CN114226736A - Method for inhibiting crack formation and promoting grain refinement of additive manufacturing aluminum alloy - Google Patents
Method for inhibiting crack formation and promoting grain refinement of additive manufacturing aluminum alloy Download PDFInfo
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- CN114226736A CN114226736A CN202111567671.2A CN202111567671A CN114226736A CN 114226736 A CN114226736 A CN 114226736A CN 202111567671 A CN202111567671 A CN 202111567671A CN 114226736 A CN114226736 A CN 114226736A
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- 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
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
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- 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]
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B22F9/00—Making metallic powder or suspensions thereof
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Abstract
The invention discloses a method for inhibiting the formation of cracks in an additive manufacturing aluminum alloy and promoting grain refinement, which comprises the steps of mixing powder by using a horizontal ball mill, uniformly assembling fine niobium particles on the surface of aluminum alloy powder in an ultra-short time and simultaneously keeping the near-spherical shape of the alloy; and melting the mixed powder by additive manufacturing to prepare a sample. The invention also provides a three-dimensional rotary swinging powder mixing device for mixing the niobium-containing alloy powder and the aluminum alloy powder with the same particle size (without steel balls and ball milling); and then melting and sampling the mixed powder by using additive manufacturing. In addition, the invention also provides the method for preparing the niobium-containing aluminum alloy powder or wire material in advance; and then melting and sampling by using additive manufacturing. The method promotes the complete transformation of columnar crystal orientation equiaxial crystals and the great refinement of crystal grains by preferentially forming a novel heterogeneous nucleating agent in the additive manufacturing solidification process, simultaneously inhibits cracks, and improves the laser additive manufacturing formability and the mechanical property of the high-strength aluminum alloy.
Description
Technical Field
The invention relates to the field of aluminum alloy additive manufacturing, in particular to a method for improving high-strength aluminum alloy additive manufacturing formability and promoting grain refinement.
Background
Metal additive manufacturing is of great interest because of its excellent near-net-shape forming ability. However, the molten pool formed by metal additive manufacturing often experiences extremely rapid cooling and steep thermal gradients, resulting in grain growth with grain extension during solidification, formation of coarse vertical columnar grains and significant texture. Meanwhile, during metal additive manufacturing, significant internal stresses may develop in the sample or part due to the presence of thermal gradients and non-uniform heat distribution and extremely fast cooling rates. These two factors can cause materials such as superalloys, intermetallics, high strength high entropy alloys, and high strength aluminum alloys (e.g., 7075 and 6061) to crack during additive manufacturing processes, exhibiting very low formability. The presence of columnar crystals also leads to severe anisotropy of mechanical properties of the material.
Through alloy design or addition of nucleation particles, a large amount of heterogeneous nucleation of the alloy is promoted in the additive manufacturing process, so that promotion of columnar crystal orientation equiaxial crystal transformation and grain refinement is an effective way for dispersing internal stress, inhibiting cracks and improving material performance. This approach is particularly effective in additive manufactured aluminum alloys. By adding elements such as Zr, Sc, Ti, Ni, Ta and the like into aluminum alloy, Al with higher melting point is precipitated in the laser additive manufacturing process3The X precipitation phase (X ═ Zr, Sc, Ti, Ni and Ta) has small lattice mismatching degree with the matrix, and can be preferentially separated out from the melt in the solidification and cooling processes due to high melting point, so the X precipitation phase is an effective heterogeneous nucleation point of alpha-Al crystal grains, greatly promotes the transformation of the crystal grain structure of the aluminum alloy from columnar crystal to isometric crystal after laser additive manufacturing, and promotes the crystal grainsThe thinning effectively inhibits the formation of cracks in the aluminum alloy. It is noted that the addition of the above elements, although effective in promoting the transformation of the aluminum alloy grain structure from columnar grains to equiaxed grains, mostly does not form complete equiaxed grains, but forms a grain structure in which columnar grains and equiaxed grains are mixed. The elements are usually added into the aluminum alloy in a melting alloying and pre-alloying powder preparation mode, so that the preparation cost is high, and the development period is long. And compound particles of the elements are added into the aluminum alloy by using the traditional ball milling method for additive manufacturing, but the sphericity of alloy powder is often damaged by using the traditional ball milling method, so that the internal porosity of a sample prepared by the additive manufacturing is high, and the performance is not favorable.
Disclosure of Invention
The invention aims to solve the problem that cracks and large columnar crystals are easily formed in the laser additive manufacturing process of high-strength aluminum alloys such as 6-series and 7-series aluminum alloys, and aims to promote the complete transformation of columnar crystal orientation equiaxial crystals and the great refinement of crystal grains by adding a novel nucleating agent, inhibit the cracks, improve the laser additive manufacturing formability and the mechanical property of the high-strength aluminum alloys, and pave the way for the popularization and application of the laser additive manufacturing technology of the high-strength aluminum alloys.
The invention also provides a horizontal ball mill for mixing powder aiming at the problem that a powder mixing device which is efficient and can keep the near-spherical shape of alloy powder particles during powder mixing is absent when the particles are added into the aluminum alloy, so that the near-spherical shape of different powder particles can be kept while the different powder particles are uniformly mixed in an ultra-short time, and the improvement of the laser melting formability of an alloy selection area is facilitated.
The invention adopts the following technical scheme:
a method for inhibiting the formation of cracks in an additive manufacturing aluminum alloy and promoting the grain refinement is used for preparing Nb-containing aluminum alloy powder or Nb-containing aluminum alloy wires; and melting and sampling the powder or wire material by using additive manufacturing. By adding Nb, on one hand, Nb is expected to react with Al to form Al in the laser additive manufacturing process3Nb precipitate phase due to Al3The melting point of Nb (1680 ℃) is much higher than that of alpha-Al (663 ℃), which means that Al is in the process of solidification3Nb particles have a large supercooling degree and precipitate a large amount of Al in the melt before the nucleation of alpha-Al3And (3) Nb particles. On the other hand, Al3The lattice mismatching degree of the Nb particles and the alpha-Al matrix is very small, and two phases are the closest arranged crystal planes {111}Al//{112}Al3NbHas a mismatching degree of interplanar spacing of only 1.71%, and {200}Al//{200}Al3NbThe mismatching degree of the interplanar spacing is only 5.14%. This low degree of lattice mismatch between the two phases means that Al is present3The Nb particles are strong heterogeneous nucleation particles that promote the formation of large numbers of alpha-Al equiaxed grains.
Further, the preparation of the Nb-containing aluminum alloy powder specifically comprises: mixing 1-5 wt% of fine Nb particles with the particle size of 50nm-5 mu m and 15-53 mu m of aluminum alloy powder in an inert atmosphere by using a horizontal ball mill, wherein the ball powder ratio is 5: 1, the rotation speed is 300-. The horizontal ball mill used in the invention utilizes the rotation of the blades on the central shaft thereof to bring the powder and the steel balls into the air for contact collision. The rotating speed of the shaft and the blades can reach 2000r/min at most, and the extremely high rotating capacity of the grinding shaft can enable the grinding medium to obtain an extremely high relative speed (14 m/s at most) which is more than 3 times that of the traditional ball milling equipment, so that different powder particles can be uniformly mixed in a short time (less than or equal to 30 min). For two kinds of powder with large particle size difference, the ball mill can efficiently and uniformly assemble fine powder particles on the surface of large particles, and simultaneously keep large particles in a nearly spherical shape, namely, the ball mill can efficiently and uniformly assemble fine Nb particles on the surface of aluminum alloy powder particles, and simultaneously keep the nearly spherical shape of the alloy powder particles. The ball mill can also be vacuumized or filled with argon in real time, and the inner part of the wall of the ball mill cavity can be cooled by water in real time, so that the alloy powder is protected from being oxidized and overheated.
Further, the preparation of the Nb-containing aluminum alloy powder specifically comprises: 1-6 wt% of niobium-containing alloy powder with the particle size of 15-53 mu m and aluminum alloy powder with the particle size of 15-53 mu m are mixed by using a three-dimensional swing powder mixer in an inert atmosphere, the rotating speed is 20-40 rpm, and the mixing time is 3-24 hours. Aluminum alloy powder particles with equivalent particle size and niobium-containing alloy powder particles by utilizing three-dimensional powder mixing deviceParticles such as Ti-22Al-25Nb (or Ti2AlNb) are mixed and then laser additive manufactured, again by forming Al3Nb or Al3(Nb, Ti) to promote nucleation and equiaxed crystallization.
Further, the preparation of the Nb-containing aluminum alloy powder specifically comprises: the preparation method comprises the steps of proportioning niobium and aluminum alloy according to a proportion, wherein the niobium accounts for 1-5 wt% of the aluminum alloy, preparing a pre-alloyed bar through smelting and casting, and preparing pre-alloyed powder by using an inert gas atomization method, a plasma atomization method or a rotary electrode powder preparation method.
Further, the preparation of the Nb-containing aluminum alloy wire specifically comprises the following steps: the method comprises the steps of proportioning niobium and aluminum alloy according to a proportion, wherein the niobium accounts for 1-5 wt% of the aluminum alloy, preparing a pre-alloyed bar through smelting and casting, and preparing the pre-alloyed bar into a metal wire.
Further, the inert atmosphere is one of argon, nitrogen and helium.
Further, the additive manufacturing is one of selective laser melting, selective electron beam melting, and laser direct deposition.
Compared with the prior art, the invention has the following beneficial effects:
(1) by adding niobium or niobium-containing alloy particles into aluminum alloy by using mixed powder and laser additive manufacturing, a large amount of Al is successfully promoted3Nb or Al3The formation of (Nb, Ti) nano nucleation particles promotes the formation of a complete equiaxial crystal structure in the aluminum alloy, the crystal grains of the material are greatly refined, the cracks of the alloy are completely inhibited, and the additive manufacturing formability of the high-strength aluminum alloy is greatly improved. Compared with the conventional aluminum alloy added with elements such as Zr, Sc, Ti, Ni, Ta and the like, the aluminum alloy is formed into a complete equiaxed crystal structure by adding Nb or Nb-containing alloy particles, and a structure in which columnar crystals and equiaxed crystals are mixed is not formed in the aluminum alloy by adding the elements. The invention can select a wider Nb powder grain size (50nm-5 μm), most Nb grains can be melted under high laser power such as 400W, and compared with the method of simply using expensive nano-scale Nb powder grains (less than or equal to 200nm), the method can obviously reduce the manufacturing cost of the aluminum alloy by selecting Nb powder grains with coarse grain size or wide grain size. Preferably, the optional particle size isNb powder particles of 300nm to 5 μm. In addition, the invention can also select niobium-containing alloy powder (15-53 μm) with the grain diameter equivalent to that of the aluminum alloy powder, wherein niobium exists in the alloy powder as an alloy element, so that the melting point is reduced, the grain diameter of the powder can be larger, and the material cost is reduced. The method ensures that the crystal grains of the aluminum alloy are equiaxially and more thoroughly refined in the additive manufacturing process, and is beneficial to improving the material performance.
(2) By introducing a novel powder mixing method and a horizontal ball milling technology, fine Nb particles (50nm-5 microns) are uniformly and efficiently assembled on the surfaces of the aluminum alloy powder particles, the alloy powder particles are ensured to be nearly spherical and have good fluidity, the uniform dispersion distribution of the added particles is realized, and finally, all parts of the material are effectively nucleated in the additive manufacturing process to obtain an excellent component structure distribution state. Compared with the traditional mechanical ball milling method such as a planetary ball mill, the powder mixing method used in the invention has the advantages that the one-time powder mixing amount is larger (2-100 kg), the powder mixing efficiency is extremely high, different powders can be uniformly mixed in only 10 minutes at a high rotating speed (500rpm), the traditional method usually needs not less than two hours, even more than ten and twenty hours, the ball milling for a long time can seriously damage the spherical appearance of alloy powder particles, the good fluidity of the alloy powder particles is not favorably maintained, and the formability of additive manufacturing and the internal defects of prepared parts are deteriorated. Compared with the method that a few international research units adopt an electrostatic assembly method to assemble fine additive particles on the surfaces of alloy powder particles, the horizontal ball milling method adopted by the invention has higher efficiency, and can process/mix powder of several kilograms to dozens of kilograms at one time.
(3) Niobium-containing alloy powder having a particle size equivalent to that of aluminum alloy powder particles, such as Ti-22Al-25Nb (or Ti2AlNb), is mixed by using a three-dimensional oscillating powder mixing device, which allows the powder to be motion-mixed in different changing directions, and more easily achieves uniform powder mixing, compared to a conventional two-way linear oscillating mixing device, such as a V-type powder mixing device. In addition, the method does not need steel balls or ball milling, does not damage the sphericity of the powder, is favorable for the fluidity of the powder in the additive manufacturing process, and reduces the defects of holes in prepared samples and parts.
(4) The invention also provides a method for adding niobium into the aluminum alloy by utilizing a pre-alloying method, then utilizing an inert gas atomization method, a plasma atomization method or a rotating electrode to prepare powder, and finally performing additive manufacturing on an alloy sample.
Drawings
FIG. 1 is a schematic view of a horizontal ball mill used in the present invention;
fig. 2 is a distribution of 7075 aluminum alloy and nano niobium particles (3 wt%) after 10 minutes of mixing using a horizontal ball mill, the white particles being niobium particles; niobium particles are uniformly assembled on the surfaces of the alloy powder particles;
FIG. 3 is an optical micrograph of selected laser melted Al7075((a) and (c)) and Al7075-3 wt% Nb ((b) and (d)) samples;
FIG. 4 is a plot of the backscatter diffraction grain distribution ((a) and (b)) and polarization (c) for a selected region laser melted Al7075-3 wt% Nb sample;
FIG. 5 is a plot of Al in a selected area laser melted Al7075-3 wt% Nb sample3The Nb particles and the matrix have a plurality of crystallographic coherent orientation relations;
FIG. 6 is an optical micrograph of selected laser melted Al7075-3 wt% Ti2AlNb samples (a)400W-50 μ s, (b)400W-80 μ s, and backscatter diffraction grain distribution plot (c) and polarization plot (d);
FIG. 7 shows selective laser melting of Al7075-3 wt% of Al in Ti2AlNb samples3The Nb particles and the matrix have a plurality of crystallographic coherent orientation relations;
FIG. 8 is a tensile engineering stress-strain curve for a selected area laser melted Al7075-3 wt% Nb sample versus an Al7075-3 wt% Ti2AlNb sample.
Detailed Description
Example one
Using a horizontal ball mill shown in fig. 1, mixing 3 wt% of fine Nb particles having a particle size of 100nm to 5 μm and 7075 aluminum alloy powder particles having a particle size of 15 to 53 μm in an argon gas at a ball-to-powder ratio of 5: 1, the rotating speed is 500rpm, the mixing time is 10min, and the uniform dispersion distribution of the added particles is realized while the alloy powder particles are ensured to keep nearly spherical and have good fluidity. After ball milling for 10 minutes, the niobium nanoparticles have been uniformly assembled on the surface of the alloy powder particles, as shown in fig. 2.
And melting and sampling the powder by using selective laser melting equipment, wherein the sampling process conditions are that the laser power is 400W, the laser point exposure time is 50 mu s, and the powder layer thickness is 30 mu m. Because of the high melting point of niobium, a greater laser power is used to ensure that most of the niobium particles melt. As shown in FIG. 3, the addition of niobium particles makes the grain structure of the aluminum alloy after selective laser melting change from complete columnar crystal to complete fine isometric crystal, and the cracks of the alloy are also completely eliminated; in contrast, the selected zone laser melted Al7075 grain structure without Nb addition was coarse columnar grains with a large number of cracks growing in the sample preparation direction. In addition, as shown in fig. 4, the niobium-containing aluminum alloy also exhibited an extremely small texture. As shown in FIG. 5, the transmission electron micrograph and the diffraction spots show that nano Al exists in the crystal grains and in the grain boundaries3Nb particles, Al inside the grains3Nb has a multi-oriented lattice coherent relationship with the matrix, and Al3The lattice matching degree of the Nb particles and the matrix is high, so that the Nb particles serve as a powerful nucleation effect in the solidification process; al on grain boundaries3The Nb particles play a role in pinning the grain boundary and inhibiting the growth of grains; both of which promote the refinement of the aluminum alloy grains.
Example two
Using a horizontal ball mill shown in fig. 1, mixing 3 wt% of fine Nb particles having a particle size of 300nm to 5 μm and 7075 aluminum alloy powder particles having a particle size of 15 to 53 μm in an argon gas at a ball-to-powder ratio of 5: 1, the rotating speed is 500rpm, the mixing time is 10min, and the uniform dispersion distribution of the added particles is realized while the alloy powder particles are ensured to keep nearly spherical and have good fluidity. After ball milling for 10 minutes, the nano niobium particles are uniformly assembled on the surfaces of the alloy powder particles.
And melting and sampling the powder by using selective laser melting equipment, wherein the sampling process conditions are that the laser power is 400W, the laser point exposure time is 50 mu s, and the powder layer thickness is 30 mu m. The addition of the niobium particles enables the grain structure of the aluminum alloy after selective laser melting to be changed from complete columnar crystal into complete fine isometric crystal, and the cracks of the alloy are also completely eliminated.
EXAMPLE III
7075 aluminum alloy powder with the equivalent grain diameter of 15-53 mu m and 3 wt% of Ti-22Al-25Nb alloy powder with the grain diameter of 15-53 mu m are mixed in argon by a three-dimensional swing powder mixer, the rotating speed is 28rpm, and the mixing time is 6 hours.
And melting and sample preparation are carried out on the mixed powder by using selective laser melting equipment, wherein the sample preparation process conditions are that the laser power is 400W, the laser point exposure time is 50 mu s, and the powder layer thickness is 30 mu m. As shown in FIG. 6, the addition of Ti-22Al-25Nb to the aluminum alloy also formed a superfine fully equiaxed grain structure in the material after selective laser melting, which suppressed the formation of cracks and had a very small grain texture. As shown in FIG. 7, Al is also found in the interior of the crystal grains3Nb particles, which are well coherent with the matrix orientation, also contain a considerable concentration of Ti (as shown in Table 1) due to Al3Nb and Al3The lattice constants of Ti are very close, so these particles can be judged as Al3(Nb, Ti) particles. These particles play a powerful heterogeneous nucleation role in the solidification process, promoting grain refinement and equiaxial transformation. As shown in fig. 8, the suppression of cracks and the refinement of grains give the material a high yield strength and good plasticity.
TABLE 1 Al3(Nb, Ti) particle component
| Precipitated particles | Al | Ti | Nb | | Cu | Zn | |
| 1 | 77.12 | 13.63 | 7.80 | 0.39 | 0.79 | 0.27 | |
| 2 | 75.80 | 11.98 | 9.85 | 1.33 | 0.80 | 0.24 | |
| 3 | 73.39 | 13.69 | 11.46 | 0.37 | 0.23 | 0.86 |
Example four
7075 aluminum alloy powder with the equivalent grain diameter of 15-53 mu m and 3 wt% of Ti2AlNb alloy powder with the grain diameter of 15-53 mu m are mixed in argon by a three-dimensional swing powder mixer, the rotating speed is 28rpm, and the mixing time is 6 hours.
And melting and sample preparation are carried out on the mixed powder by using selective laser melting equipment, wherein the sample preparation process conditions are that the laser power is 400W, the laser point exposure time is 50 mu s, and the powder layer thickness is 30 mu m. The addition of the Ti2AlNb niobium alloy powder also enables the material after selective laser melting to form a superfine complete equiaxial crystal structure, inhibits the formation of cracks and has extremely small grain texture.
EXAMPLE five
The method comprises the steps of proportioning metal raw materials according to a proportion (niobium accounts for 1-5 wt% of aluminum alloy), smelting, casting to prepare a pre-alloyed bar, preparing pre-alloyed powder by an inert gas atomization method, a plasma atomization method or a rotary electrode powder preparation method, and melting the powder by selective laser melting or selective electron beam melting or laser direct deposition equipment to prepare a sample.
EXAMPLE six
The method comprises the steps of proportioning metal raw materials in proportion (niobium accounts for 1-5 wt% of aluminum alloy), smelting, casting to prepare a pre-alloyed bar, preparing the alloy bar into a metal wire, and melting the wire by using laser direct deposition equipment to prepare a sample.
The above embodiments are only used for illustrating the design idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention accordingly, and the protection scope of the present invention is not limited to the above embodiments. Therefore, all equivalent changes and modifications made in accordance with the principles and concepts disclosed herein are intended to be included within the scope of the present invention.
Claims (9)
1. A method for inhibiting the formation of cracks and promoting the grain refinement of an additive manufacturing aluminum alloy is characterized in that Nb-containing aluminum alloy powder or Nb-containing aluminum alloy wire is prepared; and melting and sampling the powder or wire material by using additive manufacturing.
2. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to claim 1, wherein the preparing Nb-containing aluminum alloy powder is specifically: mixing 1-5 wt% of fine Nb particles with the particle size of 50nm-5 mu m and 15-53 mu m of aluminum alloy powder in an inert atmosphere by using a horizontal ball mill, wherein the ball powder ratio is 5: 1, the rotation speed is 300-.
3. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to claim 2, wherein the horizontal ball mill brings the powder and the steel balls into air for contact collision using blade rotation on a central axis thereof.
4. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to claim 1, wherein the preparing Nb-containing aluminum alloy powder is specifically: 1-6 wt% of niobium-containing alloy powder with the particle size of 15-53 mu m and aluminum alloy powder with the particle size of 15-53 mu m are mixed by using a three-dimensional swing powder mixer in an inert atmosphere, the rotating speed is 20-40 rpm, and the mixing time is 3-24 hours.
5. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to any one of claims 2-4, wherein the inert atmosphere is one of argon, nitrogen, helium.
6. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to claim 1, wherein the preparing Nb-containing aluminum alloy powder is specifically: the preparation method comprises the steps of proportioning niobium and aluminum alloy according to a proportion, wherein the niobium accounts for 1-5 wt% of the aluminum alloy, preparing a pre-alloyed bar through smelting and casting, and preparing pre-alloyed powder by using an inert gas atomization method, a plasma atomization method or a rotary electrode powder preparation method.
7. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to any one of claims 2-6, wherein the additive manufacturing is one of selective laser melting, selective electron beam melting, laser direct deposition.
8. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy according to claim 1, wherein the preparing Nb-containing aluminum alloy wire is specifically: the method comprises the steps of proportioning niobium and aluminum alloy according to a proportion, wherein the niobium accounts for 1-5 wt% of the aluminum alloy, preparing a pre-alloyed bar through smelting and casting, and preparing the pre-alloyed bar into a metal wire.
9. The method of inhibiting crack formation and promoting grain refinement in an additive manufactured aluminum alloy of claim 8, wherein the additive manufacturing is laser direct deposition.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114769604A (en) * | 2022-04-22 | 2022-07-22 | 郑州磨料磨具磨削研究所有限公司 | Method for preparing alloy powder by adding superfine crystal seeds to carry out heterogeneous nucleation |
| CN116673472A (en) * | 2023-06-30 | 2023-09-01 | 创材深造(苏州)科技有限公司 | Composite aluminum alloy powder and large-scale preparation method and application thereof |
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