CN113210629A - AlCoCrFeNi2.1Eutectic high-entropy alloy and laser selective material increase manufacturing method thereof - Google Patents
AlCoCrFeNi2.1Eutectic high-entropy alloy and laser selective material increase manufacturing method thereof Download PDFInfo
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B33Y80/00—Products made by additive manufacturing
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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Abstract
The invention provides AlCoCrFeNi2.1Eutectic high-entropy alloy and selective laser material increase manufacturing method thereofThe preparation method specifically discloses AlCoCrFeNi laser selective additive manufacturing2.1The optimal process parameters of the eutectic high-entropy alloy comprise: laser power, scanning speed, single-channel spacing and powder layer spreading thickness, and the AlCoCrFeNi prepared by the method is composed of FCC and BCC two-phase structures2.1Eutectic high entropy alloy. The invention AlCoCrFeNi2.1The eutectic high-entropy alloy has high density and fine crystal grains and better tensile mechanical property compared with casting. The preparation scheme realizes the preparation of the high-density eutectic high-entropy alloy with fine microstructure by utilizing the high cooling speed of the selective rapid material increase manufacturing, and the preparation technology has the advantages of high preparation efficiency, good quality of the obtained alloy, high automation degree and the like.
Description
Technical Field
The invention relates to a laser forming technology of a metal material, in particular to AlCoCrFeNi2.1Eutectic high-entropy alloy and a laser selective material increase manufacturing method thereof.
Background
The high-entropy alloy is a novel alloy which breaks through the traditional alloy design concept and consists of a plurality of main elements, and has attracted the attention of researchers in recent years. The high-entropy alloy is composed of a plurality of elements in equal atomic proportion or near equal atomic proportion, so that the high-entropy alloy has thermodynamic high-entropy and lattice distortion effects, kinetic delayed diffusion and a 'cocktail' effect, and the special effect enables the high-entropy alloy to have a series of unique properties. The high-entropy alloy with the FCC structure has good plasticity but low strength, and the high-entropy alloy with the BCC structure has high strength but poor plasticity, which limits the practical application of the alloy. AlCoCrFeNi2.1The eutectic high-entropy alloy consists of FCC and BCC two phases, and the combination of the FCC and the BCC phases ensures that AlCoCrFeNi2.1The eutectic high-entropy alloy has good comprehensive mechanical property, and the relatively low melting point and narrow eutectic solidification interval of the eutectic structure are beneficial to reduction of alloy defects and easy forming, and based on the characteristics, the AlCoCrFeNi alloy has good comprehensive mechanical property2.1The eutectic high-entropy alloy has excellent application prospect and commercial value.
At present, a casting method is mainly used for preparing the high-entropy alloy, because the high-entropy alloy consists of a plurality of principal elements, the phenomena of uneven components, element segregation and the like occur in the preparation process, and the defects of poor filling capability, single preparation style, large loss, complex post-processing steps and the like of a sample prepared by the casting method greatly limit the development and application of the high-entropy alloy.
The selective laser material-increasing manufacturing technology is a novel highly intelligent manufacturing technology which is based on a layered manufacturing principle, takes high-energy laser as a heat source, takes metal powder as a raw material, and can be used for accumulating and forming on a substrate layer by layer to directly manufacture a digital model into a solid part. In view of the above, the selective laser additive manufacturing technology provides a new method for preparing a high-entropy alloy component with a complex and compact shape, a uniform and fine microstructure and excellent performance.
Disclosure of Invention
The invention aims to provide AlCoCrFeNi aiming at the problems2.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy realizes the preparation of the eutectic high-entropy alloy with high compactness and fine microstructure by utilizing the high cooling speed of selective material increase manufacturing, and has the advantages of high efficiency, good quality of the obtained alloy and high automation degree.
In order to achieve the purpose, the invention adopts the technical scheme that: AlCoCrFeNi2.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy comprises the following steps:
S1、AlCoCrFeNi2.1weighing raw materials Al, Co, Cr, Fe and Ni according to the proportion of the eutectic high-entropy alloy; the purity of each raw material is more than or equal to 99.9 percent;
s2, mixing the raw materials in the step S1 and carrying out alloying treatment;
s3, preparing the sample alloyed in the step S2 into AlCoCrFeNi2.1Prealloying the powder;
s4, putting the prealloy powder in the step S3 into a drying box, heating to 120-150 ℃ in a vacuum environment for drying treatment for 3-5 hours, cooling along with the box, and adding the powder into a powder feeding cylinder of the material increase manufacturing equipment in the selective laser area;
s5, cleaning the surface of the 304 stainless steel forming substrate to be deposited, then mounting the substrate on a forming platform and leveling the substrate;
s6, starting the laser selective additive manufacturing equipment and setting a laser selective additive manufacturing scanning path and process parameters;
s7, adding AlCoCrFeNi according to the set laser selective area additive manufacturing scanning path and process parameters under the protection of inert gas2.1The prealloying powder is melted and formed on a 304 stainless steel forming substrate layer by layer to prepare a block AlCoCrFeNi2.1High entropy alloy.
Further, the alloying treatment method in step S2 is casting.
Further, AlCoCrFeNi is prepared in step S32.1The prealloying method is an atomization powder preparation method, and the AlCoCrFeNi prepared by the prealloying method2.1The prealloyed powder is a spherical structure.
Further, the AlCoCrFeNi2.1The grain size distribution of the prealloyed powder is between 10-45 μm, and the average grain size is 23.86 μm.
Further, the cleaning of the surface to be deposited of the shaped substrate in step S5 includes the following steps: the substrate was previously sandblasted on the upper surface by a sandblasting machine and washed with acetone to remove surface impurities, and then washed with alcohol and dried.
Further, the setting of the laser selective area additive manufacturing process parameters in step S6 includes: laser power is 130W-160W; the scanning speed is 800-1000 mm/s; the single-channel spacing is 0.1 mm; the thickness of the powder spreading layer is 0.2-0.4 mm.
Further, the inert gas described in step S7 is high-purity argon gas.
The invention also discloses AlCoCrFeNi2.1The eutectic high-entropy alloy is prepared by the method and has the advantages of high strength and good plasticity. The invention of AlTiCrFeNi2.1Compared with the alloy prepared by casting, the eutectic high-entropy alloy has the advantages of high density, fine crystal grains and better tensile mechanical property.
The invention AlCoCrFeNi2.1The principle of the laser selective material increase manufacturing method of the eutectic high-entropy alloy is as follows:
firstly, alloying the related alloy raw materials according to a certain proportion, preparing pre-alloyed powder from the alloyed sample by an atomization powder preparation method, and then carrying out water removal and oxygen removal treatment on the pre-alloyed powder; and finally, accumulating and forming a required high-entropy alloy sample on the surface of the cleaned 304 stainless steel substrate to be deposited by using selective laser melting deposition equipment under the protection of high-purity argon according to a reasonable planned path and process parameters, and feeding back and regulating the laser process parameters according to the microstructure and mechanical property characterization of the prepared high-entropy alloy.
The invention AlCoCrFeNi2.1Compared with the prior art, the eutectic high-entropy alloy and the laser selective material increase manufacturing method thereof have the following advantages:
according to the advantages of high automation degree, good controllability, high heating and cooling speeds, high material utilization rate, uniform, compact and fine structure formation, obvious reduction of micro defects, short process flow and the like of the selective laser melting deposition method, the eutectic high-entropy alloy component with high density and better performance than casting is prepared. The selective laser melting deposition method can change parameters such as laser power, scanning speed, scanning path and the like according to different requirements, and can prepare high-entropy alloy materials with complex shapes, high quality and excellent performance. The sample of the invention can be produced in a customized way and has high commercial value.
In conclusion, the invention provides a method for preparing the eutectic high-entropy alloy with high compactness and excellent mechanical property by using the laser selective additive manufacturing method, the method can be used for preparing the eutectic high-entropy alloy component with a complex shape and a fine microstructure in a short time, the method is high in forming speed, high in raw material utilization rate and high in working efficiency, and the alloy quality is improved.
Drawings
FIG. 1 is a schematic structural diagram of a selective laser additive manufacturing apparatus;
fig. 2 is a schematic diagram of a scanning strategy for selective laser additive manufacturing, in which (a) the scanning directions of adjacent layers are adjusted to change a certain angle, and (b) the same layer of a strip-shaped scanning strategy;
FIG. 3 shows AlCoCrFeNi2.1SEM scanning and particle size distribution diagram of the high-entropy alloy metal powder, wherein (a) is the SEM scanning diagram, and (b) is the particle size distribution diagram;
FIG. 4 shows AlCoCrFeNi2.1A high-entropy alloy laser selective additive manufacturing molding sample drawing;
FIG. 5 shows AlCoCrFeNi2.1X-ray diffraction patterns of the high-entropy alloy;
FIG. 6 shows AlCoCrFeNi2.1A secondary electron scanning image of a microstructure of the high-entropy alloy, wherein (a) is additive forming, and (b) is an as-cast state;
FIG. 7 shows AlCoCrFeNi2.1DSC curve of SLM sample of high entropy alloy;
FIG. 8 shows AlCoCrFeNi2.1Tensile stress-strain curves for high entropy alloys.
Detailed Description
The invention aims to prepare AlCoCrFeNi with high compactness and excellent performance2.1The eutectic high-entropy alloy provides a laser selective additive manufacturing method. The invention discloses a laser selective additive manufacturing process parameter range, which comprises the following steps: laser power, scanning speed, powder laying layer thickness and single-channel spacing, and summarizes the influence of melting and depositing process parameters of additive manufacturing in a laser selection area on the performance such as density, forming capability and the like of the prepared alloy, and then finds out the most appropriate additive manufacturing process parameters in the laser selection area according to the summarized rule, so as to successfully prepare AlCoCrFeNi with fine microstructure, high density and excellent mechanical property2.1Eutectic high entropy alloy.
The laser selective additive manufacturing equipment adopted by the invention is shown in figure 1 and mainly comprises a computer control system 1, a laser 2, a laser transmission system, a sample forming table, a powder feeding system and a purification system. The laser and the laser transmission system provide and transmit energy, the environment in the cavity is adjusted by utilizing the purification system, the water oxygen content is kept to be less than 40ppm, the powder is paved on the forming table through the powder feeding system, a computer control system controls a series of parameters such as a scanning path, laser power and the like, and the block sample is formed on the forming table layer by layer to obtain the block sample. The laser selective additive manufacturing equipment further comprises a scanning mirror 3, an F-theta mirror 4, shielding gas 5, a purifier 6, a forming cavity 7, a powder conveying cavity 8, a substrate 9 and a powder paving roller.
The present invention is further illustrated by the following examples and accompanying figures, in which the specific examples described herein include, but are not limited to, the following examples.
Example 1
This example provides an AlCoCrFeNi2.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy comprises the following specific steps:
(1) preparation and treatment of prealloyed powder
Mixing Al, Co, Cr, Fe and Ni 5 elements according to a certain proportion, alloying (wherein the purity of Al, Co, Cr, Fe and Ni is more than or equal to 99.9%), and atomizing the alloyed sample to prepare AlCoCrFeNi2.1The pre-alloyed powder prepared from the eutectic high-entropy alloy is of a typical spherical structure, the particle size is 10-45 mu m, and the average particle size is 23.86 mu m, as shown in figure 3. And putting the powder into a drying box, heating to the temperature of 120-150 ℃ in a vacuum environment, carrying out drying treatment for 3-5 hours, cooling along with the box, and adding the powder into a powder feeding cylinder of selective laser melting equipment.
(2) Pretreatment of shaped substrate material
The material of the forming substrate is 304 stainless steel, sand blasting is carried out on the upper surface of the forming substrate by a sand blasting machine in advance, the forming substrate is cleaned by acetone to remove surface impurities, then the forming substrate is cleaned by alcohol and dried by blowing, and finally the forming substrate is arranged on a forming platform and leveled.
(3) AlCoCrFeNi prepared by selective laser additive manufacturing2.1Eutectic high-entropy alloy
Turning on the laser melting deposition equipment, setting a scanning path as shown in fig. 2, and setting process parameters such as laser power, scanning speed, powder layer spreading thickness, single-channel spacing and the like, wherein the process parameter ranges are shown in table 1.1. AlCoCrFeNi is carried out in a closed chamber under the protection of high-purity argon2.1In a selective melting and deposition experiment of the high-entropy alloy powder, the optimal process parameters (power of 130W, scanning degree of 1000mm/s, single-channel spacing of 0.1mm and powder layer spreading thickness of 0.04mm) are determined through an orthogonal experiment. The laser selective additive manufacturing molded sample is shown in fig. 4.
(4) Laser selective additive manufacturing type sample performance test
X-ray diffractionAs can be seen from the analysis of the shots, the laser selective additive manufacturing method and the AlCoCrFeNi2.1 eutectic high-entropy alloy prepared by casting both consist of FCC and B2 phases, as shown in FIG. 5. From the secondary electron scanning image, the AlCoCrFeNi prepared by melting deposition in the specific laser selective area of casting2.1The microstructure of the eutectic high-entropy alloy is finer, as shown in fig. 6. From the DSC thermogram (FIG. 7), it can be seen that only one endothermic peak and one exothermic peak appear on the curve during the temperature rising and lowering processes, which indicates that the AlCoCrFeNi prepared by the laser selective additive manufacturing method2.1The high-entropy alloy is a eutectic structure. From the tensile stress-strain curve in fig. 8, it can be seen that the AlCoCrFeNi2.1 eutectic high-entropy alloy prepared by the laser selective additive manufacturing method has higher tensile plasticity and tensile strength than the AlCoCrFeNi prepared by casting2.1The eutectic high-entropy alloy is prepared by the method that the cooling speed of the material increase manufacturing of the laser selective area is high, the microstructure of the prepared sample is fine, the density of the prepared sample is high, and the comprehensive tensile mechanical property of the alloy is improved.
TABLE 1.1 Experimental Process parameters
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. AlCoCrFeNi2.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy is characterized by comprising the following steps of:
S1、AlCoCrFeNi2.1weighing raw materials Al, Al and Al in proportion for eutectic high-entropy alloy,Co, Cr, Fe and Ni; the purity of each raw material is more than or equal to 99.9 percent;
s2, mixing the raw materials in the step S1 and carrying out alloying treatment;
s3, preparing the sample alloyed in the step S2 into AlCoCrFeNi2.1Prealloying the powder;
s4, putting the prealloy powder in the step S3 into a drying box, heating to 120-150 ℃ in a vacuum environment for drying treatment for 3-5 hours, cooling along with the box, and adding the powder into a powder feeding cylinder of the material increase manufacturing equipment in the selective laser area;
s5, cleaning the surface of the 304 stainless steel forming substrate to be deposited, then mounting the substrate on a forming platform and leveling the substrate;
s6, starting the laser selective additive manufacturing equipment, and setting a laser selective additive manufacturing scanning path and process parameters;
s7, adding AlCoCrFeNi according to the set laser selective area additive manufacturing scanning path and process parameters under the protection of inert gas2.1The prealloying powder is melted and formed on a 304 stainless steel forming substrate layer by layer to prepare a block AlCoCrFeNi2.1High entropy alloy.
2. The AlCoCrFeNi of claim 12.1The laser selective additive manufacturing method of the eutectic high-entropy alloy is characterized in that in the step S2, the alloying treatment method is casting.
3. The AlCoCrFeNi of claim 12.1The laser selective material additive manufacturing method of the eutectic high-entropy alloy is characterized in that AlCoCrFeNi is prepared in step S32.1The prealloying method is an atomization powder preparation method, and the AlCoCrFeNi prepared by the prealloying method2.1The prealloyed powder is a spherical structure.
4. The AlCoCrFeNi of claim 12.1The laser selective material additive manufacturing method of the eutectic high-entropy alloy is characterized in that the AlCoCrFeNi alloy is prepared by adopting a laser selective material additive method2.1The grain size distribution of the prealloyed powder is between 10-45 μm, and the average grain size is 23.86 μm.
5. The AlCoCrFeNi of claim 12.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy is characterized in that the cleaning of the surface to be deposited of the forming substrate in the step S5 comprises the following steps: the substrate was previously sandblasted on the upper surface by a sandblasting machine and washed with acetone to remove surface impurities, and then washed with alcohol and dried.
6. The AlCoCrFeNi of claim 12.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy is characterized in that the step S6 of setting laser selective material increase manufacturing process parameters comprises the following steps: laser power is 130W-160W; the scanning speed is 800-1000 mm/s; the single-channel spacing is 0.1 mm; the thickness of the powder spreading layer is 0.2-0.4 mm.
7. The AlCoCrFeNi of claim 12.1The laser selective material increase manufacturing method of the eutectic high-entropy alloy is characterized in that the inert gas in the step S7 is high-purity argon.
8. AlCoCrFeNi2.1A eutectic high entropy alloy, characterized in that it is prepared by a method according to any one of claims 1 to 7.
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| CN114807719A (en) * | 2022-05-27 | 2022-07-29 | 北京理工大学 | Laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement |
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| CN115141967A (en) * | 2022-06-13 | 2022-10-04 | 哈尔滨工业大学（深圳） | High-entropy alloy composite material and preparation method and application thereof |
| CN115401214A (en) * | 2022-09-14 | 2022-11-29 | 南昌航空大学 | High-entropy alloy laser additive manufacturing method with normal temperature and high temperature corrosion resistance |
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