CN113600812A - Metal powder and preparation method thereof, metal alloy and preparation method thereof - Google Patents

Metal powder and preparation method thereof, metal alloy and preparation method thereof Download PDF

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CN113600812A
CN113600812A CN202110985530.6A CN202110985530A CN113600812A CN 113600812 A CN113600812 A CN 113600812A CN 202110985530 A CN202110985530 A CN 202110985530A CN 113600812 A CN113600812 A CN 113600812A
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metal
powder
niobium
metal powder
aluminum alloy
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CN113600812B (en
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疏达
肖飞
祝国梁
孙宝德
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10—Pre-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/10—Alloys based on aluminium with zinc as the next major constituent
    • 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
    • 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

A metal powder and a preparation method thereof, a metal alloy and a preparation method thereof belong to the technical field of alloys. The metal powder includes: the aluminum alloy powder and the niobium on the surface of the aluminum alloy powder are micron-sized, the particle size of the niobium is less than or equal to 200nm, and the mass of the niobium is 1-3% of that of the metal powder. The preparation method of the metal powder comprises the following steps: and mixing the aluminum alloy powder with niobium to obtain metal powder. The preparation method of the metal alloy comprises the following steps: and heating and melting the metal powder, and then solidifying and forming to obtain the metal alloy. The crystal grains of the metal alloy are equiaxed grains, and the size of the crystal grains is 1-5 mu m. The metal alloy made of the metal powder is fine in crystal grain and can solve the problem of crack generation.

Description

Metal powder and preparation method thereof, metal alloy and preparation method thereof
Technical Field
The application relates to the technical field of alloys, in particular to metal powder and a preparation method thereof, and a metal alloy and a preparation method thereof.
Background
Additive manufacturing technology (commonly known as 3D printing) is a very attractive rapid prototyping technology, has great advantages in particular in the preparation of complex structural components, and is commonly used for manufacturing metal parts with complex structures and excellent performance. At present, 3D printing of aluminum alloy is mostly concentrated on Al-Si series, because the weldability of the Al-Si series aluminum alloy is better, but the Al-Si series alloy belongs to aluminum alloy with medium and low strength and cannot meet the use requirement of higher strength. Aluminum alloys of 2 series (Al-Cu), 6 series (Al-Mg) and 7 series (Al-Zn) have higher strength, but these aluminum alloys have high hot cracking sensitivity and are likely to crack during solidification.
Disclosure of Invention
The application provides metal powder and a preparation method thereof, and a metal alloy and a preparation method thereof.
The embodiment of the application is realized as follows:
in a first aspect, embodiments of the present application provide a metal powder, including: the niobium-containing aluminum alloy powder comprises aluminum alloy powder and niobium on the surface of the aluminum alloy powder, the particle size of the aluminum alloy powder is micron-sized, the particle size of the niobium is less than or equal to 200nm, and the mass of the niobium is 1-3% of that of the aluminum alloy powder.
In a second aspect, embodiments of the present application provide a method for preparing a metal powder according to embodiments of the first aspect, including: and mixing the aluminum alloy powder with niobium to obtain metal powder.
In a third aspect, an embodiment of the present application provides a method for preparing a metal alloy, including: the metal powder of the embodiment of the first aspect is heated, melted and then solidified and formed to obtain the metal alloy.
In a fourth aspect, an embodiment of the present application provides a metal alloy, where the metal alloy is obtained by melting and solidifying the metal powder of the first aspect, crystal grains of the metal alloy are equiaxed crystals, and a size of the crystal grains is 1 to 5 μm.
The embodiment of the application at least comprises the following beneficial effects:
the particle size of the niobium is less than or equal to 200nm, the nano niobium has a small size effect, and in the process of mixing the nano niobium with the aluminum alloy powder, the nano niobium has a large specific surface area and insufficient coordination of surface atoms, so that the nano niobium can be spontaneously attached to the surface of the aluminum alloy powder under the action of van der Waals force to form the metal powder of the embodiment of the application.
Niobium granule cladding is showing the laser absorption rate that has improved aluminum alloy powder on aluminum alloy powder surface in this application, is favorable to printing the shaping.
In the process of heating and melting the metal powder of the embodiment of the application, niobium with the grain diameter less than or equal to 200nm is easy to melt and reacts with aluminum to generate Al3Nb, Al of fine size formed upon solidification3Nb，Al3Nb is used as an aluminum solidification primary phase and can be used as a heterogeneous nucleation core during aluminum solidification, so that the effect of grain refinement is achieved, the transformation of columnar crystal orientation to fine isometric crystal is promoted, and the probability of crack generation is reduced. The grain size of the metal alloy of the embodiment of the application is 1-5 μm through tests.
In addition, when the amount of niobium is outside the range of the examples of the present application, cracks are conspicuous in the resulting metal alloy, and it is difficult to mold.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is an SEM image of a metal powder of example 1 of the present application;
FIG. 2 is an SEM image of a metal powder of example 2 of the present application;
FIG. 3 is a laser reflectance spectrum of the metal powder of example 1 and comparative example 1 of the present application;
FIG. 4 is an optical micrograph of a metal alloy of example 3 of the present application;
FIG. 5 is an optical micrograph of a metal alloy of comparative example 7 of the present application;
FIG. 6 is a structural diagram of a metal alloy of comparative example 1 of the present application;
FIG. 7 is a structural diagram of a metal alloy according to example 1 of the present application;
FIG. 8 is a statistical plot of grain size for the metal alloy of comparative example 1 of the present application;
FIG. 9 is a statistical plot of the grain size of the metal alloy of example 1 of the present application;
FIG. 10 is a structural view of a metal alloy according to example 4 of the present application;
FIG. 11 is a structural diagram of a metal alloy of comparative example 3 of the present application;
FIG. 12 is an optical micrograph of a metal alloy of comparative example 4 of the present application.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the metal powder and the method of manufacturing the metal powder, the metal alloy and the method of manufacturing the metal alloy of the embodiments of the present application:
in a first aspect, embodiments of the present application provide a metal powder, including: the aluminum alloy powder and the niobium on the surface of the aluminum alloy powder are micron-sized, the particle size of the niobium is less than or equal to 200nm, and the mass of the niobium is 1-3% of that of the metal powder.
The inventors of the present application have found in their research that the problem of cracking of aluminum alloys can be improved by refining the grains or increasing the fluidity of the alloys. In the process of heating and melting the metal powder of the embodiment of the application, niobium with the grain diameter less than or equal to 200nm is easy to completely melt and reacts with aluminum to generate Al3Nb, Al of fine size formed upon solidification3Nb，Al3Nb is used as an aluminum solidification primary phase and can be used as a heterogeneous nucleation core during aluminum solidification, so that the effect of grain refinement is achieved, the transformation of columnar crystal orientation to fine isometric crystal is promoted, and the probability of crack generation is reduced. Among them, if the niobium on the surface of the aluminum alloy powder is not completely melted, cracks are likely to occur.
In addition, in the metal powder of the embodiment of the application, niobium is distributed on the surface of the aluminum alloy powder, so that the laser absorption rate of the metal powder can be improved, and the printing and forming are facilitated. Optionally, the niobium has a particle size of any one of 10nm, 30nm, 50nm, 80nm, 100nm, 120nm, 140nm, 160nm, 180nm, 200nm, 220nm, and 240nm, or a range between any two.
In addition, the inventors of the present application have found, in their studies, that if the aluminum alloy powder used is in the order of nanometers, the nanopowder volume fraction of the metal powder is relatively high, and that the metal powder is likely to cause a risk of explosion during heating and melting (for example, heating with a laser). Also, when the amount of niobium is outside the range of the examples of the present application, cracks of the resulting metal alloy are significant and it is difficult to mold.
Optionally, the aluminum alloy powder has a particle size of 10 to 60 μm.
Optionally, the mass of niobium is any one of, or a range between any two of, 1%, 1.5%, 2%, 2.5%, and 3% of the mass of the metal powder. In some embodiments, the mass of niobium is 1.5 to 3% of the mass of the metal powder.
In some embodiments, the aluminum alloy powder comprises, in weight percent: zn: 4.5 to 6.0 weight percent of Mg, 2.0 to 2.5 weight percent of Mg, 1.5 to 2.0 weight percent of Cu, 0.18 to 0.28 weight percent of Cr, less than 1.5 weight percent of impurity elements, less than or equal to 0.05 weight percent of O, less than or equal to 0.05 weight percent of N and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
The inventors of the present application, when studying a 7-series (Al-Zn) aluminum alloy, have found that the alloy fluidity can be improved and the thermal crack sensitivity can be reduced by adding Si, but Mg2The formation of Si phase greatly reduces the strengthening phase (MgZn) of the 7-series aluminum alloy2Phase) in the molding material, the strength of the molded article is reduced. The metal alloy prepared from the metal powder formed by the aluminum alloy powder and niobium has higher strength.
Alternatively, the Zn is 4.5 wt%, 5 wt%, 5.5 wt%, and 6 wt% in the aluminum alloy powder.
Alternatively, the Mg in the aluminum alloy powder is 2.1 wt%, 2.2 wt%, 2.3 wt%, 2.4 wt%, or 2.5 wt%.
Alternatively, the Cu in the aluminum alloy powder is 1.5 wt%, 1.6 wt%, 1.7 wt%, 1.8 wt%, 1.9 wt%, or 2 wt%.
Alternatively, the aluminum alloy powder has Cr at 0.18 wt%, 0.20 wt%, 0.22 wt%, 0.24 wt%, 0.26 wt%, or 0.28 wt%.
The metal powder of the embodiment of the present application may be used in the fields of 3D printing, laser cladding, powder metallurgy, spraying, injection molding, powder forging, and the like.
In a second aspect, embodiments of the present application provide a method for preparing a metal powder according to embodiments of the first aspect, including: and mixing the aluminum alloy powder with niobium to obtain metal powder.
The particle size of the niobium is less than or equal to 200nm, the nano niobium has a small size effect, and in the process of mixing the nano niobium with the aluminum alloy powder, the nano niobium has a large specific surface area and insufficient coordination of surface atoms, so that the nano niobium can be spontaneously attached to the surface of the aluminum alloy powder under the action of van der Waals force to form the metal powder of the embodiment of the application.
The aluminum alloy powder contains other metal elements in addition to aluminum, and the inventors of the present application have found that if aluminum fine powder, fine powder of other metal elements, and Nb nano powder are directly mixed and melted, the composition of the metal alloy tends to be uneven.
The Nb is distributed on the surface of the aluminum alloy powder, and the uniform distribution of the components of the metal alloy is facilitated after the Nb is heated and melted.
In some embodiments, the aluminum alloy powder is mixed with niobium by ball milling, wherein the ball-to-material ratio of the ball milling is 1-3: 1, and the rotation speed is 100-200 rpm.
When the aluminum alloy powder is mixed with niobium for ball milling, if the ball-to-material ratio is too large and the rotating speed is too high, the shape and the fluidity of the aluminum alloy powder are affected, so that the aluminum alloy powder is seriously deformed, and cracks are generated when the metal alloy is formed. If the ball material ratio is too small and the rotating speed is too slow, the aluminum alloy powder and the niobium are not favorably mixed uniformly, and the nano-scale niobium is easy to agglomerate together and is not favorable for printing and forming. Therefore, the ball-material ratio of ball milling is 1-3: 1, and the rotating speed is 100-200 rpm.
Further, in the ball milling process, the ball milling is suspended for 5-10 min every time the ball milling is carried out for 10-20 min, and then the ball milling is carried out, wherein the total time of the ball milling process is 2-4 h.
During the ball milling process, if the ball milling state is kept all the time, the heat generated by friction can aggravate the agglomeration of nano-niobium, and the niobium cannot be uniformly distributed on the surface of the aluminum alloy powder, so that the printing and molding are not facilitated. And the total time of ball-milling, the time of single ball-milling and the interval time of two ball-milling all can influence thermal production and thermal giving off, in the embodiment of the application, the in-process of ball-milling, every ball-milling 10 ~ 20min, pause 5 ~ 10min, carry out the ball-milling again, the total time of ball-milling process is 2 ~ 4h, be favorable to niobium to distributing on the aluminum alloy powder surface evenly more.
Illustratively, the time for a single ball mill is 10min, 12min, 15min, 18min, or 20 min. Illustratively, after a single ball milling, a pause of 5min, 6min, 7min, 8min, 9min, or 10min is made. Illustratively, the total time of the ball milling process is 2h, 2.5h, 3h, 3.5h, or 4 h.
In a third aspect, an embodiment of the present application provides a method for preparing a metal alloy, including: the metal powder of the embodiment of the first aspect is heated, melted and then solidified and formed to obtain the metal alloy.
In the process of heating and melting the metal powder of the embodiment of the application, the particle size is less than or equal to 200The nm niobium is easy to melt and reacts with aluminum to generate Al3Nb, Al of fine size formed upon solidification3Nb，Al3Nb is used as an aluminum solidification primary phase and can be used as a heterogeneous nucleation core during aluminum solidification, so that the effect of grain refinement is achieved, the transformation of columnar crystal orientation to fine isometric crystal is promoted, and the probability of crack generation is reduced. The grain size of the metal alloy of the embodiment of the application is 1-5 μm through tests.
Further, in one embodiment, the metal powder is heated and melted by laser, the laser power used for laser heating is 200-300 w, and the scanning speed is 200-1200 mm/s.
In the laser heating process, the cooling rate of the molten metal powder is high, and the metal powder can be quickly solidified and formed. In the process of laser heating of metal powder, the quality of the metal alloy is influenced by the laser power and the scanning speed, wherein the scanning speed of the laser is related to the action time of the laser, the larger the scanning speed of the laser is, the shorter the action time of the laser on the metal powder is, the smaller the scanning speed of the laser is, and the longer the action time of the laser on the metal powder is. The inventor of the present application has found that if the niobium particles have a large size, a long laser action time is required to completely melt the niobium, and a long laser action time is maintained, so that the laser scanning rate needs to be reduced, and the laser scanning rate is too low, which causes metal powder splashing and bath instability, resulting in hole defects inside the metal alloy.
Through research of the inventor of the application, the niobium in the metal powder has the particle size of less than or equal to 200nm, the laser power is 200-300 w, and when the scanning speed is 200-1200 mm/s, the niobium can be completely melted, holes cannot be generated in the metal, a compact metal alloy is obtained, and the strength of the metal alloy is further improved.
Illustratively, the laser power is 200w, 220w, 240w, 250w, 270w, 280w, or 300 w.
Illustratively, the described rate of the laser is any one of 200mm/s, 400mm/s, 600mm/s, 800mm/s, 1000mm/s, and 1200mm/s or a range between any two.
In some embodiments, the metal powder is heated to melt the metal powder by selective laser melting, which is performed by a selective laser melting device.
The selective laser melting process comprises the following steps: the three-dimensional digital model of the part is sliced and layered through special software, after contour data of each section is obtained, metal powder is selectively melted by utilizing laser beams according to the contour data, and the molded part is manufactured in a mode of spreading powder layer by layer and melting, solidifying and accumulating layer by layer. Wherein the metal powder is spread on the substrate.
Optionally, when the metal powder is heated by selective laser melting, the substrate temperature is 130-180 ℃, the layer thickness of the metal powder is 25-35 μm, the overlapping distance is 100-120 μm, and the rotation angle of the interlayer laser scanning is 67 °. Note that the overlap distance refers to a straight line distance between the centers of two laser spots.
In a fourth aspect, an embodiment of the present application further provides a metal alloy, where the metal alloy is obtained by melting and solidifying the metal powder in the embodiment of the first aspect, crystal grains of the metal alloy are equiaxial crystals, and a size of the crystal grains is 1 to 5 μm.
The metal alloy is almost free of cracks and has high strength, and through tests, the tensile strength of the metal alloy is greater than 500MPa, and the elongation is greater than or equal to 10%.
The metal powder and the method for producing the same, the metal alloy and the method for producing the same of the present application will be described in further detail with reference to examples.
Example 1
This example provides a metal powder comprising an aluminum alloy powder and niobium on the surface of the aluminum alloy powder, wherein the aluminum alloy powder has a particle size of 10 to 60 μm, the niobium has a particle size of 20 to 200nm, and the mass of niobium is 1.5% of the mass of the metal powder. Wherein the aluminum alloy powder comprises the following components in percentage by weight: zn: 4.8 wt%, Mg 2.3 wt%, Cu 1.8 wt%, Cr 0.18 wt%, impurity elements less than 0.15 wt%, O less than or equal to 0.05 wt%, N less than or equal to 0.05 wt%, and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
The present embodiment provides a method for preparing the metal powder, which includes the steps of:
(1) melting Al, Zn, Mg and Cu metal blocks at 700 ℃, preserving heat for 10min, and casting into 7-series Al-Zn-Mg-Cu alloy ingots, wherein the contents of Fe, Si, Mn and Ti are controlled to be lower than 0.15 wt%, and the contents of O, N are controlled to be lower than 0.03 wt%.
(2) And (2) melting the alloy ingot prepared in the step (1), then obtaining alloy powder by adopting an air atomization mode, drying the alloy powder, and then obtaining the aluminum alloy powder with the particle size range of 10-60 mu m by adopting a vacuum pneumatic sieve. This process can control the aluminum alloy powder O, N content to be less than 0.05 wt%.
(3) Adding the aluminum alloy powder obtained in the step (2) and niobium into a stainless steel ball milling tank with steel balls, wherein the ball-material ratio is controlled to be 2: 1, mixing at the rotation speed of 150rpm, pausing for 5min every 15min of ball milling for aeration cooling, and cumulatively mixing for 3h to obtain the metal powder of the embodiment. The metal powder maintained good sphericity and good fluidity, and the oxygen content was found to be 780 ppm.
The embodiment also provides a metal alloy, which is prepared by the following steps:
s1, inputting the preset three-dimensional model into a selective laser melting device;
s2, setting the preheating temperature of the substrate of the selective laser melting equipment to be 150 ℃, the laser power to be 225W, the laser scanning speed to be 200mm/S, the layer thickness of the metal powder to be 30 microns, the lap joint distance to be 120 microns, the scanning mode to be strip scanning, and the rotation angle of the interlaminar laser scanning to be 67 degrees;
s3, pouring the metal powder into a blanking hopper of selective laser melting equipment, vacuumizing a melting cavity after the melting cavity is sealed, introducing argon, and printing according to a set three-dimensional model and printing parameters when the oxygen content in the melting cavity reaches below 100ppm and the temperature of a substrate is stabilized at 150 ℃ to obtain the metal alloy, wherein the crystal grain of the metal alloy is isometric crystal, the size of the crystal grain is 1-5 mu m, holes and cracks are basically absent in the metal alloy, and the forming rate is high.
Example 2
This example provides a metal powder comprising an aluminum alloy powder and niobium on the surface of the aluminum alloy powder, wherein the aluminum alloy powder has a particle size of 10 to 60 μm, the niobium has a particle size of 50 to 200nm, and the mass of niobium is 2% of the mass of the metal powder. Wherein the aluminum alloy powder comprises the following components in percentage by weight: zn: 5.1 wt%, Mg 2.1 wt%, Cu 1.9 wt%, Cr 0.18 wt%, impurity elements less than 0.15 wt%, O less than or equal to 0.05 wt%, N less than or equal to 0.05 wt%, and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
The present embodiment provides a method for preparing the metal powder, which includes the steps of:
(1) melting Al, Zn, Mg and Cu metal blocks at 700 ℃, preserving heat for 10min, and casting into 7-series Al-Zn-Mg-Cu alloy ingots, wherein the contents of Fe, Si, Mn and Ti are controlled to be lower than 0.15 wt%, and the contents of O, N are controlled to be lower than 0.03 wt%.
(2) And (2) melting the alloy ingot prepared in the step (1), then obtaining alloy powder by adopting an air atomization mode, drying the alloy powder, and then obtaining the aluminum alloy powder with the particle size range of 10-60 mu m by adopting a vacuum pneumatic sieve. This process can control the aluminum alloy powder O, N content to be less than 0.05 wt%.
(3) The metal powder of this example was obtained by mixing an aluminum alloy powder having a particle size in the range of 10 to 60 μm with niobium having a particle size in the range of 50 to 200nm for 4 hours. The metal powder maintained good sphericity and good fluidity, and the oxygen content was found to be 600 ppm.
The embodiment also provides a metal alloy, which is prepared by the following steps:
s1, inputting the preset three-dimensional model into a selective laser melting device;
s2, setting the preheating temperature of the substrate of the selective laser melting equipment to be 150 ℃, the laser power to be 250W, the laser scanning speed to be 600mm/S, the layer thickness of the metal powder to be 30 microns, the lap joint distance to be 120 microns, the scanning mode to be strip scanning, and the rotation angle of the interlaminar laser scanning to be 67 degrees;
s3, pouring the metal powder into a blanking hopper of selective laser melting equipment, vacuumizing a melting cavity after the melting cavity is sealed, introducing argon, and printing according to a set three-dimensional model and printing parameters when the oxygen content in the melting cavity reaches below 100ppm and the temperature of a substrate is stabilized at 150 ℃ to obtain the metal alloy, wherein the crystal grain of the metal alloy is isometric crystal, the size of the crystal grain is 1-5 mu m, holes and cracks are basically absent in the metal alloy, and the forming rate is high.
Example 3
The present embodiment provides a metal powder, which includes an aluminum alloy powder and niobium on the surface of the aluminum alloy powder, wherein the particle size of the aluminum alloy powder is 10 to 60 μm, the particle size of the niobium is 100-200nm, and the mass of the niobium is 2.5% of the mass of the metal powder. Wherein the aluminum alloy powder comprises the following components in percentage by weight: zn: 5.7 wt%, Mg 2.1 wt%, Cu 1.7 wt%, Cr 0.21 wt%, impurity elements less than 0.15 wt%, O less than or equal to 0.05 wt%, N less than or equal to 0.05 wt%, and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
The present embodiment provides a method for preparing the metal powder, which includes the steps of:
(1) melting Al, Zn, Mg and Cu metal blocks at 700 ℃, preserving heat for 10min, and casting into 7-series Al-Zn-Mg-Cu alloy ingots, wherein the contents of Fe, Si, Mn and Ti are controlled to be lower than 0.15 wt%, and the contents of O, N are controlled to be lower than 0.03 wt%.
(2) And (2) melting the alloy ingot prepared in the step (1), then obtaining alloy powder by adopting an air atomization mode, drying the alloy powder, and then obtaining the aluminum alloy powder with the particle size range of 10-60 mu m by adopting a vacuum pneumatic sieve. This process can control the aluminum alloy powder O, N content to be less than 0.05 wt%.
(3) The metal powder of this example was obtained by mixing an aluminum alloy powder having a particle size of 10 to 60 μm with niobium having a particle size of 100 and 200nm for 5 hours. The metal powder maintained good sphericity and good flowability, with an oxygen content of 620ppm as measured.
The embodiment also provides a metal alloy, which is prepared by the following steps:
s1, inputting the preset three-dimensional model into a selective laser melting device;
s2, setting the preheating temperature of the substrate of the selective laser melting equipment to be 150 ℃, the laser power to be 300W, the laser scanning speed to be 1000mm/S, the layer thickness of the metal powder to be 30 microns, the lap joint distance to be 120 microns, the scanning mode to be strip scanning, and the rotation angle of the interlaminar laser scanning to be 67 degrees;
s3, pouring the metal powder into a blanking hopper of selective laser melting equipment, vacuumizing a melting cavity after the melting cavity is sealed, introducing argon, and printing according to a set three-dimensional model and printing parameters when the oxygen content in the melting cavity reaches below 100ppm and the temperature of a substrate is stabilized at 150 ℃ to obtain the metal alloy, wherein the crystal grain of the metal alloy is isometric crystal, the size of the crystal grain is 1-5 mu m, holes and cracks are basically absent in the metal alloy, and the forming rate is high.
Example 4
This example provides a metal powder comprising an aluminum alloy powder and niobium on the surface of the aluminum alloy powder, wherein the aluminum alloy powder has a particle size of 10 to 60 μm, the niobium has a particle size of 20 to 200nm, and the mass of niobium is 3% of the mass of the metal powder. Wherein the aluminum alloy powder comprises the following components in percentage by weight: zn: 5.3 wt%, Mg 2.2 wt%, Cu 1.6 wt%, Cr 0.27 wt%, impurity elements less than 0.15 wt%, O less than or equal to 0.05 wt%, N less than or equal to 0.05 wt%, and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
The present embodiment provides a method for preparing the metal powder, which includes the steps of:
(1) melting Al, Zn, Mg and Cu metal blocks at 700 ℃, preserving heat for 10min, and casting into 7-series Al-Zn-Mg-Cu alloy ingots, wherein the contents of Fe, Si, Mn and Ti are controlled to be lower than 0.15 wt%, and the contents of O, N are controlled to be lower than 0.03 wt%.
(2) And (2) melting the alloy ingot prepared in the step (1), then obtaining alloy powder by adopting an air atomization mode, drying the alloy powder, and then obtaining the aluminum alloy powder with the particle size range of 10-60 mu m by adopting a vacuum pneumatic sieve. This process can control the aluminum alloy powder O, N content to be less than 0.05 wt%.
(3) Adding aluminum alloy powder with the particle size range of 10-60 mu m and niobium with the particle size of 20-200nm into a stainless steel ball milling tank with steel balls, wherein the ball-material ratio is controlled to be 2: 1, mixing at the rotation speed of 200rpm, pausing for 5min every 10min of ball milling for aeration cooling, and obtaining the metal powder of the embodiment after accumulative mixing for 2 h. The metal powder maintained good sphericity and good fluidity, with an oxygen content of 750ppm measured.
The embodiment also provides a metal alloy, which is prepared by the following steps:
s1, inputting the preset three-dimensional model into a selective laser melting device;
s2, setting the preheating temperature of the substrate of the selective laser melting equipment to be 150 ℃, the laser power to be 275W, the laser scanning speed to be 600mm/S, the layer thickness of the metal powder to be 30 microns, the lapping distance to be 120 microns, the scanning mode to be strip scanning, and the rotation angle of the interlaminar laser scanning to be 67 degrees;
s3, pouring the metal powder into a blanking hopper of selective laser melting equipment, vacuumizing a melting cavity after the melting cavity is sealed, introducing argon, and printing according to a set three-dimensional model and printing parameters when the oxygen content in the melting cavity reaches below 100ppm and the temperature of a substrate is stabilized at 150 ℃ to obtain the metal alloy, wherein the crystal grain of the metal alloy is isometric crystal, the size of the crystal grain is 1-5 mu m, holes and cracks are basically absent in the metal alloy, and the forming rate is high.
Example 5
The embodiment provides a metal powder, which comprises an aluminum alloy powder and niobium on the surface of the aluminum alloy powder, wherein the particle size of the aluminum alloy powder is 30-80 mu m, the particle size of the niobium is less than 150nm, and the mass of the niobium is 1.5% of the mass of the metal powder. Wherein the aluminum alloy powder comprises the following components in percentage by weight: zn: 4.8 wt%, Mg 2.3 wt%, Cu 1.8 wt%, Cr 0.18 wt%, impurity elements less than 0.15 wt%, O less than or equal to 0.05 wt%, N less than or equal to 0.05 wt%, and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
The present embodiment provides a method for preparing the metal powder, which includes the steps of:
(1) melting Al, Zn, Mg and Cu metal blocks at 700 ℃, preserving heat for 10min, and casting into 7-series Al-Zn-Mg-Cu alloy ingots, wherein the contents of Fe, Si, Mn and Ti are controlled to be lower than 0.15 wt%, and the contents of O, N are controlled to be lower than 0.03 wt%.
(2) And (2) melting the alloy ingot prepared in the step (1), then obtaining alloy powder by adopting an air atomization mode, drying the alloy powder, and then obtaining the aluminum alloy powder with the particle size range of 30-80 microns by adopting a vacuum pneumatic sieve. This process can control the aluminum alloy powder O, N content to be less than 0.05 wt%.
(3) Adding aluminum alloy powder with the particle size range of 30-80 mu m and niobium with the particle size of less than 150nm into a stainless steel ball milling tank with steel balls, wherein the ball-material ratio is controlled to be 2: 1, mixing at the rotation speed of 150rpm, pausing for 5min every 15min of ball milling for aeration cooling, and cumulatively mixing for 3h to obtain the metal powder of the embodiment. The metal powder maintained good sphericity and good fluidity, and the oxygen content was found to be 780 ppm.
The embodiment also provides a metal alloy, which is prepared by the following steps:
s1, inputting the preset three-dimensional model into a selective laser melting device;
s2, setting the preheating temperature of the substrate of the selective laser melting equipment to be 150 ℃, the laser power to be 225W, the laser scanning speed to be 200mm/S, the layer thickness of the metal powder to be 30 microns, the lap joint distance to be 120 microns, the scanning mode to be strip scanning, and the rotation angle of the interlaminar laser scanning to be 67 degrees;
s3, pouring the metal powder into a blanking hopper of selective laser melting equipment, vacuumizing a melting cavity after the melting cavity is sealed, introducing argon, and printing according to a set three-dimensional model and printing parameters when the oxygen content in the melting cavity reaches below 100ppm and the temperature of a substrate is stabilized at 150 ℃ to obtain the metal alloy, wherein the crystal grain of the metal alloy is isometric crystal, the size of the crystal grain is 1-5 mu m, holes and cracks are basically absent in the metal alloy, and the forming rate is high.
Comparative example 1
Comparative example 1 provides a metal powder, which is different from example 1 only in that niobium is not contained in the metal powder of the present comparative example.
Comparative example 1 provides a method for preparing the above metal powder, differing from example 1 only in that step (3) is omitted.
Comparative example 1 also provides a metal alloy and a method of making the same, the method of making the metal alloy being the same as in example 1. The crystal grains of the metal alloy prepared by the comparative example are columnar crystal structures, the average crystal grain size is 18.75 mu m, and obvious cracks and holes are formed inside the metal alloy.
Comparative example 2
Comparative example 2 provides a metal powder and a method for preparing the same, which are different from example 3 only in that the particle size of niobium of the present comparative example is 300 to 500 nm.
Comparative example 2 also provides a metal alloy and a method for preparing the same, which is different from example 3 only in that the laser power is increased and the scanning rate is reduced due to the increased diameter of niobium, in order to melt niobium, the laser power is 350W and the scanning rate is 400 mm/s. The metal alloy obtained in this comparative example had cracks in the inside thereof and had unmelted niobium particles.
Comparative example 3
Comparative example 3 provides a metal powder and a method for preparing the same, which are different from example 4 only in that the mass of niobium of the present comparative example is 0.5% of the mass of the metal powder.
Comparative example 3 provides a metal alloy and a method of preparing the same, the method of preparing the metal alloy being the same as in example 4. The grains of the metal alloy obtained in comparative example 3 were columnar grains and coarse isometric grains, the average grain size was 13.2 μm, and cracks were still more conspicuously present.
Comparative example 4
Comparative example 4 provides a metal powder and a method for preparing the same, which are different from example 4 only in that the mass of niobium of the present comparative example is 4% of the mass of the metal powder.
Comparative example 4 provides a metal alloy and a method of preparing the same, the method of preparing the metal alloy being the same as in example 4. The crystal grain of the metal alloy prepared in comparative example 4 is equiaxed, the size of the crystal grain is 1-5 μm, but the inside has micro-cracks and unmelted niobium aggregates.
Comparative example 5
Comparative example 5 provides a metal powder and a method for preparing the same, which are different from example 4 only in the method for preparing a metal powder of the present comparative example in that the ball milling process parameters of step (3) are: controlling the ball material ratio to be 5: 1, mixing at the rotation speed of 300rpm, pausing for 5min every 10min of ball milling for aeration cooling, and obtaining the metal powder of the embodiment after accumulative mixing for 2 h. The metal powder is severely deformed and the sphericity is seriously deteriorated.
Comparative example 5 provides a metal alloy and a method of preparing the same, the method of preparing the metal alloy being the same as in example 4. The crystal grain of the metal alloy prepared in the comparative example 5 is columnar crystal, the size of the crystal grain is 1-5 mu m, and the interior of the metal alloy is provided with unmelted niobium, and the unfused hole in the interior is obvious.
Comparative example 6
Comparative example 6 provides a metal powder and a method for preparing the same as in example 2.
Comparative example 6 provides a metal alloy and a method for preparing the same, which are different from those of example 4 only in that the laser power of the comparative example is 325W and the scan rate is 1400 mm/s. The metal alloy obtained in comparative example 6 had unmelted aluminum alloy powder and Nb, and voids that were not fused inside were evident.
Comparative example 7
Comparative example 7 provides a metal powder and a method for preparing the same, which are different from example 1 only in that niobium of the present comparative example is in the order of micrometers.
Comparative example 7 also provides a metal alloy and a method of preparing the same, which are different from example 1 only in that the laser power is 350W and the scan rate is 100 mm/s. The metal alloy obtained in this comparative example had cracks and pores in the inside thereof and had unmelted niobium particles.
In each of the examples and comparative examples of the present application, the metal powder used in the method for producing the metal alloy is the metal powder used in the corresponding example and comparative example.
Test example 1
The metal powders obtained in examples 1 and 2 were observed under an electron scanning microscope to obtain SEM images as shown in fig. 1 and 2.
As can be seen from fig. 1 and 2, the niobium particles are on the surface of the aluminum alloy powder.
Test example 2
The metal powders obtained in example 1 and comparative example 1 were tested for laser reflectivity, and the results are shown in fig. 3.
As can be seen from the results of fig. 3, in example 1 of the present application, the surface of the aluminum alloy powder has niobium, and has a higher laser reflectance than the aluminum alloy powder alone.
Test example 3
The results of observing the metal alloys obtained in example 3 and comparative example 7 under an optical microscope are shown in fig. 4 and 5.
As can be seen from fig. 4 and 5, the metallic alloy obtained in comparative example 7 contained unmelted Nb particles and showed significant cracking, whereas the metallic alloy obtained in example 3 of the present application contained no unmelted Nb particles and showed no cracking. Among them, in the method of manufacturing the metal alloy of comparative example 7, in order to completely melt niobium, a higher laser power and a smaller laser scanning rate than those of example 1 were selected to secure more energy input, but Nb was not completely melted and the manufactured metal alloy generated cracks.
Further, it was found by comparing example 3 with comparative example 2 that in the method for preparing the metal alloy of comparative example 2, in order to completely melt niobium, a higher laser power and a smaller laser scanning rate than those of example 3 were selected to secure more energy input, but Nb was not completely melted and the prepared metal alloy generated cracks.
It is explained that when the particle size of niobium is larger than 200nm, niobium is not easily melted, and it is difficult to play a role in grain refinement and crack suppression.
Test example 4
The metal alloys obtained in comparative example 1 and example 1 were observed under a scanning electron microscope, and their structural diagrams are shown in fig. 6 and 7, respectively. The grain sizes of the metal alloys obtained in comparative example 1 and example 1 were counted, and the results are shown in fig. 8 and 9, respectively.
As can be seen from fig. 6 and 7, the metal alloy obtained in comparative example 1 has significant cracks and voids, and the grain structure thereof is columnar crystal, whereas the metal alloy obtained in example 1 of the present application has no cracks and voids, and the grain structure thereof is equiaxed crystal. It is demonstrated that the addition of Nb can improve the generation of cracks.
As can be seen from fig. 8 and 9, the average grain size of the metal alloy obtained in comparative example 1 was about 18 μm, whereas the structure of the metal alloy obtained in example 1 of the present application was significantly refined and the average grain size was about 2 μm.
Test example 5
The results of observing the structures of the metal alloys obtained in example 4 and comparative examples 3 to 4 are shown in fig. 10 to 12.
As can be seen from fig. 12, the higher Nb content in comparative example 4 is not favorable for dispersion of Nb nanoparticles, resulting in the presence of unmelted Nb agglomerates, insufficient grain refinement effect, and reduced formability.
Test example 6
(1) The compactness of the metal alloys of examples 1 to 5 and comparative examples 1 to 7 was tested by means of the archimedes drainage method, the results of which are reported in table 1.
(2) The metal alloys of examples 1 to 5 and comparative examples 1 to 7 were subjected to a standard T6 heat treatment and tested for tensile strength and elongation, the results of which are reported in Table 1. It should be noted that the metal alloys of comparative examples 1 to 7 had no data on tensile strength and elongation because cracks existed and they were broken without yielding.
TABLE 1 compactness, tensile strength and elongation
Figure BDA0003230381150000161
Figure BDA0003230381150000171
From the results in table 1, it can be known that the metal alloys of examples 1 to 5 of the present application all have higher compactness, tensile strength and elongation.
The foregoing is illustrative of the present application and is not to be construed as limiting thereof, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A metal powder, comprising: the metal powder comprises aluminum alloy powder and niobium on the surface of the aluminum alloy powder, wherein the grain size of the aluminum alloy powder is micron-sized, the grain size of the niobium is less than or equal to 200nm, and the mass of the niobium is 1-3% of that of the metal powder.
2. The metal powder according to claim 1, wherein the aluminum alloy powder has a particle size of 10 to 60 μm.
3. The metal powder according to claim 1, wherein the mass of niobium is 1.5 to 3% of the mass of the aluminum alloy powder.
4. A metal powder according to any one of claims 1 to 3, wherein the aluminium alloy powder comprises, in weight percent: zn: 4.5-6.0 wt%, Mg 2.0-2.5 wt%, Cu 1.5-2.0 wt%, Cr 0.18-0.28 wt%, impurity elements less than 1.5 wt%, O less than or equal to 0.05 wt%, N less than or equal to 0.05 wt%, and the balance of Al, wherein the impurity elements comprise Fe, Si, Mn and Ti.
5. A method for producing a metal powder according to any one of claims 1 to 4, comprising: mixing the aluminum alloy powder with the niobium to obtain the metal powder.
6. The method for preparing metal powder according to claim 5, wherein the aluminum alloy powder and the niobium are mixed by ball milling, wherein the ball-to-material ratio of the ball milling is 1-3: 1, and the rotation speed is 100-200 rpm.
7. The method for preparing metal powder according to claim 6, wherein in the ball milling process, the ball milling is suspended for 5-10 min every time the ball milling is performed for 10-20 min, and then the ball milling is performed, wherein the total time of the ball milling process is 2-4 h.
8. A method of making a metal alloy, comprising: heating and melting the metal powder according to any one of claims 1 to 4, and then solidifying and forming to obtain the metal alloy.
9. The method for preparing the metal alloy according to claim 8, wherein the heating and melting of the metal powder is laser heating, the laser power used for the laser heating is 200-300 w, and the scanning speed is 200-1200 mm/s.
10. A metal alloy obtained by melting and solidifying the metal powder according to any one of claims 1 to 4, wherein the crystal grains of the metal alloy are equiaxed grains having a grain size of 1 to 5 μm.
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