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
    • 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
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • 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
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/302—Cu as the principal 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)
  • Ceramic Products (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a high-temperature connection method for soldering a C/C composite material and a Ni-based alloy by adopting pure Cu, which aims to solve the problem of poor high-temperature resistance of a solder used for soldering a joint of the C/C composite material and the Ni-based alloy. The high-temperature connection method comprises the following steps: 1. polishing the surface to be welded of the C/C composite material; 2. coating Sn-Cr metal paste on the surface to be welded of the pretreated C/C composite material, heating at 800-1050 ℃, and then placing the modified C/C composite material into a nitric acid solution to obtain a C/C composite material with the modified Cr-C coating surface; 3. and placing the Cu foil between the C/C composite material and the surface to be welded of the Ni-based alloy, and placing the Cu foil in a vacuum heating furnace for braze welding connection. According to the invention, pure Cu with high plasticity and excellent high temperature resistance is adopted as a brazing filler metal to realize the brazing of the C/C composite material and the Ni-based alloy, the obtained joint forms tight interface connection, and the joint has excellent room temperature and high temperature mechanical properties.

Description

High-temperature connection method for soldering C/C composite material and Ni-based alloy by adopting pure Cu
Technical Field
The invention belongs to the field of dissimilar material connection, and particularly relates to a high-temperature connection method for a pure Cu brazing C/C composite material and Ni-based alloy.
Background
The C/C composite is an excellent carbon fiber reinforced carbon-based composite with a low density (-1.8 g/cm) 3 ) Low thermal expansion coefficient (-1.5X10) -6 K -1 ) High temperature resistant>2000 deg.c), high specific strength and specific modulus, high heat and electric conductivity, excellent heat shock resistance, corrosion resistance, etc. Therefore, it is increasingly used in the aerospace, nuclear power and automotive industries. However, the C/C composite material has a complicated manufacturing process and high processing cost, and is difficult to manufacture structural members with large size and complex shape, which greatly limits the practical application thereof in engineering structures. This problem can be effectively solved by connecting it with a metal having good workability. The Ni-based alloy is a high-temperature structural material widely applied in the fields of aerospace, nuclear energy and the like at present due to the good processability, excellent high temperature resistance, corrosion resistance, creep resistance, high strength and the like. The C/C composite material is connected with the Ni-based alloy, so that on one hand, the structural weight can be remarkably reduced, the working efficiency of parts such as an engine is improved, on the other hand, the excellent performances of the two materials can be fully combined, the manufacturing cost is reduced, and the two materials are promoted to be widely applied as high-temperature structural materials.
At present, brazing is an effective method for achieving the connection of the C/C composite material and the Ni-based alloy. However, there are a number of difficulties with the brazed connection of the two. Firstly, the C/C composite material is combined by covalent bonds, the chemical property is stable, the melting is difficult, and metals such as Ni and the like are difficult to wet the surface of the C/C composite material. Next, the C/C composite material has a low coefficient of thermal expansion, which is approximately that of Ni-based alloys (about 14X10) -6 K -1 ) This large difference in thermal expansion coefficients can result in significant residual stresses in the two post-weld joints. Especially, the C/C composite material is a brittle material, while the Ni-based alloy often contains a large amount of strengthening phases, the plastic deformation capability of the base metal at two sides is poor, and the residual stress in the joint is difficult to release. As a result, residual stresses in the joint will induce cracks at the interface, thereby losing the jointThe effect is achieved. Therefore, proper brazing filler metal is selected to relieve the residual stress of the joint. At present, researchers have developed solders with higher plasticity, such as AgCuTi, agTi and the like, to realize the connection of the C/C composite material and the Ni-based alloy. However, these solders are not sufficiently resistant to high temperatures, and often are used at temperatures not exceeding 500 ℃. However, the high temperature brazing filler metals such as NiTi, cuTi, coTi, which are commonly used at present, have poor plasticity due to the fact that the brazing filler metals contain a large amount of brittle compounds, so that reliable connection between the C/C composite material and the Ni-based alloy is difficult to realize. In addition, research also shows that the commonly used high-temperature brazing filler metals such as NiCrSiB and the like are easy to generate cracks at joint interfaces when the C/C composite material and the Ni-based alloy are brazed due to insufficient plasticity, and the reliability of the joint is reduced. Therefore, there is a great need to develop a new brazing method to achieve reliable interface connection of the two while providing a joint with excellent high temperature resistance.
Disclosure of Invention
The invention aims to solve the problems of poor high temperature resistance and low plasticity of the brazing filler metal used for the current C/C composite material and Ni-based alloy brazing joint, and provides a high temperature connection method for brazing the C/C composite material and the Ni-based alloy by adopting pure Cu.
The invention adopts a high-temperature connection method of pure Cu brazing C/C composite material and Ni-based alloy, and is realized according to the following steps:
polishing the surface to be welded of the C/C composite material by adopting SiC abrasive paper, and cleaning and drying to obtain a pretreated C/C composite material;
preparing a Cr-C coating on the surface of the C/C composite material, wherein the specific steps are as follows:
a. mechanically ball milling Cr powder with the mass percentage of 2.5-15% and Sn powder with the mass percentage of 97.5-85%, uniformly mixing to obtain Sn-Cr metal powder, and then adding a binder and uniformly mixing to obtain Sn-Cr metal paste;
b. coating Sn-Cr metal paste on the surface to be welded of the pretreated C/C composite material, heating the surface to be welded in a vacuum heating furnace at 800-1050 ℃, and cooling the surface to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid solution to remove Sn by corrosion, and performing ultrasonic cleaning to obtain a Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the modified Cr-C coating surface and the Ni-based alloy, wherein the specific steps are as follows:
d. polishing the surfaces to be welded of the Ni-based alloy and the Cu foil by adopting SiC abrasive paper, and cleaning and drying to obtain the cleaned Ni-based alloy and Cu foil;
e. placing Cu foil between the C/C composite material modified on the surface of the Cr-C coating and the surface to be welded of the Ni-based alloy to form a sandwich structure, placing the sandwich structure into a vacuum heating furnace, and carrying out brazing connection at the temperature of 1100-1180 ℃;
f. and after the heat preservation is finished, cooling, taking out the weldment, and completing the high-temperature brazing connection of the C/C composite material and the Ni-based alloy.
The high-temperature connection method adopting the pure Cu brazing C/C composite material and the Ni-based alloy mainly comprises the following beneficial effects:
1. the Sn-Cr alloy reacts with the C/C composite material and combines an acid corrosion method to prepare a uniform and compact Cr-C modified layer on the surface of the C/C composite material at a lower temperature, so that the pure Cu is converted into the Cr-C modified C/C composite material surface from a completely non-wetting state on the surface of the original C/C composite material to be well wetted;
2. the pure Cu with high plasticity and excellent high temperature resistance is adopted as the brazing filler metal to realize the brazing of the C/C composite material and the Ni-based alloy, the obtained joint forms tight interface connection, and the joint has excellent room temperature and high temperature mechanical properties;
3. in the obtained braze welding joint, the braze welding joint mainly consists of Cu solid solution, a brittle compound is not formed, the joint tissue structure is simple, and the property is stable;
4. the solder has the advantages of wide sources of components, low cost, simple and convenient operation and convenient industrial application.
Drawings
FIG. 1 is an optical photograph of the wet state of pure Cu in the original C/C composite (left panel) and the C/C composite modified by surface Cr-C (right panel) in the examples;
FIG. 2 is a scanning electron micrograph of a micro joint of a DD3 joint of a single crystal alloy and a Ni-based alloy using a pure Cu braze surface modified C/C composite in the example;
FIG. 3 is a scanning electron microscope photograph of a microstructure of a C/C interface in a DD3 joint of a single crystal alloy and a Ni-based alloy by adopting pure Cu to braze the surface modified C/C composite material in the embodiment;
FIG. 4 is a scanning electron microscope photograph of DD3 interface microstructure in DD3 joints of single crystal alloys and Ni-based alloys using pure Cu braze surface modified C/C composites in the examples.
Detailed Description
The first embodiment is as follows: the high-temperature connection method of the pure Cu brazing C/C composite material and the Ni-based alloy is implemented according to the following steps:
polishing the surface to be welded of the C/C composite material by adopting SiC abrasive paper, and cleaning and drying to obtain a pretreated C/C composite material;
preparing a Cr-C coating on the surface of the C/C composite material, wherein the specific steps are as follows:
a. mechanically ball milling Cr powder with the mass percentage of 2.5-15% and Sn powder with the mass percentage of 97.5-85%, uniformly mixing to obtain Sn-Cr metal powder, and then adding a binder and uniformly mixing to obtain Sn-Cr metal paste;
b. coating Sn-Cr metal paste on the surface to be welded of the pretreated C/C composite material, heating the surface to be welded in a vacuum heating furnace at 800-1050 ℃, and cooling the surface to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid solution to remove Sn by corrosion, and performing ultrasonic cleaning to obtain a Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the modified Cr-C coating surface and the Ni-based alloy, wherein the specific steps are as follows:
d. polishing the surfaces to be welded of the Ni-based alloy and the Cu foil by adopting SiC abrasive paper, and cleaning and drying to obtain the cleaned Ni-based alloy and Cu foil;
e. placing Cu foil between the C/C composite material modified on the surface of the Cr-C coating and the surface to be welded of the Ni-based alloy to form a sandwich structure, placing the sandwich structure into a vacuum heating furnace, and carrying out brazing connection at the temperature of 1100-1180 ℃;
f. and after the heat preservation is finished, cooling, taking out the weldment, and completing the high-temperature brazing connection of the C/C composite material and the Ni-based alloy.
According to the embodiment, the C/C composite material is subjected to surface modification, and then pure Cu with high plasticity and excellent high temperature resistance is used as a brazing filler metal for brazing, so that the joint can form reliable interface connection, and excellent high temperature mechanical property is obtained.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that the binder in the step a is an aqueous carboxymethyl cellulose solution.
And a third specific embodiment: the difference between the present embodiment and the first or second embodiment is that the heating treatment time in the step b is 10 to 60 minutes.
The specific embodiment IV is as follows: this embodiment differs from one to three embodiments in that the volume fraction of the nitric acid solution in step c is 10% to 30%.
Fifth embodiment: the present embodiment differs from the first to fourth embodiments in that the Cu foil in step d has a thickness of 0.05 to 0.5mm.
Specific embodiment six: this embodiment differs from one to five of the embodiments in that the Ni-based alloy in step d is a single-crystal Ni-based superalloy, a GH superalloy, an Inconel alloy, or a Monel alloy.
Seventh embodiment: the present embodiment differs from the first to sixth embodiments in that the vacuum degree in the vacuum heating furnace in step e is lower than 3×10 -3 Pa。
Eighth embodiment: the difference between the embodiment and one of the first to seventh embodiments is that the temperature rising rate is controlled to be 5-15 ℃/min to rise to the brazing temperature in the step e.
Detailed description nine: the difference between the present embodiment and the eighth embodiment is that the heat preservation time of the braze joint in the step e is 10 to 60 minutes.
Detailed description ten: the difference between the embodiment and one of the first to ninth embodiments is that the cooling in the step f is to cool the weldment to 380-420 ℃ at a cooling rate of 5 ℃/min, and then cool the weldment to room temperature along with the furnace.
Examples: the embodiment adopts a high-temperature connection method of pure Cu brazing C/C composite material and Ni-based alloy, and is realized according to the following steps:
firstly, polishing the surface to be welded of the C/C composite material by using 1200# SiC sand paper, putting the surface to be welded into absolute ethyl alcohol, ultrasonically cleaning for 3 times, 5 minutes each time, and drying to obtain a pretreated C/C composite material;
preparing a Cr-C coating on the surface of the C/C composite material, wherein the specific steps are as follows:
a. mechanically ball milling Cr powder with the mass percentage of 10% and Sn powder with the mass percentage of 90%, uniformly mixing to obtain Sn-Cr metal powder, and then adding a binder and uniformly mixing to obtain Sn-Cr metal paste;
b. coating Sn-Cr metal paste on the surface to be welded of the pretreated C/C composite material, heating the surface to be welded in a vacuum heating furnace at 800 ℃ for 30min, and cooling the surface to obtain a modified C/C composite material;
c. putting the modified C/C composite material into 30% nitric acid (water) solution for corrosion for 60min, removing Sn, and putting into absolute ethyl alcohol for ultrasonic cleaning to obtain the Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the modified Cr-C coating surface and the Ni-based alloy, wherein the specific steps are as follows:
d. sequentially polishing the surfaces to be welded of the Ni-based alloy by using 400# SiC abrasive paper, 800# SiC abrasive paper and 1200# SiC abrasive paper, polishing the two surfaces of the Cu foil by using 1200# SiC abrasive paper, placing the polished Ni-based alloy and Cu foil into absolute ethyl alcohol, ultrasonically cleaning for 3 times, 5 minutes each time, and drying to obtain the cleaned Ni-based alloy and Cu foil;
e. placing Cu foil between the C/C composite material modified on the surface of Cr-C coating and the surface to be welded of Ni-based alloy to form a sandwich structure, and placing into a vacuum heating furnace with vacuum degree lower than 3×10 -3 When Pa, a heating switch is started, the heating rate is controlled to be 15 ℃/min to 450 ℃, the heating rate is controlled to be 10 ℃/min to 800 ℃, and the heating rate is controlled to be 5 ℃/min to 1140 ℃, and the brazing connection is performed after the heating is performed for 30 min;
f. and after the heat preservation is finished, cooling the weldment to about 400 ℃ at a cooling rate of 5 ℃/min, then cooling to room temperature along with a furnace, taking out the test piece, and completing the high-temperature brazing connection of the C/C composite material and the Ni-based alloy.
In this example, a 10 mm. Times.10 mm. Times.3 mm C/C composite material and a 5mm. Times.5 mm. Times.3 mm DD3 alloy were joined by brazing with a pure Cu foil at 1140℃for 30 minutes. The test result shows that the room temperature shear strength of the braze welding joint of the C/C composite material and the Ni-based alloy can reach 30.3MPa, and the high temperature shear strength of 800 ℃ can reach 22.8MPa.
FIG. 1 is an optical photograph of pure Cu in a wet state of an original C/C composite material and a C/C composite material modified by Cr-C on the surface, and it can be seen that pure Cu does not wet on the surface of the original C/C composite material, but forms good wetting and spreading on the surface of the C/C composite material modified by Cr-C.
FIG. 2 is a scanning electron micrograph of a micro joint of a DD3 joint of a single crystal alloy based on Ni with a pure Cu braze surface modified C/C composite, showing that the joint forms a tight joint, the braze joint being composed principally of a Cu solid solution, wherein no brittle compound is formed.
FIG. 3 is a scanning electron microscope photograph of a microstructure of a C/C interface in a DD3 joint of a single crystal alloy and a Ni-based alloy by adopting pure Cu to braze the surface modified C/C composite material, and the defects of cracks, holes and the like of the interface between the brazing filler metal and the C/C composite material can be seen.
FIG. 4 is a scanning electron microscope photograph of DD3 interface microstructure in a DD3 joint of a single crystal alloy and a Ni-based alloy by adopting pure Cu brazing surface modified C/C composite material, and can be used for showing that the brazing filler metal is well connected with the DD3 alloy interface, so that a layer of obvious solid solution and diffusion layer is formed.

Claims (10)

1. The high-temperature connection method for soldering the C/C composite material and the Ni-based alloy by adopting pure Cu is characterized in that the high-temperature connection method for soldering the C/C composite material and the Ni-based alloy is realized according to the following steps:
polishing the surface to be welded of the C/C composite material by adopting SiC abrasive paper, and cleaning and drying to obtain a pretreated C/C composite material;
preparing a Cr-C coating on the surface of the C/C composite material, wherein the specific steps are as follows:
a. mechanically ball milling Cr powder with the mass percentage of 2.5-15% and Sn powder with the mass percentage of 97.5-85%, uniformly mixing to obtain Sn-Cr metal powder, and then adding a binder and uniformly mixing to obtain Sn-Cr metal paste;
b. coating Sn-Cr metal paste on the surface to be welded of the pretreated C/C composite material, heating the surface to be welded in a vacuum heating furnace at 800-1050 ℃, and cooling the surface to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid solution to remove Sn by corrosion, and performing ultrasonic cleaning to obtain a Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the modified Cr-C coating surface and the Ni-based alloy, wherein the specific steps are as follows:
d. polishing the surfaces to be welded of the Ni-based alloy and the Cu foil by adopting SiC abrasive paper, and cleaning and drying to obtain the cleaned Ni-based alloy and Cu foil;
e. placing Cu foil between the C/C composite material modified on the surface of the Cr-C coating and the surface to be welded of the Ni-based alloy, placing the Cu foil in a vacuum heating furnace, and carrying out brazing connection at the temperature of 1100-1180 ℃;
f. and after the heat preservation is finished, cooling, taking out the weldment, and completing the high-temperature brazing connection of the C/C composite material and the Ni-based alloy.
2. The method for high temperature joining of a pure Cu braze C/C composite to a Ni-based alloy according to claim 1, characterized in that the binder in step a is an aqueous carboxymethyl cellulose solution.
3. The high temperature joining method using pure Cu brazing C/C composite material and Ni-based alloy according to claim 1, characterized in that the heating treatment time in step b is 10 to 60min.
4. The high temperature joining method using pure Cu brazing C/C composite material with Ni-based alloy according to claim 1, characterized in that the volume fraction of the nitric acid solution in step C is 10% to 30%.
5. The high temperature joining method using pure Cu brazing C/C composite material with Ni-based alloy as claimed in claim 1, characterized in that the Cu foil in step d has a thickness of 0.05-0.5 mm.
6. The high temperature joining method using pure Cu brazing C/C composite material with Ni-based alloy according to claim 1, characterized in that in step d the Ni-based alloy is a single crystal Ni-based superalloy, a GH superalloy, an Inconel alloy or a Monel alloy.
7. The high temperature joining method using pure Cu brazing C/C composite material and Ni-based alloy according to claim 1, wherein the vacuum degree in the vacuum heating furnace in step e is lower than 3X 10 -3 Pa。
8. The high temperature connection method using pure Cu brazing C/C composite material and Ni-based alloy according to claim 1, characterized in that in step e the temperature rising rate is controlled to be 5-15 ℃/min to rise to the brazing temperature.
9. The high temperature joining method using pure Cu brazing C/C composite material and Ni-based alloy according to claim 8, characterized in that the heat preservation time of the brazing joining in step e is 10-60 min.
10. The high temperature joining method using pure Cu brazing C/C composite material and Ni-based alloy according to claim 1, characterized in that the cooling in step f is cooling the weldment to 380-420 ℃ at a cooling rate of 5 ℃/min, followed by furnace cooling to room temperature.
CN202210439214.3A 2022-04-25 2022-04-25 High-temperature connection method for soldering C/C composite material and Ni-based alloy by adopting pure Cu Active CN114749743B (en)

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