CN116944503A - Preparation method of amorphous powder for titanium alloy brazing - Google Patents
Preparation method of amorphous powder for titanium alloy brazing Download PDFInfo
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- CN116944503A CN116944503A CN202311182415.0A CN202311182415A CN116944503A CN 116944503 A CN116944503 A CN 116944503A CN 202311182415 A CN202311182415 A CN 202311182415A CN 116944503 A CN116944503 A CN 116944503A
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- brazing
- amorphous powder
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 113
- 239000000843 powder Substances 0.000 title claims abstract description 95
- 238000005219 brazing Methods 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 74
- 239000000956 alloy Substances 0.000 claims abstract description 74
- 238000000498 ball milling Methods 0.000 claims abstract description 48
- 238000003723 Smelting Methods 0.000 claims abstract description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- 239000010949 copper Substances 0.000 claims abstract description 38
- 230000006698 induction Effects 0.000 claims abstract description 37
- 238000002844 melting Methods 0.000 claims abstract description 37
- 230000008018 melting Effects 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 230000009471 action Effects 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims description 33
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000002074 melt spinning Methods 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 7
- 239000012634 fragment Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000000945 filler Substances 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 abstract description 2
- 238000003892 spreading Methods 0.000 abstract description 2
- 230000007480 spreading Effects 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 14
- 229910052719 titanium Inorganic materials 0.000 description 14
- 230000008569 process Effects 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 229910000679 solder Inorganic materials 0.000 description 8
- 238000007789 sealing Methods 0.000 description 6
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 238000005280 amorphization Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 235000008429 bread Nutrition 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/048—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by pulverising a quenched ribbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a preparation method of amorphous powder for titanium alloy brazing, which comprises the following steps: 1. preparing a metal raw material, and then carrying out vacuum suspension smelting to obtain a master alloy ingot; 2. after induction heating and melting of the master alloy ingot, spraying out from a crucible nozzle, and rapidly cooling under the action of a copper roller rotating at a high speed to form a continuous amorphous titanium alloy strip; 3. and (3) carrying out vacuum ball milling after preliminary crushing on the titanium alloy amorphous strip, and screening to obtain amorphous powder for titanium alloy brazing. The amorphous powder for titanium alloy brazing has the advantages of simple preparation process, low cost, uniform and stable components, low impurity content, convenient spreading during use, reduced brazing temperature, contribution to improving the performance of welded parts, suitability for different brazing environments and satisfaction of technical requirements of titanium alloy brazing on high-quality amorphous brazing filler metal powder.
Description
Technical Field
The invention belongs to the technical field of titanium alloy brazing material manufacturing, and particularly relates to a preparation method of amorphous powder for titanium alloy brazing.
Background
The brazing piece of the titanium alloy has wide application in the fields of aerospace industry and the like. The common titanium alloy brazing materials mainly comprise three large brazing filler metal series of Ag base, al base and Ti base. Ag-based solder is sensitive to chloride ions and has low strength at high temperature; the joint brazed by the Al-based brazing filler metal is fragile and has poor strength. Titanium-based solders are currently considered to be the best solders for brazing titanium alloys. However, titanium-based solders are brittle and have poor processability, and foils are difficult to prepare, so that the titanium-based solders are blended into paste form for use in powder form or with glue. Compared with the traditional titanium-based crystalline powder, the titanium-based amorphous powder has the advantages of low melting point, simple process, adjustable components and the like, and can greatly promote the development and progress of the titanium alloy brazing technology.
Besides being applied to titanium alloy brazing, the titanium-based amorphous powder also has wide application prospect in the fields of aerospace, laser 3D printing and the like. For example, in the field of aerospace, the titanium-based amorphous powder can be used for manufacturing high-strength and light-weight aviation parts, so that the performance and the safety of an airplane are greatly improved; in the laser 3D printing field, the titanium-based amorphous powder can be used for preparing titanium-based amorphous parts, and is not limited by size and complexity.
There are various methods for preparing titanium-based amorphous powders, such as atomization, rapid solidification, mechanical alloying, etc. The gas atomization has high equipment requirement precision, the powder components and granularity are not easy to control, and the amorphous degree is low; the powder prepared by the rapid solidification method has low amorphization degree and large granularity; the mechanical alloying method has long period, and the impurity content and the oxygen content of the powder are not easy to control. In summary, the existing method has the defects for preparing the titanium-based amorphous powder, and can not completely meet the requirement of the titanium-based amorphous powder on the service performance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of amorphous powder for titanium alloy brazing, aiming at the defects of the prior art. The amorphous powder for titanium alloy brazing is successfully prepared by adopting a smelting-melt-spinning-ball milling process, the amorphous degree and the grain diameter of the amorphous powder for titanium alloy brazing are effectively controlled by controlling a melt-spinning process and a ball milling crushing process, the amorphous powder for titanium alloy brazing is uniform and stable in component and low in impurity content, the technical requirement of titanium alloy brazing on high-quality amorphous solder powder is met, and the problem that the amorphous degree and the grain diameter of the amorphous powder are difficult to control in the existing preparation method is solved.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing amorphous powder for titanium alloy brazing, which is characterized by comprising the following steps:
step one, preparing master alloy: preparing a metal raw material according to the composition of amorphous powder for the target product titanium alloy brazing, and then placing the metal raw material into a vacuum suspension smelting furnace for smelting to prepare a master alloy cast ingot with uniform components;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting a master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller, starting the copper roller with water cooling function, controlling the rotating speed to be 2500 r/min-3500 r/min, continuously heating for 3-10 min after the master alloy ingot is completely melted and stabilizing the temperature, then introducing high-purity argon to enable the master alloy ingot melt to be sprayed out from the crucible nozzle, and rapidly cooling under the action of the copper roller rotating at a high speed to form a continuous titanium alloy amorphous strip;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing by a crusher, and then the obtained amorphous fragments are transferred into a vacuum ball milling tank, sealed and vacuumized to 3.0x10 -3 Pa, ball milling is carried out by using a planetary ball mill, and amorphous powder for titanium alloy brazing is obtained through screening.
The method for preparing amorphous powder for titanium alloy brazing is characterized in that in the first step, the mass purity of the metal raw material is more than 99.95%, and the metal raw material is in a block shape. The invention reduces the introduction of impurities by controlling the purity of the metal raw material, and is beneficial to forming amorphous powder solder.
The method for preparing the amorphous powder for titanium alloy brazing is characterized in that the vacuum degree of smelting in the step one at least reaches 3.0 multiplied by 10 -3 Pa, the smelting times are at least 4 times. According to the invention, the alloy oxidation phenomenon in the smelting process is avoided by controlling the vacuum degree of smelting in the vacuum suspension smelting furnace, and the component uniformity of the master alloy cast ingot is ensured by controlling the smelting times.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that after the master alloy ingot is completely melted and stabilized in the second step, high-purity argon is introduced into an induction smelting crucible to increase the air pressure in the induction smelting crucible, and a pressure difference of 0.5-1.0 MPa is formed between the induction smelting crucible and a vacuum chamber, so that the master alloy ingot solution is rapidly sprayed out from a crucible nozzle to the surface of a copper roller rotating at high speed under the action of pressure, and continuous titanium alloy amorphous strip is formed through rapid cooling. According to the invention, high-purity argon is introduced into the crucible to promote the formation of pressure difference between the induction smelting crucible and the vacuum chamber, so that the melt of the master alloy ingot is sprayed out to perform melt-spinning, and the amorphous titanium alloy strip is formed, and meanwhile, the phenomenon of alloy oxidation in the process of alloy melt-spinning is avoided, and the quality of amorphous powder for titanium alloy brazing is ensured.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that the distance between the crucible nozzle and the surface of the copper roller in the second step is 0.7 mm-1.2 mm.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that the rotation speed of the copper roller is 2500 r/min-3000 r/min when the master alloy ingot casting solution is sprayed out of the crucible nozzle in the second step.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that the temperature of the master alloy ingot casting solution is stabilized at 50-200 ℃ above the alloy melting point when the master alloy ingot casting solution is sprayed out from a crucible nozzle.
The technological parameters of the preparation process are closely related to the formation and the characteristics of the amorphous strip.
In the research process, the larger the pressure difference between the crucible and the vacuum chamber is, the more mother alloy cast ingot melt sprayed on the surface of the copper roller is, and the larger the thickness of the formed titanium alloy amorphous strip is, and the problems that the amorphous strip cannot be formed due to the fact that the pressure difference is too large and the solution is sprayed discontinuously and the titanium alloy amorphous strip is formed discontinuously are avoided while the amorphous strip is formed due to the fact that the pressure difference is controlled to be 0.5-1.0 MPa. Secondly, the distance between the crucible nozzle and the surface of the copper roller influences the thickness of the titanium alloy amorphous strip, and the method solves the problems that the interval is too large, too much molten liquid is accumulated on the surface of the copper roller and the amorphous strip cannot be formed by controlling the distance between the crucible nozzle and the surface of the copper roller to be 0.7 mm-1.2 mm, and meanwhile, the interval is too small so that the crucible nozzle and the copper roller are rubbed or even damaged to seriously leak the liquid, and even the amorphous strip is formed, the head and the tail of the amorphous strip are basically unusable, and the middle part of the amorphous strip is provided with too many meshes to have poor quality. Meanwhile, the rotating speed of the copper roller directly determines the thickness of the titanium alloy amorphous strip. The faster the speed of the copper roller, the thinner the prepared amorphous strip of titanium alloy, whereas the slower the speed of the copper roller, the thicker the prepared amorphous strip of titanium alloy, even not the amorphous strip. In addition, the temperature of the master alloy ingot casting solution sprayed out of the crucible nozzle greatly affects the amorphous strip of the titanium alloy, the viscosity coefficient of the solution with too high temperature is reduced, the amorphous strip of the titanium alloy formed after being sprayed out is subjected to the phenomena of burrs, discontinuity, uneven thickness and the like, and the solution with too low temperature is solidified or completely solidified at the mouth part of the crucible nozzle, so that the amorphous strip of the titanium alloy is failed to prepare. Within the parameters that enable the formation of amorphous strips of titanium alloy, the thinner the strip, the better the toughness and the thicker the strip the greater the brittleness.
According to the invention, by adjusting the pressure difference between the induction smelting crucible and the vacuum chamber in the melt-spinning process, the distance between the crucible nozzle and the surface of the copper roller, the rotating speed of the copper roller, the melt-spinning temperature and other technological parameters, the amorphization degree of the amorphous titanium alloy strip is ensured, and meanwhile, the amorphous titanium alloy strip has a certain brittleness, is easy to break, and is beneficial to the preparation of subsequent amorphous powder.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that the vacuum ball milling tank and the adopted grinding balls in the third step are made of zirconium oxide. The active elements titanium and zirconium contained in the amorphous powder for brazing the target product titanium alloy are extremely easy to react with ball milling tank and grinding ball materials to different degrees to introduce impurities, so that the zirconium oxide with high hardness and good wear resistance is adopted as the grinding ball material, and the phenomenon that the brazing material is impure due to the fact that other impurities are introduced in the ball milling process is avoided, and further the brazing performance of the brazing material is reduced.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that the grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, and the total ball-material ratio is 30:1-50:1. The large ball has large weight and large impact force, is easy to crush large materials, has small ball volume and large collision times, and can refine small particles. The invention adopts the grinding balls with the two diameters and reasonably configures the quality of the grinding balls, so that the grinding balls are crushed by ball milling, and the amorphous powder for titanium alloy brazing with proper particle size is obtained.
The preparation method of the amorphous powder for titanium alloy brazing is characterized in that the ball milling rotating speed in the third step is 200-500 r/min, the ball milling time is 20-50 h, and the machine is stopped for 15min every 1h of ball milling. According to the invention, by controlling the ball-material ratio, the ball-milling rotating speed and the ball-milling time and adopting an intermittent process, the conditions that the temperature in a tank is too high and amorphous alloy is converted into a crystalline state due to the too high rotating speed and the continuous long-time ball-milling are avoided, meanwhile, the titanium alloy amorphous strip is difficult to break into a powder state due to the too low rotating speed and the small rotating speed are avoided, the titanium alloy amorphous strip is fully broken and thinned, and the high-quality amorphous powder for titanium alloy brazing is obtained.
Compared with the prior art, the invention has the following advantages:
1. the amorphous powder for titanium alloy brazing is successfully prepared by adopting a smelting-melt-spinning-ball milling process, and the amorphous degree and the grain diameter of the amorphous powder for titanium alloy brazing are effectively controlled by controlling the melt-spinning process and the ball milling crushing process.
2. The amorphous powder for titanium alloy brazing prepared by the invention has low melting point and is powdery, and can be conveniently spread on the surface of a piece to be welded in subsequent use, so that the influence of the welding temperature on the piece to be welded is effectively reduced, and the actual spreading operation of brazing solder is simplified.
3. The prepared amorphous powder of the titanium-based alloy for brazing has high activity, good heat resistance and corrosion resistance and good brazing process performance, and the amorphous brazing material is molten and has lower reaction temperature than the crystalline brazing material, so that the brazing temperature is prevented from being too high to a certain extent, the amorphous powder effectively reduces the brazing temperature of the titanium alloy, and the performance of a welded part is improved.
4. The amorphous powder for titanium alloy brazing prepared by the invention has lower welding temperature than crystalline brazing material, thereby effectively avoiding microstructure change of titanium alloy at higher welding temperature and keeping good mechanical property of a welded part.
5. Compared with the method for preparing the powder by directly and quickly cooling the melted titanium alloy block, the method provided by the invention has the advantages that the melted titanium alloy block is quickly cooled to prepare the strip, then the strip is crushed to obtain the amorphous powder, and the amorphous powder with smaller grain size is obtained by adding one step of operation, so that the method is suitable for different brazing environments, and especially meets the requirement of thin brazing sheet with the thickness of less than 1mm on a thinner brazing material layer.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is an XRD pattern of an amorphous strip of titanium alloy prepared in example 1 of the present invention.
FIG. 2 is a graph showing the microscopic morphology of amorphous powder for brazing titanium alloy prepared in example 1 of the present invention.
FIG. 3 is an XRD pattern of amorphous powder for brazing titanium alloy prepared in example 1 of the present invention.
Fig. 4 is an XRD pattern of an amorphous strip of titanium alloy prepared in example 2 of the present invention.
FIG. 5 is a graph showing the microscopic morphology of amorphous powder for brazing titanium alloy prepared in example 3 of the present invention.
Fig. 6 is an XRD pattern of amorphous powder for brazing of titanium alloy prepared in example 3 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, preparing master alloy: preparing metal raw material blocks with the mass purity of more than 99.95 percent according to the mass percentage of elements corresponding to 37.5 percent Ti-37.5 percent Zr-15 percent Cu-10 percent Ni of amorphous powder for brazing the target product titanium alloy, and then sequentially placing the metal raw material blocks into a vacuum suspension smelting furnace for smelting, wherein the vacuum degree of smelting is at least 3.0 multiplied by 10 -3 Pa, smelting times are 4 times, and mother alloy cast ingots with uniform components are prepared;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting a master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller to 0.7mm, starting the copper roller with water cooling effect, controlling the rotating speed to 2500r/min, continuously heating for 3min after the master alloy ingot is completely melted, keeping the temperature of the master alloy ingot to be 200 ℃ above the melting point of the alloy, introducing argon with the mass purity of 99.999% into an induction melting crucible to increase the air pressure in the induction melting crucible, forming a pressure difference of 1.0MPa between the induction melting crucible and a vacuum chamber, so that the master alloy ingot melt is rapidly sprayed out from the crucible nozzle under the action of the pressure, and rapidly cooling to form a continuous amorphous strip of the titanium alloy under the action of the copper roller rotating at a high speed;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing through a crusher, the obtained amorphous fragments are transferred into a zirconia vacuum ball milling tank, zirconia grinding balls are added until the total ball-to-material ratio is 30:1, the zirconia grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, and the sealing is carried out and then the sealing is carried outVacuum to 3.0X10 -3 Pa, ball milling is carried out by using a planetary ball mill, the ball milling rotating speed is 200r/min, the ball milling time is 50h, the machine is stopped for 15min every 1h of ball milling, and amorphous powder for titanium alloy brazing is obtained through screening.
Fig. 1 is an XRD pattern of an amorphous titanium alloy strip prepared in this example, and the steamed bread peak in fig. 1 indicates that the strip is an amorphous alloy.
Fig. 2 is a microscopic morphology of the amorphous powder for titanium alloy brazing prepared in this example, and it can be seen from fig. 2 that the particle size of the amorphous powder for titanium alloy brazing is less than 10 μm.
Fig. 3 is an XRD pattern of the amorphous powder for titanium alloy brazing prepared in this example, and it can be seen from fig. 3 that the amorphous powder for titanium alloy brazing has the characteristics of an amorphous alloy.
Example 2
The embodiment comprises the following steps:
step one, preparing master alloy: preparing metal raw material blocks with the mass purity of more than 99.95 percent according to the mass percentage of elements corresponding to 37.5 percent Ti-37.5 percent Zr-15 percent Cu-10 percent Ni of amorphous powder for brazing the target product titanium alloy, and then sequentially placing the metal raw material blocks into a vacuum suspension smelting furnace for smelting, wherein the vacuum degree of smelting is at least 3.0 multiplied by 10 -3 Pa, smelting times are 5 times, and mother alloy cast ingots with uniform components are prepared;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting a master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller to 1.0mm, starting the copper roller with water cooling function, controlling the rotating speed to 2500r/min, continuously heating for 8min after the master alloy ingot is completely melted, keeping the temperature of the master alloy ingot to be 150 ℃ above the melting point of the alloy, introducing argon with the mass purity of 99.999% into an induction melting crucible to increase the internal pressure of the induction melting crucible, forming a pressure difference of 0.8MPa between the induction melting crucible and a vacuum chamber, so that the master alloy ingot is rapidly sprayed out from the crucible nozzle under the pressure effect, and rotating at a high speedRapidly cooling to form a continuous amorphous strip of titanium alloy under the action of a copper roller;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing through a crusher, the obtained amorphous fragments are transferred into a zirconia vacuum ball milling tank, zirconia grinding balls are added until the total ball-to-material ratio is 40:1, the zirconia grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, and the sealing is carried out, and then the vacuum pumping is carried out until the total ball-to-material ratio is 3.0x10 -3 Pa, ball milling is carried out by using a planetary ball mill, the ball milling rotating speed is 300r/min, the ball milling time is 30h, the machine is stopped for 15min every 1h of ball milling, and amorphous powder for titanium alloy brazing is obtained through screening.
Fig. 4 is an XRD pattern of the amorphous titanium alloy strip prepared in this example, and the steamed bread peak in fig. 4 indicates that the strip is an amorphous alloy.
Example 3
The embodiment comprises the following steps:
step one, preparing master alloy: preparing metal raw material blocks with the mass purity of more than 99.95 percent according to the mass percentage of elements corresponding to 37.5 percent Ti-37.5 percent Zr-15 percent Cu-10 percent Ni of amorphous powder for brazing the target product titanium alloy, and then sequentially placing the metal raw material blocks into a vacuum suspension smelting furnace for smelting, wherein the vacuum degree of smelting is at least 3.0 multiplied by 10 -3 Pa, smelting times are 6 times, and mother alloy cast ingots with uniform components are prepared;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting a master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller to 1.2mm, starting the copper roller with water cooling function, controlling the rotating speed to 3500r/min, continuously heating for 5min after the master alloy ingot is completely melted, keeping the temperature of the master alloy ingot to be 100 ℃ above the melting point of the alloy, introducing argon with the mass purity of 99.999% into an induction melting crucible to increase the internal pressure of the induction melting crucible, and forming a pressure difference of 0.5MPa between the induction melting crucible and a vacuum chamber to ensure that the master alloy ingot is melted from the crucible nozzle under the pressure effectRapidly spraying and rapidly cooling under the action of a copper roller rotating at a high speed to form a continuous titanium alloy amorphous strip;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing through a crusher, the obtained amorphous fragments are transferred into a zirconia vacuum ball milling tank, zirconia grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, the zirconia grinding balls are added until the total ball-to-material ratio is 50:1, and the sealing is carried out and then the vacuum pumping is carried out until the total ball-to-material ratio is 3.0x10 -3 Pa, ball milling is carried out by using a planetary ball mill, the ball milling rotating speed is 200r/mi, the ball milling time is 40h, the machine is stopped for 15min every 1h of ball milling, and amorphous powder for titanium alloy brazing is obtained through screening.
Fig. 5 is a microscopic morphology of the amorphous powder for titanium alloy brazing prepared in this example, and as can be seen from fig. 5, the amorphous powder for titanium alloy brazing is an irregular powder.
Fig. 6 is an XRD pattern of the amorphous powder for titanium alloy brazing prepared in this example, and as can be seen from fig. 6, the amorphous powder for titanium alloy brazing has the characteristics of an amorphous alloy.
Example 4
The embodiment comprises the following steps:
step one, preparing master alloy: preparing metal raw material blocks with the mass purity of more than 99.95 percent according to the mass percentage of elements corresponding to 37.5 percent Ti-37.5 percent Zr-15 percent Cu-10 percent Ni of amorphous powder for brazing the target product titanium alloy, and then sequentially placing the metal raw material blocks into a vacuum suspension smelting furnace for smelting, wherein the vacuum degree of smelting is at least 3.0 multiplied by 10 -3 Pa, smelting times are 6 times, and mother alloy cast ingots with uniform components are prepared;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting the master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller to 0.8mm, starting the copper roller with water cooling function, controlling the rotating speed to 2500r/min, continuously heating for 10min after the master alloy ingot is completely melted, and keeping the master alloy ingotThe temperature of the molten liquid is stabilized at 50 ℃ above the melting point of the alloy, argon with the mass purity of 99.999% is introduced into the induction smelting crucible to increase the air pressure in the induction smelting crucible, and a pressure difference of 0.5MPa is formed between the induction smelting crucible and the vacuum chamber, so that the mother alloy ingot casting molten liquid is rapidly sprayed out from a crucible nozzle under the action of pressure, and is rapidly cooled under the action of a copper roller rotating at a high speed to form a continuous amorphous strip of the titanium alloy;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing through a crusher, the obtained amorphous fragments are transferred into a zirconia vacuum ball milling tank, zirconia grinding balls are added until the total ball-to-material ratio is 40:1, the zirconia grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, and the sealing is carried out, and then the vacuum pumping is carried out until the total ball-to-material ratio is 3.0x10 -3 Pa, ball milling is carried out by using a planetary ball mill, the ball milling rotating speed is 200r/min, the ball milling time is 50h, the machine is stopped for 15min every 1h of ball milling, and amorphous powder for titanium alloy brazing is obtained through screening.
Example 5
The embodiment comprises the following steps:
step one, preparing master alloy: preparing metal raw material blocks with the mass purity of more than 99.95 percent according to the mass percentage of elements corresponding to 37.5 percent Ti-37.5 percent Zr-15 percent Cu-10 percent Ni of amorphous powder for brazing the target product titanium alloy, and then sequentially placing the metal raw material blocks into a vacuum suspension smelting furnace for smelting, wherein the vacuum degree of smelting is at least 3.0 multiplied by 10 -3 Pa, smelting times are 5 times, and mother alloy cast ingots with uniform components are prepared;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting a master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller to 1.2mm, starting the copper roller with water cooling function, controlling the rotating speed to be 3000r/min, continuously heating for 3min after the master alloy ingot is completely melted, keeping the temperature of the master alloy ingot to be 200 ℃ above the melting point of the alloy, and introducing argon with the mass purity of 99.999% into an induction melting crucible to increase the inductionThe pressure in the melting crucible is required to be increased, and a pressure difference of 0.5MPa is formed between the induction melting crucible and the vacuum chamber, so that master alloy ingot casting molten liquid is rapidly sprayed out from a crucible nozzle under the action of pressure, and is rapidly cooled under the action of a copper roller rotating at a high speed to form a continuous amorphous strip of the titanium alloy;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing through a crusher, the obtained amorphous fragments are transferred into a zirconia vacuum ball milling tank, zirconia grinding balls are added until the total ball-to-material ratio is 30:1, the zirconia grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, and the sealing is carried out, and then the vacuum pumping is carried out until the total ball-to-material ratio is 3.0x10 -3 Pa, ball milling is carried out by using a planetary ball mill, the ball milling rotating speed is 500r/min, the ball milling time is 20h, the machine is stopped for 15min every 1h of ball milling, and amorphous powder for titanium alloy brazing is obtained through screening.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (10)
1. A method for preparing amorphous powder for titanium alloy brazing, which is characterized by comprising the following steps:
step one, preparing master alloy: preparing a metal raw material according to the composition of amorphous powder for the target product titanium alloy brazing, and then placing the metal raw material into a vacuum suspension smelting furnace for smelting to prepare a master alloy cast ingot with uniform components;
step two, preparing an amorphous strip: placing the master alloy ingot obtained in the step one into an induction melting crucible of a vacuum melt-spinning machine, and vacuumizing a cavity to 3.0X10 -3 Pa, heating and melting the master alloy ingot through an induction coil, adjusting the distance between a crucible nozzle and the surface of a copper roller, starting the copper roller with water cooling function, controlling the rotating speed to 2500-3500 r/min, continuously heating for 3-10 min after the master alloy ingot is completely melted and stabilizing the temperature, and then introducing high-purity argon to melt the master alloy ingotSpraying the liquid from a crucible nozzle, and rapidly cooling under the action of a copper roller rotating at a high speed to form a continuous amorphous strip of the titanium alloy;
step three, preparing amorphous powder: the titanium alloy amorphous strip formed in the second step is subjected to preliminary crushing by a crusher, and then the obtained amorphous fragments are transferred into a vacuum ball milling tank, sealed and vacuumized to 3.0x10 -3 Pa, ball milling is carried out by using a planetary ball mill, and amorphous powder for titanium alloy brazing is obtained through screening.
2. The method for producing an amorphous powder for brazing a titanium alloy according to claim 1, wherein in the step one, the metal raw material has a mass purity of 99.95% or more and is in the form of a block.
3. The method for producing amorphous powder for brazing titanium alloy as recited in claim 1, wherein said vacuum degree of melting in the step one is at least 3.0x10 -3 Pa, the smelting times are at least 4 times.
4. The method for preparing amorphous powder for titanium alloy brazing according to claim 1, wherein after the master alloy ingot is completely melted and stabilized in the second step, high-purity argon is introduced into the induction smelting crucible to increase the air pressure in the induction smelting crucible, and a pressure difference of 0.5-1.0 MPa is formed between the induction smelting crucible and the vacuum chamber, so that the master alloy ingot solution is rapidly sprayed out from a crucible nozzle to the surface of a copper roller rotating at a high speed under the action of pressure, and is rapidly cooled to form a continuous titanium alloy amorphous strip.
5. The method for preparing amorphous powder for titanium alloy brazing according to claim 1, wherein in the second step, the distance between the crucible nozzle and the surface of the copper roller is 0.7 mm-1.2 mm.
6. The method for producing amorphous powder for titanium alloy brazing according to claim 1, wherein the rotation speed of the copper roller is 2500r/min to 3000r/min when the master alloy ingot casting solution is ejected from the crucible nozzle in the second step.
7. The method for producing amorphous powder for titanium alloy brazing according to claim 1, wherein the temperature of the master alloy ingot melt is stabilized at 50 ℃ to 200 ℃ above the alloy melting point when the master alloy ingot melt is ejected from the crucible nozzle in the second step.
8. The method for preparing amorphous powder for titanium alloy brazing according to claim 1, wherein in the third step, the vacuum ball milling tank and the grinding balls are made of zirconia.
9. The preparation method of the amorphous powder for titanium alloy brazing according to claim 8, wherein the grinding balls consist of grinding balls with the diameter of 8mm and grinding balls with the diameter of 5mm according to the mass ratio of 1.6:1, and the total ball-to-material ratio is 30:1-50:1.
10. The method for preparing amorphous powder for titanium alloy brazing according to claim 1, wherein the ball milling rotating speed in the third step is 200-500 r/min, the ball milling time is 20-50 h, and the machine is stopped for 15min every 1h of ball milling.
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