CN110549032B - Copper-based brazing filler metal with gradient thermal expansion coefficient and preparation method thereof - Google Patents
Copper-based brazing filler metal with gradient thermal expansion coefficient and preparation method thereof Download PDFInfo
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- CN110549032B CN110549032B CN201910775011.XA CN201910775011A CN110549032B CN 110549032 B CN110549032 B CN 110549032B CN 201910775011 A CN201910775011 A CN 201910775011A CN 110549032 B CN110549032 B CN 110549032B
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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
- B23K35/22—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
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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
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3601—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with inorganic compounds as principal constituents
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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
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Abstract
The invention discloses a copper-based brazing filler metal with gradient thermal expansion coefficient and a preparation method thereof, which comprises metal powder, thermal expansion coefficient adjusting powder, an active agent and a dispersing agent, wherein the preparation method comprises the steps of mixing mechanically alloyed metal powder with the active agent to obtain mixed powder A, equally dividing the mixed powder A into n equal parts, mixing the thermal expansion coefficient adjusting powder with the dispersing agent to obtain mixed powder B, and equally dividing the mixed powder B into n (n-1)/2 equal parts; mixing the first part of mixed powder A with 0 part of mixed powder B to obtain mixed powder AB1, and mixing the nth part of mixed powder A with n-1 part of mixed powder B to obtain mixed powder ABn; uniformly scattering mixed powder AB1 in a hot-pressing sintering grinding tool to obtain a first powder layer, preparing an nth powder layer by the same method, performing vacuum hot isostatic pressing on the n powder layers to obtain a static-pressure blank, and performing multi-pass cold rolling on the static-pressure blank to obtain the copper-based brazing filler metal.
Description
Technical Field
The invention relates to the technical field of brazing materials and dissimilar materials, in particular to a copper-based brazing filler metal with gradient thermal expansion coefficient and a preparation method thereof.
Background
The ceramic or ceramic matrix composite has high hardness, strong wear resistance, good high-temperature mechanical property, high-temperature oxidation resistance and thermal shock resistance, and is widely applied in the fields of aerospace, automobiles and petrochemical industry, but the complex ceramic component is difficult to machine and form due to the characteristics of poor plasticity and high brittleness of the ceramic. The metal material has good toughness and processability, but has poor high-temperature mechanical property. Therefore, an effective connecting method is selected to connect the ceramic and the metal to obtain the ceramic-metal composite member, so that the advantages of the ceramic and the metal are combined, the excellent performance of the ceramic material is fully exerted, and the application range of the ceramic material is widened.
The brazing has the advantages of simple working procedure, wide application range of joint forms, low cost and the like, and is widely applied to ceramic-metal connection. However, the thermal expansion coefficients of ceramic and metal are very different, so that the soldered joint generates large residual stress, even has local stress concentration, is easy to generate welding cracks, and greatly reduces the strength of the joint. Therefore, reducing residual stresses is critical to achieving high strength ceramic-to-metal braze joints.
In order to reduce the residual stress, the common solution is: (1) and (3) reducing the brazing temperature: the brazing temperature is mainly determined by the brazing material, so that the brazing material with lower melting temperature is selected for reducing the brazing temperature. For ceramic-metal brazing, common brazing filler metals comprise silver-based brazing filler metals, nickel-based brazing filler metals and copper-based brazing filler metals, wherein the silver-based brazing filler metals are mainly Ag-Cu-Ti brazing filler metals, the melting temperature of the silver-based brazing filler metals is low, but the cost is high due to the existence of silver, and the silver-based brazing filler metals are low in strength and are not suitable for brazed joints with strength requirements; the nickel-based brazing filler metal is mainly Ni-Cr, Ni-Cr-B-Si and Ni-Cr-B-Si-Mo brazing filler metal, the brazing filler metal has high strength, but the melting temperature is high, and the residual stress of a brazed joint is large; compared with the nickel-based and silver-based active solder, the copper-based solder has moderate melting temperature, low production cost and better economy, but the copper-based solder sold in the market at present is mainly CuSnTi solder, and Sn element in the solderThe content is high, the microstructure contains a large amount of massive or strip SnTi compounds, the brittleness of the brazing filler metal is obviously increased, the strength of the brazing filler metal is low, and the performance is unstable; (2) adding an intermediate slow-release layer: in order to compensate for plastic deformation caused by difference of thermal expansion coefficients, a single-layer or multi-layer copper ribbon or nickel ribbon (slow release layer) with good plasticity is often added into a soldered joint in a manner of 'solder-slow release layer-solder' or 'solder-slow release layer 1-solder-slow release layer 2-solder', however, the straight-chain slow release layer not only easily generates soldering defects, but also generates interaction stress between the solder and the slow release layer, so that the soldering performance is unstable; (3) compounding the brazing filler metal: the composite solder is prepared by adding reinforced particles with low expansion coefficient into the solder, and the commonly used reinforced particles are WC particles, TiN particles, SiC particles and Al2O3Particles, Cr2O3The brazing filler metal comprises particles, high-melting-point metal simple substance powder (such as Mo powder), carbon fibers and the like, and aims to improve the strength of the silver-based brazing filler metal and strengthen the particles in the silver-based brazing filler metal, but the content of the particles cannot exceed 10 vol%, the reduction of the thermal expansion coefficient of the composite brazing filler metal is not obvious, and meanwhile, because the traditional brazing filler metal has poor wettability on the reinforced particles, the reinforced particles are mechanically coupled with a brazing filler metal matrix, so that interface defects such as incomplete fusion, microcracks and the like are formed, and the improvement of the strength of a brazed joint is not facilitated. Therefore, in order to solve the problems existing in the method, the thermal expansion coefficient gradient brazing filler metal which is more suitable for brazing the dissimilar joint with larger difference of the thermal expansion coefficients is developed, and the method has great significance for realizing high-strength connection of metal-ceramic.
Disclosure of Invention
In order to solve the problems, the invention provides the copper-based brazing filler metal with the gradient thermal expansion coefficient and the preparation method thereof, which can reduce the residual stress of a joint and improve the strength of the joint, so that the ceramic or ceramic matrix composite material is not easy to crack when being in brazing connection with metal.
The invention is realized by the following technical scheme:
the copper-based brazing filler metal with the gradient thermal expansion coefficient comprises 70-85 parts by weight of metal powder and 15-30 parts by weight of thermal expansion coefficient adjusting powder;
the metal powder comprises the following components in parts by weight: 5-10 parts of tin, 1-5 parts of titanium, 1-5.5 parts of phosphorus, 1-5 parts of cobalt, 1-3 parts of zinc, 1-3 parts of indium, 0.1-2.5 parts of manganese, 0.1-0.5 part of silicon, 0.1-0.5 part of cerium and the balance of copper;
the thermal expansion coefficient adjusting powder comprises, by weight, 2-8 parts of nickel-coated titanium carbide, 40-60 parts of nickel-coated molybdenum and 15-40 parts of nickel-coated tungsten.
Further, the copper-based brazing filler metal with the gradient thermal expansion coefficient also comprises 0.1-1 part of an active agent in parts by weight.
Further, the active agent is a mixture of boron, borax, boric anhydride, potassium fluoride and potassium fluoborate.
Further, the copper-based brazing filler metal with the gradient thermal expansion coefficient also comprises 0.1-2 parts by weight of a dispersing agent.
Further, the dispersant is at least one of silane coupling agent, polyethyleneimine, sodium dodecyl sulfate, cetyl trimethyl ammonium bromide and polyoxyethylene monoacrylate.
Further, the particle size of the metal powder is 10-150 μm; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
A preparation method of a copper-based brazing filler metal with gradient thermal expansion coefficient mainly comprises the following steps:
respectively weighing copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder and copper-cerium intermediate alloy powder for later use according to the weight parts of the metal powder;
respectively weighing nickel-coated titanium carbide powder, nickel-coated molybdenum powder and nickel-coated tungsten powder according to the weight parts of the thermal expansion coefficient adjusting powder for later use;
step two, carrying out mechanical alloying on the metal powder weighed in the step one to obtain mechanical alloying metal powder;
step three, putting the mechanical alloying metal powder prepared in the step two and an active agent into a mixing tank, and vacuumizing to 1 × 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the working pressure in the mixing tank is 1-100 Pa, mixing for 1-5 h under the condition that the rotating speed is 50-200 r/min, and obtaining mixed powder A;
putting the nickel-coated titanium carbide powder, the nickel-coated molybdenum powder, the nickel-coated tungsten powder and the dispersing agent weighed in the step one into a mixer, and mixing for 1-5 hours at the rotating speed of 50-200 r/min to obtain mixed powder B;
dividing the mixed powder A prepared in the third step into n equal parts by weight, and respectively marking as 1 st part, 2 nd part, … th part and nth part; dividing the mixed powder B prepared in the step four into n (n-1)/2 equal parts according to equal weight; the n equal parts are 3-10 parts;
step six, uniformly mixing the 1 st part of mixed powder A and 0 part of mixed powder B to obtain mixed powder AB 1; uniformly mixing the 2 nd part of mixed powder A and 1 part of mixed powder B to obtain mixed powder AB 2; uniformly mixing the 3 rd part of mixed powder A and 2 parts of mixed powder B to obtain mixed powder AB 3; and analogy is carried out in sequence, the nth mixed powder A and the n-1 mixed powder B are uniformly mixed to obtain mixed powder ABn;
step seven, taking a hot-pressing sintering grinding tool, and uniformly scattering the mixed powder AB1 obtained in the step six in the hot-pressing sintering grinding tool to form a first powder layer; then, uniformly scattering mixed powder AB2 on the first powder layer by the same method to form a second powder layer; uniformly scattering the mixed powder ABn on the (n-1) th powder layer by analogy to form an nth powder layer;
step eight, carrying out vacuum hot isostatic pressing on the n layers of powder prepared in the step seven to prepare a static-pressure blank, wherein the vacuum degree of the static-pressure forming is 1 multiplied by 10-3～5×10-3Pa, the pressure is 15-100 MPa, the temperature is 600-650 ℃, and the time is 10-120 min; after the static pressure is finished, cooling to room temperature and taking out the static pressure blank; the thickness of the static pressure blank is not more than 3 mm;
and step nine, performing multi-pass cold rolling on the static-pressure blank prepared in the step eight, wherein the pass deformation is 5% -30%, and then trimming and trimming to obtain the copper-based brazing filler metal with the gradient thermal expansion coefficient and the gradient thickness of 0.1-0.5 mm.
Further, the step two of preparing the mechanical alloying metal powder comprises the following specific steps: the method comprises the steps of putting weighed copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder, copper-cerium intermediate alloy powder and grinding balls into a ball-milling tank under the conditions that the ball-material ratio is 10-15: 1 and the filler ratio is 35% -50%, vacuumizing the ball-milling tank to 1 x 10-3～5×10-3And introducing argon with the purity of 99.99% after Pa to ensure that the working pressure in the ball milling tank is 1-100 Pa, and then carrying out ball milling for 3-24 h at the rotating speed of 150-300 r/min to obtain the mechanical alloying metal powder.
Further, the material of the grinding ball in the second step is TiC.
The invention has the beneficial effects that:
(1) according to the invention, copper is selected as a brazing filler metal substrate, so that the high cost of the silver-based brazing filler metal and the high melting temperature of the nickel-based brazing filler metal are avoided, and the content of tin is reduced by compositely adding indium, phosphorus, zinc, manganese and silicon to replace part of tin, so that the melting temperature of the brazing filler metal is reduced, massive or strip-shaped SnTi compounds are prevented from being formed in brazing seams, the microstructure of the brazing seams is optimized, and the joint strength is improved; titanium is an active element and can form a compound with a ceramic component, so that the wettability of the brazing filler metal to the ceramic is improved, and firm combination is formed; cerium can remove oxygen in the brazing filler metal and purify a crystal boundary; the cobalt has a small thermal expansion coefficient and is used for compensating the increase of the thermal expansion coefficient caused by zinc and manganese; setting the mass parts of the selected elements based on the mixing theory of the thermal expansion coefficient;
(2) according to the invention, nickel-coated titanium carbide, nickel-coated molybdenum and nickel-coated tungsten are selected as thermal expansion coefficient adjusting powder, and soft/hard double-layer buffer particles with micro-nano scale are constructed, namely an external nickel soft layer and an internal titanium carbide, molybdenum and tungsten hard layer, so that stress relaxation is promoted, and the thermal expansion coefficient of the composite brazing filler metal can be reduced;
wherein the titanium carbide, molybdenum and tungsten have high melting point, high strength, high hardness and smaller thermal expansion coefficient, according to the mixing theory, the addition of titanium carbide, molybdenum and tungsten to the metal material with larger thermal expansion coefficient can reduce the thermal expansion coefficient of the mixed metal material, but because the titanium carbide, the molybdenum and the tungsten have larger thermal expansion coefficient difference with the metal material with larger thermal expansion coefficient, therefore, larger interface stress and other interface defects are generated between the titanium carbide, the molybdenum and the tungsten and the metal material with larger thermal expansion coefficient, the titanium carbide, the molybdenum and the tungsten are coated by the nickel with good plasticity and moderate thermal expansion coefficient, so that the outer layers of the titanium carbide, the molybdenum and the tungsten contain the metal nickel with good plasticity, the interface stress and the interface defects caused by the titanium carbide, the molybdenum and the tungsten reinforced particles are obviously reduced, and the effect of the titanium carbide, the molybdenum and the tungsten on reducing the thermal expansion coefficient is ensured;
(3) according to the copper-based brazing filler metal with the gradient thermal expansion coefficient, the content of powder is adjusted by increasing the thermal expansion coefficient layer by layer, so that the thermal expansion coefficient of the brazing filler metal is gradually changed from the gradient of the ceramic side to the metal side, the residual stress of a joint is reduced, the strength of the joint is improved, and the problem of poor reliability when the traditional brazing filler metal is used for brazing ceramic-metal is solved;
(4) the optimal preparation method of the copper-based brazing filler metal with the gradient of the thermal expansion coefficient has the advantages of short required process flow, simple equipment and easy operation, can realize the mass production of the copper-based brazing filler metal with the gradient of the thermal expansion coefficient, and has good stability and lower cost.
Drawings
FIG. 1 is a schematic powder assembly of example 1 of the present invention;
FIG. 2 is a schematic view of powder assembly of example 2 of the present invention;
FIG. 3 is a schematic view of powder assembly of example 3 of the present invention;
reference numerals: 1. thermal expansion coefficient adjusting powder 11 and a first powder layer I; 12. a second powder layer I; 13. a third powder layer I; 21. a first powder layer II; 22. a second powder layer II; 23. a third powder layer II; 24. a fourth powder layer II; 25. a fifth powder layer II; 31. a first powder layer III; 32. a second powder layer III; 33. a third powder layer III; 34. a fourth powder layer III; 35. a fifth powder layer III; 36. a sixth powder layer III; 37. a seventh powder layer III; 38. an eighth powder layer III; 39. a ninth powder layer III; 40. the tenth powder layer III.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention.
Example 1
The copper-based brazing filler metal with the gradient thermal expansion coefficient comprises, by weight, 72 parts of metal powder, 27 parts of thermal expansion coefficient adjusting powder, 0.2 part of an active agent and 0.8 part of a dispersing agent. The active agent is a mixture of at least two of boron, borax, boric anhydride, potassium fluoride and potassium fluoborate, and the dispersing agent is at least one of a silane coupling agent, polyethyleneimine, sodium dodecyl sulfate, hexadecyl trimethyl ammonium bromide and polyoxyethylene monoacrylate.
Specifically, the metal powder comprises 5 parts of tin, 5 parts of titanium, 5.5 parts of phosphorus, 5 parts of cobalt, 1 part of zinc, 1 part of indium, 1 part of manganese, 0.2 part of silicon, 0.1 part of cerium and the balance of copper; the thermal expansion coefficient adjusting powder comprises 8 parts by weight of nickel-coated titanium carbide, 60 parts by weight of nickel-coated molybdenum and 32 parts by weight of nickel-coated tungsten. The particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
The preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient comprises the following steps:
respectively weighing copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder and copper-cerium intermediate alloy powder for later use according to the weight parts of the metal powder;
respectively weighing nickel-coated titanium carbide powder, nickel-coated molybdenum powder and nickel-coated tungsten powder according to the weight parts of the thermal expansion coefficient adjusting powder for later use;
step two, grinding balls made of the copper powder, the tin powder, the titanium powder, the cobalt powder, the zinc powder, the manganese powder, the copper-silicon intermediate alloy powder, the copper-indium intermediate alloy powder, the copper-phosphorus intermediate alloy powder, the copper-cerium intermediate alloy powder and the TiC material and weighed in the step one are subjected to ball material ratio of 10-15: 1 and filler material ratio35 to 50 percent of the total weight of the mixture is put into a ball milling tank, and the ball milling tank is vacuumized to 1 multiplied by 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the working pressure in the ball milling tank is 1-100 Pa, and then carrying out ball milling for 3-24 h at the rotating speed of 150-300 r/min to obtain mechanical alloying metal powder;
step three, putting the mechanical alloying metal powder and the activator into a mixing tank, and vacuumizing to 1 × 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the pressure in the material mixing tank is 1-100 Pa, mixing materials for 1-5 hours at the rotating speed of 50-200 r/min, and obtaining mixed powder A;
putting the nickel-coated titanium carbide powder, the nickel-coated molybdenum powder, the nickel-coated tungsten powder and the dispersing agent into a mixer, and mixing for 1-5 hours at the rotating speed of 50-200 r/min to obtain mixed powder B;
dividing the mixed powder A into 3 equal parts by equal weight, and respectively recording as 1 st part, 2 nd part and 3 rd part; dividing the mixed powder B into 3 equal parts by weight;
step six, uniformly mixing the 1 st part of mixed powder A with 0 part of mixed powder B to obtain mixed powder AB 1; uniformly mixing the 2 nd part of mixed powder A with 1 part of mixed powder B to obtain mixed powder AB 2; uniformly mixing the 3 rd part of mixed powder A with the 2 nd part of mixed powder B to obtain mixed powder AB 3;
step seven, taking the hot-pressing sintering grinding tool, and uniformly scattering the mixed powder AB1 in the hot-pressing sintering grinding tool to form a first powder layer I11; then, the mixed powder AB2 was uniformly sprinkled on the first powder layer I11 in the same way to form a second powder layer I12; uniformly scattering the mixed powder AB3 on the second powder layer I12 to form a third powder layer I13, as shown in FIG. 1, wherein the second powder layer I12 and the third powder layer I13 contain thermal expansion coefficient adjusting powder 1;
step eight, putting the hot-pressing sintering grinding tool filled with 3 layers of powder into a hot-pressing sintering furnace for vacuum hot isostatic pressing, wherein the vacuum degree of the static-pressing forming is 1 multiplied by 10-3～5×10-3Pa, pressure of 15-100 MPa, temperature of 600-650 ℃, time of 10-120 DEG Cmin; after the static pressure is finished, cooling to room temperature and taking out the static pressure blank; the thickness of the static pressure blank is not more than 3 mm;
and step nine, performing multi-pass cold rolling on the static pressure blank, wherein the pass deformation is 5% -30%, and then trimming and trimming to obtain the copper-based brazing filler metal with the gradient thermal expansion coefficient and the gradient thickness of 0.1-0.5 mm.
Example 2
The copper-based brazing filler metal with the gradient thermal expansion coefficient comprises, by weight, 72 parts of metal powder, 27 parts of thermal expansion coefficient adjusting powder, 0.2 part of an active agent and 0.8 part of a dispersing agent. The activating agent is a mixture of boron, borax, boric anhydride, potassium fluoride and potassium fluoborate, and the dispersing agent is at least one of silane coupling agent, polyethyleneimine, sodium dodecyl sulfate, hexadecyl trimethyl ammonium bromide and polyoxyethylene-based monoacrylate.
The metal powder comprises 5 parts of tin, 5 parts of titanium, 5.5 parts of phosphorus, 5 parts of cobalt, 1 part of zinc, 1 part of indium, 1 part of manganese, 0.2 part of silicon, 0.1 part of cerium and the balance of copper; the thermal expansion coefficient adjusting powder comprises 8 parts by weight of nickel-coated titanium carbide, 60 parts by weight of nickel-coated molybdenum and 32 parts by weight of nickel-coated tungsten. The particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
The preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient comprises the following steps:
respectively weighing copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder and copper-cerium intermediate alloy powder for later use according to the weight parts of the metal powder;
respectively weighing nickel-coated titanium carbide powder, nickel-coated molybdenum powder and nickel-coated tungsten powder according to the weight parts of the thermal expansion coefficient adjusting powder for later use;
step two, putting the copper powder, the tin powder, the titanium powder, the cobalt powder, the zinc powder, the manganese powder, the copper-silicon intermediate alloy powder, the copper-indium intermediate alloy powder, the copper-phosphorus intermediate alloy powder, the copper-cerium intermediate alloy powder and the grinding balls weighed in the step one into a ball-milling tank under the conditions that the ball-material ratio is 10-15: 1 and the packing ratio is 35% -50%, and aligning the ballsGrinding the pot and vacuumizing to 1 × 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the working pressure in the ball milling tank is 1-100 Pa, and then carrying out ball milling for 3-24 h at the rotating speed of 150-300 r/min to obtain mechanical alloying metal powder;
step three, putting the mechanical alloying metal powder and the activator into a mixing tank, and vacuumizing to 1 × 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the pressure in the material mixing tank is 1-100 Pa, mixing materials for 1-5 hours at the rotating speed of 50-200 r/min, and obtaining mixed powder A;
putting the nickel-coated titanium carbide powder, the nickel-coated molybdenum powder, the nickel-coated tungsten powder and the dispersing agent into a mixer, and mixing for 1-5 hours at the rotating speed of 50-200 r/min to obtain mixed powder B;
dividing the mixed powder A into 5 equal parts by equal weight, and respectively recording as 1 st part, 2 nd part, 3 rd part, 4 th part and 5 th part; dividing the mixed powder B into 10 equal parts by weight;
step six, uniformly mixing the 1 st part of mixed powder A with 0 part of mixed powder B to obtain mixed powder AB 1; uniformly mixing the 2 nd part of mixed powder A with 1 part of mixed powder B to obtain mixed powder AB 2; uniformly mixing the 3 rd part of mixed powder A with the 2 nd part of mixed powder B to obtain mixed powder AB 3; and the rest in sequence, uniformly mixing the 5 th mixed powder A with the 4 th mixed powder B to obtain mixed powder AB 5;
step seven, taking the hot-pressing sintering grinding tool, and uniformly scattering the mixed powder AB1 in the hot-pressing sintering grinding tool to form a first powder layer II 21; then, uniformly scattering the mixed powder AB2 on the first powder layer II21 by the same method to form a second powder layer II 22; uniformly scattering the mixed powder AB3 on the second powder layer II22 to form a third powder layer II 23; by analogy, uniformly scattering the mixed powder AB5 on the fourth powder layer II24 to form a fifth powder layer II25, as shown in FIG. 2, wherein the second powder layer II22, the third powder layer II23, the fourth powder layer II24 and the fifth powder layer II25 contain thermal expansion coefficient adjusting powder 1;
step eight, will be equipped withThe hot-pressing sintering grinding tool with 5 layers of powder is put into a hot-pressing sintering furnace for vacuum hot isostatic pressing, and the vacuum degree of the static-pressing forming is 1 multiplied by 10-3～5×10-3Pa, the pressure is 15-100 MPa, the temperature is 600-650 ℃, and the time is 10-120 min; after the static pressure is finished, cooling to room temperature and taking out the static pressure blank; the thickness of the static pressure blank is not more than 3 mm;
and step nine, performing multi-pass cold rolling on the static pressure blank, wherein the pass deformation is 5% -30%, and then trimming and trimming to obtain the copper-based brazing filler metal with the gradient thermal expansion coefficient and the gradient thickness of 0.1-0.5 mm.
Example 3
The copper-based brazing filler metal with the gradient thermal expansion coefficient comprises, by weight, 72 parts of metal powder, 27 parts of thermal expansion coefficient adjusting powder, 0.2 part of an active agent and 0.8 part of a dispersing agent. The activating agent is a mixture of boron, borax, boric anhydride, potassium fluoride and potassium fluoborate, and the dispersing agent is at least one of silane coupling agent, polyethyleneimine, sodium dodecyl sulfate, hexadecyl trimethyl ammonium bromide and polyoxyethylene-based monoacrylate.
Specifically, the metal powder comprises 5 parts of tin, 5 parts of titanium, 5.5 parts of phosphorus, 5 parts of cobalt, 1 part of zinc, 1 part of indium, 1 part of manganese, 0.2 part of silicon, 0.1 part of cerium and the balance of copper; the thermal expansion coefficient adjusting powder comprises 8 parts by weight of nickel-coated titanium carbide, 60 parts by weight of nickel-coated molybdenum and 32 parts by weight of nickel-coated tungsten. The particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
The preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient comprises the following steps:
respectively weighing copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder and copper-cerium intermediate alloy powder for later use according to the weight parts of the metal powder;
respectively weighing nickel-coated titanium carbide powder, nickel-coated molybdenum powder and nickel-coated tungsten powder according to the weight parts of the thermal expansion coefficient adjusting powder for later use;
step two, weighing the copper powder and the tin in the step oneThe ball material ratio of the powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder, copper-cerium intermediate alloy powder and grinding balls is 10-15: 1. filling the mixture into a ball milling tank under the condition that the filler ratio is 35 to 50 percent, and vacuumizing the ball milling tank to 1 multiplied by 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the working pressure in the ball milling tank is 1-100 Pa, and then carrying out ball milling for 3-24 h at the rotating speed of 150-300 r/min to obtain mechanical alloying metal powder;
step three, putting the mechanical alloying metal powder and the activator into a mixing tank, and vacuumizing to 1 × 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the pressure in the material mixing tank is 1-100 Pa, mixing materials for 1-5 hours at the rotating speed of 50-200 r/min, and obtaining mixed powder A;
putting the nickel-coated titanium carbide powder, the nickel-coated molybdenum powder, the nickel-coated tungsten powder and the dispersing agent into a mixer, and mixing for 1-5 hours at the rotating speed of 50-200 r/min to obtain mixed powder B;
dividing the mixed powder A into 10 equal parts by weight, and respectively recording as 1 st part, 2 nd part, 3 rd part, … th part and 10 th part; dividing the mixed powder B into 45 equal parts by weight;
step six, uniformly mixing the 1 st part of mixed powder A with 0 part of mixed powder B to obtain mixed powder AB 1; uniformly mixing the 2 nd part of mixed powder A with 1 part of mixed powder B to obtain mixed powder AB 2; uniformly mixing the 3 rd part of mixed powder A with the 2 nd part of mixed powder B to obtain mixed powder AB 3; and the rest in sequence, uniformly mixing the 10 th mixed powder A with the 9 th mixed powder B to obtain mixed powder AB 10;
step seven, taking the hot-pressing sintering grinding tool, and uniformly scattering the mixed powder AB1 in the hot-pressing sintering grinding tool to form a first powder layer III 31; then, uniformly scattering the mixed powder AB2 on the first powder layer III31 by the same method to form a second powder layer III 32; uniformly scattering the mixed powder AB3 on the second powder layer III32 to form a third powder layer III 33; by analogy, uniformly scattering the mixed powder AB10 on the ninth powder layer III39 to form a tenth powder layer III 40; as shown in fig. 3, the second powder layer III32 and the third powder layer III33 …. the ninth powder layer III39 contains thermal expansion coefficient adjusting powder 1;
step eight, putting the hot-pressing sintering grinding tool filled with 10 layers of powder into a hot-pressing sintering furnace for vacuum hot isostatic pressing, wherein the vacuum degree of the static-pressing forming is 1 multiplied by 10-3～5×10-3Pa, the pressure is 15-100 MPa, the temperature is 600-650 ℃, and the time is 10-120 min; after the static pressure is finished, cooling to room temperature and taking out the static pressure blank; the thickness of the static pressure blank is not more than 3 mm;
and step nine, performing multi-pass cold rolling on the static pressure blank, wherein the pass deformation is 5% -30%, and then trimming and trimming to obtain the copper-based brazing filler metal with the gradient thermal expansion coefficient and the gradient thickness of 0.1-0.5 mm.
Example 4
The copper-based brazing filler metal with the gradient thermal expansion coefficient comprises 82 parts of metal powder, 16 parts of thermal expansion coefficient adjusting powder, 0.5 part of active agent and 1.5 parts of dispersing agent in parts by weight.
Specifically, the metal powder comprises 8 parts of tin, 3 parts of titanium, 4.5 parts of phosphorus, 5 parts of cobalt, 2 parts of zinc, 2 parts of indium, 2 parts of manganese, 0.3 part of silicon, 0.3 part of cerium and the balance of copper; the thermal expansion coefficient adjusting powder comprises, by weight, 5 parts of nickel-coated titanium carbide, 55 parts of nickel-coated molybdenum and 40 parts of nickel-coated tungsten. The particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
Specifically, the specific steps of the preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient are the same as those in example 1.
Specifically, the active agent is a mixture of boron, borax and potassium fluoride.
Specifically, the dispersing agent is a silane coupling agent.
Example 5
The copper-based brazing filler metal with the gradient thermal expansion coefficient comprises 82 parts of metal powder, 16 parts of thermal expansion coefficient adjusting powder, 0.5 part of active agent and 1.5 parts of dispersing agent in parts by weight.
The metal powder comprises 8 parts of tin, 3 parts of titanium, 4.5 parts of phosphorus, 5 parts of cobalt, 2 parts of zinc, 2 parts of indium, 2 parts of manganese, 0.3 part of silicon, 0.3 part of cerium and the balance of copper; the thermal expansion coefficient adjusting powder comprises, by weight, 5 parts of nickel-coated titanium carbide, 55 parts of nickel-coated molybdenum and 40 parts of nickel-coated tungsten. The particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
The specific steps of the preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient are the same as those in the embodiment 2.
Specifically, the active agent is a mixture of boron and potassium fluoride.
Specifically, the dispersant is polyethyleneimine.
Example 6
The copper-based brazing filler metal with the gradient thermal expansion coefficient comprises 82 parts of metal powder, 16 parts of thermal expansion coefficient adjusting powder, 0.5 part of active agent and 1.5 parts of dispersing agent in parts by weight.
Specifically, the metal powder comprises 8 parts of tin, 3 parts of titanium, 4.5 parts of phosphorus, 5 parts of cobalt, 2 parts of zinc, 2 parts of indium, 2 parts of manganese, 0.3 part of silicon, 0.3 part of cerium and the balance of copper; the thermal expansion coefficient adjusting powder comprises, by weight, 5 parts of nickel-coated titanium carbide, 55 parts of nickel-coated molybdenum and 40 parts of nickel-coated tungsten. The particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
Specifically, the specific steps of the preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient are the same as those in example 3.
Specifically, the activating agent is a mixture of borax, boric anhydride and potassium fluoborate.
Specifically, the dispersing agent is a mixture of sodium dodecyl sulfate and hexadecyl trimethyl ammonium bromide.
The melting temperature and the bending strength of the soldered 05Cr17Ni4Cu4Nb stainless steel and Si3N4 ceramic joint of the copper-based brazing filler metal with gradient thermal expansion coefficient prepared in the above examples are shown in Table 1.
TABLE 1
The optimal preparation method of the copper-based solder with the gradient thermal expansion coefficient is not limited to the preparation of copper-based solder, but also can be used for preparing other metal-based solders such as silver-based solder, nickel-based solder, gold-based solder, tin-based solder and the like, and the prepared solder is not limited to ceramic-metal solders and can be used for the soldering connection of any dissimilar materials with larger difference of thermal expansion coefficients.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (8)
1. The copper-based brazing filler metal with the gradient thermal expansion coefficient is characterized in that: the powder comprises 70-85 parts by weight of metal powder and 15-30 parts by weight of thermal expansion coefficient adjusting powder;
the metal powder comprises the following components in parts by weight: 5-10 parts of tin, 1-5 parts of titanium, 1-5.5 parts of phosphorus, 1-5 parts of cobalt, 1-3 parts of zinc, 1-3 parts of indium, 0.1-2.5 parts of manganese, 0.1-0.5 part of silicon, 0.1-0.5 part of cerium and the balance of copper;
the thermal expansion coefficient adjusting powder comprises 2-8 parts of nickel-coated titanium carbide, 40-60 parts of nickel-coated molybdenum and 15-40 parts of nickel-coated tungsten by weight;
the preparation method of the copper-based brazing filler metal with the gradient thermal expansion coefficient mainly comprises the following steps:
respectively weighing copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder and copper-cerium intermediate alloy powder for later use according to the weight parts of the metal powder;
respectively weighing nickel-coated titanium carbide powder, nickel-coated molybdenum powder and nickel-coated tungsten powder according to the weight parts of the thermal expansion coefficient adjusting powder for later use;
step two, carrying out mechanical alloying on the metal powder weighed in the step one to obtain mechanical alloying metal powder;
step three, putting the mechanical alloying metal powder prepared in the step two and an active agent into a mixing tank, and vacuumizing to 1 × 10-3～5×10-3Introducing argon with the purity of 99.99% after Pa, ensuring that the working pressure in the mixing tank is 1-100 Pa, mixing for 1-5 h under the condition that the rotating speed is 50-200 r/min, and obtaining mixed powder A;
putting the nickel-coated titanium carbide powder, the nickel-coated molybdenum powder, the nickel-coated tungsten powder and the dispersing agent weighed in the step one into a mixer, and mixing for 1-5 hours at the rotating speed of 50-200 r/min to obtain mixed powder B;
dividing the mixed powder A prepared in the third step into n equal parts by weight, and respectively marking as 1 st part, 2 nd part, … th part and nth part; dividing the mixed powder B prepared in the step four into n (n-1)/2 equal parts according to equal weight; the n equal parts are 3-10 parts;
step six, uniformly mixing the 1 st part of mixed powder A and 0 part of mixed powder B to obtain mixed powder AB 1; uniformly mixing the 2 nd part of mixed powder A and 1 part of mixed powder B to obtain mixed powder AB 2; uniformly mixing the 3 rd part of mixed powder A and 2 parts of mixed powder B to obtain mixed powder AB 3; and analogy is carried out in sequence, the nth mixed powder A and the n-1 mixed powder B are uniformly mixed to obtain mixed powder ABn;
step seven, taking a hot-pressing sintering grinding tool, and uniformly scattering the mixed powder AB1 obtained in the step six in the hot-pressing sintering grinding tool to form a first powder layer; then, uniformly scattering mixed powder AB2 on the first powder layer by the same method to form a second powder layer; uniformly scattering the mixed powder ABn on the (n-1) th powder layer by analogy to form an nth powder layer;
step eight, carrying out vacuum hot isostatic pressing on the n layers of powder prepared in the step seven to prepare a static-pressure blank, wherein the vacuum degree of the static-pressure forming is 1 in a large scale10-3～5×10-3Pa, the pressure is 15-100 MPa, the temperature is 600-650 ℃, and the time is 10-120 min; after the static pressure is finished, cooling to room temperature and taking out the static pressure blank; the thickness of the static pressure blank is not more than 3 mm;
and step nine, performing multi-pass cold rolling on the static-pressure blank prepared in the step eight, wherein the pass deformation is 5% -30%, and then trimming and trimming to obtain the copper-based brazing filler metal with the gradient thermal expansion coefficient and the gradient thickness of 0.1-0.5 mm.
2. The gradient copper-based solder with thermal expansion coefficient as claimed in claim 1, wherein: the copper-based brazing filler metal with the gradient thermal expansion coefficient further comprises 0.1-1 part of an active agent in parts by weight.
3. The gradient copper-based solder with thermal expansion coefficient as claimed in claim 2, wherein: the activating agent is a mixture of boron, borax, boric anhydride, potassium fluoride and potassium fluoborate.
4. The gradient copper-based solder with thermal expansion coefficient as claimed in claim 1, wherein: the copper-based brazing filler metal with the gradient thermal expansion coefficient also comprises 0.1-2 parts by weight of a dispersing agent.
5. The gradient copper-based solder with thermal expansion coefficient as claimed in claim 4, wherein: the dispersing agent is at least one of silane coupling agent, polyethyleneimine, sodium dodecyl sulfate, hexadecyl trimethyl ammonium bromide and polyoxyethylene monoacrylate.
6. The gradient copper-based solder with thermal expansion coefficient as claimed in claim 1, wherein: the particle size of the metal powder is 10-150 mu m; the particle size of the thermal expansion coefficient adjusting powder is 20-500 nm.
7. The copper-based solder with gradient coefficient of thermal expansion according to claim 1The preparation method is characterized by comprising the following steps: the step two of preparing the mechanical alloying metal powder comprises the following specific steps: the method comprises the steps of putting weighed copper powder, tin powder, titanium powder, cobalt powder, zinc powder, manganese powder, copper-silicon intermediate alloy powder, copper-indium intermediate alloy powder, copper-phosphorus intermediate alloy powder, copper-cerium intermediate alloy powder and grinding balls into a ball-milling tank under the conditions that the ball-material ratio is 10-15: 1 and the filler ratio is 35% -50%, vacuumizing the ball-milling tank to 1 x 10-3～5×10-3And introducing argon with the purity of 99.99% after Pa to ensure that the working pressure in the ball milling tank is 1-100 Pa, and then carrying out ball milling for 3-24 h at the rotating speed of 150-300 r/min to obtain the mechanical alloying metal powder.
8. The method for preparing the copper-based solder with the gradient thermal expansion coefficient according to claim 7, is characterized in that: the grinding ball is made of TiC.
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| CN111014867B (en) * | 2019-12-24 | 2022-03-01 | 新疆大学 | Laser brazing method for titanium alloy and ceramic dissimilar materials |
| CN112059470A (en) * | 2020-09-08 | 2020-12-11 | 中物院成都科学技术发展中心 | Active brazing filler metal for brazing titanate microwave dielectric ceramic and metal and preparation method thereof |
| CN112222671B (en) * | 2020-09-22 | 2021-12-28 | 西南交通大学 | Fuzzy algorithm-based composite solder component design method and system |
| CN117604307B (en) * | 2024-01-24 | 2024-03-26 | 崇义章源钨业股份有限公司 | Rare earth tungsten rod and preparation method thereof |
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