CN114749743A - High-temperature connection method for brazing C/C composite material and Ni-based alloy by adopting pure Cu - Google Patents

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

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CN114749743A
CN114749743A CN202210439214.3A CN202210439214A CN114749743A CN 114749743 A CN114749743 A CN 114749743A CN 202210439214 A CN202210439214 A CN 202210439214A CN 114749743 A CN114749743 A CN 114749743A
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composite material
brazing
based alloy
temperature
pure
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CN114749743B (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)
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Abstract

The invention discloses a high-temperature connection method for brazing a C/C composite material and a Ni-based alloy by adopting pure Cu, and aims to solve the problem of poor high-temperature resistance of brazing filler metal used for brazing joints of the C/C composite material and the Ni-based alloy. The high-temperature connection method comprises the following steps: firstly, grinding the surface to be welded of the C/C composite material; secondly, coating Sn-Cr metal paste on the surface to be welded of the pretreated C/C composite material, heating at 800-1050 ℃, and then putting the modified C/C composite material into a nitric acid solution to obtain the Cr-C coating surface modified C/C composite material; and thirdly, placing the Cu foil between the surfaces to be welded of the C/C composite material and the Ni-based alloy, and placing the C/C composite material and the Ni-based alloy into a vacuum heating furnace for brazing connection. The invention adopts pure Cu with high plasticity and excellent high temperature resistance 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.

Description

High-temperature connection method for brazing 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 brazing a C/C composite material and a Ni-based alloy by adopting pure Cu.
Background
The C/C composite is an excellent carbon fiber reinforced carbon-based composite with low density (-1.8 g/cm)3) Low thermal expansion coefficient (-1.5X 10)-6K-1) High temperature resistance (C)>2000 ℃), high specific strength and specific modulus, high thermal conductivity and electrical conductivity, excellent thermal shock resistance and corrosion resistance, etc. Therefore, the composite material has increasingly wide application in the industries of aerospace, nuclear power, automobiles and the like. However, the C/C composite material has complicated manufacturing process, high processing cost and difficulty in manufacturing large-sized and complex-shaped structural members, which greatly limits the practical application thereof in engineering structures. The problem can be effectively solved by connecting the metal with good processing performance. 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 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 the structural weight can be obviously reduced, the working efficiency of components such as an engine and the like can be improved, 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.
Currently, brazing is an effective method for achieving the connection of C/C composite materials with Ni-based alloys. However, the braze joint between the two presents a number of difficulties. Firstly, the C/C composite material is combined by covalent bonds, the chemical property of the C/C composite material is stable, the C/C composite material is difficult to melt, and metals such as Ni are difficult to wet the surface of the C/C composite material. Secondly, the C/C composite material has a low coefficient of thermal expansion, which is about that of Ni-based alloy (14X 10)-6K-1) One tenth of this large difference in thermal expansion coefficient can result in significant residual stresses in the welded joint. Particularly, the C/C composite material is a brittle material, while the Ni-based alloy often contains a large amount of strengthening phases, the plasticity of parent metals on 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 causing the joint to fail. Therefore, it is crucial to select a suitable solder to relieve the residual stress of the joint. At present, researchers have developed brazing filler metals with high plasticity such as AgCuTi, AgTi and the like, and connection of the C/C composite material and the Ni-based alloy is achieved. However, these solders have insufficient high temperature resistance and are often used at temperatures not exceeding 500 ℃. However, the poor plasticity of the currently commonly used high-temperature solders, such as NiTi, CuTi, CoTi and the like, caused by the large amount of brittle compounds, is difficult to realize the reliable connection between the C/C composite material and the Ni-based alloy. In addition, research also shows that the common high-temperature brazing filler metal such as NiCrSiB is easy to generate cracks at the joint interface 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 strong need to develop a new brazing method to achieve reliable interface connection between the two, and simultaneously provide 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 brazing filler metal used for the existing C/C composite material and Ni-based alloy brazed 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:
step one, polishing the surface to be welded of the C/C composite material by using SiC sand paper, and cleaning and drying to obtain a pretreated C/C composite material;
step two, preparing a Cr-C coating on the surface of the C/C composite material, which comprises the following specific steps:
a. carrying out mechanical ball milling on 2.5-15% of Cr powder and 97.5-85% of Sn powder in percentage by mass, uniformly mixing to obtain Sn-Cr metal powder, 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 in a vacuum heating furnace at the temperature of 800-1050 ℃, and cooling to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid solution to corrode and remove Sn, and carrying out ultrasonic cleaning to obtain a Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the Cr-C coating surface modified and the Ni-based alloy, and specifically comprises the following steps:
d. polishing the surfaces to be welded of the Ni-based alloy and the Cu foil by using SiC sand paper, and cleaning and drying to obtain the cleaned Ni-based alloy and the cleaned Cu foil;
e. placing a Cu foil between the Cr-C coating surface modified C/C composite material and the to-be-welded surface 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 and taking out the weldment to finish 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 has the following beneficial effects:
1. the Sn-Cr alloy is adopted to react with the C/C composite material and an acid corrosion method is combined 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 complete non-wetting state of pure Cu on the surface of the original C/C composite material is changed into good wetting on the surface of the Cr-C modified C/C composite material;
2. pure Cu with high plasticity and excellent high temperature resistance is used as the brazing filler metal to realize 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 brazing joint, the brazing seam mainly consists of a Cu solid solution, no brittle compound is formed, and the joint has a simple structure and stable properties;
4. the solder has wide component sources, low cost, simple and convenient operation and convenient industrial application.
Drawings
FIG. 1 is an optical photograph of pure Cu in the wet state of an original C/C composite (left panel) and a surface Cr-C modified C/C composite (right panel) in the examples;
FIG. 2 is a scanning electron microscope photograph of a micro joint of a surface modified C/C composite material brazed with pure Cu and a Ni-based single crystal alloy DD3 joint in an example;
FIG. 3 is a scanning electron microscope photograph of the microstructure of the C/C interface in the joint of the surface modified C/C composite material brazed by pure Cu and the Ni-based single crystal alloy DD3 in the example;
FIG. 4 is a scanning electron microscope photograph of the DD3 interface microstructure in the joint of the surface modified C/C composite material brazed by pure Cu and the Ni-based single crystal alloy DD3 in the embodiment.
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:
step one, polishing the surface to be welded of the C/C composite material by using SiC abrasive paper, and cleaning and drying to obtain a pretreated C/C composite material;
step two, preparing a Cr-C coating on the surface of the C/C composite material, which comprises the following specific steps:
a. carrying out mechanical ball milling on 2.5-15% of Cr powder and 97.5-85% of Sn powder in percentage by mass, uniformly mixing to obtain Sn-Cr metal powder, 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 in a vacuum heating furnace at 800-1050 ℃, and cooling to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid solution to corrode and remove Sn, and carrying out ultrasonic cleaning to obtain a Cr-C coating surface modified C/C composite material;
thirdly, brazing the Cr-C coating surface modified C/C composite material and the Ni-based alloy, and specifically comprises the following steps:
d. polishing the surfaces to be welded of the Ni-based alloy and the Cu foil by using SiC sand paper, and cleaning and drying to obtain the cleaned Ni-based alloy and the cleaned Cu foil;
e. placing a Cu foil between the Cr-C coating surface modified C/C composite material and the to-be-welded surface 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 and taking out the weldment to finish 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 firstly, and then pure Cu with high plasticity and excellent high-temperature resistance is adopted as the brazing filler metal for brazing, so that the joint can form reliable interface connection, and excellent high-temperature mechanical properties are obtained.
The second embodiment is as follows: the difference between this embodiment and the first embodiment is that the binder in step a is an aqueous solution of carboxymethyl cellulose.
The third concrete implementation mode: the present embodiment is different from the first or second embodiment in that the heating time in step b is 10 to 60 min.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is that the volume fraction of the nitric acid solution in step c is 10% to 30%.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that the thickness of the Cu foil in step d is 0.05 to 0.5 mm.
The sixth specific implementation mode: the present embodiment is different from one of the first to fifth 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.
The seventh embodiment: this embodiment is different from the first to sixth embodiments in that the degree of vacuum in the vacuum heating furnace in the step e is less than 3X 10-3Pa。
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is that in step e, the temperature is raised to the brazing temperature at a rate of 5 to 15 ℃/min.
The specific implementation method nine: the difference between the embodiment and the eighth embodiment is that the heat preservation time of the braze welding connection in the step e is 10-60 min.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is that the temperature reduction in step f is to cool the weldment to 380-420 ℃ at a cooling rate of 5 ℃/min, and then to cool the weldment to room temperature along with the furnace.
Example (b): the embodiment adopts a high-temperature connection method of a pure Cu brazing C/C composite material and a Ni-based alloy, and is realized according to the following steps:
step one, polishing the surface to be welded of the C/C composite material by using 1200# SiC abrasive paper, putting the surface into absolute ethyl alcohol for ultrasonic cleaning for 3 times, wherein each time lasts for 5min, and drying the surface to obtain a pretreated C/C composite material;
step two, preparing a Cr-C coating on the surface of the C/C composite material, which comprises the following specific steps:
a. carrying out mechanical ball milling on 10 mass percent of Cr powder and 90 mass percent of Sn powder, uniformly mixing to obtain Sn-Cr metal powder, and then adding a binder to uniformly mix 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 for 30min at the temperature of 800 ℃ in a vacuum heating furnace, and cooling to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid (water) solution with the volume fraction of 30% to corrode for 60min, removing Sn, putting the C/C composite material into absolute ethyl alcohol to carry out ultrasonic cleaning, and obtaining the Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the Cr-C coating surface modified and the Ni-based alloy, and specifically comprises the following steps:
d. sequentially polishing the to-be-welded surfaces of the Ni-based alloy by using 400#, 800#, 1200# SiC abrasive paper, polishing the two surfaces of the Cu foil by using 1200# SiC abrasive paper, ultrasonically cleaning the polished Ni-based alloy and Cu foil in absolute ethyl alcohol for 3 times, 5min each time, and drying to obtain the cleaned Ni-based alloy and Cu foil;
e. placing a Cu foil between the Cr-C coating surface modified C/C composite material and the Ni-based alloy surface to be welded to form a sandwich structure, and placing the sandwich structure into a vacuum heating furnace, wherein the vacuum degree is lower than 3 multiplied by 10-3When Pa is needed, a heating switch is started, the heating rate is controlled to be 15 ℃/min to 450 ℃, 10 ℃/min to 800 ℃, 5 ℃/min to 1140 ℃, and the temperature is kept for 30min for braze welding connection;
f. and after the heat preservation is finished, cooling the weldment to about 400 ℃ at the cooling rate of 5 ℃/min, then cooling the weldment to room temperature along with the furnace, taking out the test piece, and finishing the high-temperature brazing connection of the C/C composite material and the Ni-based alloy.
In this example, pure Cu foil was used to braze a 10mm × 10mm × 3mm C/C composite material to a 5mm × 5mm × 3mm DD3 alloy at 1140 deg.C for 30 min. Test results show that the room-temperature shear strength of the soldered joint of the C/C composite material and the Ni-based alloy can reach 30.3MPa, and the high-temperature shear strength at 800 ℃ can reach 22.8 MPa.
FIG. 1 is an optical photograph of the wet state of pure Cu in the original C/C composite material and the C/C composite material with Cr-C modified surface, and it can be seen that pure Cu is not wet on the surface of the original C/C composite material, but forms good wet spreading on the C/C surface with Cr-C modified surface.
FIG. 2 is a scanning electron micrograph of a microscopic joint of a surface modified C/C composite material brazed with pure Cu and a Ni-based single crystal alloy DD3, and it can be seen that the joint forms a tight connection, and a brazing seam is mainly composed 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 joint of a pure Cu brazing surface modified C/C composite material and a Ni-based single crystal alloy DD3, and it can be seen that the interface connection between the brazing filler metal and the C/C composite material is good, and the interface has no defects such as cracks, holes and the like.
FIG. 4 is a scanning electron micrograph of a DD3 interface microstructure in a joint of a pure Cu brazing surface modified C/C composite material and a Ni-based single crystal alloy DD3, and it can be seen that the interface of the brazing filler metal and the DD3 alloy is well connected, and an obvious solid solution and diffusion layer is formed.

Claims (10)

1. The high-temperature connection method of the pure Cu brazing C/C composite material and the Ni-based alloy is characterized by being realized according to the following steps:
step one, polishing the surface to be welded of the C/C composite material by using SiC sand paper, and cleaning and drying to obtain a pretreated C/C composite material;
step two, preparing a Cr-C coating on the surface of the C/C composite material, which comprises the following specific steps:
a. carrying out mechanical ball milling on 2.5-15% of Cr powder and 97.5-85% of Sn powder in percentage by mass, uniformly mixing to obtain Sn-Cr metal powder, and then adding a binder to uniformly mix 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 in a vacuum heating furnace at the temperature of 800-1050 ℃, and cooling to obtain a modified C/C composite material;
c. putting the modified C/C composite material into a nitric acid solution to corrode and remove Sn, and ultrasonically cleaning to obtain a Cr-C coating surface modified C/C composite material;
step three, brazing the C/C composite material with the Cr-C coating surface modified and the Ni-based alloy, and specifically comprises the following steps:
d. polishing the surfaces to be welded of the Ni-based alloy and the Cu foil by using SiC sand paper, and cleaning and drying to obtain the cleaned Ni-based alloy and the cleaned Cu foil;
e. placing a Cu foil between the Cr-C coating surface modified C/C composite material and the to-be-welded surface of the Ni-based alloy, placing the C/C composite material and the Ni-based alloy 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 and taking out the weldment to finish the high-temperature brazing connection of the C/C composite material and the Ni-based alloy.
2. The high temperature joining method of pure Cu brazing C/C composite material with Ni base alloy according to claim 1, wherein the binder in step a is an aqueous solution of carboxymethyl cellulose.
3. The high-temperature connection method of pure Cu brazing C/C composite material and Ni-based alloy according to claim 1, wherein the heating treatment time in step b is 10-60 min.
4. The high temperature joining method of pure Cu brazing C/C composite material with Ni base alloy according to claim 1, wherein the volume fraction of the nitric acid solution in step C is 10% to 30%.
5. The high temperature joining method of pure Cu brazing C/C composite material and Ni based alloy according to claim 1, wherein the thickness of Cu foil in step d is 0.05-0.5 mm.
6. The high temperature joining method of pure Cu brazing C/C composite material with Ni based alloy according to claim 1, characterized in that Ni based alloy in step d is single crystal Ni based superalloy, GH superalloy, Inconel alloy or Monel alloy.
7. The method for joining a Ni-based alloy to a C/C composite material by brazing with pure Cu according to claim 1, wherein the degree of vacuum in the vacuum furnace is less than 3X 10 in step e-3Pa。
8. The high-temperature connection method for brazing the C/C composite material and the Ni-based alloy by using the pure Cu according to claim 1, wherein the temperature rise rate is controlled to be 5-15 ℃/min to the brazing temperature in the step e.
9. The high temperature joining method of pure Cu brazing C/C composite material and Ni based alloy according to claim 8, wherein the brazing joining in step e is performed with a holding time of 10-60 min.
10. The high-temperature connection method for brazing the C/C composite material and the Ni-based alloy by adopting the pure Cu as claimed in claim 1, wherein the temperature reduction in the step f is to cool the weldment to 380-420 ℃ at the temperature reduction rate of 5 ℃/min, and then the weldment is cooled to room temperature along with a furnace.
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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CN115121893A (en) * 2022-08-03 2022-09-30 哈尔滨工业大学 Method for brazing carbon-based material and nickel-based superalloy by adopting high-temperature CuPdW low-thermal expansion coefficient composite brazing filler metal
CN115121893B (en) * 2022-08-03 2024-03-19 哈尔滨工业大学 Method for brazing carbon-based material and nickel-based superalloy by adopting high-temperature CuPdW low-thermal expansion coefficient composite solder

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