CN113122837A - AgCuTiX alloy foil brazing filler metal based on cold spraying process and preparation method thereof - Google Patents
AgCuTiX alloy foil brazing filler metal based on cold spraying process and preparation method thereof Download PDFInfo
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- CN113122837A CN113122837A CN202110446105.XA CN202110446105A CN113122837A CN 113122837 A CN113122837 A CN 113122837A CN 202110446105 A CN202110446105 A CN 202110446105A CN 113122837 A CN113122837 A CN 113122837A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
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Abstract
The invention belongs to the technical field of metal material manufacturing, and particularly relates to a preparation method of an AgCuTiX alloy foil brazing filler metal based on a cold spraying process, which comprises the following steps: preparing AgCu alloy powder according to the component proportion of the AgCuTiX alloy brazing filler metal; uniformly mixing AgCu alloy powder and Ti powder according to the component proportion of the AgCuTiX alloy brazing filler metal; inputting the mixed powder into a powder feeding system of a cold spraying system, carrying out ultrasonic rapid cold spraying by adopting inactive gas, colliding the mixed powder particles to an AgCuTiX matrix made of the same material at supersonic speed, and depositing to a certain thickness to form an AgCuTiX alloy blank plate; and annealing the AgCuTiX alloy blank, and then performing multi-pass cold rolling forming treatment to finally obtain the AgCuTiX alloy foil brazing filler metal. In the forming process of the cold spraying blank plate, the pre-alloyed silver-copper alloy powder is taken as a base, and pure titanium powder/X powder is doped according to the proportion of the final alloy. The cold spraying process is close to the plastic deformation, cold welding and mechanical alloying of powder particles, and the Ti element is always in a stable state in the processing flow, so that the Ti element still has high activity during brazing.
Description
Technical Field
The invention belongs to the technical field of metal material manufacturing, and particularly relates to an AgCuTiX alloy foil brazing filler metal based on a cold spraying process and a preparation method thereof.
Background
The AgCuTi solder as an active solder has excellent conductivity and corrosion resistance, proper solid/liquid phase line temperature, excellent wettability and higher soldered joint strength. The AgCuTi brazing filler metal is mainly applied to brazing between ceramics and between metals and ceramics; and the successful brazing of ceramics and ceramic and metal components can be realized without carrying out complex metallization pretreatment on the surface of the ceramics. The active brazing filler metal containing Ti is always the key point and hot direction of ceramic connection research, but the processing and forming performance of the AgCuTi active brazing filler metal is poor, the difficulty of foil strip preparation is high, and the technical bottleneck which troubles the processing of the AgCuTi active brazing filler metal foil strip is formed.
The AgCuTi active brazing filler metal foil strip on the market at present has two main flow manufacturing process flows:
the first method is to adopt electric arc melting or vacuum induction melting AgCuTi alloy, cast a spindle, and then plastically process the alloy into foil strip-shaped brazing filler metal through subsequent hot rolling and cold rolling processes. The process has the following process difficulties: 1) the density difference of several metals is large, and the problems of uneven internal structure and segregation of alloy components of the ingot are difficult to solve when the ingot is smelted; 2) The activity of Ti element is very high, and Ti is easy to combine with O, N and other gas elements in the processes from smelting, ingot casting to the subsequent plastic pressing processing, so that the performance of AgCuTi solder is deteriorated and the activity of the solder is reduced. 3) During vacuum melting, Ti element is easy to react with crucible materials, so that the quality of an alloy ingot is influenced, and the difficulty of large-scale production of the active brazing filler metal is caused. 4) When the alloy is smelted at high temperature, Ti element and alloy components such as Ag, Cu and the like can form brittle intermediate phases such as Ag-Ti, Cu-Ti and the like, so that the processing performance and the mechanical property of the AgCuTi alloy are further reduced, and the AgCuTi alloy is difficult to roll into a high-quality foil strip.
The second method is to adopt a powder metallurgy process to process Ag powder, Cu powder and Ti powder into foil strips through ball milling, hot isostatic pressing, vacuum sintering, multi-pass rolling-annealing and other processes.
Therefore, the two traditional methods have limitations in the preparation of the AgCuTi foil brazing filler metal. Therefore, a new process technology is urgently needed to fundamentally solve the process problems.
The invention aims to overcome the defects of the existing AgCuTi brazing filler metal forming technology, provides a new process technology, and innovatively applies a high-pressure pneumatic cold spraying technology to the manufacturing process of the AgCuTiX brazing filler metal for the first time. Specifically, in the cold spray forming process, pre-alloyed silver-copper alloy powder is used as a base, pure titanium powder and X powder are doped according to the proportion of the final alloy, then the mixed powder is collided to an AgCuTiX matrix made of the same material at supersonic speed by a cold spray process, the process is close to the situation that powder particles are subjected to plastic deformation and cold welding, and mechanical alloying is completed in the cold spray process. And then, performing compression plastic processing on the blank plate obtained by cold spraying, so as to further promote the homogenization and fusion of the AgCuTiX alloy elements. The process can produce high-quality AgCuTiX foil brazing filler metal which has uniform components, low oxygen content, average grain size of below 10 microns, excellent mechanical property and density of more than 99.8 percent and meets the technical requirement of vacuum welding. Meanwhile, because the temperature in the cold spraying process is lower, the Ti element is always in a stable state in the whole process flow, and the high activity of the Ti element during brazing is ensured. The process directly avoids a series of process problems of component segregation of alloy components, high-temperature oxidation and nitridation of active element Ti, reaction with crucible materials, material brittleness caused by the generation of brittle intermediate phases such as Ag-Ti, Cu-Ti and the like in smelting and the like in the traditional process, and has important application value.
In addition, the present invention has a high production flexibility: ti elements which have highest activity and are easy to cause process problems in the brazing alloy components are independently controlled in a powder form and added according to the formula proportion in the cold spraying process stage, so that the diversified requirements of the AgCuTiX foil brazing alloy product formula are met in a simpler mode, and AgCu28 required by the market is produced; AgCuTi; AgCuTiSn; series of foil brazing filler metal products such as AgCuInTi.
The AgCuTiX alloy foil brazing filler metal product can meet the brazing application requirements of ceramics, metals, ceramics and carbon materials in the field of vacuum welding, and has a good commercial application prospect.
Disclosure of Invention
The invention aims to: aiming at the technical problem that the existing AgCuTi alloy brazing filler metal is difficult to produce high-quality foil strips, the preparation method of the AgCuTiX alloy foil strip brazing filler metal based on the cold spraying process is provided, and the ultra-sonic cold spraying technology is innovatively applied to the manufacturing flow of the AgCuTiX brazing filler metal for the first time. Specifically, in the cold spray forming process, pre-alloyed silver-copper alloy powder is used as a base, pure titanium powder and X powder are doped according to the proportion of the final alloy, then the AgCuTiX brazing filler metal blank plate capable of accurately controlling the components is prepared by a cold spray process, and then the blank plate is subjected to rolling processing, so that the high-activity AgCuTiX foil brazing filler metal which is uniform in components, low in oxygen content, excellent in mechanical property, high in density of 99.8% and capable of meeting the technical requirements of vacuum welding is finally produced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of AgCuTiX alloy foil brazing filler metal based on a cold spraying process at least comprises the following steps:
firstly, preparing Ag and Cu raw material ingots into AgCu alloy powder according to the component proportion of the AgCuTiX alloy brazing filler metal;
step two, weighing cold spraying Ti powder and X powder according to the component proportion of the AgCuTiX alloy brazing filler metal, and uniformly mixing the AgCu alloy powder obtained in the step one with the cold spraying Ti powder to obtain mixed powder;
inputting the mixed powder obtained in the step two into a powder feeding system of a cold spraying system, and carrying out cold spraying by adopting inactive gas to form an AgCuTiX alloy blank;
step four, annealing the AgCuTiX alloy blank obtained in the step three to eliminate internal stress generated in the blank processing process to obtain an AgCuTiX blank;
step five, carrying out multi-pass cold rolling forming treatment on the AgCuTiX blank obtained in the step four until the AgCuTiX alloy foil strip brazing filler metal with the required thickness is obtained;
wherein X is at least one of In, Zr, Sn, Zn, Cd and Ni, and the sum of the mass fractions of X and Ti is 0-10%. Wherein, the mass fractions of Ti and X can both be 0 or not, preferably, the mass fraction of Ti is not 0, and the mass fraction of X is 0; or the mass fraction of Ti is not 0, and the mass fraction of X is not 0, namely the formula of the invention is not limited to adding pure Ti powder, and other metal materials can be additionally added as components to obtain better comprehensive performance.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, the preparation process of AgCu alloy powder in the step one is as follows: and putting the Ag ingot and the Cu ingot into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu alloy spherical powder by adopting a gas atomization process.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, the AgCu alloy spherical powder prepared in the first step consists of 40-95% of Ag and 5-60% of Cu by mass percent, and the temperature of vacuum induction melting is 950-1150 ℃; the gas adopted by the atomization process is high-purity nitrogen, and a supersonic gas atomization nozzle is adopted, wherein the atomization pressure is 2.5-4.5 MPa.
Before the second step, the method further comprises the step of selecting AgCu alloy powder with the size meeting the requirement from the AgCu alloy powder obtained in the first step, wherein the AgCu alloy powder with the size meeting the requirement refers to powder with the particle size distribution of 1-45 microns, and the preferable particle size range is 5-38 microns; the cold spraying Ti powder is spherical titanium powder prepared by a fuse wire atomization method or a plasma atomization method, the purity is 4N grade, the particle size range is 1-45 micrometers, and the preferred particle size range is 5-38 micrometers. The purity of the X powder is higher than 3N grade, and the particle size range is 0.1-20 microns.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, in the mixed powder obtained in the step two, except for AgCu, Ti and other components X account for 0-10% by weight; and mixing in the second step adopts a V-shaped mixer, and the mixing time is 12-24 hours.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, the cold spraying system in the third step comprises a powder feeding system, a high-pressure gas source, a gas heater for heating the high-pressure gas source, a gas adjusting and controlling system for adjusting the pressure of gas sent out by the high-pressure gas source and a spray gun. The spray gun is a Laval spray gun, and the inactive gas is high-purity argon or high-purity helium. During cold spraying, the working temperature of gas is room temperature to 650 ℃, the preferred temperature is 450 to 550 ℃, the cold spraying pressure is 1.5 to 3.5Mpa, the preferred pressure is 2.5 to 3.0Mpa, the powder conveying capacity is 0.1 to 400g/min, and the preferred condition is 250 to 300 g/min; when the device works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the spray gun is arranged on a mechanical arm, and the spray gun performs spraying and reciprocating movement at the same time according to a designed path, so that a layer of AgCuTi alloy blank with controllable thickness is finally formed on the substrate.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, the cold spraying substrate in the step III is an AgCuTiX alloy plate which has the same formula and material quality as the AgCuTiX alloy foil brazing filler metal, the thickness of a blank obtained after spraying is 0.5-100 mm, and the size of the blank can be designed according to the process requirements.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, the annealing treatment temperature in the step four is 600-750 ℃, the annealing treatment time is 0.5-1 hour, and the preferred condition is 650 ℃ and 1 hour.
As an improvement of the preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process, the cold rolling forming treatment in the step five is a conventional strip rolling forming process, and according to the initial thickness of a blank plate and the final required thickness of a foil, cold rolling processing is usually carried out for 3-8 times, and the pass reduction is 5-25% until the typical AgCuTiX foil brazing filler metal with the thickness of 0.08-1.2 mm is obtained.
The invention also provides a formula of the AgCuTiX alloy foil brazing filler metal prepared by the preparation method based on the cold spraying process, and the brazing filler metal consists of 40-95% of Ag, 3-60% of Cu and 0-10% of Ti and X in percentage by mass.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions of the present invention are described below with specific examples, but the scope of the present invention is not limited thereto.
Example 1
The embodiment provides a preparation method of an AgCu28 eutectic alloy foil brazing filler metal, which comprises the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag72% and Cu28%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu28 eutectic alloy spherical powder by adopting a gas atomization process, wherein an atomization medium is high-purity nitrogen. The temperature of melting vacuum induction melting is 1000 ℃, a supersonic gas atomizing nozzle is adopted, and the atomizing gas pressure is 3.7 Mpa.
And step two, standard screening is carried out on the AgCu28 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the average particle size of the powder is 15-20 microns.
And step three, firstly carrying out ultrasonic cleaning, drying and sand blasting treatment on a pre-prepared AgCu28 base plate (when in continuous production, the blank plate prepared in the front is cold-rolled to a certain thickness, can be cut into a proper size and is used as a cold spraying substrate when in later production). And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And step four, inputting the AgCu28 powder with qualified particle size screened in the step two into a powder feeding system of a cold spraying system, wherein the cold spraying gas adopts high-purity nitrogen. The cold spraying pressure is 2.6Mpa, and the powder conveying capacity is 250 g/min. When the device works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the spray gun for cold spraying is arranged on a mechanical arm, the spray gun adopts a scaling type Laval spray gun, the spray gun performs spraying and reciprocating movement at the same time according to a designed path, and finally a layer of AgCu28 alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spray gun moves, and meanwhile, the dust removal system moves synchronously with the cold spray gun to collect the non-deposited powder, so that the non-deposited powder is prevented from being mixed into the blank plate, and the density and the purity of the blank plate are ensured. Wherein, the cold spraying substrate is an AgCu alloy plate with the same formula material.
And step five, carrying out vacuum annealing treatment on the AgCu28 alloy blank plate obtained after the spraying in the step four is completed so as to eliminate the internal stress of the blank. The annealing temperature is 650 ℃, and the annealing time is 0.8 h.
And step six, carrying out cold rolling forming treatment on the AgCu28 blank subjected to annealing treatment in the step five by a multi-pass strip rolling forming process, and carrying out cold rolling processing for 3-8 times, wherein the pass reduction is 5-25% until the AgCu28 alloy foil strip brazing filler metal with the thickness of 0.08mm is obtained.
Example 2
As shown in fig. 1, this embodiment provides a method for preparing an Ag69Cu27Ti4 alloy foil solder, which includes the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag72% and Cu28%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu28 alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 1100 deg.C, and supersonic gas atomizing nozzle is adopted, and the gas pressure is 3.6 Mpa during atomization.
And step two, standard screening is carried out on the AgCu28 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the median particle size of the powder is 15-20 microns.
Step three, adding spherical Ti powder with the particle size range of 10-38 micrometers and the purity of 4N, which is produced by a fuse wire atomization method, into the AgCu28 alloy spherical powder obtained in the step two according to the proportion that the total weight percentage is 4%, and fully and uniformly mixing the powder by using a V-shaped mixer for 18 hours;
and step four, carrying out ultrasonic cleaning, drying and sand blasting treatment on the pre-prepared Ag69Cu27Ti4 base plate (when in continuous production, the blank plate prepared in the front is cold-rolled to a certain thickness, and then can be cut into a proper size to be used as a cold spraying substrate in the later production). And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The cold spraying medium gas is high-purity argon, the temperature of the medium gas is 480 ℃, the cold spraying pressure is 2.75Mpa, and the powder conveying capacity is 230 g/min. When the device works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the spray gun for cold spraying is installed on a mechanical arm, the spray gun adopts a Laval spray gun, the Laval spray gun performs spraying and reciprocating movement at the same time according to a designed path, and finally a layer of AgCuTi alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spray gun moves, and meanwhile, the dust removal system moves synchronously with the cold spray gun to collect the non-deposited powder, so that the non-deposited powder is prevented from being mixed into the blank plate, and the density and the purity of the blank plate are ensured. Wherein, the cold spraying base plate is an AgCuTi alloy plate with the same formula material.
And step six, carrying out vacuum annealing treatment on the Ag69Cu27Ti4 alloy blank plate obtained after the cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 650 ℃, and the annealing time is 0.8 h.
And seventhly, carrying out multi-pass cold rolling forming treatment on the Ag69Cu27Ti4 blank subjected to annealing treatment in the sixth step by using a strip rolling forming process, and carrying out 3-8 times of cold rolling processing with the pass reduction of 5-25% until the Ag69Cu27Ti4 alloy foil strip solder with the thickness of 0.35mm is obtained.
Example 3
As shown in fig. 1, this embodiment provides a method for preparing an ag68.8cu26.7ti4.5 alloy foil brazing filler metal, including the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag72% and Cu28%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu28 alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 1100 deg.C, and supersonic gas atomizing nozzle is adopted, and the gas pressure is 3.8Mpa during atomization.
And step two, standard screening is carried out on the AgCu28 alloy spherical powder obtained in the step one, and powder within the range of 325-600 meshes is selected. The median particle size of the powder is 15-20 μm.
Step three, adding spherical Ti powder with the particle size range of 10-38 micrometers and the purity of 4N grade, which is produced by a plasma atomization method, into the AgCu28 alloy spherical powder obtained in the step two according to the proportion that the total weight percentage is 4.5%, and fully and uniformly mixing the powder by using a V-shaped mixer for 18 hours;
and step four, carrying out ultrasonic cleaning, drying and sand blasting on a pre-prepared Ag68.8Cu26.7Ti4.5 matrix plate (when in continuous production, the previously prepared blank plate is cold-rolled to a certain thickness, can be cut into a proper size and is used as a cold spraying substrate when in later production). And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The cold spraying medium gas is high-purity argon, the temperature of the medium gas is 400 ℃, the cold spraying pressure is 2.76Mpa, and the powder conveying capacity is 200 g/min. When the device works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the spray gun for cold spraying is installed on a mechanical arm, the spray gun adopts a Laval spray gun, the Laval spray gun performs spraying and reciprocating movement at the same time according to a designed path, and finally a layer of AgCuTi alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spray gun moves, and meanwhile, the dust removal system moves synchronously with the cold spray gun to collect the non-deposited powder, so that the non-deposited powder is prevented from being mixed into the blank plate, and the density and the purity of the blank plate are ensured. Wherein, the cold spraying base plate is an AgCuTi alloy plate with the same formula material.
And step six, carrying out vacuum annealing treatment on the Ag68.8Cu26.7Ti4.5 alloy blank plate obtained after cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 650 ℃, and the annealing time is 0.8 h.
And step seven, carrying out cold rolling forming treatment on the Ag68.8Cu26.7Ti4.5 blank subjected to annealing treatment in the step six by using a multi-pass strip rolling forming process, and carrying out cold rolling processing for 3-8 times, wherein the pass reduction is 5-25%, until the Ag68.8Cu26.7Ti4.5 alloy foil strip brazing filler metal with the thickness of 0.12mm is obtained.
Example 4
As shown in fig. 1, this example provides a method for preparing an ag71.2cu27.6ti1.2 alloy foil brazing filler metal, comprising the steps of:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag72% and Cu28%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu28 eutectic alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 1000 deg.C, supersonic gas atomizing nozzle is adopted, and gas pressure is 3.9 Mpa during atomizing.
And step two, standard screening is carried out on the AgCu28 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the median particle size of the powder is 15-20 microns.
Step three, adding spherical Ti powder with the particle size range of 10-38 micrometers and the purity of 4N, which is produced by a plasma atomization method, into the AgCu28 alloy spherical powder obtained in the step two according to the proportion of 1.2 percent of the total weight percent, and fully and uniformly mixing the powder by using a V-shaped mixer for 15 hours;
and step four, carrying out ultrasonic cleaning, drying and sand blasting on the pre-prepared Ag71.2Cu27.6Ti1.2 base plate (when in continuous production, the previously prepared blank plate is cold-rolled to a certain thickness and can be cut into a proper size to be used as a cold spraying substrate in later production). And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The medium gas of cold spraying is high-purity helium. The temperature of the medium gas is 300 ℃, the pressure of the cold spraying is 1.8Mpa, and the powder conveying capacity is 150 g/min. When the device works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the spray gun for cold spraying is installed on a mechanical arm, the spray gun adopts a Laval spray gun, the Laval spray gun performs spraying and reciprocating movement at the same time according to a designed path, and finally a layer of AgCuTi alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spray gun moves, and meanwhile, the dust removal system moves synchronously with the cold spray gun to collect the non-deposited powder, so that the non-deposited powder is prevented from being mixed into the blank plate, and the density and the purity of the blank plate are ensured. Wherein, the cold spraying base plate is an AgCuTi alloy plate with the same formula material.
And step six, carrying out vacuum annealing treatment on the Ag71.2Cu27.6Ti1.2 alloy blank plate obtained after cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 630 ℃, and the annealing time is 1 h.
And step seven, carrying out cold rolling forming treatment on the Ag71.2Cu27.6Ti1.2 blank subjected to annealing treatment in the step six by a multi-pass strip rolling forming process, and carrying out cold rolling processing for 3-8 times, wherein the pass reduction is 5-25% until the Ag71.2Cu27.6Ti1.2 alloy foil brazing filler metal with the thickness of 0.1mm is obtained.
Example 4
As shown in fig. 1, this embodiment provides a method for preparing an Ag63Cu34Ti2Sn1 alloy foil solder, which includes the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag65% and Cu35%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing Ag65Cu35 alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 1050 deg.C, supersonic gas atomizing nozzle is adopted, and the gas pressure is 3.9 Mpa during atomization.
And step two, standard screening is carried out on the Ag65Cu35 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the average particle size of the powder is 15-20 microns.
Step three, adding the spherical Ti powder with the particle size range of 10-38 micrometers and the purity of 4N produced by the plasma atomization method and the spherical Sn powder with the particle size range of 10-38 micrometers and the purity of 4N produced by the gas atomization method into the AgCu28 alloy spherical powder obtained in the step two according to the proportion of 1% of the total weight percentage, and fully and uniformly mixing the powder by using a V-shaped mixer for 18 hours;
and step four, carrying out ultrasonic cleaning, drying and sand blasting treatment on the pre-prepared Ag63Cu34Ti2Sn1 base plate (when in continuous production, the blank plate prepared in the front is cold-rolled to a certain thickness, and then can be cut into a proper size to be used as a cold spraying substrate when in later production). And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The cold spraying medium gas is high-purity helium, the temperature of the medium gas is 300 ℃, the cold spraying air pressure is 1.8Mpa, and the powder conveying capacity is 150 g/min. When the spraying machine works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then are deposited on the surface of the prefabricated cold spraying substrate, the spray gun for cold spraying is arranged on a mechanical arm, the spray gun adopts a zoom type Laval spray gun, the spray gun performs reciprocating motion while spraying according to a designed path, and finally, a layer of Ag63Cu34Ti2Sn1 alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spray gun moves, and meanwhile, the dust removal system moves synchronously with the cold spray gun to collect the non-deposited powder, so that the non-deposited powder is prevented from being mixed into the blank plate, and the density and the purity of the blank plate are ensured. The cold spraying substrate is an Ag63Cu34Ti2Sn1 alloy plate with the same formula material.
And step six, carrying out vacuum annealing treatment on the Ag63Cu34Ti2Sn1 alloy blank plate obtained after cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 630 ℃, and the annealing time is 1 h.
And step seven, carrying out cold rolling forming treatment on the Ag71.2Cu27.6Ti1.2 blank subjected to annealing treatment in the step six by a multi-pass strip rolling forming process, and carrying out cold rolling processing for 3-8 times with the pass reduction of 5-25% until the Ag63Cu34Ti2Sn1 alloy foil strip solder with the thickness of 1.1mm is obtained.
Example 5
As shown In fig. 1, this embodiment provides a method for preparing an Ag59Cu28In12Ti1 alloy foil solder, which includes the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag67.8% and Cu32.2%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction smelting, and then preparing Ag67.8Cu32.2 alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 1050 deg.C, supersonic gas atomizing nozzle is adopted, and the gas pressure is 3.9 Mpa during atomization.
And step two, standard screening is carried out on the Ag67.8Cu32.2 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the median particle size of the powder is 15-20 microns.
Step three, adding spherical Ti powder with the particle size range of 10-38 microns and the purity of 4N, which is produced by a plasma atomization method, into the Ag67.8Cu32.2 alloy spherical powder obtained in the step two according to the proportion of 1 percent of the total weight percentage; adding spherical In powder with the particle size range of 10-38 micrometers and the purity of 4N, which is produced by a gas atomization method, into the Ag67.8Cu32.2 alloy spherical powder obtained In the step two according to the proportion of 1% of the total weight percent, and fully and uniformly mixing the powder by using a V-shaped mixer for 15 hours;
and step four, carrying out ultrasonic cleaning, drying and sand blasting on a pre-prepared Ag59Cu28In12Ti1 base plate (when In continuous production, the blank plate prepared In the front is cold-rolled to a certain thickness, and then can be cut into a proper size to be used as a cold spraying substrate when In later production). And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The cold spraying medium gas is high-purity helium, the temperature of the medium gas is 300 ℃, the cold spraying air pressure is 1.8Mpa, and the powder conveying capacity is 150 g/min. When the device works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the spray gun for cold spraying is arranged on a mechanical arm, the spray gun adopts a Laval spray gun, the spray gun performs spraying and reciprocating movement according to a designed path, and finally a layer of Ag59Cu28In12Ti1 alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spraying substrate is an Ag59Cu28In12Ti1 alloy plate with the same formula material.
And step six, carrying out vacuum annealing treatment on the Ag59Cu28In12Ti1 alloy blank plate obtained after the cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 650 ℃, and the annealing time is 0.9 h.
And seventhly, carrying out cold rolling forming treatment on the Ag59Cu28In12Ti1 blank subjected to annealing treatment In the sixth step by a multi-pass strip rolling forming process, and carrying out cold rolling processing for 3-8 times, wherein the pass reduction is 5-25% until the Ag59Cu28In12Ti1 alloy foil strip solder with the thickness of 0.3mm is obtained.
Example 6
As shown in fig. 1, this embodiment provides a method for preparing an ag64.8cu25.2ti10 alloy foil brazing filler metal, including the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag72% and Cu28%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu28 eutectic alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 1000 deg.C, supersonic gas atomizing nozzle is adopted, and gas pressure is 3.5Mpa during atomizing.
And step two, standard screening is carried out on the AgCu28 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the median particle size of the powder is 15-20 microns.
And step three, adding spherical Ti powder with the particle size range of 15-40 micrometers and the purity of 4N, which is produced by a fuse wire atomization method, into the AgCu28 alloy spherical powder obtained in the step two according to the proportion of 10 percent of the total weight percentage, and fully and uniformly mixing the powder by using a V-shaped mixer for 24 hours.
And step four, carrying out ultrasonic cleaning, drying and sand blasting treatment on the pre-prepared Ag64.8Cu25.2Ti10 matrix plate. And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The cold spraying medium gas is high-purity helium, the temperature of the medium gas is 250 ℃, the cold spraying air pressure is 3.2Mpa, and the powder conveying capacity is 120 g/min. A spray gun for cold spraying is installed on a mechanical arm, the spray gun adopts a scaling type Laval spray gun, the spray gun performs spraying and moves back and forth according to a designed path, and finally a layer of Ag64.8Cu25.2Ti10 alloy coating with controllable thickness is formed on a substrate to become a blank. The cold spraying substrate is an Ag64.8Cu25.2Ti10 alloy plate with the same formula and material.
And step six, carrying out vacuum annealing treatment on the Ag64.8Cu25.2Ti10 alloy blank plate obtained after the cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 700 ℃, and the annealing time is 0.8 h.
And step seven, carrying out cold rolling forming treatment on the Ag64.8Cu25.2Ti10 blank subjected to the annealing treatment in the step six by a multi-pass strip rolling forming process, and carrying out cold rolling processing for 2-5 times, wherein the pass reduction is 5-25% until the Ag64.8Cu25.2Ti10 alloy foil strip brazing filler metal with the thickness of 0.5mm is obtained.
Example 7
As shown in fig. 1, this embodiment provides a method for preparing Ag59Cu28Sn12Ti1 alloy foil solder, which includes the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the weight percentage of Ag67.8% and Cu32.2%, putting the two metals into a graphite crucible of a medium-frequency induction furnace for vacuum induction smelting, and then preparing Ag67.8Cu32.2 alloy spherical powder by adopting a gas atomization process, wherein a gas medium is high-purity nitrogen. The vacuum induction melting temperature is 950 deg.C, supersonic gas atomizing nozzle is adopted, and gas pressure is 3.9 Mpa during atomizing.
And step two, standard screening is carried out on the Ag67.8Cu32.2 alloy spherical powder obtained in the step one, powder within the range of 325-600 meshes is selected, and the average particle size of the powder is 15-20 microns.
Step three, adding spherical Ti powder with the particle size range of 10-38 microns and the purity of 4N, which is produced by a plasma atomization method, into the Ag67.8Cu32.2 alloy spherical powder obtained in the step two according to the proportion of 1 percent of the total weight percentage; adding spherical Sn powder with the particle size range of 10-38 micrometers and the purity of 4N, which is produced by a gas atomization method, into the Ag67.8Cu32.2 alloy spherical powder obtained in the step two according to the proportion of 1% of the total weight percent, fully and uniformly mixing the powder by using a V-type mixer for 15 hours, wherein the weight percent of each element of the uniformly mixed powder is Ag59Cu28Sn12Ti 1;
and step four, carrying out ultrasonic cleaning, drying and sand blasting treatment on the pre-prepared Ag59Cu28Sn12Ti1 base plate. And carrying out sand blasting treatment by using corundum sand, wherein the granularity of the corundum sand is 16-30 meshes.
And fifthly, inputting the uniformly mixed powder into a powder feeding system of a cold spraying system for cold spraying. The cold spraying medium gas is high-purity helium, the temperature of the medium gas is 300 ℃, the cold spraying air pressure is 1.8Mpa, and the powder conveying capacity is 150 g/min. When the spraying machine works, mixed powder on the powder feeding system is accelerated by airflow sprayed by a spray gun and then collides with a cold spraying substrate at a high speed, powder particles are subjected to plastic deformation and then deposited on the surface of the prefabricated cold spraying substrate, the cold spraying spray gun is installed on a mechanical arm, the spray gun adopts a scaling type Laval spray gun, the spray gun performs spraying and reciprocating movement according to a designed path, and finally, a layer of Ag59Cu28Sn12Ti1 alloy coating with controllable thickness is formed on the substrate to form a blank. The cold spraying substrate is an Ag59Cu28Sn12Ti1 alloy plate with the same formula material.
And step six, carrying out vacuum annealing treatment on the Ag59Cu28Sn12Ti1 alloy blank plate obtained after the cold spraying is finished so as to eliminate the internal stress of the blank. The annealing temperature is 700 ℃, and the annealing time is 0.9 h.
And seventhly, carrying out cold rolling forming treatment on the Ag59Cu28Sn12Ti1 blank subjected to annealing treatment in the sixth step by a multi-pass strip rolling forming process, and carrying out cold rolling processing for 3-8 times, wherein the pass reduction is 5-25% until the Ag59Cu28Sn12Ti1 alloy foil strip brazing filler metal with the thickness of 1mm is obtained.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and the related alloy element ratio changes within the formula scope of the present invention should also fall within the protection scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A preparation method of AgCuTiX alloy foil brazing filler metal based on a cold spraying process is characterized by at least comprising the following steps:
firstly, weighing Ag ingot and Cu ingot raw materials according to the component proportion of the AgCuTiX alloy brazing filler metal to prepare AgCu alloy powder;
step two, weighing cold spraying Ti and X powder according to the component proportion of the AgCuTi alloy brazing filler metal, and uniformly mixing the AgCu alloy powder obtained in the step one with the cold spraying Ti powder and the cold spraying X powder to obtain mixed powder;
inputting the mixed powder obtained in the step two into a powder feeding system of a cold spraying system, and carrying out cold spraying by adopting inactive gas to form an AgCuTiX alloy blank;
step four, annealing the AgCuTiX alloy blank obtained in the step three to eliminate the internal stress of the blank and obtain an AgCuTiX blank plate;
step five, carrying out multi-pass cold rolling forming treatment on the AgCuTiX blank obtained in the step four until the AgCuTiX alloy foil strip brazing filler metal with the required thickness is obtained;
wherein X is at least one of In, Zr, Sn, Zn, Cd and Ni, and the sum of the mass fractions of X and Ti is 0-10%.
2. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process according to claim 1, wherein the preparation process of AgCu alloy powder in the first step is as follows: and putting the Ag ingot and the Cu ingot into a graphite crucible of a medium-frequency induction furnace for vacuum induction melting, and then preparing AgCu alloy spherical powder by adopting a gas atomization process.
3. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process according to claim 2, wherein the AgCu alloy spherical powder prepared in the first step consists of 40-95% of Ag and 5-60% of Cu by mass percent, and the temperature of vacuum induction melting is 950-1150 ℃; the gas adopted by the atomization powder preparation process is high-purity nitrogen, and the atomization pressure is 2.5-4.5 MPa.
4. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process according to claim 1, characterized by further comprising the step of selecting AgCu alloy powder with the size meeting the requirements from the AgCu alloy powder obtained in the step one before the step two, wherein the AgCu alloy powder with the size meeting the requirements is powder with the particle size distribution of 1-45 micrometers; the purity of the Ti powder is 4N grade, and the particle size range is 1-45 microns; the purity of the X powder is higher than 3N grade, and the particle size range is 0.1-20 microns.
5. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process according to claim 1, wherein a V-shaped mixer is adopted for mixing in the second step, and the mixing time is 12-24 hours.
6. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process according to claim 1, wherein the supersonic cold spraying system in the third step comprises a powder feeding system, a high-pressure gas source, a gas heater for heating the high-pressure gas source, a gas regulation control system for regulating the pressure of gas fed by the high-pressure gas source and a spray gun; the spray gun is a Laval spray gun, and the inactive gas is high-purity nitrogen, high-purity argon or high-purity helium; during cold spraying, the working temperature of gas is room temperature to 650 ℃, the pressure of cold spraying is 1.5 to 3.5Mpa, and the powder conveying capacity is 0.1 to 400 g/min; when the device works, the spray gun is arranged on the mechanical arm, and moves back and forth while spraying according to a designed path, and finally a layer of AgCuTiX alloy blank with controllable thickness is formed on the cold spraying substrate.
7. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process as claimed in claim 6, wherein the cold spraying substrate in the third step is an AgCuTiX alloy plate with the same formula and material as the AgCuTiX alloy foil brazing filler metal, and the thickness of the blank obtained after spraying is 0.5-100 mm.
8. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process according to claim 1, wherein the annealing treatment temperature in the step four is 600-700 ℃, and the annealing treatment time is 0.5-1.5 hours.
9. The preparation method of the AgCuTiX alloy foil brazing filler metal based on the cold spraying process as claimed in claim 1, wherein the cold rolling forming treatment in the fifth step is a strip rolling forming process, the cold rolling processing is performed for 3-8 times, the pass reduction is 5-25%, and the thickness of the AgCuTiX foil brazing filler metal is 0.08-1.2 mm.
10. An AgCuTiX alloy foil brazing filler metal based on a cold spraying process, prepared by the preparation method of claims 1-9, is characterized in that: the brazing filler metal consists of 40-95% of Ag, 3-60% of Cu and 0-10% of Ti and X in percentage by mass.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113953609A (en) * | 2021-09-16 | 2022-01-21 | 黎铭坚 | AMB ceramic-metal brazing method |
| CN114293155A (en) * | 2021-10-22 | 2022-04-08 | 紫金矿业集团黄金珠宝有限公司 | Preparation method of silver-palladium-copper alloy target material |
| CN114769585A (en) * | 2022-04-20 | 2022-07-22 | 昆明冶金研究院有限公司北京分公司 | Cold spray forming method of Cu-Cr-Nb series alloy |
| CN115786762A (en) * | 2022-11-24 | 2023-03-14 | 南京理工大学 | High-strength active brazing filler metal |
-
2021
- 2021-04-25 CN CN202110446105.XA patent/CN113122837A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113953609A (en) * | 2021-09-16 | 2022-01-21 | 黎铭坚 | AMB ceramic-metal brazing method |
| CN114293155A (en) * | 2021-10-22 | 2022-04-08 | 紫金矿业集团黄金珠宝有限公司 | Preparation method of silver-palladium-copper alloy target material |
| CN114769585A (en) * | 2022-04-20 | 2022-07-22 | 昆明冶金研究院有限公司北京分公司 | Cold spray forming method of Cu-Cr-Nb series alloy |
| CN114769585B (en) * | 2022-04-20 | 2024-01-05 | 中铝科学技术研究院有限公司 | Cold spray forming method of Cu-Cr-Nb alloy |
| CN115786762A (en) * | 2022-11-24 | 2023-03-14 | 南京理工大学 | High-strength active brazing filler metal |
| CN115786762B (en) * | 2022-11-24 | 2024-05-07 | 南京理工大学 | High-strength active brazing filler metal |
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