CN112122826A - Soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and method and application thereof - Google Patents
Soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and method and application thereof Download PDFInfo
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- CN112122826A CN112122826A CN202010988739.3A CN202010988739A CN112122826A CN 112122826 A CN112122826 A CN 112122826A CN 202010988739 A CN202010988739 A CN 202010988739A CN 112122826 A CN112122826 A CN 112122826A
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- silicon nitride
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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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- 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
- B23K1/20—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
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
-
- 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
- B23K35/3006—Ag as the principal constituent
Abstract
The invention discloses a soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and a method and application thereof, wherein the soldering method comprises the following steps: pretreating a titanium-based composite material and silicon nitride ceramics, processing foamed nickel to the same size as a base material to be welded, stacking the foamed nickel in a graphite die according to the sequence of the titanium-based composite material/soldering paste/foamed nickel/soldering paste/silicon nitride ceramics to obtain a composite solder, and putting the composite solder into a vacuum brazing furnace after briquetting; controlling the vacuum degree of the vacuum brazing furnace not to be lowAt 8.0X 10‑3Pa, sequentially heating to 300 ℃ and keeping for 5-30 min, heating to 810-930 ℃ and keeping for 5-30 min, cooling to 300 ℃ and cooling to room temperature along with the furnace. The invention adopts the foam nickel as the middle layer to enable the stress in the joint to form gradient transition, effectively inhibits the generation of brittle compounds, improves the strength of the joint, and has simple operation in the brazing process, low cost and higher application value.
Description
Technical Field
The invention relates to the field of brazing, in particular to a soldering paste for brazing a titanium-based composite material and silicon nitride ceramics, and a method and application thereof.
Background
The silicon nitride ceramic has the advantages of high strength, high hardness, good corrosion resistance and thermal shock resistance and the like, and has wide application prospect in the field of aerospace. However, silicon nitride ceramics are very brittle and difficult to process into a member having a complicated shape, and the range of application thereof is greatly limited. Therefore, the silicon nitride ceramic is connected with the metal material, so that the excellent high-temperature performance of the silicon nitride ceramic can be utilized, the good plasticity and toughness of the metal material can be exerted, and the requirements of modern engineering application are met. The titanium-based composite material has the characteristics of low density, high strength, good high-temperature creep resistance and the like, and is widely applied to the fields of aerospace, automobile industry and the like. Therefore, the realization of the connection between the titanium-based composite material and the silicon nitride ceramic is of great practical significance.
At present, in a connection method of ceramics and metal, brazing has the advantages of simple process, low cost, small requirements on the size and the shape of a joint and the like, and is widely applied. However, the thermal expansion coefficients of the ceramic and the metal are not matched, so that residual stress is easily generated at a brazing interface, and the mechanical property of the joint is influenced. In addition, due to the dissolution and diffusion behaviors of the brazing filler metal in the brazing process, a brittle compound can be formed on a joint interface, and the reliability of the brazed joint in the service process is reduced.
Therefore, a method for brazing the titanium-based composite material and the silicon nitride ceramic is needed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a soldering paste for brazing a titanium-based composite material and silicon nitride ceramics, and a method and application thereof.
The invention adopts the following specific technical scheme:
a preparation method of a soldering paste for brazing a titanium-based composite material and silicon nitride ceramics comprises the following specific steps:
a silver-based solder of 68.8Ag-26.7Cu-4.5Ti in wt.% was mixed with carbon nanotubes as follows (1-x%): mixing x% in percentage by mass to obtain a composite solder, wherein x is 1-5; ball-milling the composite solder by using a ball mill, and removing a ball-milling medium to obtain composite powder; and mixing the composite powder with a welding intermediate agent to obtain the soldering paste.
Preferably, the ball milling is performed for 8 hours by using a centrifugal ball mill, using steel balls as milling balls and alcohol as a milling medium under the condition that the ball milling rotating speed is 100 r/min.
Further, the method for removing the ball milling medium adopts a rotary evaporator to heat in water bath to 60 ℃ so as to completely volatilize the alcohol.
Preferably, the composite powder is mixed with the welding intermediate agent in a ratio of 9: 1.
The second purpose of the invention is to provide a soldering paste prepared by any one of the above soldering paste preparation methods.
The third purpose of the invention is to provide a method for brazing a titanium-based composite material and silicon nitride ceramic based on the soldering paste, which comprises the following steps:
s1: pretreating the titanium-based composite material and the silicon nitride ceramic to obtain a base material to be welded;
s2: processing the foamed nickel to the same size as the parent metal to be welded, cleaning and drying to obtain a foamed nickel parent metal;
s3: stacking the base material to be welded, the foam nickel base material and the soldering paste in a graphite mould according to the sequence of titanium-based composite material/soldering paste/foam nickel/soldering paste/silicon nitride ceramic to obtain composite solder, and placing a pressing block above the composite solder into a vacuum brazing furnace;
s4: controlling the vacuum degree of the vacuum brazing furnace to be not less than 8.0 multiplied by 10-3Pa, sequentially heating to 300 ℃ and keeping for 5-30 min, heating to 810-930 ℃ and keeping for 5-30 min, cooling to 300 ℃ and cooling to room temperature along with the furnace, and completing the brazing process of the titanium-based composite material and the silicon nitride ceramic.
Preferably, the pretreatment in S1 means that the surfaces of the titanium-based composite material and the silicon nitride ceramic are sequentially polished with 180-2000 mesh sandpaper step by step, then the surfaces to be welded of the polished titanium-based composite material and the polished silicon nitride ceramic are respectively polished on a polishing machine until no scratch is formed, and finally the surfaces are cleaned with alcohol and dried.
Preferably, the thickness of the solder paste in S3 is 100 to 200 μm.
Preferably, the thickness of the nickel foam in S3 is 0.5mm to 1 mm.
Preferably, the temperature increase rate in S4 is 10 ℃/min, and the temperature decrease rate is 5 ℃/min.
And cooling to room temperature along with the furnace at 300 ℃, thus completing the connection of the titanium-based composite material and the silicon nitride ceramic.
Compared with the prior art, the invention has the beneficial effects that:
1) the brazing method can realize effective connection of the titanium-based composite material and the silicon nitride ceramic, has no defects of cracks, air holes and the like in a joint, the shear strength of the joint obtained when the temperature is kept at 840 ℃ for 20min is 83MPa, and the preparation and brazing processes of the composite brazing filler metal are simple and efficient, thereby being convenient for batch production;
2) according to the brazing method, the carbon nano tubes are added into the silver-based brazing filler metal to prepare the composite powder brazing filler metal, so that the joint filling capacity of the brazing filler metal is improved, and the brazing is carried out by adopting a titanium-based composite material/brazing filler metal soldering paste/nickel foam/brazing filler metal soldering paste/silicon nitride ceramic structure, so that the residual stress in a joint is reduced, and the mechanical property of a brazed joint is improved;
3) the brazing method of the invention utilizes the unique three-dimensional structure of the nickel foam to promote the diffusion of elements, so that the compound generated in the brazing process is uniformly and dispersedly distributed in the brazing seam, and the Ti from the titanium-based composite material is consumed by the Ni in the brazing process, thereby inhibiting the generation of brittle compound at the ceramic interface, effectively relieving the problem of residual stress concentration in the joint and remarkably improving the mechanical property of the joint;
4) the invention adopts the foam nickel as the middle layer to lead the stress in the joint to form gradient transition and effectively inhibit the generation of brittle compounds, the addition of the carbon nano tube leads the joint tissue to be evenly refined, the joint strength is improved, and the brazing process has simple operation, low cost and higher application value.
Drawings
FIG. 1 is a schematic view showing the assembly of S3 composite filler metal in example 1;
FIG. 2 is a graph of the brazing process in S4 in example 1;
in the figure: titanium-based composite material 1, solder paste 2, foam nickel 3 and silicon nitride ceramic 4.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and the detailed description. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
Example 1
Silver-based solder (68.8Ag-26.7Cu-4.5Ti in wt.%) was mixed with carbon nanotubes as (1-x%): and mixing x% (x is 1-5) in percentage by weight to obtain the composite solder. The composite solder is ball-milled for 8 hours by using a centrifugal ball mill with steel balls as milling balls and alcohol as a ball-milling medium at the ball-milling rotating speed of 100r/min, and then a rotary evaporator is adopted to carry out water bath heating to 60 ℃ so that the alcohol as the ball-milling medium is completely volatilized to obtain composite powder. And mixing the composite powder and the welding intermediate agent according to the ratio of 9:1 to obtain the soldering paste.
The prepared soldering paste is used for soldering the titanium-based composite material and the silicon nitride ceramic, and the specific method comprises the following steps:
s1: and (3) pretreating the titanium-based composite material and the silicon nitride ceramic to obtain a base material to be welded.
The pretreatment process mainly comprises the following steps: sequentially polishing the surfaces of the titanium-based composite material and the silicon nitride ceramic by 180-2000 meshes of abrasive paper step by step, respectively polishing the surfaces to be welded of the polished titanium-based composite material and the polished silicon nitride ceramic on a polishing machine until no scratch is generated, and finally cleaning and drying by using alcohol.
S2: and (4) processing the foamed nickel to the size which is the same as the size of the to-be-welded surface of the base material to be welded obtained in S1, wherein the thickness is 0.5mm, and cleaning and drying to obtain the foamed nickel base material.
S3: and stacking the obtained base material to be welded, the foamed nickel base material and the soldering paste in a graphite mould according to the sequence of titanium-based composite material/soldering paste/foamed nickel/soldering paste/silicon nitride ceramic to obtain the composite solder. Wherein the thickness of the solder paste is about 100 μm. And placing a pressing block on the top of the obtained composite solder into a vacuum brazing furnace.
S4: controlling the vacuum degree of the vacuum brazing furnace to be not less than 8.0 multiplied by 10-3Pa, heating to 300 ℃ at the adding rate of 10 ℃/min, preserving heat for 30min, heating to 840 ℃ at the heating rate of 10 ℃/min, preserving heat for 20min, cooling to 300 ℃ at the cooling rate of 5 ℃/min after heat preservation, and cooling to room temperature along with the furnace, thereby completing the brazing process of the titanium-based composite material and the silicon nitride ceramic. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 1.
Example 2
In this example, the same solder paste and method as in example 1 were used to braze the titanium-based composite material and the silicon nitride ceramic, except that in S4, the temperature was increased to 300 ℃ at a rate of 10 ℃/min and then maintained for 30min, and then increased to 810 ℃ at a rate of 10 ℃/min and then maintained for 20 min. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 2.
Example 3
In this example, the same solder paste and method as in example 1 were used to braze the titanium-based composite material and the silicon nitride ceramic, except that in S4, the temperature was increased to 300 ℃ at a rate of 10 ℃/min and then maintained for 30min, and then increased to 870 ℃ at a rate of 10 ℃/min and then maintained for 20 min. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 3.
Example 4
In this example, the same solder paste and method as in example 1 were used to braze the titanium-based composite material and the silicon nitride ceramic, except that in S4, the temperature was increased to 300 ℃ at a rate of 10 ℃/min and then maintained for 30min, and then increased to 900 ℃ at a rate of 10 ℃/min and then maintained for 20 min. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 4.
Example 5
In this example, the same solder paste and method as in example 1 were used to braze the titanium-based composite material and the silicon nitride ceramic, except that in S4, the temperature was increased to 300 ℃ at a rate of 10 ℃/min and then maintained for 30min, and then increased to 930 ℃ at a rate of 10 ℃/min and then maintained for 20 min. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 5.
Comparative example 1
In this example, the same method as in example 1 was used to braze a titanium-based composite material and a silicon nitride ceramic, except that only a silver-based solder (68.8Ag-26.7Cu-4.5Ti wt.%) was used in the preparation of the solder paste, i.e., no carbon nanotubes were added; meanwhile, the brazing structure is titanium-based composite material/soldering paste/silicon nitride ceramic, namely, foam nickel is not added. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 6.
Comparative example 2
This example uses the same solder paste and method as in example 1 for brazing titanium matrix composites to silicon nitride ceramics, except that the brazed structure is titanium matrix composite/solder paste/silicon nitride ceramics, i.e. no nickel foam is added. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 7.
Comparative example 3
This example uses the same method as in example 1 for brazing a titanium matrix composite with a silicon nitride ceramic, except that only a silver-based solder (68.8Ag-26.7Cu-4.5Ti wt.%) is used in the preparation of the solder paste, i.e., no carbon nanotubes are added. And obtaining a titanium-based composite material and silicon nitride ceramic brazing joint sample 8.
The titanium-based composite materials obtained in examples 1 to 5 and comparative examples 1 to 3 and the silicon nitride ceramic soldered joints were placed on a universal testing machine to test the shear strength, and the test results are shown in table 1.
TABLE 1 shear strength of brazed joints of titanium-based composites and silicon nitride ceramics
The data in Table 1 demonstrate that higher shear strengths of brazed joints can be obtained by the method of brazing titanium-based composites with silicon nitride ceramic using the solder paste of the present invention. Compared with the comparative examples 1-3, the brazing structure with a proper amount of carbon nano tubes and foam nickel as the middle layer added into the silver-based brazing filler metal plays an important role in relieving residual stress in the brazed joint, and the effect of improving the shear strength of the brazed joint is remarkable.
The invention adopts the foam nickel as the middle layer to lead the stress in the joint to form gradient transition and effectively inhibit the generation of brittle compounds, the addition of the carbon nano tube leads the joint tissue to be evenly refined, the joint strength is improved, and the brazing process has simple operation, low cost and higher application value.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (10)
1. A preparation method of a soldering paste for brazing a titanium-based composite material and silicon nitride ceramics is characterized by comprising the following steps:
a silver-based solder of 68.8Ag-26.7Cu-4.5Ti in wt.% was mixed with carbon nanotubes as follows (1-x%): mixing x% in percentage by mass to obtain a composite solder, wherein x is 1-5; ball-milling the composite solder by using a ball mill, and removing a ball-milling medium to obtain composite powder; and mixing the composite powder with a welding intermediate agent to obtain the soldering paste.
2. The method for preparing solder paste according to claim 1, wherein the ball milling is performed for 8 hours by using a centrifugal ball mill, using steel balls as milling balls and alcohol as a milling medium at a milling speed of 100 r/min.
3. A method of preparing solder paste according to claim 2, wherein the method of removing the ball milling medium is carried out by heating in a water bath to 60 ℃ using a rotary evaporator to completely volatilize the alcohol.
4. A paste preparation method according to claim 1, wherein said composite powder is mixed with a solder intermediate in a ratio of 9: 1.
5. A solder paste prepared by the method of any one of claims 1 to 4.
6. A method for brazing a titanium-based composite material and a silicon nitride ceramic based on the solder paste of claim 5, which comprises the following steps:
s1: pretreating the titanium-based composite material and the silicon nitride ceramic to obtain a base material to be welded;
s2: processing the foamed nickel to the same size as the parent metal to be welded, cleaning and drying to obtain a foamed nickel parent metal;
s3: stacking the base material to be welded, the foam nickel base material and the soldering paste in a graphite mould according to the sequence of titanium-based composite material/soldering paste/foam nickel/soldering paste/silicon nitride ceramic to obtain composite solder, and placing a pressing block above the composite solder into a vacuum brazing furnace;
s4: controlling the vacuum degree of the vacuum brazing furnace to be not less than 8.0 multiplied by 10-3Pa, sequentially heating to 300 ℃ and keeping for 5-30 min, heating to 810-930 ℃ and keeping for 5-30 min, cooling to 300 ℃ and cooling to room temperature along with the furnace, and completing the brazing process of the titanium-based composite material and the silicon nitride ceramic.
7. The brazing method according to claim 6, wherein the pretreatment in S1 is to sequentially polish the surfaces of the titanium-based composite material and the silicon nitride ceramic with 180-2000 mesh sand paper step by step, then polish the surfaces to be welded of the titanium-based composite material and the silicon nitride ceramic on a polishing machine respectively until no scratch is formed, and finally clean and dry the surfaces with alcohol.
8. The method according to claim 6, wherein the thickness of the solder paste in S3 is 100 μm to 200 μm.
9. The brazing method according to claim 6, wherein the foamed nickel in S3 has a thickness of 0.5mm to 1 mm.
10. The brazing method according to claim 6, wherein the temperature increase rate in S4 is 10 ℃/min, and the temperature decrease rate is 5 ℃/min.
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