CN112222413B - Cold rolling composite laser additive manufacturing process method of gradient structure high-entropy alloy - Google Patents
Cold rolling composite laser additive manufacturing process method of gradient structure high-entropy alloy Download PDFInfo
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- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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Abstract
The invention provides a cold-rolling composite laser additive manufacturing process method of a high-entropy alloy with a gradient structure, which comprises the following steps of: firstly, preparing a high-entropy alloy ingot by adopting a vacuum induction melting process under the atmosphere of high-purity argon according to the set chemical components of the high-entropy alloy, carrying out homogenization annealing, hot forging and cold rolling on the ingot, finally adopting a selective laser melting technology, selecting pre-alloyed high-entropy alloy powder as a raw material, and directly carrying out laser additive manufacturing on a rolled plate blank. Because the high-entropy alloy has a delayed diffusion effect and the grain size of the high-entropy alloy in a deposition state is in a micron order, namely the grain size of the cold-rolled sheet is relatively fine, and the grain size of the additive sheet is relatively coarse, a gradient structure is finally formed. The high-entropy alloy with the gradient structure prepared by the invention has excellent strength and plasticity due to the strong back stress strengthening effect generated by geometrical necessary dislocation and the strong work hardening capacity of the coarse crystal layer.
Description
Technical Field
The invention belongs to the technical field of metal material additive manufacturing, and particularly relates to a cold-rolling composite laser additive manufacturing process method of a high-entropy alloy with a gradient structure.
Background
The additive manufacturing technology has the characteristics of short flow, high material utilization rate and the like, is applied to the fields of aerospace, automobile part manufacturing, biomedicine and the like at present, and has a wide application prospect in the preparation of complex components. However, the additive manufacturing technology has a bottleneck problem of insufficient mechanical property of the deposited metal. That is, the mechanical properties of the laser additive manufacturing high-entropy alloy are relatively poor compared with the high-entropy alloy after plastic deformation and heat treatment.
For this reason, many patent applicants propose a rolling-based composite additive manufacturing technique, a shot-peening-based composite additive manufacturing technique, a laser-assisted composite additive manufacturing technique, and the like for improving the mechanical properties of the as-deposited metal. The patent with application number 201810528056.2 provides a device and a method for rolling a laser three-dimensional forming part layer by layer, namely, the deposited metal is subjected to cold rolling or hot rolling layer by layer, crystal grains are refined by using the rolling force of a roller, and dislocation is increased, so that the mechanical property of the laser three-dimensional forming part is improved; the patent with application number 201911146571.5 proposes a composite manufacturing device and method of arc additive and laser-assisted thermoplastic forming, which utilizes laser to heat the surface of a deposition layer, and then applies plastic deformation to the material through a roller or an impact tool head, thereby refining crystal grains, improving microstructure and improving comprehensive mechanical properties of parts.
However, the deformation amount of plastic deformation such as deposition interlayer rolling is small, and the deposition interlayer cold rolling reduces the plasticity of the material and aggravates the crack tendency, so the existing composite additive manufacturing technology can convert dendrites into equiaxed crystals, namely improve the anisotropy of the material, but the improvement range of the mechanical property of the metal material is limited. Therefore, a process method capable of remarkably improving the mechanical property of the laser additive manufacturing high-entropy alloy is urgently needed to be proposed.
Disclosure of Invention
The invention provides a cold-rolling composite laser additive manufacturing process method of a high-entropy alloy with a gradient structure based on the principle that the strength of a metal material is improved by cold rolling and the strength and plasticity of the traditional metal material cannot be combined by changing the gradient structure, thereby improving the strength and plasticity of the high-entropy alloy manufactured by laser additive manufacturing.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a cold rolling composite laser additive manufacturing process method of a gradient structure high-entropy alloy is carried out according to the following steps:
(1) preparing a high-entropy alloy ingot by adopting a vacuum induction melting process under a high-purity argon atmosphere according to the set chemical components of the high-entropy alloy;
(2) carrying out homogenization annealing heat treatment on the high-entropy alloy cast ingot, wherein the homogenization annealing heat preservation temperature is 1000-1250 ℃, and the homogenization annealing heat preservation time is 8-30 h;
(3) hot forging the high-entropy alloy cast ingot subjected to the homogenizing annealing heat treatment into a plate blank, wherein the forging temperature is 1080-1140 ℃;
(4) rolling the plate blank at room temperature, wherein the pass reduction is 0.3-3 mm, and the total reduction rate is more than or equal to 82%;
(5) the selective laser melting technology is adopted, pre-alloyed high-entropy alloy powder is selected as a raw material, laser additive manufacturing is directly carried out on a rolled plate blank, the diameter of a light spot is 50-100 mu m, the thickness of the layer is 40-90 mu m, the laser power is 170-325W, the scanning speed is 750-2000 mm/s, the lap joint rate is 15-50%, and argon is used as protective gas.
Preferably, the smelting in the step (1) needs to be repeated for 4-7 times.
Preferably, a water cooling mode is adopted after the homogenization annealing and heat preservation in the step (2).
Preferably, the heating temperature of the high-entropy alloy cast ingot in the step (3) before hot forging is 1200 +/-20 ℃, and the heat preservation time is 2 hours.
Preferably, the thickness of the high-entropy alloy after cold rolling in the step (4) is 2-5 mm, and the high-entropy alloy after cold rolling is subjected to surface mechanical grinding treatment.
Preferably, the powder particle size of the high-entropy alloy powder in the step (5) is 15-53 μm, and the high-entropy alloy powder is prepared by adopting a gas atomization forming mode.
The invention also provides the gradient structure high-entropy alloy prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention obtains the high-entropy alloy with submicron or nanometer grain size through multi-pass cold rolling deformation. And the high-entropy alloy after cold rolling is used as a substrate for laser additive manufacturing, namely, the laser additive manufacturing is directly carried out on the cold-rolled high-entropy alloy plate. Because the high-entropy alloy has a delayed diffusion effect and the grain size of the high-entropy alloy in a deposition state is in a micron order, namely the grain size of the cold-rolled sheet is relatively fine, and the grain size of the additive sheet is relatively coarse, a gradient structure is finally formed.
(2) The existing rolling composite additive manufacturing process needs a specific device, namely, a roller which moves simultaneously with a welding gun is used for rolling and deforming an arc deposition layer, but the invention can be realized by using the existing cold rolling mill and additive manufacturing equipment, so that the equipment investment is reduced.
(3) The high-entropy alloy with the gradient structure prepared by the invention has excellent strength and plasticity due to the strong back stress strengthening effect generated by geometrical necessary dislocation and the strong work hardening capacity of the coarse crystal layer.
Drawings
FIG. 1 is a schematic diagram of a laser additive manufacturing process performed directly on a cold rolled sheet according to the present invention;
FIG. 2 is a schematic diagram of the grain size distribution of the gradient structure high-entropy alloy prepared by the present invention.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
The gradient structure high-entropy alloy is subjected to a room temperature tensile test on an INSTRON 3369 type universal material testing machine according to GB/T228-.
The specific embodiment of the cold-rolling composite laser additive manufacturing process method of the gradient structure high-entropy alloy according to the invention is as follows:
example 1
(1) In a high-purity argon atmosphere, a CoCrFeMnNi high-entropy alloy ingot is prepared by adopting a vacuum induction melting process and repeatedly melted for 5 times, and the CoCrFeMnNi high-entropy alloy ingot comprises the chemical components of, by weight, 21.22% of Co, 18.34% of Cr, 19.70% of Fe, 19.32% of Mn, 20.94% of Ni and the balance of Si, Al, S, P and the like.
(2) And carrying out homogenization annealing heat treatment on the cast ingot, wherein the homogenization annealing heat preservation temperature is 1200 ℃, the homogenization annealing heat preservation time is 20h, and a water cooling mode is adopted after the homogenization annealing heat preservation.
(3) And (3) carrying out homogenization annealing heat treatment on the cast ingot, then carrying out heat preservation at 1180 ℃ for 2 hours, and carrying out hot forging at 1090-1120 ℃ to obtain a plate blank.
(4) And rolling the plate blank at room temperature, wherein the pass reduction is 0.5-2 mm, the total reduction rate is 93.3%, the thickness of the high-entropy alloy after cold rolling is 2mm, and mechanically grinding the surface of the high-entropy alloy.
(5) By adopting a selective laser melting technology, CoCrFeMnNi high-entropy alloy powder (gas atomization forming) with the powder particle size of 15-53 mu m is selected, as shown in figure 1, laser additive manufacturing is directly carried out on a cold-rolled plate blank 1, the spot diameter of a laser beam 2 is required to be 70 mu m, the layer thickness is 80 mu m, the laser power is 170W, the scanning rate is 750mm/s, the lap joint rate is 20%, and the protective gas is argon.
The grain size distribution of the gradient structure high-entropy alloy of the embodiment is schematically shown in FIG. 2, namely, the grain size gradually transits from submicron or nanometer to micron from cold-rolled sheet to additive sheet. The tensile strength of the gradient structure CoCrFeMnNi high-entropy alloy is 1085MPa, and the elongation after fracture is 31.2%.
Example 2
(1) In a high-purity argon atmosphere, a CoCrFeMnNi high-entropy alloy cast ingot is prepared by adopting a vacuum induction melting process and repeatedly melted for 4 times, and the chemical components of the alloy ingot comprise, by weight, 20.90% of Co, 18.61% of Cr, 20.03% of Fe, 19.29% of Mn, 20.61% of Ni and the balance of Si, Al, S, P and the like.
(2) And carrying out homogenization annealing heat treatment on the cast ingot, wherein the homogenization annealing heat preservation temperature is 1250 ℃, the homogenization annealing heat preservation time is 15h, and a water cooling mode is adopted after homogenization annealing heat preservation.
(3) And (3) carrying out homogenization annealing heat treatment on the cast ingot, then preserving heat for 2h at 1200 ℃, and carrying out hot forging at 1080-1100 ℃ to obtain a plate blank.
(4) And rolling the plate blank at room temperature, wherein the pass reduction is 0.5-2.5 mm, the total reduction rate is 82.8%, the thickness of the high-entropy alloy after cold rolling is 5mm, and mechanically grinding the surface of the high-entropy alloy.
(5) By adopting a selective laser melting technology, CoCrFeMnNi high-entropy alloy powder (gas atomization forming) with the powder particle size of 15-53 mu m is selected, and laser additive manufacturing is directly carried out on a cold-rolled plate blank, wherein the spot diameter is 50 mu m, the layer thickness is 40 mu m, the laser power is 230W, the scanning speed is 1100mm/s, the lap joint rate is 30%, and the protective gas is argon.
The grain size of the gradient structure high-entropy alloy of the embodiment is gradually transited from submicron or nanometer to micron from a cold-rolled sheet to a reinforced sheet. The tensile strength of the gradient structure CoCrFeMnNi high-entropy alloy is 1012MPa, and the elongation after fracture is 36.3%.
Example 3
(1) In a high-purity argon atmosphere, a CoCrFeMnNi high-entropy alloy ingot is prepared by adopting a vacuum induction melting process and repeatedly melted for 5 times, and the CoCrFeMnNi high-entropy alloy ingot comprises the chemical components of, by weight, 21.08% of Co, 18.70% of Cr, 19.89% of Fe, 19.41% of Mn, 20.58% of Ni and the balance of Si, Al, S, P and the like.
(2) And carrying out homogenization annealing heat treatment on the cast ingot, wherein the homogenization annealing heat preservation temperature is 1200 ℃, the homogenization annealing heat preservation time is 24h, and a water cooling mode is adopted after the homogenization annealing heat preservation.
(3) And (3) carrying out homogenization annealing heat treatment on the cast ingot, then carrying out heat preservation for 2h at 1210 ℃, and carrying out hot forging at 1100-1140 ℃ to obtain a plate blank.
(4) And rolling the plate blank at room temperature, wherein the pass reduction is 0.3-2 mm, the total reduction rate is 90.0%, the thickness of the high-entropy alloy after cold rolling is 3mm, and mechanically grinding the surface of the high-entropy alloy.
(5) By adopting a selective laser melting technology, CoCrFeMnNi high-entropy alloy powder (gas atomization forming) with the powder particle size of 15-53 mu m is selected, and laser additive manufacturing is directly carried out on a cold-rolled plate blank, wherein the spot diameter is 80 mu m, the layer thickness is 50 mu m, the laser power is 325W, the scanning speed is 2000mm/s, the lap joint rate is 50%, and the protective gas is argon.
The grain size of the gradient structure high-entropy alloy of the embodiment is gradually transited from submicron or nanometer to micron from a cold-rolled sheet to a reinforced sheet. The tensile strength of the gradient structure CoCrFeMnNi high-entropy alloy is 878MPa, and the elongation after fracture is 38.4%.
Example 4
(1) In a high-purity argon atmosphere, a CoCrFeMnNi high-entropy alloy cast ingot is prepared by adopting a vacuum induction melting process and repeatedly melted for 7 times, and the chemical components of the alloy ingot comprise, by weight, 21.11% of Co, 18.49% of Cr, 19.63% of Fe, 19.68% of Mn, 20.71% of Ni and the balance of Si, Al, S, P and the like.
(2) And carrying out homogenization annealing heat treatment on the cast ingot, wherein the homogenization annealing heat preservation temperature is 1150 ℃, the homogenization annealing heat preservation time is 30h, and a water cooling mode is adopted after homogenization annealing heat preservation.
(3) And (3) carrying out homogenization annealing heat treatment on the cast ingot, then carrying out heat preservation for 2h at 1220 ℃, and carrying out hot forging at 1080-1120 ℃ to obtain a plate blank.
(4) And rolling the plate blank at room temperature, wherein the pass reduction is 0.5-3 mm, the total reduction rate is 86.7%, the thickness of the high-entropy alloy after cold rolling is 4mm, and mechanically grinding the surface of the high-entropy alloy.
(5) By adopting a selective laser melting technology, CoCrFeMnNi high-entropy alloy powder (gas atomization forming) with the powder particle size of 15-53 mu m is selected, and laser additive manufacturing is directly carried out on a cold-rolled plate blank, wherein the spot diameter is 100 mu m, the layer thickness is 90 mu m, the laser power is 250W, the scanning speed is 1500mm/s, the lap joint rate is 15%, and the protective gas is argon.
The grain size of the gradient structure high-entropy alloy of the embodiment is gradually transited from submicron or nanometer to micron from a cold-rolled sheet to a reinforced sheet. The tensile strength of the gradient structure CoCrFeMnNi high-entropy alloy is 994MPa, and the elongation after fracture is 35.9%.
Example 5
(1) In a high-purity argon atmosphere, a vacuum induction melting process is adopted to prepare a CoCuFeMnNi high-entropy alloy ingot, and the CoCuFeMnNi high-entropy alloy ingot is repeatedly melted for 5 times, wherein the chemical components comprise, by weight, 19.96% of Co, 21.65% of Cu, 19.32% of Fe, 18.63% of Mn, 19.98% of Ni, and the balance of Si, Al, S, P and the like.
(2) And carrying out homogenizing annealing heat treatment on the cast ingot, wherein the homogenizing annealing heat preservation temperature is 1000 ℃, the homogenizing annealing heat preservation time is 8h, and a water cooling mode is adopted after homogenizing annealing heat preservation.
(3) And (3) carrying out homogenization annealing heat treatment on the cast ingot, then carrying out heat preservation at 1180 ℃ for 2 hours, and carrying out hot forging at 1080-1100 ℃ to obtain a plate blank.
(4) And rolling the plate blank at room temperature, wherein the pass reduction is 0.5-1.5 mm, the total reduction rate is 90.0%, the thickness of the high-entropy alloy after cold rolling is 3mm, and mechanically grinding the surface of the high-entropy alloy.
(5) By adopting a selective laser melting technology, CoCuFeMnNi high-entropy alloy powder (gas atomization forming) with the powder particle size of 15-53 mu m is selected, and laser additive manufacturing is directly carried out on a cold-rolled plate blank, wherein the spot diameter is 70 mu m, the layer thickness is 50 mu m, the laser power is 200W, the scanning speed is 1500mm/s, the lap joint rate is 20%, and the protective gas is argon.
The grain size of the gradient structure high-entropy alloy of the embodiment is gradually transited from submicron or nanometer to micron from a cold-rolled sheet to a reinforced sheet. The tensile strength of the gradient structure CoCuFeMnNi high-entropy alloy is 709MPa, and the elongation after fracture is 40.7%.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (7)
1. A cold rolling composite laser additive manufacturing process method of a gradient structure high-entropy alloy is characterized by comprising the following steps:
(1) preparing a high-entropy alloy ingot by adopting a vacuum induction melting process under a high-purity argon atmosphere according to the set chemical components of the high-entropy alloy;
(2) carrying out homogenization annealing heat treatment on the high-entropy alloy cast ingot, wherein the homogenization annealing heat preservation temperature is 1000-1250 ℃, and the homogenization annealing heat preservation time is 8-30 h;
(3) hot forging the high-entropy alloy cast ingot subjected to the homogenizing annealing heat treatment into a plate blank, wherein the forging temperature is 1080-1140 ℃;
(4) rolling the plate blank at room temperature, wherein the pass reduction is 0.3-3 mm, and the total reduction rate is more than or equal to 82%;
(5) the selective laser melting technology is adopted, pre-alloyed high-entropy alloy powder is selected as a raw material, laser additive manufacturing is directly carried out on a rolled plate blank, the diameter of a light spot is 50-100 mu m, the thickness of the layer is 40-90 mu m, the laser power is 170-325W, the scanning speed is 750-2000 mm/s, the lap joint rate is 15-50%, and argon is used as protective gas.
2. The cold-rolling composite laser additive manufacturing process method of the gradient structure high-entropy alloy is characterized in that in the step (1), the melting is repeatedly carried out for 4-7 times.
3. The cold-rolling composite laser additive manufacturing process method of the gradient structure high-entropy alloy according to claim 1, wherein a water-cooling mode is adopted after the homogenization annealing and heat preservation in the step (2).
4. The cold-rolling composite laser additive manufacturing process method of the gradient-structure high-entropy alloy is characterized in that in the step (3), the heating temperature of the high-entropy alloy ingot before hot forging is 1200 +/-20 ℃, and the heat preservation time is 2 hours.
5. The cold-rolling composite laser additive manufacturing process method of the gradient structure high-entropy alloy is characterized in that the thickness of the cold-rolled high-entropy alloy in the step (4) is 2-5 mm, and the surface of the cold-rolled high-entropy alloy is subjected to mechanical grinding treatment.
6. The cold-rolling composite laser additive manufacturing process method of the gradient-structure high-entropy alloy is characterized in that in the step (5), the powder particle size of the high-entropy alloy powder is 15-53 μm, and the high-entropy alloy powder is prepared in a gas atomization forming mode.
7. The gradient structure high-entropy alloy prepared by the method of any one of claims 1 to 6.
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| CN113427021A (en) * | 2021-06-28 | 2021-09-24 | 哈尔滨工业大学 | Cryogenic treatment method for additive manufacturing high-entropy alloy |
| CN113881885B (en) * | 2021-09-05 | 2022-07-01 | 安徽中科春谷激光产业技术研究院有限公司 | Selective laser melting particle reinforced high-entropy alloy material and preparation method thereof |
| CN113957366B (en) * | 2021-10-21 | 2022-07-22 | 温州大学 | Laser surface heat treatment method of high-entropy alloy with reverse gradient nano structure |
| CN114226750B (en) * | 2021-11-22 | 2024-02-23 | 南京联空智能增材研究院有限公司 | Shell-structure-imitated alloy laser additive manufacturing method |
| CN115229207A (en) * | 2022-07-26 | 2022-10-25 | 北京科技大学 | Preparation method for manufacturing CoCrFeMnNi hydrogen embrittlement-resistant high-entropy alloy by additive manufacturing and high-entropy alloy |
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| CN111118496A (en) * | 2020-01-19 | 2020-05-08 | 中国人民解放军陆军装甲兵学院 | Tough high-entropy alloy forming structure and preparation method thereof |
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Application publication date: 20210115 Assignee: ZHEJIANG WUMA REDUCER Co.,Ltd. Assignor: Wenzhou University Contract record no.: X2023330000100 Denomination of invention: A Cold Rolled Composite Laser Additive Manufacturing Process for Gradient Structure High Entropy Alloy Granted publication date: 20220531 License type: Common License Record date: 20230311 |
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