CN115635097A - High-entropy alloy composite material with stable cellular structure and preparation method thereof - Google Patents
High-entropy alloy composite material with stable cellular structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of metal materials, and particularly relates to a laser powder bed melting high-entropy alloy composite material with stable cell structure and a preparation method thereof. The laser powder bed melting high-entropy alloy composite material with the stable cell structure has the advantages that the yield strength, the tensile strength, the hardness and other properties of the laser powder bed melting high-entropy alloy composite material are improved besides the high-stability cell structure, the yield strength of the composite material is larger than or equal to 800 MPa, the tensile strength of the composite material is larger than or equal to 1000 MPa, and the hardness of the composite material is larger than or equal to 350 HV.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a high-entropy alloy composite material with a stable cell structure and a preparation method thereof, and more particularly relates to a laser powder bed melting high-entropy alloy composite material with a stable cell structure and a preparation method thereof.
Background
The high-entropy alloy (HEA) has excellent performances such as high strength, high hardness, high wear resistance, high corrosion resistance and the like, so that the high-entropy alloy has wide development space and use value; the high-entropy alloy also has unique performance characteristics, including four major effects, namely a high-entropy effect on thermodynamics, a lattice distortion effect on a structure, a delayed diffusion effect on kinetics and a cocktail effect on performance, and the performance characteristics provide a wider design idea for the microstructure and performance research of the high-entropy alloy. At present, the traditional process for preparing the high-entropy alloy block comprises an electric arc melting method, an induction melting method, a powder metallurgy method and the like. As a novel processing technology, the additive manufacturing technology can directly manufacture complex parts according to the three-dimensional data of parts, and the advantage attracts people's extensive attention. Meanwhile, the high-entropy alloy has higher heating speed and cooling speed, so that a finer-grained tissue structure is formed, the uniformity of the tissue is improved, and the effect of improving the comprehensive performance of the high-entropy alloy is achieved. The additive manufacturing technology for preparing the high-entropy alloy at the present stage mainly comprises laser powder bed melting (PBF-LB), laser Melting Deposition (LMD), electron beam selective melting (SEBM) and other technologies, wherein the laser powder bed melting technology is the most commonly used technology in additive manufacturing.
The laser powder bed melting technology is a high-energy transient metallurgical process, the melting, solidification and cooling of materials are completed in a very short time, and the large temperature gradient enables the crystal grains to have the characteristics of columnar and textured characteristics and non-uniform distribution of elements in the crystal grains. Meanwhile, the periodic expansion and contraction causes the generation of microscopic substructures, such as cellular dislocation structures, inside the grains. The special cellular dislocation structures have the characteristics that individual elements (or precipitated phases) are enriched at cell walls and high-density dislocations exist at the cell walls, and the special substructures have obvious influence on the mechanical properties and the corrosion behavior of the additive manufacturing metal. At present, the cellular structure of the laser powder bed melting high-entropy alloy FeCoCrNiMn diffuses and disappears along with the increase of the heat treatment temperature (for example, the cellular structure disappears when the heat treatment temperature is 1100 ℃), and is unstable under the high-temperature condition; and the thermal stability of the cellular structure is beneficial to improving the structural structure and performance stability of the additive manufacturing high-entropy alloy. Therefore, it is necessary to design a laser powder bed melting high-entropy alloy with stable cell structure to meet the practical requirements of production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention mainly aims to provide a laser powder bed melting high-entropy alloy composite material with a stable cell structure and a preparation method thereof.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
a laser powder bed melting high-entropy alloy composite material with a stable cell structure, wherein the cell structure still stably exists after being subjected to heat treatment at the temperature of more than or equal to 1100 ℃.
As a preferable scheme of the laser powder bed melting high-entropy alloy composite material with stable cellular structure, the laser powder bed melting high-entropy alloy composite material is characterized in that: the composite material comprises laser powder bed melting high-entropy alloy and carbide, wherein the mass fraction of the carbide is 2-6 wt.%.
As a preferable scheme of the laser powder bed melting high-entropy alloy composite material with stable cellular structure, the laser powder bed melting high-entropy alloy composite material is characterized in that: the high entropy alloy is a single phase solid solution.
As a preferable scheme of the laser powder bed melting high-entropy alloy composite material with the stable cellular structure, the laser powder bed melting high-entropy alloy composite material is characterized in that: the high-entropy alloy comprises at least four of Fe, co, cr, ni, mn and Cu, and the carbide comprises at least one of titanium carbide, niobium carbide and chromium carbide; preferably, the high-entropy alloy is FeCoCrNiMn, and the carbide is niobium carbide.
As a preferable scheme of the laser powder bed melting high-entropy alloy composite material with stable cellular structure, the laser powder bed melting high-entropy alloy composite material is characterized in that: the yield strength of the composite material is more than or equal to 800 MPa, the tensile strength is more than or equal to 1000 MPa, and the hardness is more than or equal to 350 HV. Preferably, the yield strength of the composite material is more than or equal to 850 MPa, the tensile strength is more than or equal to 1050 MPa, and the hardness is more than or equal to 370 HV.
In order to solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solutions:
a preparation method of a laser powder bed melting high-entropy alloy composite material with a stable cellular structure comprises the following steps:
s1, mixing laser powder bed melting high-entropy alloy powder with carbide powder to obtain composite material powder;
and S2, printing the composite material powder obtained in the step S1 by adopting a laser powder bed melting process to form a printed product.
As a preferable scheme of the preparation method of the laser powder bed melting high-entropy alloy composite material with the stable cellular structure, the method comprises the following steps: in the step S1, the ball-to-material ratio of a mixer is 1 to 2, the rotating speed is 150 to 200 r/min, and the mixing time is 5 to 8 hours during mixing.
As a preferable scheme of the preparation method of the laser powder bed melting high-entropy alloy composite material with the stable cellular structure, the method comprises the following steps: in the step S1, the particle size of the high-entropy alloy powder is 25 to 53 mu m; the carbide powder is nano powder, and the particle size of the carbide powder is 40-70 nm.
As a preferable scheme of the preparation method of the laser powder bed melting high-entropy alloy composite material with the stable cellular structure, the method comprises the following steps: in the step S2, the parameters of the laser powder bed melting process are as follows: the scanning power is 150 to 200W, the scanning distance is 0.07 to 0.10 mm, the scanning speed is 800 to 950 mm/s, and the powder layer thickness is 0.01 to 0.03 mm; the preheating temperature of the substrate is 70 to 90 ℃, and the rotation angle of the interlayer optical path is 67 degrees.
As a preferable scheme of the preparation method of the laser powder bed melting high-entropy alloy composite material with the stable cellular structure, the method comprises the following steps: in the step S2, the protective atmosphere in the process of the laser powder bed melting process is nitrogen.
The invention has the following beneficial effects:
the invention provides a laser powder bed melting high-entropy alloy composite material with stable cell structure and a preparation method thereof, wherein the laser powder bed melting alloy powder and carbide powder are uniformly mixed, the high-entropy alloy composite material with stable cell structure is prepared by a laser powder bed melting technology, and the cell structure of the prepared high-entropy alloy composite material still stably exists after heat treatment at the temperature of more than or equal to 1100 ℃. The laser powder bed melting high-entropy alloy composite material with the stable cell structure has the advantages that the yield strength, the tensile strength, the hardness and other properties of the laser powder bed melting high-entropy alloy composite material are improved besides the high-stability cell structure. The high-entropy alloy composite material realizes the performance of improving yield strength and the like, has thermal stability of the cell structure, realizes the rapid forming of the high-entropy alloy manufactured by additive manufacturing and the reasonable allocation of the cell structure elements and the structure, and provides a new solution for preparing the laser powder bed melting high-entropy alloy composite material with stable cell structure.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a transmission electron micrograph of a composite material according to example 1 of the present invention;
FIG. 2 is a graph showing the results of room temperature tensile tests of examples 1 to 3 of the present invention and comparative examples 1 to 2;
FIG. 3 is a graph showing hardness results of examples 1 to 3 of the present invention and comparative examples 1 to 2.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a laser powder bed melting high-entropy alloy composite material with a stable cell structure and a preparation method thereof, the prepared high-entropy alloy composite material realizes the performance of improving yield strength and the like, the cell structure has thermal stability, the rapid forming of high-entropy alloy manufactured by additive manufacturing and the reasonable allocation of cell structure elements and structures are realized, and a new solution is provided for preparing the laser powder bed melting high-entropy alloy composite material with the stable cell structure. The invention mixes the laser powder bed melting alloy powder and the carbide powder uniformly, and prepares the high-entropy alloy composite material with stable cell structure by the laser powder bed melting technology, and the cell structure of the prepared high-entropy alloy composite material still exists stably after the heat treatment at the temperature of more than or equal to 1100 ℃. The laser powder bed melting high-entropy alloy composite material with the stable cell structure has the advantages that the yield strength, the tensile strength, the hardness and other properties of the laser powder bed melting high-entropy alloy composite material are improved besides the high-stability cell structure.
According to one aspect of the invention, the invention provides the following technical scheme:
a laser powder bed melting high-entropy alloy composite material with stable cell structure, wherein the cell structure is still stable after being subjected to heat treatment at 1100 ℃ or more, for example, the cell structure is still stable at the heat treatment temperature of 1100 ℃, 1200 ℃ and the like.
Preferably, the composite material comprises laser powder bed melting high-entropy alloy and carbide, the mass fraction of the carbide is 2-6 wt.%, can ensure that the carbide is uniformly coated on the high-entropy alloy spherical powder, and particularly, the mass fraction of the carbide can be, for example and without limitation, any one of 2 wt.%, 2.5 wt.%, 3 wt.%, 3.5 wt.%, 4 wt.%, 4.5 wt.%, 5 wt.%, 5.5 wt, 6 wt.%, or a range between any two of the two;
further preferably, the high-entropy alloy is a single-phase solid solution, specifically, the high-entropy alloy comprises at least four of Fe, co, cr, ni, mn and Cu, and the carbide comprises at least one of titanium carbide, niobium carbide and chromium carbide. Further preferably, the high entropy alloy may be, for example, but not limited to, any one of fecoccrni, feCoCrMn, fecoccrcu, fecomnmn, feCoNiCu, fecomnmn, feCrNiCu, fecrmnccu, feNiMnCu, coCrNiMn, coCrNiCu, cocrmnccu, coNiMnCu, crnimnccu, feCoCrNiMn, fecocnicu, fecoccrmnccu, fecomncmncu, fecronimncu, fecrnimnnccu, coCrNiMnCu, feCoCrNiMnCu, and the carbide may be, for example, but not limited to, any one of titanium carbide, niobium carbide, chromium carbide, titanium carbide + niobium carbide, titanium carbide + chromium carbide, niobium carbide + chromium carbide.
The yield strength of the composite material is more than or equal to 800 MPa, the tensile strength is more than or equal to 1000 MPa, and the hardness is more than or equal to 350 HV. Preferably, the yield strength of the composite material is more than or equal to 850 MPa, the tensile strength is more than or equal to 1050 MPa, and the hardness is more than or equal to 370 HV.
The invention also provides a preparation method of the laser powder bed melting high-entropy alloy composite material with stable cellular structure, which comprises the following steps:
s1, mixing laser powder bed melting high-entropy alloy powder with carbide powder to obtain composite material powder;
and S2, printing the composite material powder obtained in the step S1 by adopting a laser powder bed melting process to form a printed product.
Preferably, in the step S1, the ball-to-material ratio of the mixer during mixing is 1 to 2, the rotation speed is 150 to 200 r/min, and the mixing time is 5 to 8 hours. Specifically, the ball-to-feed ratio can be, for example but not limited to, any one or a range between 1; the rotational speed may be, for example, but is not limited to, any one of 150 r/min, 160 r/min, 170 r/min, 180 r/min, 190 r/min, 200 r/min, or a range between any two thereof; the mixing time may be, for example, without limitation, any one or a range between any two of 5 h, 6 h, 7 h, 8 h; the particle size of the high-entropy alloy powder is 25 to 53 mu m; the carbide powder is nano powder, and the particle size of the carbide powder is 40 to 70 nm. Specifically, the particle size of the high entropy alloy powder may be, for example, but not limited to, a range between any two of 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 53 μm; the carbide powder may have a particle size in a range between, for example, but not limited to, any two of 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm.
In the step S2, the parameters of the laser powder bed melting process are as follows: the scanning power is 150 to 200W, the scanning distance is 0.07 to 0.10 mm, the scanning speed is 800 to 950 mm/s, and the powder layer thickness is 0.01 to 0.03 mm; the preheating temperature of the substrate is 70 to 90 ℃, and the rotation angle of an interlayer light path is 67 degrees. The protective atmosphere in the process of the laser powder bed melting process is nitrogen. Specifically, the scan power may be, for example, but not limited to, any one of 150W, 160W, 170W, 180W, 190W, 200W, or a range between any two; the scan pitch may be, for example, but is not limited to, any one of, or a range between, 0.07 mm, 0.08 mm, 0.09 mm, 0.10 mm; the scan speed may be, for example, but is not limited to, any one or a range between any two of 800 mm/s, 850 mm/s, 900 mm/s, 950 mm/s; the layer thickness may be, for example, but is not limited to, any one of or a range between any two of 0.01 mm, 0.015 mm, 0.02 mm, 0.025mm, 0.03 mm; the substrate preheat temperature may be, for example, without limitation, any one of 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, or a range between any two.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
A laser powder bed melting high-entropy alloy composite material with stable cellular structure comprises a laser powder bed melting high-entropy alloy FeCoCrNiMn and niobium carbide with the mass fraction of 5 wt%;
the preparation method of the composite material comprises the following steps:
s1, mixing the laser powder bed melting high-entropy alloy powder and niobium carbide powder according to the proportion, wherein the ball-material ratio of a mixer is 1:7, the rotating speed is 150 r/min, and the mixing time is 8 h; the high-entropy alloy powder is FeCoCrNiMn, and the particle size of the high-entropy alloy powder is 25 to 53 mu m; the grain diameter of the niobium carbide powder is 40 to 70 nm;
s2, printing the high-entropy alloy mixed powder obtained in the step S1 by adopting a laser powder bed melting process to form a printed product;
the scanning power of the laser powder bed melting process is 180W, the scanning interval is 0.08 mm, the scanning speed is 900 mm/s, the powder spreading layer thickness is 0.025mm, the substrate preheating temperature is 80 ℃, the interlayer light path rotation angle is 67 degrees, and the density of a printed sample is 99.6 percent.
FIG. 1 is a transmission electron micrograph of the composite material of example 1, wherein (a) and (d) in FIG. 1 are transmission electron micrographs of the composite material prepared in example 1, (b) and (e) in FIG. 1 are transmission electron micrographs of the composite material prepared in example 1 after heat treatment at 800 deg.C, and (c) and (f) in FIG. 1 are transmission electron micrographs of the composite material prepared in example 1 after heat treatment at 1100 deg.C.
Example 2
Example 2 differs from example 1 in the printing process:
the scanning speed of the laser powder bed melting process of example 2 was 800 mm/s, and the density of the prepared sample was 99.4%.
Example 3
Example 3 differs from example 1 in the carbide content:
example 3 niobium carbide powder was used at a mass fraction of 3 wt%.
Comparative example 1
Comparative example 1 differs from example 1 in that no carbides are included.
Comparative example 2
Comparative example 2 differs from example 1 in that it includes 1 wt% niobium carbide powder.
Fig. 1 is a transmission electron microscope image of the composite material of example 1, the composite material of example 1 after being subjected to a heat treatment at 800 ℃, and the composite material of example 1 after being subjected to a heat treatment at 1100 ℃, which can be seen from fig. 1 that the cellular structure of the composite material of the present invention still stably exists after being subjected to a heat treatment at 800 ℃ and 1100 ℃, and elements segregated on the cell wall still exist, and the cellular structure of the composite material of the present invention has thermal stability, so that rapid forming of the high-entropy alloy manufactured by additive manufacturing and reasonable blending of the cellular structure elements and the structure are realized.
FIG. 2 shows the room temperature tensile test results of examples 1-3 and comparative examples 1-2 of the present invention, and it can be seen from FIG. 2 that the yield strength of the laser powder bed melting high-entropy alloy composite material after adding a certain amount of carbide is significantly improved compared with that of the laser powder bed melting high-entropy alloy FeCoCrNiMn, and the yield strength of the composite material with the added carbide not in the content range of the present invention is better than that of the laser powder bed melting high-entropy alloy FeCoCrNiMn but lower than that of the laser powder bed melting high-entropy alloy composite material of the present invention.
FIG. 3 shows hardness results of examples 1-3 and comparative examples 1-2 of the present invention, and it can be seen from FIG. 3 that the hardness increase and yield strength change are similar, the hardness of the laser powder bed melting high-entropy alloy composite material of the present invention added with a certain amount of carbide is significantly increased compared with the hardness of the laser powder bed melting high-entropy alloy FeCoCrNiMn, and the hardness of the composite material added with carbide out of the content range of the present invention is better than that of the laser powder bed melting high-entropy alloy FeCoCrNiMn but lower than that of the laser powder bed melting high-entropy alloy composite material of the present invention.
In conclusion, the invention can realize the preparation of the laser powder bed melting high-entropy alloy composite material with stable cell structure, improve the thermal stability of the cell structure, realize the improvement of mechanical properties such as yield strength, and achieve better mechanical properties and the laser powder bed melting high-entropy alloy composite material with stable cell structure.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. The laser powder bed melting high-entropy alloy composite material with the stable cell structure is characterized in that the cell structure still exists stably after being subjected to heat treatment at the temperature of more than or equal to 1100 ℃.
2. The composite material as claimed in claim 1, wherein the composite material comprises a laser powder bed melting high entropy alloy and a carbide, and the mass fraction of the carbide is 2 to 6 wt.%.
3. The composite material according to claim 2, wherein the high entropy alloy is a single phase solid solution.
4. A composite material according to claim 3, wherein the high entropy alloy comprises at least four of Fe, co, cr, ni, mn, cu, and the carbides comprise at least one of titanium carbide, niobium carbide, chromium carbide.
5. The composite material according to any one of claims 1 to 4, wherein the composite material has a yield strength of 800 MPa or more, a tensile strength of 1000 MPa or more, and a hardness of 350 HV or more.
6. A method for preparing a composite material according to any one of claims 1 to 5, comprising the steps of:
s1, mixing laser powder bed melting high-entropy alloy powder with carbide powder to obtain composite material powder;
and S2, printing the composite material powder obtained in the step S1 by adopting a laser powder bed melting process to form a printed product.
7. The preparation method according to claim 6, wherein in the step S1, the ball-to-feed ratio of a mixer during mixing is 1-2, the rotation speed is 150-200 r/min, and the mixing time is 5-8 h.
8. The preparation method according to claim 6, wherein in the step S1, the particle size of the high-entropy alloy powder is 25 to 53 μm; the carbide powder is nano powder, and the particle size of the carbide powder is 40-70 nm.
9. The method according to claim 6, wherein in the step S2, the parameters of the laser powder bed melting process are: the scanning power is 150 to 200W, the scanning distance is 0.07 to 0.10 mm, the scanning speed is 800 to 950 mm/s, and the powder layer thickness is 0.01 to 0.03 mm; the preheating temperature of the substrate is 70 to 90 ℃, and the rotation angle of the interlayer optical path is 67 degrees.
10. The method according to claim 6, wherein in step S2, the process protective atmosphere of the laser powder bed melting process is nitrogen.
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| CN116144962A (en) * | 2023-04-17 | 2023-05-23 | 北京科技大学 | High-strength and high-toughness hastelloy and preparation process thereof |
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