CN112404631A - Method for soldering dissimilar materials with assistance of carbon nanotube sponge intermediate layer - Google Patents
Method for soldering dissimilar materials with assistance of carbon nanotube sponge intermediate layer Download PDFInfo
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- CN112404631A CN112404631A CN202011165414.1A CN202011165414A CN112404631A CN 112404631 A CN112404631 A CN 112404631A CN 202011165414 A CN202011165414 A CN 202011165414A CN 112404631 A CN112404631 A CN 112404631A
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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
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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
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
- B23K1/206—Cleaning
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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
- B23K3/00—Tools, devices, or special appurtenances for soldering, e.g. brazing, or unsoldering, not specially adapted for particular methods
- B23K3/08—Auxiliary devices therefor
- B23K3/085—Cooling, heat sink or heat shielding means
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Abstract
A method for soldering a dissimilar material with the aid of a carbon nanotube sponge intermediate layer relates to a method for soldering a dissimilar material. The problem of current metallic material and dissimilar material brazing joint low strength is solved in order to solve. The method comprises the following steps: mixing carbon nanotubes with a strong acid solution, ultrasonically cleaning, dispersing into deionized water, filtering, ultrasonically dispersing a filter cake into absolute ethyl alcohol, and centrifuging to obtain a supernatant; then pumping filtration and drying are carried out, and finally the dissimilar materials are brazed. Or mixing the carbon nano tube with a strong acid solution, carrying out ultrasonic cleaning, then dispersing the solution into deionized water, carrying out suction filtration, ultrasonically dispersing a filter cake into absolute ethyl alcohol, and centrifuging to obtain a supernatant; adding brazing filler metal powder into the supernatant, then performing suction filtration and drying, and finally brazing the dissimilar materials. The preparation method of the carbon nanotube sponge is simple and low in cost, can avoid the carbon nanotubes from agglomerating in the brazing process, is beneficial to regulating and controlling interface tissues, enhances the brazing seam performance, relieves the residual stress of joints and improves the joint strength. The invention is suitable for brazing dissimilar materials.
Description
Technical Field
The invention relates to a method for brazing dissimilar materials.
Background
The reliable connection of dissimilar materials is always the hot direction of research, the member prepared by multiple materials together can realize the advantage complementation of the materials, give full play to the respective advantageous performance, and better meet the production requirements of modern industry, especially the welding of metal materials and other dissimilar materials, other dissimilar materials such as ceramics, composite materials and the like, and the welding of metal materials and other dissimilar materials can selectively realize the performances such as high temperature resistance, wear resistance, corrosion resistance, wave transmission and filtration property, heat conductivity and the like of the member. However, due to the difference in physical and chemical properties of the to-be-welded parent metal, problems of poor wettability of the brazing filler metal, large residual stress of the joint, generation of a large amount of brittle compounds on the interface and the like can occur, so that reliable joints of dissimilar materials are difficult to realize, and particularly, when the active brazing filler metal containing elements such as Ti, Zr, Cr and the like and the alloy parent metal are used, the strength of the joints can be greatly reduced due to the formation of a large amount of agglomerated brittle compounds on the brazing interface.
The carbon nano tube is a one-dimensional nano material, has excellent thermal property and electrical property, and also has better stability and mechanical property, the average Young modulus of the carbon nano tube is up to 1.8TPa, and the density is only 1.7g/cm3The thermal expansion perpendicular to the axial direction is almost zero. Carbon nanotubes have been widely used in the fields of electronic devices, energy storage, high strength composites, and the like. The carbon nano tube and the brazing filler metal are mixed for braze welding connection, the linear expansion coefficient of a brazing seam is adjusted, the residual stress of a joint is relieved to a certain extent, however, in the adding process, the carbon nano tube has a serious agglomeration phenomenon, the adding content of the carbon nano tube is greatly limited, and the brittle compound generated in the interface is not effectively controlled.
Disclosure of Invention
The invention provides a method for assisting in brazing dissimilar materials by a carbon nanotube sponge intermediate layer, aiming at solving the problem of low strength of a brazed joint of the existing metal material and the dissimilar materials.
The method for soldering the dissimilar materials with the aid of the carbon nanotube sponge intermediate layer comprises the following steps:
step one, mixing carbon nanotube powder with a strong acid solution, and then carrying out ultrasonic cleaning at a constant temperature of 60 ℃ to obtain a suspension;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
step four, carrying out vacuum filtration on the supernatant obtained in the step three, stripping to obtain a filter cake, and finally drying to obtain the carbon nanotube sponge;
and fifthly, arranging brazing filler metal on two sides of the carbon nano tube sponge to form composite brazing filler metal, and performing brazing connection on the dissimilar materials by using the composite brazing filler metal.
The other method for soldering the dissimilar materials with the carbon nanotube sponge intermediate layer in an auxiliary manner is carried out according to the following steps:
step one, mixing carbon nanotube powder with a strong acid solution, and then carrying out ultrasonic cleaning at a constant temperature of 60 ℃ to obtain a suspension;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
step four, adding brazing filler metal powder into the supernatant obtained in the step three, uniformly mixing, then carrying out vacuum filtration, stripping to obtain a filter cake, and finally drying to obtain the carbon nano tube sponge composite brazing filler metal;
and fifthly, carrying out brazing connection on the dissimilar materials by using the carbon nanotube sponge composite brazing filler metal.
The principle and the beneficial effects of the invention are as follows:
1. the vacuum filtration method of the invention prepares the one-dimensional carbon nano tube into the carbon nano tube sponge with the three-dimensional structure, and the method has the advantages of simplicity, high efficiency and low cost; in the preparation process, the density, the thickness and the porosity of the carbon nanotube sponge intermediate layer can be regulated and controlled by changing the weight of the carbon nanotube, the suction filtration pressure and the acid washing time.
2. The three-dimensional net structure of the carbon nanotube sponge middle layer has a certain supporting effect, and can effectively avoid the carbon nanotubes from agglomerating in the brazing process.
3. The carbon nanotube sponge provided by the invention keeps the excellent mechanical properties and higher reactivity of the carbon nanotubes, the three-dimensional network structure has extremely high specific surface area, and the carbon nanotube sponge is used as an intermediate layer in the brazing of dissimilar materials, so that the problems of agglomeration, insufficient reaction and the like caused by directly adding the carbon nanotubes are effectively avoided, the interface structure is favorably regulated and controlled, the brazing seam performance is enhanced, the residual stress of a joint is relieved, and the joint strength is improved.
4. The carbon nanotube sponge intermediate layer is easy to react with active elements such as Ti, Zr, Cr and the like existing in brazing filler metal and dissolved from a base metal to a brazing seam preferentially in the brazing process, so that a large amount of intermetallic compounds generated due to excessive active elements in the brazing seam are avoided, the generation and agglomeration of brittle intermetallic compounds at a joint interface are inhibited, and the mechanical property of a brazed joint is ensured.
5. By using the carbon nano tube sponge as the middle layer and adopting the C/C composite material and the metal Nb which are connected by the TiCu brazing filler metal, the TiCu phase in the obtained joint interface is obviously reduced, and the TiCu is used4The phase and the Cu (s, s) phase are main, and the shearing strength of a soldered joint reaches 35-45 MPa.
6. The carbon nanotube sponge is used as an intermediate layer, the C/C composite material welded by the TiCu brazing filler metal and the TC4 titanium alloy are adopted, the dissolving distance of the TC4 titanium alloy base metal in an interface of the joint to a brazing seam is reduced to 40-50 mu m from 100-130 mu m, Ti (s, s) in the interface is obviously reduced, and the shearing strength of the joint reaches 30-50 MPa.
Drawings
FIG. 1 is a scanned photograph of a brazed joint obtained in example 1; FIG. 2 is a photograph of a scan of a brazed joint obtained in comparative example 1; as can be seen from the comparison of FIG. 1 and FIG. 2, after the carbon nanotube sponge intermediate layer is added, the TiCu phase in the joint interface is obviously reduced, the brittle compounds are hardly agglomerated, and the TiCu phase is used in the joint interface4The phases and the Cu (s, s) phase are dominant.
FIG. 3 is a scanned photograph of a brazed joint obtained in example 2; FIG. 4 is a photograph of a scan of a brazed joint obtained in comparative example 2; as can be seen from a comparison of fig. 3 and 4, Ti (s, s) dissolution was significantly reduced after the addition of the carbon nanotube sponge intermediate layer.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: the method for soldering the dissimilar materials with the aid of the carbon nanotube sponge intermediate layer in the embodiment comprises the following steps:
step one, mixing carbon nanotube powder with a strong acid solution, and then carrying out ultrasonic cleaning at a constant temperature of 60 ℃ to obtain a suspension;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
step four, carrying out vacuum filtration on the supernatant obtained in the step three, stripping to obtain a filter cake, and finally drying to obtain the carbon nanotube sponge;
and fifthly, arranging brazing filler metal on two sides of the carbon nano tube sponge to form composite brazing filler metal, and performing brazing connection on the dissimilar materials by using the composite brazing filler metal.
The principle and the beneficial effects of the implementation mode are as follows:
1. the vacuum filtration method of the embodiment prepares the one-dimensional carbon nano tube into the carbon nano tube sponge with the three-dimensional structure, and has the advantages of simplicity, high efficiency and low cost; in the preparation process, the density, the thickness and the porosity of the carbon nanotube sponge intermediate layer can be regulated and controlled by changing the weight of the carbon nanotube, the suction filtration pressure and the acid washing time.
2. The three-dimensional net structure of the carbon nanotube sponge middle layer has a certain supporting effect, and can effectively avoid the carbon nanotubes from agglomerating in the brazing process.
3. The carbon nanotube sponge of the embodiment keeps the excellent mechanical property and the higher reaction activity of the carbon nanotube, the three-dimensional network structure has extremely high specific surface area, and the carbon nanotube sponge is used as an intermediate layer in the brazing of dissimilar materials, so that the problems of agglomeration, insufficient reaction and the like caused by directly adding the carbon nanotube are effectively avoided, the interface structure is favorably regulated and controlled, the brazing seam performance is enhanced, the residual stress of a joint is relieved, and the joint strength is improved.
4. The carbon nanotube sponge intermediate layer of the embodiment is easy to react with active elements such as Ti, Zr, Cr and the like existing in brazing filler metal and dissolved from a base metal to a brazing seam preferentially in the brazing process, so that a large amount of intermetallic compounds generated due to excessive active elements in the brazing seam are avoided, the generation and agglomeration of brittle intermetallic compounds at a joint interface are inhibited, and the mechanical property of a brazed joint is ensured.
5. The carbon nanotube sponge of the embodiment is used as an intermediate layer, the C/C composite material and the metal Nb are connected by the TiCu brazing filler metal, the TiCu phase in the obtained joint interface is obviously reduced, and the TiCu phase is used4The phase and the Cu (s, s) phase are main, and the shearing strength of a soldered joint reaches 35-45 MPa.
6. By using the carbon nanotube sponge as the middle layer and adopting the C/C composite material welded by the TiCu brazing filler metal and the TC4 titanium alloy, the dissolving distance of the TC4 titanium alloy base metal in the joint interface to a brazing seam is reduced from 100-130 mu m to 40-50 mu m, the Ti (s, s) phase in the interface is obviously reduced, and the shear strength of the joint reaches 30-50 MPa.
7. The invention carries out suction filtration and drying on brazing filler metal powder and supernatant fluid together to obtain the carbon nano tube sponge composite brazing filler metal: the brazing filler metal powder is compounded with the carbon nanotube sponge in advance, so that the brazing filler metal can completely permeate the carbon nanotube sponge middle layer in the brazing process, and joint failure caused by incomplete reaction of the carbon nanotube sponge middle layer is avoided.
According to the embodiment, the carbon nano tubes can be purified by using the strong acid solution, and the method can ensure that the carbon nano tubes are not damaged, so that the strength of the carbon nano tube sponge is ensured.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one, the carbon nanotube powder is a single-walled carbon nanotube, a double-walled carbon nanotube or a multi-walled carbon nanotube.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: step one, the ratio of the mass of the carbon nanotube powder to the volume of the strong acid solution is (10-200) mg: (10-30) mL.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the strong acid in the step one is concentrated sulfuric acid, concentrated nitric acid or a mixed solution of the concentrated sulfuric acid and the concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is not less than 98%, the mass fraction of the concentrated nitric acid is not less than 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution of the concentrated sulfuric acid and the concentrated nitric acid is (2-5): 1.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: step one, the ultrasonic cleaning time is 0-12 h.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the filter cake washing process in the step two comprises the following steps: and after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into the filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7-8, wherein the vacuum filtration pressure in the filter cake washing process is 0.01-100 Pa.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and step two, the organic solvent adopted when the filter cake and the filter membrane are stripped is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol, n-hexane and the like.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and the vacuum filtration pressure of the mixed liquid in the step two is 0.01 Pa-100 Pa.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: the filter membrane is a water system filter membrane or an organic system filter membrane when the mixed solution is subjected to vacuum filtration, the diameter of the filter membrane is 20-80 mm, and the aperture of the filter membrane is 0.2-2 mu m.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and step three, the rotating speed during the centrifugal treatment is 3000-10000 r, and the centrifugal time is 10-20 min.
The concrete implementation mode eleven: the present embodiment differs from one of the first to tenth embodiments in that: and step four, stripping is carried out in an organic solvent, wherein the organic solvent is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol, n-hexane and the like.
The specific implementation mode twelve: this embodiment is different from one of the first to eleventh embodiments in that: fifthly, the dissimilar materials are a parent metal 1 and a parent metal 2; the parent metal 1 is C/C composite material, C/SiC composite material, graphite and Ti3SiC2、Ti3AlC2Or oxide ceramics, etc.; the base material 2 is Nb, TC4 titanium alloy, Ti600 titanium alloy, TiAl alloy, Ni-based high-temperature alloy, etc.
The specific implementation mode is thirteen: the present embodiment differs from the first to twelfth embodiments in that: and fifthly, the brazing filler metal is Cu-based brazing filler metal, Ag-based brazing filler metal, Ni-based brazing filler metal, Sn-based brazing filler metal, Ti-based brazing filler metal or Zr brazing filler metal and the like.
The specific implementation mode is fourteen: the method for soldering the dissimilar materials with the aid of the carbon nanotube sponge intermediate layer in the embodiment comprises the following steps:
step one, mixing carbon nanotube powder with a strong acid solution, and then carrying out ultrasonic cleaning at a constant temperature of 60 ℃ to obtain a suspension;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
step four, adding brazing filler metal powder into the supernatant obtained in the step three, uniformly mixing, then carrying out vacuum filtration, stripping to obtain a filter cake, and finally drying to obtain the carbon nano tube sponge composite brazing filler metal;
and fifthly, carrying out brazing connection on the dissimilar materials by using the carbon nanotube sponge composite brazing filler metal.
The principle and the beneficial effects of the implementation mode are as follows:
1. the vacuum filtration method of the embodiment prepares the one-dimensional carbon nano tube into the carbon nano tube sponge with the three-dimensional structure, and has the advantages of simplicity, high efficiency and low cost; in the preparation process, the density, the thickness and the porosity of the carbon nanotube sponge intermediate layer can be regulated and controlled by changing the weight of the carbon nanotube, the suction filtration pressure and the acid washing time.
2. The three-dimensional net structure of the carbon nanotube sponge middle layer has a certain supporting effect, and can effectively avoid the carbon nanotubes from agglomerating in the brazing process.
3. The carbon nanotube sponge of the embodiment keeps the excellent mechanical property and the higher reaction activity of the carbon nanotube, the three-dimensional network structure has extremely high specific surface area, and the carbon nanotube sponge is used as an intermediate layer in the brazing of dissimilar materials, so that the problems of agglomeration, insufficient reaction and the like caused by directly adding the carbon nanotube are effectively avoided, the interface structure is favorably regulated and controlled, the brazing seam performance is enhanced, the residual stress of a joint is relieved, and the joint strength is improved.
4. The carbon nanotube sponge intermediate layer of the embodiment is easy to react with active elements such as Ti, Zr, Cr and the like existing in brazing filler metal and dissolved from a base metal to a brazing seam preferentially in the brazing process, so that a large amount of intermetallic compounds generated due to excessive active elements in the brazing seam are avoided, the generation and agglomeration of brittle intermetallic compounds at a joint interface are inhibited, and the mechanical property of a brazed joint is ensured.
5. The carbon nanotube sponge is used as an intermediate layer, and the C/C composite material and the TiCu brazing filler metal are connectedMetal Nb with a significant reduction of TiCu phase at the resulting joint interface, with TiCu4The phase and the Cu (s, s) phase are main, and the shearing strength of a soldered joint reaches 35-45 MPa.
6. By using the carbon nanotube sponge as the middle layer and adopting the C/C composite material welded by the TiCu brazing filler metal and the TC4 titanium alloy, the dissolving distance of the TC4 titanium alloy base metal in the joint interface to a brazing seam is reduced from 100-130 mu m to 40-50 mu m, the Ti (s, s) phase in the interface is obviously reduced, and the shear strength of the joint reaches 30-50 MPa.
The embodiment can purify the carbon nano tube by using the strong acid solution, and the method can control the process to ensure that the carbon nano tube is not damaged, thereby ensuring the strength of the carbon nano tube sponge.
The brazing filler metal that can be used in the present embodiment includes Cu-based brazing filler metal, Ag-based brazing filler metal, Ni-based brazing filler metal, Sn-based brazing filler metal, and the like.
In the embodiment, the brazing filler metal powder and the supernatant are filtered and dried together to obtain the carbon nanotube sponge composite brazing filler metal: the brazing filler metal powder is compounded with the carbon nanotube sponge in advance, so that the brazing filler metal can completely permeate the carbon nanotube sponge middle layer in the brazing process, and joint failure caused by incomplete reaction of the carbon nanotube sponge middle layer is avoided.
The concrete implementation mode is fifteen: the present embodiment is different from the specific embodiment in the fourteenth aspect: step one, the carbon nanotube powder is a single-walled carbon nanotube, a double-walled carbon nanotube or a multi-walled carbon nanotube.
The specific implementation mode is sixteen: this embodiment is fourteen or fifteen different from the specific embodiment: the strong acid in the step one is concentrated sulfuric acid, concentrated nitric acid or a mixed solution of the concentrated sulfuric acid and the concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is not less than 98%, the mass fraction of the concentrated nitric acid is not less than 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution of the concentrated sulfuric acid and the concentrated nitric acid is (2-5): 1.
Seventeenth embodiment: this embodiment is different from the specific embodiment in one of fourteen to sixteen: step one, the ultrasonic cleaning time is 0-12 h.
The specific implementation mode is eighteen: this embodiment is different from one of the fourteenth to seventeenth embodiments in that: step one, the ratio of the mass of the carbon nanotube powder to the volume of the strong acid solution is (10-200) mg: (10-30) mL.
The detailed embodiment is nineteen: this embodiment is different from one of the fourteenth to eighteen embodiments in that: the filter cake washing process in the step two comprises the following steps: and after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into the filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7-8, wherein the vacuum filtration pressure in the filter cake washing process is 0.01-100 Pa.
The specific implementation mode twenty: this embodiment is different from one of the fourteenth to nineteenth embodiments in that: and step two, the organic solvent adopted when the filter cake and the filter membrane are stripped is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol, n-hexane and the like.
The specific implementation mode is twenty one: this embodiment is different from one of the fourteenth to twenty specific embodiments in that: and the vacuum filtration pressure of the mixed liquid in the step two is 0.01 Pa-100 Pa.
Specific embodiment twenty-two: the present embodiment is different from the fourteenth embodiment in one of twenty-one: and step two, when the mixed solution is subjected to vacuum filtration, the filter membrane is a water system filter membrane or an organic system filter membrane, the diameter of the filter membrane is 20-80 mm, and the aperture of the filter membrane is 0.2-2 mu m.
Specific embodiment twenty-three: this embodiment is different from one of the fourteenth to twenty-second embodiments in that: and step three, the rotating speed during the centrifugal treatment is 3000-10000 r, and the centrifugal time is 10-20 min.
Twenty-four specific embodiments: this embodiment is different from one of the fourteenth to twenty-third embodiments in that: and step four, the brazing filler metal is Cu-based brazing filler metal, Ag-based brazing filler metal, Ni-based brazing filler metal, Sn-based brazing filler metal and the like.
The specific implementation mode is twenty five: this embodiment is different from one of the fourteenth to the twenty-fourth embodiment in that: and step four, stripping is carried out in an organic solvent, wherein the organic solvent is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol, n-hexane and the like.
The specific implementation mode is twenty-six: book (I)Embodiments are different from one of the fourteenth to the twenty-fifth embodiments in that: fifthly, the dissimilar materials are a parent metal 1 and a parent metal 2; the parent metal 1 is C/C composite material, C/SiC composite material, graphite and Ti3SiC2、Ti3AlC2Or oxide ceramics, etc.; the base material 2 is Nb, TC4 titanium alloy, Ti600 titanium alloy, TiAl alloy, Ni-based high-temperature alloy, etc.
Example 1:
the method for soldering the dissimilar materials with the aid of the carbon nanotube sponge intermediate layer comprises the following steps:
step one, mixing 30mg of multi-walled carbon nanotube powder with 18mL of strong acid solution, and then carrying out ultrasonic cleaning for 1h in a constant-temperature water bath environment at 60 ℃ to obtain a suspension;
the strong acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the concentrated nitric acid is 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution is 3: 1;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
the vacuum filtration pressure of the mixed solution is 10 Pa;
and when the mixed solution is subjected to vacuum filtration, the filter membrane is an organic filter membrane, the diameter of the filter membrane is 50mm, and the aperture of the filter membrane is 0.45 mu m.
The organic solvent adopted when the filter cake and the filter membrane are stripped is normal hexane.
The filter cake washing process comprises the following steps: after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into a filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7, wherein the vacuum filtration pressure in the filter cake washing process is 10 Pa;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
the rotating speed during the centrifugal treatment is 7800 revolutions, and the centrifugal time is 15 min;
step four, carrying out vacuum filtration on the supernatant obtained in the step three, stripping to obtain a filter cake, and finally drying to obtain carbon nanotube sponge with the thickness of 50 microns; the stripping is carried out in an organic solvent, and the organic solvent is n-hexane;
step five, mixing pure Cu powder and TiH2Uniformly mixing the powder according to the mass ratio of 77:23 to prepare a TiCu brazing filler metal, blending the TiCu brazing filler metal with alcohol to form brazing filler metal paste, coating the brazing filler metal paste on two surfaces of the carbon nano tube sponge to form composite brazing filler metal, placing the composite brazing filler metal between dissimilar materials, and performing brazing connection;
fifthly, the dissimilar materials are a parent metal 1 and a parent metal 2; the parent metal 1 is a C/C composite material; the base material 2 is Nb, the thickness of the C/C composite material is 5mm, and the thickness of the metal Nb is 3 mm; before brazing, the surfaces to be welded of the C/C composite material and the metal Nb are sequentially polished by No. 240 abrasive paper, No. 400 abrasive paper, No. 600 abrasive paper and No. 1000 abrasive paper, then the C/C composite material and the metal Nb are placed into acetone for ultrasonic cleaning for 10min, and the C/C composite material and the metal Nb are taken out and dried.
The brazing process comprises the following steps: vacuumizing in the furnace until the vacuum rate reaches 3 multiplied by 10-3Pa, starting heating, heating to 450 ℃ at the speed of 15 ℃/min, heating to 800 ℃ at the speed of 10 ℃/min, heating to 950 ℃ at the speed of 5 ℃/min, keeping the temperature for 10min, cooling to 450 ℃ at the speed of 10 ℃/min, cooling to 200 ℃ at the speed of 5 ℃/min, closing the heating, and cooling to room temperature along with the furnace.
Comparative example 1: the method for brazing dissimilar materials is carried out according to the following steps:
mixing pure Cu powder with TiH2Uniformly mixing the powder according to the mass ratio of 77:23 to prepare a TiCu brazing filler metal, blending the TiCu brazing filler metal with alcohol to form brazing filler metal paste, coating the brazing filler metal paste between the C/C composite material and the Nb, and performing brazing connection;
the brazing process comprises the following steps: vacuumizing in the furnace until the vacuum rate reaches 3 multiplied by 10-3Pa, starting heating, heating to 450 ℃ at the speed of 15 ℃/min, heating to 800 ℃ at the speed of 10 ℃/min, heating to 950 ℃ at the speed of 5 ℃/min, keeping the temperature for 10min, cooling to 450 ℃ at the speed of 10 ℃/min, cooling to 200 ℃ at the speed of 5 ℃/min, closing the heating, and cooling to room temperature along with the furnace. Before brazing, the surfaces to be welded of the C/C composite material and the metal Nb are treated by using 240#, 400#, 600# and 100 # in sequenceAnd polishing the No. 0 sand paper, then putting the polished No. 0 sand paper into acetone for ultrasonic cleaning for 10min, taking out and airing.
FIG. 1 is a scanned photograph of a brazed joint obtained in example 1; FIG. 2 is a photograph of a scan of a brazed joint obtained in comparative example 1; as can be seen from the comparison of FIG. 1 and FIG. 2, after the carbon nanotube sponge intermediate layer is added, the TiCu phase in the joint interface is obviously reduced, the brittle compounds are hardly agglomerated, and the TiCu phase is used in the joint interface4The phases and the Cu (s, s) phase are dominant. The shear strength of the joint reaches 43 MPa.
Example 2:
the method for soldering the dissimilar materials with the aid of the carbon nanotube sponge intermediate layer comprises the following steps:
step one, mixing 30mg of multi-walled carbon nanotube powder with 18mL of strong acid solution, and then carrying out ultrasonic cleaning for 1h in a constant-temperature water bath environment at 60 ℃ to obtain a suspension;
the strong acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the concentrated nitric acid is 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution is 3: 1;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
the vacuum filtration pressure of the mixed solution is 10 Pa;
and when the mixed solution is subjected to vacuum filtration, the filter membrane is an organic filter membrane, the diameter of the filter membrane is 50mm, and the aperture of the filter membrane is 0.45 mu m.
The organic solvent adopted when the filter cake and the filter membrane are stripped is normal hexane.
The filter cake washing process comprises the following steps: after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into a filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7, wherein the vacuum filtration pressure in the filter cake washing process is 10 Pa;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
the rotating speed during the centrifugal treatment is 7800 revolutions, and the centrifugal time is 15 min;
step four, carrying out vacuum filtration on the supernatant obtained in the step three, stripping to obtain a filter cake, and finally drying to obtain carbon nanotube sponge with the thickness of 50 microns; the stripping is carried out in an organic solvent, and the organic solvent is n-hexane;
step five, mixing pure Cu powder and TiH2The powder is evenly mixed according to the mass ratio of 77:23 to prepare the TiCu solder,
firstly, pre-flattening TiCu brazing filler metal powder, then placing carbon nano tube sponge, and then placing the rest TiCu brazing filler metal powder for pressing, wherein the pressure is 6MPa (within the range of 5-10 MPa), so that the composite brazing filler metal with the thickness of 0.5mm is obtained, and the middle layer of the carbon nano tube sponge has certain strength and cannot crack during pressing; placing the composite brazing filler metal between dissimilar materials for brazing connection;
fifthly, the dissimilar materials are a parent metal 1 and a parent metal 2; the parent metal 1 is a C/C composite material; the base material 2 is TC4 titanium alloy, the thickness of the C/C composite material is 5mm, and the thickness of the TC4 titanium alloy is 3 mm; before brazing, the surfaces to be welded of the C/C composite material and the TC4 titanium alloy are sequentially polished by 240#, 400#, 600# and 1000# sandpaper, then are placed into acetone for ultrasonic cleaning for 10min, and are taken out and dried.
The brazing process comprises the following steps: vacuumizing in the furnace until the vacuum rate reaches 3 multiplied by 10-3Pa, starting heating, heating to 450 ℃ at the speed of 15 ℃/min, heating to 800 ℃ at the speed of 10 ℃/min, heating to 950 ℃ at the speed of 5 ℃/min, keeping the temperature for 10min, cooling to 450 ℃ at the speed of 10 ℃/min, cooling to 200 ℃ at the speed of 5 ℃/min, closing the heating, and cooling to room temperature along with the furnace.
Comparative example 2: the method for brazing dissimilar materials is carried out according to the following steps:
mixing pure Cu powder with TiH2The powder is evenly mixed according to the mass ratio of 77:23 to prepare the TiCu solder,
pressing TiCu brazing filler metal powder under the pressure of 6MPa to obtain brazing filler metal sheets with the thickness of 0.5mm, and placing the brazing filler metal sheets between the C/C composite material and the TC4 titanium alloy for brazing connection;
the brazing process comprises the following steps: vacuumizing the furnace to vacuumThe rate reaches 3 x 10-3Pa, starting heating, heating to 450 ℃ at the speed of 15 ℃/min, heating to 800 ℃ at the speed of 10 ℃/min, heating to 950 ℃ at the speed of 5 ℃/min, keeping the temperature for 10min, cooling to 450 ℃ at the speed of 10 ℃/min, cooling to 200 ℃ at the speed of 5 ℃/min, closing the heating, and cooling to room temperature along with the furnace. Before brazing, the surfaces to be welded of the C/C composite material and the TC4 titanium alloy are sequentially polished by 240#, 400#, 600# and 1000# sandpaper, then are placed into acetone for ultrasonic cleaning for 10min, and are taken out and dried.
FIG. 3 is a scanned photograph of a brazed joint obtained in example 2; FIG. 4 is a photograph of a scan of a brazed joint obtained in comparative example 2; as can be seen from a comparison of fig. 3 and 4, Ti (s, s) dissolution was significantly reduced after the addition of the carbon nanotube sponge intermediate layer. The shear strength of the joint reaches 40 MPa.
Example 3:
the method for soldering the dissimilar materials with the aid of the carbon nanotube sponge intermediate layer comprises the following steps:
step one, mixing 30mg of multi-walled carbon nanotube powder with 18mL of strong acid solution, and then carrying out ultrasonic cleaning for 1h in a constant-temperature water bath environment at 60 ℃ to obtain a suspension;
the strong acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the concentrated nitric acid is 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution is 3: 1;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
the vacuum filtration pressure of the mixed solution is 10 Pa;
and when the mixed solution is subjected to vacuum filtration, the filter membrane is an organic filter membrane, the diameter of the filter membrane is 50mm, and the aperture of the filter membrane is 0.45 mu m.
The organic solvent adopted when the filter cake and the filter membrane are stripped is normal hexane.
The filter cake washing process comprises the following steps: after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into a filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7, wherein the vacuum filtration pressure in the filter cake washing process is 10 Pa;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
the rotating speed during the centrifugal treatment is 7800 revolutions, and the centrifugal time is 15 min;
step four, adding brazing filler metal powder into the supernatant obtained in the step three, uniformly mixing, then carrying out vacuum filtration, stripping to obtain a filter cake, and finally drying to obtain the carbon nanotube sponge composite brazing filler metal with the thickness of 200 microns;
the brazing filler metal powder is AgCu brazing filler metal and is formed by uniformly mixing pure Cu powder and Ag powder with the grain sizes of 40nm according to the mass ratio of 72: 28;
the stripping is carried out in an organic solvent, and the organic solvent is n-hexane;
and fifthly, carrying out brazing connection on the dissimilar materials by using the carbon nanotube sponge composite brazing filler metal.
The dissimilar materials are a parent metal 1 and a parent metal 2; the base material 1 is Ti3SiC2(ii) a The parent material 2 is TC4, Ti3SiC2The thickness is 5mm, and the thickness of TC4 is 3 mm; before brazing, Ti3SiC2And sequentially grinding the surface to be welded with TC4 with 240#, 400#, 600# and 1000# sandpaper, then placing into acetone for ultrasonic cleaning for 10min, taking out and drying.
The brazing process comprises the following steps: vacuumizing in the furnace until the vacuum rate reaches 3 multiplied by 10-3Pa, starting heating, heating to 450 ℃ at the speed of 15 ℃/min, heating to 800 ℃ at the speed of 10 ℃/min, heating to 880 ℃ at the speed of 5 ℃/min, keeping the temperature for 10min, cooling to 450 ℃ at the speed of 10 ℃/min, cooling to 200 ℃ at the speed of 5 ℃/min, closing the heating, and cooling to room temperature along with the furnace.
The content of the brittle compound at the interface of the joint obtained in the embodiment is reduced, the dissolution range of the base metal into the brazing seam is obviously reduced, the residual stress of the brazing joint is relieved by the brazing seam structure with good plasticity, and the shear strength of the brazing joint reaches 118 MPa.
Claims (10)
1. A method for soldering a dissimilar material with the aid of a carbon nanotube sponge intermediate layer is characterized by comprising the following steps: the method comprises the following steps:
step one, mixing carbon nanotube powder with a strong acid solution, and then carrying out ultrasonic cleaning at a constant temperature of 60 ℃ to obtain a suspension;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
step four, carrying out vacuum filtration on the supernatant obtained in the step three, stripping to obtain a filter cake, and finally drying to obtain the carbon nanotube sponge;
and fifthly, arranging brazing filler metal on two sides of the carbon nano tube sponge to form composite brazing filler metal, and performing brazing connection on the dissimilar materials by using the composite brazing filler metal.
2. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 1, wherein:
step one, the carbon nanotube powder is a single-walled carbon nanotube, a double-walled carbon nanotube or a multi-walled carbon nanotube;
step one, the ratio of the mass of the carbon nanotube powder to the volume of the strong acid solution is (10-200) mg: (10-30) mL;
the strong acid in the step one is concentrated sulfuric acid, concentrated nitric acid or a mixed solution of the concentrated sulfuric acid and the concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is not less than 98%, the mass fraction of the concentrated nitric acid is not less than 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution of the concentrated sulfuric acid and the concentrated nitric acid is (2-5): 1;
step one, the ultrasonic cleaning time is 0-12 h.
3. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 1, wherein:
the filter cake washing process in the step two comprises the following steps: after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into a filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7-8, wherein in the filter cake washing process, the vacuum filtration pressure is 0.01-100 Pa;
the organic solvent adopted when the filter cake and the filter membrane are stripped in the second step is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol or normal hexane;
the vacuum filtration pressure of the mixed liquid in the step two is 0.01 Pa-100 Pa;
and step two, when the mixed solution is subjected to vacuum filtration, the filter membrane is a water system filter membrane or an organic system filter membrane, the diameter of the filter membrane is 20-80 mm, and the aperture of the filter membrane is 0.2-2 mu m.
4. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 1, wherein:
rotating speed during the centrifugal treatment in the third step is 3000-10000 r, and the centrifugal time is 10-20 min;
and fourthly, stripping is carried out in an organic solvent, wherein the organic solvent is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol or normal hexane.
5. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 1, wherein:
fifthly, the dissimilar materials are a parent metal 1 and a parent metal 2; the parent metal 1 is C/C composite material, C/SiC composite material, graphite and Ti3SiC2、Ti3AlC2Or an oxide ceramic; the base material 2 is Nb, TC4 titanium alloy, Ti600 titanium alloy, TiAl alloy or Ni-based high-temperature alloy;
and fifthly, the brazing filler metal is Cu-based brazing filler metal, Ag-based brazing filler metal, Ni-based brazing filler metal, Sn-based brazing filler metal, Ti-based brazing filler metal or Zr brazing filler metal.
6. A method for soldering a dissimilar material with the aid of a carbon nanotube sponge intermediate layer is characterized by comprising the following steps: the method comprises the following steps:
step one, mixing carbon nanotube powder with a strong acid solution, and then carrying out ultrasonic cleaning at a constant temperature of 60 ℃ to obtain a suspension;
step two, dispersing the suspension obtained in the step one into deionized water to obtain a mixed solution, then carrying out vacuum filtration on the mixed solution to obtain a filter cake, continuing washing the filter cake, and finally stripping the filter cake and the filter membrane;
step three, ultrasonically dispersing the filter cake obtained by stripping in the step two into absolute ethyl alcohol, carrying out centrifugal treatment, and keeping supernatant;
step four, adding brazing filler metal powder into the supernatant obtained in the step three, uniformly mixing, then carrying out vacuum filtration, stripping to obtain a filter cake, and finally drying to obtain the carbon nano tube sponge composite brazing filler metal;
and fifthly, carrying out brazing connection on the dissimilar materials by using the carbon nanotube sponge composite brazing filler metal.
7. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 6, wherein:
step one, the carbon nanotube powder is a single-walled carbon nanotube, a double-walled carbon nanotube or a multi-walled carbon nanotube;
the strong acid in the step one is concentrated sulfuric acid, concentrated nitric acid or a mixed solution of the concentrated sulfuric acid and the concentrated nitric acid; the mass fraction of the concentrated sulfuric acid is not less than 98%, the mass fraction of the concentrated nitric acid is not less than 65%, and the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid in the mixed solution of the concentrated sulfuric acid and the concentrated nitric acid is (2-5): 1;
step one, the ultrasonic cleaning time is 0-12 h;
step one, the ratio of the mass of the carbon nanotube powder to the volume of the strong acid solution is (10-200) mg: (10-30) mL.
8. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 6, wherein:
the filter cake washing process in the step two comprises the following steps: after the mixed liquid is subjected to vacuum filtration to obtain a filter cake, sequentially adding deionized water and absolute ethyl alcohol into a filtration device to serve as a washing liquid, and performing vacuum filtration until the pH of the washing liquid is 7-8, wherein in the filter cake washing process, the vacuum filtration pressure is 0.01-100 Pa;
the organic solvent adopted when the filter cake and the filter membrane are stripped in the second step is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol or normal hexane;
the vacuum filtration pressure of the mixed liquid in the step two is 0.01 Pa-100 Pa;
and step two, when the mixed solution is subjected to vacuum filtration, the filter membrane is a water system filter membrane or an organic system filter membrane, the diameter of the filter membrane is 20-80 mm, and the aperture of the filter membrane is 0.2-2 mu m.
9. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 6, wherein:
rotating speed during the centrifugal treatment in the third step is 3000-10000 r, and the centrifugal time is 10-20 min;
the solder in the fourth step is Cu-based solder, Ag-based solder, Ni-based solder or Sn-based solder;
and fourthly, stripping is carried out in an organic solvent, wherein the organic solvent is absolute ethyl alcohol, acetone, ethylene glycol, isopropanol or normal hexane.
10. The method for brazing dissimilar materials with the aid of the carbon nanotube sponge intermediate layer as recited in claim 6, wherein:
fifthly, the dissimilar materials are a parent metal 1 and a parent metal 2; the parent metal 1 is C/C composite material, C/SiC composite material, graphite and Ti3SiC2、Ti3AlC2Or an oxide ceramic; the base material 2 is Nb, TC4 titanium alloy, Ti600 titanium alloy, TiAl alloy or Ni-based high-temperature alloy.
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