CN106825984A - The method for welding and solder preparation method of a kind of high-volume fractional SiCp/Al composites - Google Patents

Abstract

The invention relates to a brazing method of high volume fraction SiCp/Al composite material and a brazing filler metal preparation method. Brazing filler metal of the present invention is Al-Cu-Si-Mg quenching foil-shaped brazing filler metal, and its preparation method comprises the steps: one, material mixing; Two, prepare brazing filler metal blank; Three, refining brazing filler metal becomes alloy cylinder; Four, The alloy cylinder is made into a quenched foil-like solder by rapid stripping; it relates to a brazing method for a SiCp/Al composite material with a high volume fraction, which includes the following steps: 1. Pretreating the surface of the SiCp/Al composite material; 2. 1. Magnetron sputtering a Ti active layer on the pretreated surface of the SiCp/Al composite material; 3. Pretreatment of the surface to be welded; Step 4, vacuum brazing. The quenched foil-shaped brazing material obtained in the present invention can undergo metallurgical reaction with the Ti active layer and form a dense reaction layer, the brazing seam is well formed, the joint has high shear strength and air tightness, and can be widely used in high volume fraction SiCp/Al composite materials field of welding.

Description

A kind of brazing method and solder preparation of high volume fraction SiCp/Al composite material method

technical field

The invention belongs to the welding field of metal matrix composite materials, and relates to a brazing method and a brazing material preparation method of high volume fraction SiCp/Al composite materials.

Background technique

High volume fraction (55-75%) silicon carbide particle reinforced aluminum matrix composite (SiCp/Al) is one of the most promising materials among new materials, because of its high specific strength, high specific stiffness, high thermal conductivity Excellent characteristics such as low density and low thermal expansion coefficient have important application prospects in key components such as electronic packaging and aerospace, and become an ideal choice for replacing traditional electronic packaging materials such as Kovar, W/Cu and Mo/Cu, but due to high The introduction of the proportional SiC ceramic phase results in poor weldability of the aluminum matrix composite material, which makes its welding process quite difficult.

At present, the joining methods of high volume fraction SiCp/Al composite materials mainly include fusion welding, solid phase welding and brazing, among which brazing has the advantages of low heating temperature, small damage to the reinforcement phase, and large freedom of weldment size and shape. It is considered to be one of the more effective methods for welding such composite materials. A large number of studies have shown that improving the wettability of high volume fraction SiCp/Al composites can significantly improve the strength and airtightness of their brazed joints, which can be achieved by surface metallization and the development of active solders. Patent CN201510051866X proposes a vacuum brazing method for electroless Ni-plating assisted brazing of high volume fraction SiCp/Al composite materials, and the wettability of composite materials is greatly improved, but the electroless Ni-plating process introduces non-metallic element P into the coating, while The P element remaining in the brazing joint is easy to form welding defects such as inclusions, holes and cracks. Patent ZL2007100725364 proposes a welding method for ultrasonic-assisted brazing of high volume fraction SiCp/Al composite materials. The strength of the joint reaches the strength of the base metal. Since the brazing filler metal is Zn-Al brazing filler metal, the corrosion resistance and high temperature resistance of the brazing joint are poor, and the increase A set of ultrasonic equipment and the introduction of ultrasonic waves are affected when the shape is complex. The present invention aims to propose a brazing method and brazing filler metal preparation method for high volume fraction SiCp/Al composite materials, thereby effectively solving the problems of poor wettability and difficult connection of high volume fraction SiCp/Al composite materials, in order to obtain high strength , Brazed joints with good airtightness.

Contents of the invention

The purpose of the present invention is to provide a high volume fraction SiCp/Al composite material in order to solve the problems of poor wettability of the high volume fraction SiCp/Al composite material and low brazed joint strength and low air tightness under the existing welding process Brazing method and solder preparation method.

The technical scheme that the present invention adopts for solving its technical problem is:

A kind of brazing material preparation method of high volume fraction SiCp/Al composite material is carried out according to the following steps:

The first step, mixing materials: put Al, Cu elemental substance and Al-20Si master alloy with a good ratio of purity higher than 99.99% in the graphite crucible of the high vacuum induction melting furnace, and put the Al-50Mg master alloy in a rectangular In the stainless steel mold, the stainless steel mold is evacuated to 1×10 ^-3 Pa ~ 3×10 ^-3 Pa, and then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank: turn on the induction heating power supply, preheat the graphite crucible to 300 ° C ~ 400 ° C, and then heat the graphite crucible to 1500 ° C ~ 1600 ° C within 6 minutes ~ 10 minutes, so that the metal raw materials in the graphite crucible Melt completely and keep it warm for 20-30 minutes, then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution fully mix with the Al-50Mg master alloy, then cool naturally to room temperature for shaping, Prepared into brazing material blank;

The third step is to refine the brazing material into an alloy cylinder: firstly, the brazing material blank prepared in the second step is taken out from the stainless steel mold, and after removing the surface oxide skin, it is placed in the graphite crucible of the induction melting furnace again, and then it is processed according to the first step. According to the method in the second step, vacuumize the melting furnace and then fill it with argon, heat the graphite crucible to 750 ° C ~ 800 ° C, so that the metal raw materials in the graphite crucible are completely melted, use a stirring rod to stir the alloy solution for 1 min ~ 2 min, And keep it warm for 10min~20min, finally shake the crucible so that the alloy liquid breaks through the surface oxide film shell and smoothly pours into the columnar stainless steel mold, and obtains the solder alloy cylinder with the furnace cooling;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed on the In the induction coil in the furnace cavity of the vacuum belt throwing machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be 1.5 mm to ^1.7 mm ^; After ³ Pa, argon gas is introduced; then start the copper roller rotation control switch, adjust the copper roller speed to 1200r/min~1500r/min, turn on the induction heating power supply, adjust the current to 11A~12A, heat for 2min~4min, the brazing in the quartz tube After the material alloy is completely melted, 1 × 10 ^-2 Pa ~ 5 × 10 ^-2 Pa argon gas is introduced into the quartz tube, and the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating On the copper roll, the Al-Si-Cu-Mg foil-like solder is finally obtained.

The composition of the Al-Si-Cu-Mg foil-shaped solder obtained by the solder preparation method is: 5.0% to 6.2% Si, 19.6% to 28.6% Cu, 1.2% to 2.5% Mg and the balance by mass percentage Al composition.

A kind of brazing method of high volume fraction SiCp/Al composite material, utilizes the Al-Si-Cu-Mg foil-shaped brazing material that above-mentioned preparation method makes, according to following steps:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, and then etched in an aqueous NaOH solution with a concentration of 6% to 8% for 25s to 30s. Then ultrasonically wash for 15min-20min, then ultrasonically clean in alcohol-acetone mixture for 15min-20min, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material pretreated in the first step in a vacuum magnetron sputtering equipment, and sputter and deposit Ti with a thickness of 4 μm to 6 μm active layer;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 15-20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Cu-Si-Mg foil solder, and place it in vacuum brazing at 15°C/min～20 Heat up to 450°C at the speed of ℃/min, keep it warm for 5min-8min, then raise the temperature to 545°C-575°C at the speed of 10°C/min-15°C/min, keep it warm for 10min-30min, then cool down to room temperature with the furnace, and the process is complete Welding of high volume fraction SiCp/Al composites.

Further, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a volume content of SiC ceramic phase higher than 55%.

Compared with the prior art, the present invention has the beneficial effects that: the present invention adopts Al-Cu-Si-Mg quenching foil-shaped solder to vacuum braze the high volume fraction SiCp/Al composite material after magnetron sputtering Ti active layer , the metallurgical reaction between the brazing filler metal and the Ti active layer generates ternary intermetallic compounds such as rod-shaped Ti-Al-Si or Ti-Al-Cu, the interface is well bonded, the brazing filler metal and the base metal are tightly connected, and the joint strength is high; the invention obtains The SiCp/Al composite material vacuum brazed joint can achieve the performance index of shear strength up to 120MPa and air tightness up to 10 ^-9 Pa∙m ³ /s.

Description of drawings

Figure 1 is the light microscope image of the microstructure of the 60% volume fraction SiCp/Al composite material.

Fig. 2 is a scanning electron microscope image after magnetron sputtering Ti active layer on the surface of SiCp/Al composite material with high volume fraction to be welded.

Fig. 3 is a typical scanning electron microscope image of the brazed joint of the present invention.

detailed description

The present invention will be further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.

Example 1

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 26.7%Cu, 5.25%Si, 1.5%Mg and the balance of Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank: turn on the induction heating power supply, preheat the graphite crucible to 300 ° C ~ 400 ° C, and then heat the graphite crucible to 1500 ° C ~ 1600 ° C within 10 minutes to completely melt the metal raw materials in the graphite crucible , and keep it warm for 20min, and then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution and the Al-50Mg master alloy fully mixed, and then naturally cool to room temperature and shape to prepare a brazing filler metal blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder refined alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed on the In the induction coil in the furnace cavity of the vacuum strip machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be 1.5mm; then vacuumize the cavity of the strip machine to 1×10 ^-3 Pa and then pass in argon gas; then start Copper roller rotation control switch, adjust the copper roller speed to 1500r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the solder alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon gas into the quartz tube , and the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain a solder foil, and the resulting Al-Si-Cu-Mg foil-shaped solder The composition is 26.7% Cu, 5.25% Si, 1.5% Mg, 66.55% Al.

A brazing method of a high volume fraction SiCp/Al composite material, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a volume content of 60% of the SiC ceramic phase, as shown in Figure 1, using the above method The Al-Si-Cu-Mg foil solder of gained, according to the steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the alcohol-acetone mixture for 20 minutes, take it out and dry it;

The second step is to carry out magnetron sputtering Ti active layer on the surface to be welded: the SiCp/Al composite material treated in the first step is placed in a vacuum magnetron sputtering device, and a Ti active layer with a thickness of 5 μm is deposited by sputtering (such as as shown in Figure 2);

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 5 minutes, then raise the temperature to 550°C at a rate of 10°C/min, hold for 20 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this embodiment reaches 121.2 MPa. The scanning electron microscope photo of the brazed joint in this embodiment is shown in Figure 3. The interface of the joint is well bonded, the solder and the base metal are tightly connected, and there is an obvious reaction layer. It is a rod-shaped Ti-Al-Si or Ti-Al-Cu ternary intermetallic compound phase, and these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the joint strength.

Example 2

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 20.0%Cu, 6.0%Si, 1.5%Mg and the balance of Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank: turn on the induction heating power supply, preheat the graphite crucible to 300 ° C ~ 400 ° C, and then heat the graphite crucible to 1500 ° C ~ 1600 ° C within 10 minutes to completely melt the metal raw materials in the graphite crucible , and keep it warm for 20min, and then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution and the Al-50Mg master alloy fully mixed, and then naturally cool to room temperature and shape to prepare a brazing filler metal blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed in a vacuum In the induction coil in the furnace chamber of the belt throwing machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be ^1.5mm ; Roller rotation control switch, adjust the copper roller speed to 1500r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the brazing alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon gas into the quartz tube, And the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain the solder foil. The composition of the obtained Al-Si-Cu-Mg foil-shaped solder is It is 20% Cu, 6% Si, 1.5% Mg, 72.5% Al.

A brazing method of a high volume fraction SiCp/Al composite material, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a volume content of 60% of the SiC ceramic phase, as shown in Figure 1, using the above method The Al-Si-Cu-Mg foil solder of gained, according to the steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the alcohol-acetone mixture for 20 minutes, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material treated in the first step in a vacuum magnetron sputtering device, and sputter deposit a Ti active layer with a thickness of 5 μm;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 5 minutes, then raise the temperature to 550°C at a rate of 10°C/min, hold for 20 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this example reaches 122 MPa. The interface of the brazed joint in this example is well bonded, the solder and the base metal are closely connected, and there is an obvious reaction layer, mainly rod-shaped Ti-Al-Si or Ti-Al -Cu ternary intermetallic compound phase, these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the joint strength.

Example 3

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 28% Cu, 6% Si, 2% Mg and the balance Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank, turn on the induction heating power supply, preheat the graphite crucible to 300 ℃ ~ 400 ℃, and then heat the graphite crucible to 1500 ℃ ~ 1600 ℃ within 10 minutes to completely melt the metal raw materials in the graphite crucible , and keep it warm for 20min, and then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution and the Al-50Mg master alloy fully mixed, and then naturally cool to room temperature and shape to prepare a brazing filler metal blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed in a vacuum In the induction coil in the furnace chamber of the belt throwing machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be ^1.5mm ; Roller rotation control switch, adjust the copper roller speed to 1500r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the brazing alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon gas into the quartz tube, And the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain the solder foil. The composition of the obtained Al-Si-Cu-Mg foil-shaped solder is It is 28% Cu, 6% Si, 2% Mg, 64% Al.

A brazing method of a high volume fraction SiCp/Al composite material, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a volume content of 60% of the SiC ceramic phase, as shown in Figure 1, using the above method The Al-Si-Cu-Mg foil solder of gained, according to the steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the mixture of alcohol and acetone for 20 minutes, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material treated in the first step in a vacuum magnetron sputtering device, and sputter deposit a Ti active layer with a thickness of 5 μm;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 5 minutes, then raise the temperature to 550°C at a rate of 10°C/min, hold for 20 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this example reaches 120 MPa. The interface of the brazed joint in this example is well bonded, the solder and the base metal are closely connected, and there is an obvious reaction layer, mainly rod-shaped Ti-Al-Si or Ti-Al -Cu ternary intermetallic compound phase, these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the joint strength.

Example 4

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 26.7%Cu, 5.25%Si, 1.5%Mg and the balance of Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank: turn on the induction heating power supply, preheat the graphite crucible to 300 ° C ~ 400 ° C, and then heat the graphite crucible to 1500 ° C ~ 1600 ° C within 10 minutes to completely melt the metal raw materials in the graphite crucible , and keep it warm for 20min, and then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution and the Al-50Mg master alloy fully mixed, and then naturally cool to room temperature and shape to prepare a brazing filler metal blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed in a vacuum In the induction coil in the furnace chamber of the belt throwing machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be ^1.5mm ; Roller rotation control switch, adjust the copper roller speed to 1500r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the brazing alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon gas into the quartz tube, And the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain the solder foil. The composition of the obtained Al-Si-Cu-Mg foil-shaped solder is It is 26.7% Cu, 5.25% Si, 1.5% Mg, 66.55% Al.

A brazing method for a high volume fraction SiCp/Al composite material, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a SiC ceramic phase volume content higher than 55%, and the Al- Si-Cu-Mg foil solder, follow the steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the alcohol-acetone mixture for 20 minutes, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material treated in the first step in a vacuum magnetron sputtering device, and sputter deposit a Ti active layer with a thickness of 6 μm;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 8 minutes, then raise the temperature to 560°C at a rate of 10°C/min, hold for 20 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this example reaches 121 MPa. The interface of this example is well bonded, the solder and the base metal are closely connected, and there is an obvious reaction layer, mainly rod-shaped Ti-Al-Si or Ti-Al-Cu three Elemental intermetallic compound phase, these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the strength of the joint.

Example 5

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 26.7%Cu, 5.25%Si, 1.5%Mg and the balance of Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank, turn on the induction heating power supply, preheat the graphite crucible to 300 ℃ ~ 400 ℃, and then heat the graphite crucible to 1500 ℃ ~ 1600 ℃ within 10 minutes to completely melt the metal raw materials in the graphite crucible , and keep it warm for 20min, and then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution and the Al-50Mg master alloy fully mixed, and then naturally cool to room temperature and shape to prepare a brazing filler metal blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed in a vacuum In the induction coil in the furnace chamber of the belt throwing machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be ^1.5mm ; Roller rotation control switch, adjust the copper roller speed to 1250r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the brazing alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon into the quartz tube, And the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain the solder foil. The composition of the obtained Al-Si-Cu-Mg foil-shaped solder is It is 26.7% Cu, 5.25% Si, 1.5% Mg, 66.55% Al.

A brazing method for a high volume fraction SiCp/Al composite material, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a volume content of 60% of the SiC ceramic phase, and the Al-Si- Cu-Mg foil solder, follow the steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the alcohol-acetone mixture for 20 minutes, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material treated in the first step in a vacuum magnetron sputtering device, and sputter deposit a Ti active layer with a thickness of 4 μm;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 5 minutes, then raise the temperature to 570°C at a rate of 10°C/min, hold for 20 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this example reaches 121.5 MPa. The interface of the brazed joint in this example is well bonded, the brazing filler metal is closely connected with the base metal, and there is an obvious reaction layer, which is mainly rod-shaped Ti-Al-Si or Ti- Al-Cu ternary intermetallic compound phase, these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the joint strength.

Example 6

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 26.7%Cu, 5.25%Si, 1.5%Mg and the balance of Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank, turn on the induction heating power supply, preheat the graphite crucible to 300 ° C ~ 400 ° C, and then heat the graphite crucible to 1500 ° C ~ 1600 ° C within 6 minutes ~ 10 minutes, so that the metal raw materials in the graphite crucible Melt completely, keep it warm for 20 minutes, then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution fully mix with the Al-50Mg master alloy, then cool naturally to room temperature and shape, and prepare the Brazing blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder refined alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed on the In the induction coil in the furnace cavity of the vacuum strip machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be 1.5mm; then vacuumize the cavity of the strip machine to 1×10 ^-3 Pa and then pass in argon gas; then start Copper roller rotation control switch, adjust the copper roller speed to 1400r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the solder alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon gas into the quartz tube , and the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain a solder foil, and the resulting Al-Si-Cu-Mg foil-shaped solder The composition is 26.7% Cu, 5.25% Si, 1.5% Mg, 66.55% Al.

A brazing method for a high volume fraction SiCp/Al composite material, the high volume fraction SiCp/Al composite material is an aluminum-based composite material with a SiC ceramic phase volume content higher than 55%, and the Al- Si-Cu-Mg foil solder, follow the steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the alcohol-acetone mixture for 20 minutes, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material treated in the first step in a vacuum magnetron sputtering device, and sputter deposit a Ti active layer with a thickness of 5 μm;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 5 minutes, then raise the temperature to 550°C at a rate of 10°C/min, hold for 20 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this example reaches 121.2MPa. The interface of the brazed joint in this example is well bonded, the brazing filler metal is closely connected with the base metal, and there is an obvious reaction layer, which is mainly rod-shaped Ti-Al-Si or Ti- Al-Cu ternary intermetallic compound phase, these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the joint strength.

Example 7

A method for preparing brazing material of high volume fraction SiCp/Al composite material, comprising the steps of:

The first step, mixing materials: according to the mass ratio of 26.7%Cu, 5.25%Si, 1.5%Mg and the balance of Al, the raw materials of pure Al, pure Cu, Al-20Si, Al-50Mg are mixed, and then pure Al, Cu simple substance and Al-20Si master alloy are placed in the graphite crucible of the high vacuum induction melting furnace, and the Al-50Mg master alloy is placed in the stainless steel mold, and the stainless steel mold is evacuated to 1×10 ^-3 Pa～3× 10 ^-3 Pa, then filled with high-purity argon until the pressure inside the stainless steel mold is 0MPa;

The second step is to prepare the brazing material blank, turn on the induction heating power supply, preheat the graphite crucible to 300 ℃ ~ 400 ℃, and then heat the graphite crucible to 1500 ℃ ~ 1600 ℃ within 10 minutes to completely melt the metal raw materials in the graphite crucible , and keep it warm for 20min, and then quickly pour the alloy solution into a stainless steel mold to melt the Al-50Mg master alloy, and make the alloy solution and the Al-50Mg master alloy fully mixed, and then naturally cool to room temperature and shape to prepare a brazing filler metal blank;

The third step is to refine the brazing material into an alloy cylinder: first, take out the brazing material blank prepared in the second step from the stainless steel mold, remove the surface oxide skin and put it back in the graphite crucible of the induction melting furnace, and then follow the first step to process the Vacuumize the melting furnace and fill it with argon. Follow the second step to heat the graphite crucible to 750°C to 800°C to completely melt the metal material in the graphite crucible. Use a stirring rod to stir the alloy solution for 1 minute and keep it warm for 10 minutes. Finally, shake the crucible to make The alloy liquid breaks through the shackles of the oxide film shell on the surface and pours smoothly into the columnar stainless steel mold, and at the same time keeps the oxide film shell in the graphite crucible, and the solder cools with the furnace to obtain the alloy column;

The fourth step is to make the alloy cylinder into a quenched state foil-shaped solder through rapid stripping: firstly, the solder refined alloy cylinder prepared in the third step is cleaned and placed in a quartz tube, and the quartz tube is fixed on the In the induction coil in the furnace cavity of the vacuum strip machine, adjust the distance between the nozzle at the lower end of the quartz tube and the copper roller to be 1.5mm; then vacuumize the cavity of the strip machine to 1×10 ^-3 Pa and then pass in argon gas; then start Copper roller rotation control switch, adjust the copper roller speed to 1500r/min, turn on the induction heating power supply, adjust the current to 11A, heat for 3min, after the solder alloy in the quartz tube is completely melted, pass 1×10 ^-2 Pa argon gas into the quartz tube , and the molten solder is sprayed from the nozzle at the lower end of the quartz tube to the high-speed rotating copper roller under the action of the gas pressure difference to obtain a solder foil, and the resulting Al-Si-Cu-Mg foil-shaped solder The composition is 26.7% Cu, 5.25% Si, 1.5% Mg, 66.55% Al.

A kind of brazing method of high volume fraction SiCp/Al composite material, described high volume fraction SiCp/Al composite material as shown in Figure 1 is the aluminum matrix composite material of the volume content 60% of SiC ceramic phase, as shown in Figure 1 Show, utilize the Al-Si-Cu-Mg foil shape brazing material that above-mentioned method gains, according to steps as follows:

The first step is to pretreat the surface of the SiCp/Al composite material to be welded: firstly, the surface of the SiCp/Al composite material is smoothed with 400# sandpaper, then etched in a 7% NaOH aqueous solution for 26 seconds, and then ultrasonically washed for 15 minutes. Then ultrasonically clean the alcohol-acetone mixture for 20 minutes, take it out and dry it;

The second step is to perform magnetron sputtering Ti active layer on the surface to be welded: place the SiCp/Al composite material treated in the first step in a vacuum magnetron sputtering device, and sputter deposit a Ti active layer with a thickness of 6 μm;

The third step, retreatment of the surface to be welded and solder pretreatment: put the SiCp/Al composite material and Al-Si-Cu-Mg foil solder after the magnetron sputtering Ti active layer into the alcohol-acetone mixture Ultrasonic cleaning for 20 minutes, take out the cold air and dry it for later use;

The fourth step, vacuum brazing: assemble the SiCp/Al composite material of the surface magnetron sputtered Ti active layer with Al-Si-Cu-Mg foil solder, and place it in vacuum brazing at a speed of 20°C/min Raise the temperature to 450°C, hold for 5 minutes, then raise the temperature to 570°C at a rate of 10°C/min, hold for 10 minutes, and then cool to room temperature with the furnace to complete the welding of high volume fraction SiCp/Al composite materials.

The shear strength of the brazed joint obtained in this example reaches 125.2 MPa. The interface of the brazed joint in this example is well bonded, the brazing material is closely connected with the base metal, and there is an obvious reaction layer, mainly rod-shaped Ti-Al-Si or Ti- Al-Cu ternary intermetallic compound phase, these compounds exist at the connection interface between the Ti active layer and the solder, and play a pinning role, thereby improving the joint strength.

The scope of protection of this invention is not limited to the content on the description, and any technical deformation that is the same as the above-mentioned implementation structure or based on the technical principle of the present invention belongs to the scope of protection required by the present invention.

Claims (4)

1. a kind of solder preparation method of high-volume fractional SiCp/Al composites, it is characterised in that enter in accordance with the following steps OK：

The first step, batch mixing：Al, Cu simple substance of the purity that will have been matched higher than 99.99% and Al-20Si intermediate alloys are placed in height In the graphite crucible of vacuum induction melting furnace, and Al-50Mg intermediate alloys are placed in rectangle stainless steel mould, and by stainless steel Mould is evacuated to 1 × 10^-3Pa~3 × 10^-3Pa, it is 0MPa to be then charged with air pressure in high-purity argon gas to stainless steel mould；

Second step, prepares solder blank：Open induction heating power, preheating graphite crucible to 300 DEG C~400 DEG C, Ran Hou Graphite crucible is heated to 1500 DEG C~1600 DEG C in 6min~10min times, makes the raw metal in graphite crucible melt Entirely, and 20min~30min is incubated, then alloy solution is poured into stainless steel mould rapidly, so as to rush in the middle of molten Al-50Mg Alloy, and cause that alloy solution is sufficiently mixed with Al-50Mg intermediate alloys, it is moulding then to naturally cool to normal temperature, is prepared into pricker Material blank；

3rd step, concise solder is into alloy cylinder：The solder blank that will be prepared in second step first takes out from stainless steel mould, goes Except being replaced in the graphite crucible of induction melting furnace after surface scale, smelting furnace is entered according to the method in the first step then Row vacuumizes then applying argon gas, and graphite crucible is heated to 750 DEG C~800 DEG C according to the method in second step, makes in graphite crucible Raw metal fusing it is complete, stir aluminium alloy 1min~2min using stirring rod, and be incubated 10min~20min, finally shake Crucible makes aluminium alloy break through the constraint of surface film oxide shell and smoothly pour into column stainless steel mould, and furnace cooling obtains solder Alloy cylinder；

4th step, by alloy cylinder through quickly getting rid of band is made chilling state foil-shaped brazing material：To prepare by the 3rd step first Brazing filler metal alloy cylinder is placed in quartz ampoule after cleaning up, and quartz ampoule is fixed on into vacuum gets rid of with the induction coil in machine furnace chamber In, the spacing of adjustment quartz ampoule lower end nozzle to copper roller is 1.5mm~1.7mm；Then it is evacuated to 1 to getting rid of band machine cavity body × 10^-3Pa~3 × 10^-3Argon gas is passed through after Pa；Then start copper roller rotary control switch, regulation copper roller rotating speed to 1200r/min~ 1500r/min, opens induction heating power, and regulation electric current to 11A~12A heats 2min~4min, and the solder in quartz ampoule is closed Gold be completely melt after to being passed through 1 × 10 in quartz ampoule^-2Pa~5 × 10^-2Pa argon gas, and molten solder is made in gas pressure difference Under, it is sprayed onto from the nozzle of quartz ampoule lower end on the copper roller of rotation at a high speed, it is final to obtain Al-Si-Cu-Mg foil-shaped brazing materials.

2. a kind of solder preparation method of high-volume fractional SiCp/Al composites according to claim 1, its feature exists In the composition of the Al-Si-Cu-Mg foil-shaped brazing materials as obtained by solder preparation method is：By mass percentage by 5.0%~6.2% The Al compositions of Si, 19.6%~28.6%Cu, 1.2%~2.5%Mg and surplus.

3. a kind of method for welding of high-volume fractional SiCp/Al composites, it is characterised in that using described in claim 2 Al-Si-Cu-Mg foil-shaped brazing materials, in accordance with the following steps：

The first step, SiCp/Al composite welding surfaces are pre-processed：SiCp/Al composite material surfaces are used first 400# sand paperings are smooth, and 25s~30s is then corroded in the NaOH aqueous solution that concentration is 6%~8%, then ultrasound washing 15min~20min, then ultrasound cleaning 15min~20min in alcohol-acetone mixture, taking-up are dried；

Second step, welding surface carries out magnetron sputtering Ti active layers：Will be by the pretreated SiCp/Al composites of the first step It is placed in vacuum magnetic-control sputtering equipment, sputtering sedimentation thickness is 4 μm~6 μm of Ti active layers；

3rd step, welding surface reprocessing and solder pretreatment：By the SiCp/Al composites after magnetron sputtering Ti active layers and Al-Si-Cu-Mg foil-shaped brazing materials are put into ultrasound cleaning 15min~20min in alcohol-acetone mixture, take out cold wind drying and treat With；

4th step, vacuum brazing：The SiCp/Al composites of surface magnetic control sputtering Ti active layers are assembled into Al-Cu-Si-Mg paper tinsels Shape solder, is placed in vacuum brazing, and 450 DEG C are warming up to the speed of 15 DEG C/min~20 DEG C/min, is incubated 5min~8min, then 545 DEG C~575 DEG C are warming up to the speed of 10 DEG C/min~15 DEG C/min, 10min~30min is incubated, then cooled to the furnace Room temperature, that is, complete the welding of high-volume fractional SiCp/Al composites.

4. the method for welding of a kind of high-volume fractional SiCp/Al composites according to claim 3, it is characterised in that Described high-volume fractional SiCp/Al composites are the aluminum matrix composite of the volume content higher than 55% of SiC ceramic phase.