CN112157261A - Preparation method and application of high-entropy alloy part with laser melting deposition reaction structure - Google Patents
Preparation method and application of high-entropy alloy part with laser melting deposition reaction structure Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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Abstract
The invention relates to the technical field of high-entropy alloy, and provides a preparation method of a high-entropy alloy part with a laser melting deposition reaction structure, which comprises the following steps: s1, mixing or alloying the metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 90 percent according to a certain proportion; s2, screening the powder after mixing or alloying treatment, and drying the screened powder in a vacuum drying oven; s3, setting laser melting deposition process parameters and a laser scanning path; and S4, starting a laser melting and depositing system, melting and depositing the powder on the forming substrate layer by layer, and preparing the high-entropy alloy component with the reaction structure. According to the method provided by the embodiment of the invention, different laser scanning paths are set as required, so that high-entropy alloy components with different shapes of reaction structures can be prepared; according to the specific metal simple substance proportion and the laser melting deposition process parameters, the reaction structure high-entropy alloy component with uniform structure, stable structure and excellent performance can be prepared.
Description
Technical Field
The invention relates to the technical field of high-entropy alloy, in particular to a preparation method and application of a high-entropy alloy part with a laser melting deposition reaction structure.
Background
High entropy alloys are alloys formed from five or more equal or approximately equal amounts of metals. The high-entropy alloy has four main effects different from the traditional alloy, namely a high-entropy effect, a lattice distortion effect, a delayed diffusion effect and a 'cocktail' effect, so that the high-entropy alloy has a plurality of unique properties. At present, the high-entropy alloy has proved excellent properties including low-layer fault energy, thermal stability, radiation resistance, corrosion resistance and easy overcoming of the 'trade-off' effect on the properties, and the like, and has excellent application prospect and commercial value based on the excellent properties.
However, the preparation and forming of the high-entropy alloy are difficult due to the multi-principal-element characteristics of the high-entropy alloy, and for example, the existing mainstream method for preparing the high-entropy alloy is a 'fusion casting' method, so that the existing components are not uniform in the preparation process, even the element segregation phenomenon is generated, and the mechanical property of the high-entropy alloy is poor; and the method has the defects of single preparation style, weak mold filling capability, complex post-processing steps, large loss and the like, and greatly limits the application and development of the high-entropy alloy as a structural and functional material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method and application of a high-entropy alloy part with a laser melting deposition reaction structure, so as to prepare a high-performance high-entropy alloy with the reaction structure.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the high-entropy alloy part with the laser melting deposition reaction structure comprises the following steps:
s1, mixing or alloying the metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 90 percent according to a certain proportion; wherein, the mixture ratio of the five metal simple substances is as follows: al: 15 at.% to 20 at.%; co: 15 at.% to 20 at.%; cr: 15 at.% to 20 at.%; fe: 15 at.% to 20 at.%; ni: 20 at.% to 40 at.%;
s2, screening the powder subjected to mixing or alloying treatment in the step S1 through a metal powder screen, then putting the screened powder into a vacuum drying box, heating to 100-150 ℃ in a vacuum environment, preserving heat for 1-3 hours, and cooling along with the box for later use;
s3, cleaning the surface to be deposited of the forming substrate; setting laser melting deposition process parameters and a laser scanning path in a laser melting deposition system; wherein, the laser melting deposition process parameters are as follows: the laser power is 400-1200W; the scanning speed is 200-800 mm/min; the powder feeding speed is 0.8 to 1.5 rad/min; the flow rate of inert powder feeding gas is 20-35L/min; the flow rate of the inert protective gas is 2-10L/min; the lifting amount is 0.1-1 mm; the lapping rate is 10% -90%;
s4, under the protection of inert gas, putting the powder dried in the step S2 into a powder feeder of a laser melting deposition system; and then starting a laser melting deposition system, and melting and depositing powder on a forming substrate layer by layer under the protection of inert gas according to set laser melting deposition process parameters and a scanning path to prepare the reaction structure high-entropy alloy component.
Further, in step S1, the mixture ratio of the five metal simple substances is: al: 15 at.% to 17 at.%; co: 15 at.% to 17 at.%; cr: 15 at.% to 17 at.%; fe: 15 at.% to 17 at.%; ni: 34 at.% to 40 at.%.
Further, in step S3, the laser melting deposition process parameters are: the laser power is 700-800W; the scanning speed is 400-450 mm/min; the powder feeding speed is 1-1.2 rad/min; the flow rate of inert powder feeding gas is 28-30L/min; the flow rate of the inert protective gas is 5-10L/min; the lifting amount is 0.2-0.25 mm; the lapping rate is 40-60%.
Further, in step S1, the mixing method of the five simple metals is as follows: mechanically stirring and mixing for 1-5 h or ball-milling and mixing for 5-30 h.
Further, in step S1, the alloying treatment method of the five simple metals includes: inert gas atomization powder preparation method, rotating electrode method, rotating disc electron beam melting method, rotating electrode plasma melting method or rotating electrode electron beam melting method.
Further, in step S2, the particle size of the powder dried in the vacuum drying oven is 50 to 150 μm.
Further, in step S2, the particle size of the powder dried in the vacuum drying oven is 55 to 120 μm.
Further, the forming substrate is a stainless steel plate or a zirconium alloy plate.
Further, the method is adopted to prepare AlCoCrFeNi2.1Application of reaction structure high-entropy alloy
The invention has the beneficial effects that: according to the preparation method of the high-entropy alloy component with the laser melting deposition reaction structure, different laser scanning paths are set according to requirements, and the high-entropy alloy components with different shapes can be prepared; according to the specific metal simple substance proportion and the laser melting deposition process parameters, the reaction structure high-entropy alloy part with uniform structure, stable structure and excellent performance can be prepared; the AlCoCrFeNi prepared by the method of the embodiment of the invention2.1The reaction structure high-entropy alloy part has excellent energy release characteristic and armor penetration performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be 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 described in the present invention, and that other drawings can be obtained from these drawings by a person skilled in the art without inventive effort.
FIGS. 1A and 1B are laser scanning path planning diagrams for preparing a high-entropy alloy block component in an embodiment of the invention;
FIGS. 2A to 2D are laser scanning path planning diagrams for preparing a high-entropy alloy cylindrical component in an embodiment of the invention;
FIG. 3 is a physical representation of a high entropy alloy block member produced in example 1 of the present invention;
FIG. 4 is a physical diagram of a cylindrical member of a high-entropy alloy produced in example 1 of the present invention;
FIG. 5 is a physical representation of a high entropy alloy bulk part produced in example 3 of this invention;
FIG. 6 is a physical diagram of a high-entropy alloy block member produced in a comparative example;
FIG. 7 is an X-ray diffraction pattern of the high entropy alloy components of examples 1-3 and comparative example;
FIG. 8 is a differential scanning calorimetry plot of the reaction structure high entropy alloy component of example 1 and the comparative example;
FIG. 9 is a scanning electron mirror backscattered electron image of a high entropy alloy part of examples 1-3 and comparative example;
FIG. 10 is a tensile stress-strain curve for the high entropy alloy components of examples 1-3 and comparative examples;
11A-11C are high-speed photographic images of the detonation process after the high-entropy alloy component of example 2 was prepared into a fragment.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following further description is provided in conjunction with the accompanying drawings and examples. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. The embodiments and features of the embodiments of the invention may be combined with each other without conflict.
The preparation method of the high-entropy alloy part with the laser melting deposition reaction structure comprises the following steps:
s1, mixing or alloying the metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 90 percent according to a certain proportion; wherein, the mixture ratio of the five metal simple substances is as follows: al: 15 at.% to 20 at.%; co: 15 at.% to 20 at.%; cr: 15 at.% to 20 at.%; fe: 15 at.% to 20 at.%; ni: 20 at.% to 40 at.%;
s2, screening the powder subjected to mixing or alloying treatment in the step S1 through a metal powder screen, then putting the screened powder into a vacuum drying box, heating to 100-150 ℃ in a vacuum environment, preserving heat for 1-3 hours, and cooling along with the box for later use;
s3, cleaning the surface to be deposited of the forming substrate; setting laser melting deposition process parameters and a laser scanning path in a laser melting deposition system; wherein, the laser melting deposition process parameters are as follows: the laser power is 400-1200W; the scanning speed is 200-800 mm/min; the powder feeding speed is 0.8 to 1.5 rad/min; the flow rate of inert powder feeding gas is 20-35L/min; the flow rate of the inert protective gas is 2-10L/min; the lifting amount is 0.1-1 mm; the lapping rate is 10% -90%;
s4, under the protection of inert gas, putting the powder dried in the step S2 into a powder feeder of a laser melting deposition system; and then starting a laser melting deposition system, and melting and depositing powder on a forming substrate layer by layer under the protection of inert gas according to set laser melting deposition process parameters and a scanning path to prepare the reaction structure high-entropy alloy component.
In step S1, metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 90% are selected as raw materials, and then the five metal simple substances are mixed or alloyed according to a certain proportion to prepare mechanical mixed powder or pre-alloyed powder with the particle size range of approximately 40-180 mu m.
For example, the mixture ratio of the five metal simple substances is as follows: al: 15 at.% to 20 at.%; co: 15 at.% to 20 at.%; cr: 15 at.% to 20 at.%; fe: 15 at.% to 20 at.%; ni: 20 at.% to 40 at.%.
In a preferred embodiment, the mixture ratio of the five simple metals is as follows: al: 15 at.% to 17 at.%; co: 15 at.% to 17 at.%; cr: 15 at.% to 17 at.%; fe: 15 at.% to 17 at.%; ni: 34 at.% to 40 at.%.
The mixing method of the five metal simple substances comprises the following steps: mechanically stirring and mixing for 1-5 h or ball-milling and mixing for 5-30 h. The alloying treatment method of the five metal simple substances comprises the following steps: the method of powder preparation by inert gas atomization, the method of rotating electrode, the method of rotating disk electron beam melting, the method of rotating electrode plasma melting or the method of rotating electrode electron beam melting, although other methods of alloying treatment may be used, and is not specifically limited herein.
In step S2, the powder mixed or alloyed in step S1 is sieved with a metal powder sieve for the purpose of removing powder having a particle size not satisfying the requirement. And after the screening is finished, putting the screened powder into a vacuum drying box, heating to 100-150 ℃ in a vacuum environment, preserving heat for 1-3 h, and cooling along with the box for later use. For example, the particle size of the powder dried in a vacuum drying oven is 50 to 150. mu.m. By drying the sieved powder, the moisture in the powder can be removed and the oxygen content in the metal powder can be reduced. In a preferred embodiment, the particle size of the powder dried in the vacuum drying oven is 55 to 120 μm.
In the embodiment of the present invention, the powder after the mixing or alloying treatment in step S1 may be sieved by using metal powder sieves having 360 mesh, 340 mesh, 320 mesh, 300 mesh, 280 mesh, 260 mesh, 240 mesh, 220 mesh, 200 mesh, 180 mesh, 160 mesh, 140 mesh, 120 mesh, 100 mesh, 80 mesh, and the like.
In step S3, the surface to be deposited of the shaped substrate is cleaned. The forming substrate is a stainless steel plate or a zirconium alloy plate, and the surface to be deposited of the forming substrate refers to the surface for depositing the high-entropy alloy component of the reaction structure.
The cleaning of the surface to be deposited of the shaped substrate comprises the following steps carried out in sequence: s3.1, carrying out machining treatment or polishing treatment by adopting an angle grinder on the surface to be deposited of the forming substrate; s3.2, soaking the formed substrate into acetone for at least 5 minutes; s3.3, placing the formed substrate into absolute ethyl alcohol for ultrasonic cleaning; s3.4, repeating the step S3.1 to the step S3.3 at least once.
And after the surface to be deposited of the forming substrate is cleaned, drying the forming substrate, putting the dried forming substrate into a forming chamber protected by inert gas, and fixing the forming substrate on a workbench of a laser melting deposition system for later use. In the embodiment of the present invention, the inert gas is argon, but may be other inert gases, and is not limited specifically herein.
In step S3, laser melting deposition process parameters are set in the laser melting deposition system, and a laser scanning path is set according to the structure of the reaction-structure high-entropy alloy member. The laser melting deposition system is a common device in powder injection molding technologies such as laser 3D printing and spraying, and has the characteristics of good forming, high bonding strength, high automation degree, customizable operation and the like. In the embodiment of the present invention, a laser melting and depositing system developed by Nanjing Zhongkoyu laser technology company Limited is used, and of course, a laser melting and depositing system developed by another company may be used, which is not specifically limited herein.
The laser melting deposition process parameters in the embodiment of the invention are as follows: the laser power is 400-1200W; the scanning speed is 200-800 mm/min; the powder feeding speed is 0.8 to 1.5 rad/min; the flow rate of inert powder feeding gas is 20-35L/min; the flow rate of the inert protective gas is 2-10L/min; the lifting amount is 0.1-1 mm; the lapping rate is 10-90%.
As a preferred embodiment, the laser melting deposition process parameters are as follows: the laser power is 700-800W; the scanning speed is 400-450 mm/min; the powder feeding speed is 1-1.2 rad/min; the flow rate of inert powder feeding gas is 28-30L/min; the flow rate of the inert protective gas is 5-10L/min; the lifting amount is 0.2-0.25 mm; the lapping rate is 40-60%.
In step S4, the powder dried in step S2 is first put into a powder feeder of a laser melting deposition system under the protection of inert gas, so as to avoid the change of dryness and oxygen content of the powder caused by the contact with air; and then, under the protection of inert gas, melting and depositing the powder on a forming substrate layer by layer through a laser melting and depositing system, and further preparing the high-entropy alloy part with the reaction structure.
According to the preparation method of the high-entropy alloy component with the laser melting deposition reaction structure, different laser scanning paths are set according to requirements, and the high-entropy alloy components with different shapes can be prepared; according to the specific metal simple substance proportion and the laser melting deposition process parameters, the reaction structure high-entropy alloy part with uniform structure, stable structure and excellent performance can be prepared.
Example 1:
AlCoCrFeNi2.1the preparation method of the reaction structure high-entropy alloy block-shaped component comprises the following steps:
s1, carrying out inert gas atomization powder preparation on metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 99.5% according to a certain proportion; wherein, the mixture ratio of the five metal simple substances is as follows: al: 16.39 at.%; co: 16.39 at.%; cr: 16.39 at.%; fe: 16.39 at.%; ni: 34.44 at.%;
s2, sieving the powder subjected to alloying treatment in the step S1 through a 280-mesh and 100-mesh metal powder sieve, collecting the powder with the particle size of 50-150 mu m, putting the powder into a vacuum drying box, heating the powder to 100 ℃ in a vacuum environment, preserving the heat for 1 hour, and cooling the powder along with the box for later use;
s3, selecting a 316L stainless steel plate as a forming substrate, cleaning the surface to be deposited of the forming substrate, and fixing the forming substrate on a workbench of a laser melting deposition system for later use under the protection of argon gas;
setting the technological parameters of laser melting deposition in a laser melting deposition system: the laser power is 800W; the scanning speed is 400 mm/min; the powder feeding speed is 1.2 rad/min; the flow rate of inert powder feeding gas is 28L/min; the flow rate of the inert protective gas is 5L/min; the lifting amount is 0.25 mm; the lapping rate is 50 percent;
setting a laser scanning path in the laser melting deposition system; for example, the odd layers follow the path shown in FIG. 1A, and the even layers follow the path shown in FIG. 1B;
s4, under the protection of argon, putting the powder dried in the step S2 into a powder feeder of a laser melting deposition system; and then starting a laser melting deposition system, and melting and depositing powder on a forming substrate layer by layer under the protection of argon according to set laser melting deposition process parameters and a scanning path to prepare the massive component of the high-entropy alloy with the reaction structure.
FIG. 3 shows AlCoCrFeNi in example 12.1A physical diagram of the high-entropy alloy block-shaped component of the reaction structure.
Example 2:
AlCoCrFeNi2.1the preparation method of the high-entropy alloy cylindrical component with the reaction structure comprises the following steps:
s1, carrying out inert gas atomization powder preparation on metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 99.8% according to a certain proportion; wherein, the mixture ratio of the five metal simple substances is as follows: al: 16.5 at.%; co: 16.5 at.%; cr: 16.5 at.%; fe: 16.5 at.%; ni: 34 at.%;
s2, sieving the powder subjected to alloying treatment in the step S1 through a 260-mesh and 120-mesh metal powder sieve, collecting the powder with the particle size of 55-120 mu m, putting the powder into a vacuum drying box, heating the powder to 120 ℃ in a vacuum environment, preserving the heat for 2 hours, and cooling the powder along with the box for later use;
s3, selecting a 316L stainless steel plate as a forming substrate, cleaning the surface to be deposited of the forming substrate, and fixing the forming substrate on a workbench of a laser melting deposition system for later use under the protection of argon gas;
setting the technological parameters of laser melting deposition in a laser melting deposition system: the laser power is 700W; the scanning speed is 450 mm/min; the powder feeding speed is 1.0 rad/min; the flow rate of inert powder feeding gas is 30L/min; the flow rate of the inert protective gas is 5L/min; the lifting amount is 0.2 mm; the lapping rate is 50 percent;
setting a laser scanning path in the laser melting deposition system; for example, a first layer follows the path shown in FIG. 2A, a second layer follows the path shown in FIG. 2B, a third layer follows the path shown in FIG. 2C, and a fourth layer follows the path shown in FIG. 2D; and then circularly and sequentially superposed according to the paths in fig. 2A to 2D.
S4, under the protection of argon, putting the powder dried in the step S2 into a powder feeder of a laser melting deposition system; and then starting a laser melting deposition system, and melting and depositing powder on a forming substrate layer by layer under the protection of argon according to set laser melting deposition process parameters and a scanning path to prepare the cylindrical part of the high-entropy alloy with the reaction structure.
FIG. 4 shows AlCoCrFeNi in example 22.1A physical diagram of a high-entropy alloy cylindrical part with a reaction structure.
Example 3:
the preparation method of the reaction structure high-entropy alloy block-shaped component comprises the following steps:
s1, carrying out inert gas atomization powder preparation on metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 99.8% according to a certain proportion; wherein, the mixture ratio of the five metal simple substances is as follows: al: 15.4 at.%; co: 15.4 at.%; cr: 15.4 at.%; fe: 15.4 at.%; ni: 38.4 at.%;
s2, sieving the powder subjected to alloying treatment in the step S1 through a 260-mesh and 120-mesh metal powder sieve, collecting the powder with the particle size of 50-150 mu m, putting the powder into a vacuum drying box, heating the powder to 120 ℃ in a vacuum environment, preserving the heat for 2 hours, and cooling the powder along with the box for later use;
s3, selecting a 316L stainless steel plate as a forming substrate, cleaning the surface to be deposited of the forming substrate, and then placing the forming substrate on a workbench of a laser melting deposition system for standby application under the protection of argon gas;
setting the technological parameters of laser melting deposition in a laser melting deposition system: the laser power is 800W; the scanning speed is 400 mm/min; the powder feeding speed is 1.2 rad/min; the flow rate of inert powder feeding gas is 30L/min; the flow rate of inert protective gas is 10L/min; the lifting amount is 0.2 mm; the lapping rate is 50 percent;
setting a laser scanning path in the laser melting deposition system, wherein in particular, odd layers follow the path shown in FIG. 1A, and even layers follow the path shown in FIG. 1B;
s4, under the protection of argon, putting the powder dried in the step S2 into a powder feeder of a laser melting deposition system; and then starting a laser melting deposition system, and melting and depositing powder on a forming substrate layer by layer under the protection of argon according to set laser melting deposition process parameters and a scanning path to prepare the massive component of the high-entropy alloy with the reaction structure.
Fig. 5 shows a physical diagram of the reaction structure high-entropy alloy block member produced in example 3.
Comparative example:
preparing the high-entropy alloy block by using metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 99.5 percent according to a certain proportion by adopting the existing casting method. Wherein, the mixture ratio of the five metal simple substances is as follows: al: 16.4 at.%; co: 16.4 at.%; cr: 16.4 at.%; fe: 16.4 at.%; ni: 34.4 at.%. Fig. 6 shows a physical diagram of the high-entropy alloy block member produced in the comparative example.
FIG. 7 shows X-ray diffraction patterns of high-entropy alloy members of examples 1 to 3 and comparative example. Wherein curve A in FIG. 7 is the X-ray diffraction pattern of the part of example 1; FIG. 7 is an X-ray diffraction pattern of the part of example 2 along curve B; FIG. 7 is an X-ray diffraction pattern of the part of example 3 along curve C; the curve D in fig. 7 is the X-ray diffraction pattern of the part in the comparative example.
As can be seen from FIG. 7, the reaction structure high entropy alloy members in examples 1 to 3 are each composed of a face centered cubic structure (FCC) and a body centered cubic structure (BCC).
FIG. 8 shows differential scanning method spectra of high entropy alloy components in example 1 and comparative example.
As can be seen from fig. 8, the part of example 1 has one endothermic peak and one exothermic peak, indicating that the part of example 1 is a bidirectional eutectic high entropy alloy.
Fig. 9 shows the scanning-mirror backscattered electron images of the components of examples 1-3 and comparative example. Wherein, a in FIG. 9 illustrates a scanning electron mirror backscattered electron image of the component in embodiment 1; figure 9 b illustrates the scanning electron mirror backscattered electron image of the component of example 2; figure 9 c illustrates the scanning electron mirror backscattered electron image of the components of example 3; figure 9 d shows the scanning-mirror backscattered electron image of the component of the comparative example.
As can be seen from fig. 9, the microstructure of the reaction structure high entropy alloy member in examples 1 to 3 is a lamellar heterostructure formed of an FCC phase and a BCC phase.
Tensile specimens were produced using the parts of examples 1 to 3 and comparative example, and were subjected to tensile tests in accordance with the requirements of GB/T228.1-2010 metallic Material tensile test method.
Fig. 10 shows the tensile stress strain curves of tensile specimens produced using the components of examples 1-3 and comparative example. Wherein, curve a in fig. 10 is a tensile stress strain curve of the tensile specimen in example 1; curve B in fig. 10 is the tensile stress strain curve of the tensile specimen in example 2; the C-curve in fig. 10 is the tensile stress strain curve of the tensile specimen in example 3; the D-curve in fig. 10 is a tensile stress strain curve of the tensile specimen in the comparative example.
The mechanical property test results of the high-entropy alloy parts of examples 1 to 3 and comparative example are shown in the following table:
in summary, by performing X-ray diffraction analysis, differential scanning calorimeter analysis, scanning electron microscope analysis and tensile test on the high-entropy alloy components prepared in examples 1 to 3 and comparative examples, the reaction structure high-entropy alloy components prepared by the method of the present invention are two-phase eutectic high-entropy alloys composed of a face-centered cubic structure (FCC) and a body-centered cubic structure (BCC), and the microstructure thereof is a lamellar eutectic structure formed by the FCC phase and the BCC phase, and the microstructure is stable. Compared with the high-entropy alloy part prepared by a casting method, the high-entropy alloy part prepared by the method disclosed by the embodiment of the invention has the advantages of fine eutectic structures, more uniform distribution, more excellent tensile strength and elongation and greatly improved mechanical properties.
The reaction structure high-entropy alloy cylindrical component prepared in example 2 was cut into cubic pieces having a size of 6 to 10mm, and the pieces were subjected to an explosive-driven steel plate impact test.
Fig. 11A shows a high-speed photographic image of a fragment during flight, fig. 11B shows a high-speed photographic image of a fragment at the time of initial collision, and fig. 11C shows a high-speed photographic image of a fragment during collision discharge.
From this test it is possible to obtain: referring to FIG. 11A, the fragment spontaneously combusts during flight under explosive detonation-driven conditions to release a significant amount of heat; referring to fig. 11B, the fragments further release huge heat when striking the steel plate, so that the striking surfaces of the fragments and the steel plate generate fiercely burning flame groups, and the fragments are promoted to rapidly penetrate through the steel plate; referring to fig. 11C, the fragments still have high activity during penetration through the steel plate, releasing strong airflow after penetration.
Therefore, the reaction structure high-entropy alloy part prepared by the method disclosed by the embodiment of the invention not only has higher strength and elongation, but also has excellent energy release characteristics and armor penetration performance, shows an excellent armor penetration combustion effect, and improves the application and development of the high-entropy alloy as a structure and functional material.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the high-entropy alloy part with the laser melting deposition reaction structure is characterized by comprising the following steps of:
s1, mixing or alloying the metal simple substances Al, Co, Cr, Fe and Ni with the purity of more than or equal to 90 percent according to a certain proportion; wherein, the mixture ratio of the five metal simple substances is as follows: al: 15 at.% to 20 at.%; co: 15 at.% to 20 at.%; cr: 15 at.% to 20 at.%; fe: 15 at.% to 20 at.%; ni: 20 at.% to 40 at.%;
s2, screening the powder subjected to mixing or alloying treatment in the step S1 through a metal powder screen, then putting the screened powder into a vacuum drying box, heating to 100-150 ℃ in a vacuum environment, preserving heat for 1-3 hours, and cooling along with the box for later use;
s3, cleaning the surface to be deposited of the forming substrate; setting laser melting deposition process parameters and a laser scanning path in a laser melting deposition system; wherein, the laser melting deposition process parameters are as follows: the laser power is 400-1200W; the scanning speed is 200-800 mm/min; the powder feeding speed is 0.8 to 1.5 rad/min; the flow rate of inert powder feeding gas is 20-35L/min; the flow rate of the inert protective gas is 2-10L/min; the lifting amount is 0.1-1 mm; the lapping rate is 10% -90%;
s4, under the protection of inert gas, putting the powder dried in the step S2 into a powder feeder of a laser melting deposition system; and then starting a laser melting deposition system, and melting and depositing powder on a forming substrate layer by layer under the protection of inert gas according to set laser melting deposition process parameters and a scanning path to prepare the reaction structure high-entropy alloy component.
2. The method for preparing a high-entropy alloy component with a laser melting deposition reaction structure according to claim 1, wherein in step S1, the mixture ratio of five metal simple substances is as follows: al: 15 at.% to 17 at.%; co: 15 at.% to 17 at.%; cr: 15 at.% to 17 at.%; fe: 15 at.% to 17 at.%; ni: 34 at.% to 40 at.%.
3. A method for preparing a high-entropy alloy component with a laser melting deposition reaction structure according to claim 2, wherein in step S3, the laser melting deposition process parameters are as follows: the laser power is 700-800W; the scanning speed is 400-450 mm/min; the powder feeding speed is 1-1.2 rad/min; the flow rate of inert powder feeding gas is 28-30L/min; the flow rate of the inert protective gas is 5-10L/min; the lifting amount is 0.2-0.25 mm; the lapping rate is 40-60%.
4. The method for producing a high-entropy alloy member with a laser fused deposition reaction structure according to claim 1, wherein in step S1, the mixing method of five metal elements is as follows: mechanically stirring and mixing for 1-5 h or ball-milling and mixing for 5-30 h.
5. The method for producing a high-entropy alloy member with a laser melting deposition reaction structure according to claim 1, wherein in step S1, the alloying treatment method for five kinds of simple metals is as follows: inert gas atomization powder preparation method, rotating electrode method, rotating disc electron beam melting method, rotating electrode plasma melting method or rotating electrode electron beam melting method.
6. A method for producing a high-entropy alloy member with a laser fused deposition reaction structure according to claim 1, 2, 3, 4 or 5, wherein in step S2, the particle size of the powder subjected to the drying treatment in the vacuum drying oven is 50 to 150 μm.
7. A method for preparing a high-entropy alloy member with a laser melting deposition reaction structure according to claim 6, wherein in step S2, the particle size of the powder dried in the vacuum drying oven is 55-120 μm.
8. A method of producing a laser fused deposition reaction structure high entropy alloy component according to claim 1, wherein the forming substrate is a stainless steel plate or a zirconium alloy plate.
9. Use of the process according to any of claims 1 to 8 for the production of AlCoCrFeNi2.1Application in reaction structure high-entropy alloy.
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