CN115815585A - Light high-entropy alloy spherical powder and preparation method and application thereof - Google Patents
Light high-entropy alloy spherical powder and preparation method and application thereof Download PDFInfo
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Abstract
A light high-entropy alloy spherical powder and a preparation method and application thereof are disclosed, wherein the light high-entropy alloy spherical powder comprises the following raw materials in parts by mass: a1:
parts by weight, fe:
parts by weight, cr:
parts by weight, mn:
parts by weight, ti:
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy materials, and particularly relates to light high-entropy alloy spherical powder and a preparation method and application thereof.
Background
The flexible preparation of the special alloy spherical powder with low cost and high quality in small batches is a high-point manufacturing point of metal laser 3D printing, and the future of metal laser 3D printing is mastered to a certain extent by mastering the technology. The existing mature powder preparation method has great defects, for example, satellite spherical powder can be generated when the spherical powder is prepared by a smelting atomization method, and oxide inclusions can be easily generated when the plasma rotating electrode is used for powder preparation.
For example, the application number is CN202011213632.8, the name is: the patent of the application of a discharge plasma modification method in the treatment of spherical/spheroidal metal powder prepared by an atomization method adopts the atomization method, and the adverse effects of spheroidal powder, hollow sphere powder and the like can be generated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide light high-entropy alloy spherical powder and a preparation method and application thereof, proper alloying element types and relative contents are selected, the high-entropy alloy is combined with a mechanical alloying technology, the solid solution of aluminum elements is realized through mechanical alloying, the melting point of the powder reaches 1350K, and the light high-entropy alloy spherical powder can be widely applied to the field of high-temperature alloys; the high-entropy alloy coating is prepared after 3D printing, the hardness can reach 680HV, and the light high-entropy alloy is expected to be applied to important fields of aerospace, vehicle and ship industries and the like.
In order to achieve the purpose, the preparation technical scheme adopted by the invention is as follows:
a light high-entropy spherical alloy powder with the granularity of raw material
According to the parts by mass: a1:
Fe：
Cr：
Mn：
Ti：
the preparation method of the light high-entropy alloy comprises the following steps:
(1) The components in parts by mass: a1:
Fe：
Cr：
Mn：
Ti：
the particle size is
Mixing the powders, placing into a rod mill, and vacuumizing to 1 × 10 -1 —1×10 -2 And Pa, filling argon, repeating the process at least twice, vacuumizing and pressing into n-heptane again, wherein the mass fraction ratio of the n-heptane to the powder is 1: (2-4), finally introducing argon until the tank body is filled with argon;
(2) Alloying the alloy powder with a vibrating rod mill for 2-3 hours, vacuumizing the rod mill tank to 1 × 10 -1 Filling industrial alcohol into a rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10: (3-4), after continuously grinding for 10-12 minutes, taking out the mixture of the alloy powder and the alcohol;
(3) Standing the mixture for 15-25 hours, filtering out supernatant, and placing the mixture in a vacuum drying oven, wherein the vacuum of the drying oven is always kept to 0.1-0.12 pa, the temperature is kept to 60-65 ℃, the mixture is dried for 8-10 hours under the condition of heat preservation to obtain high-entropy alloy powder, and finally the powder is packaged and stored in vacuum;
(4) And opening a power supply of the vertical heating furnace, and setting a temperature rise process: heating to 50-1650 deg.C at 5-10 deg.C/min, heating to set temperature, and maintaining for 120-180 min; filling the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, and feeding the powder out by using a nozzle, wherein the actual powder feeding speed of the powder feeder is 2g/min-2.4g/min, and simultaneously introducing argon as a protective gas;
(5) The powder is melted and condensed through the vertical long pipe and falls into the bottom collecting device, after the powder all falls into the collecting device, the argon gas for the protective gas is continuously introduced and the cooling circulating device is started, and after the temperature of the powder is reduced to the room temperature, the collecting device is taken down, and the light high-entropy alloy spherical powder is obtained.
Based on the application of the light high-entropy alloy, the prepared light high-entropy alloy spherical powder is loaded into an annular powder feeder of a selected laser melting 3D printer, the high-entropy alloy powder is conveyed under the protection of argon, the parameters of the coaxial powder feeding 3D printer are set to be 700-1000W of laser power, the powder supply speed is 1.6-3 g/min, the scanning speed is 50-70%, the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating, and finally the light high-entropy alloy coating is obtained on a substrate.
Compared with the prior art, the invention has the beneficial effects and innovations that:
(1) The newly designed new components of the AlFeCrMnTi alloy are alloyed after metals (aluminum powder, manganese powder, chromium powder, iron powder and titanium powder) are uniformly mixed according to a certain proportion by means of mechanical alloying, and finally the single-phase body-centered cubic solid solution diagram high-entropy alloy powder is successfully prepared by drying the alloy powder.
(2) By means of a mechanical alloying and drop tube fusing duplex process, a feasible scheme for preparing small-batch special alloy spherical powder with low cost and high quality is formed.
(3) The high-entropy alloy coating material is manufactured by using a laser melting deposition process, and compared with an original substrate, the high-entropy alloy coating material is excellent in corrosion resistance and improved in hardness by 2-3 times.
Drawings
FIG. 1 is an XRD spectrum of high-entropy alloy powder of example I, II, III and IV.
FIG. 2 is an SEM topography of four high entropy alloy powders with different Ti contents.
FIG. 3 is an XRD pattern of Al4FeCrMnTix series light high entropy alloy spherical powder with different Ti contents at a fusing temperature of 1700 ℃.
FIG. 4 is an SEM morphology of spherical powder of high-entropy alloy of the first, second, third and fourth examples. In fig. 4, (a) is Ti content x =0, (b) is Ti content x =0.25, (c) is Ti content x =0.5; (d) is Ti content x =1.
FIG. 5 is XRD patterns of high entropy alloy coatings with different Ti contents for examples one, two, three and four.
Fig. 6 is SEM images of high entropy alloy coatings of examples one, two, three, and four different Ti contents, where (a) the Ti content x =0.25, (b) the Ti content x =0.5, and (c) the Ti content x =1.
FIG. 7 is a graph of the electrochemical properties of Al4FeCrMnTix high entropy alloy laser cladding coatings of examples one, two, three, four different Ti contents, wherein (a) is a polarization curve of the high entropy alloy coating, and (b) is an impedance plot.
FIG. 8 is a microhardness distribution curve of the laser cladding coating of the high-entropy alloy of the first, second, third and fourth examples.
Detailed Description
The invention is described in detail below with reference to the figures and examples
Example one
The light high-entropy alloy of the embodiment comprises the following components in parts by weight: al:39.9 parts, fe:20.6 parts, cr:19.2 parts, mn:20.2 parts of Ti:0 part of (A).
The preparation method of the light-weight high-entropy alloy comprises the following steps:
(1) According to the mass parts: al:39.9 parts of Fe:20.6 parts, cr:19.2 parts, mn:20.2 parts of Ti:0 portion, the powder is evenly mixed and then put into a rod mill pot, and the pot is vacuumized to 1 multiplied by 10 -1 Pa, filling argon, and repeatedly operating the process twice to prevent the powder from being oxidized in the alloying process; 100ml of n-heptane were introduced under pressure to lower the entropy of mixing of the powders during grinding in a high-energy rod mill, and argon gas was introduced again.
The total weight of the above powder is 300g;
(2) Alloying the powder for 2h by a vibrating rod mill, vacuumizing the rod mill tank to 1 × 10 -1 Pa, filling industrial alcohol into the rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10:3, continuously grinding for 10min, and taking out the mixture of the high-entropy alloy powder and the alcohol;
(3) Standing the mixture obtained in the step for 15h, filtering to remove supernatant, placing in a vacuum drying oven, wherein the vacuum of the drying oven is always kept at 0.1pa, the temperature is kept to 60 ℃, and the heat preservation and drying are carried out for 8h to obtain high-entropy alloy powder, finally, the powder is packaged and stored in vacuum, the XRD pattern of the powder is shown in figure 1, the SEM picture is shown in figure 2, and the powder is seen to be in a lamellar shape.
(4) Turning on a power supply of the vertical heating furnace, and setting a temperature rise process: heating to 50-1650 ℃ at 5 ℃/min, keeping the temperature for 120 minutes after heating to the set temperature, loading the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, opening a controller, wherein the actual powder feeding speed of the powder feeder is 2g/min, and simultaneously introducing argon as protective gas.
(5) The powder is melted and condensed through the vertical long pipe and falls into the bottom collecting device, and the powder is taken out to finally obtain the superfine spherical alloy powder. The XRD pattern of the spherical powder is shown in fig. 3, and it can be seen that the spherical powder is completely alloyed to form a solid solution with a single body-centered cubic phase structure. The SEM image of the powder is shown in fig. 4, and the sphericity ratio exceeds 95%.
Based on the application of the light-weight high-entropy alloy, in the embodiment, a steel product of Q235 is selected as a base material, and a large-sized steel product of Q235 is cut into rectangular steel products of 150mm × 90mm × 12mm by a wire cutting device. And (3) polishing the surface of the steel by using abrasive paper to remove oxides on the surface of the steel, cleaning by using alcohol and drying.
The prepared light high-entropy alloy spherical powder is filled into a ring-shaped powder feeder of a selected laser melting 3D printer, argon is introduced to provide a protective atmosphere environment, and the powder is blown out; opening a power switch and a protective atmosphere valve of the powder feeder to ensure that protective gas is filled in the container to avoid powder oxidation; opening a laser condensation circulating water system, opening a laser for positioning when the water temperature is raised to the room temperature, and setting a scanning path; and conveying the high-entropy alloy powder under the protection of argon gas, and starting to print the laser cladding coating.
The machining precision of the printer is 1mm, the parameters of the coaxial powder feeding 3D printer are set to be laser power 1000W, the powder supply speed is 1.6g/min, the scanning speed is 60%, and the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating with the thickness of 30 x 15 mm. Finally, obtaining a 4mm light high-entropy alloy coating on the Q235 steel plate. After the coating is printed, closing a power supply of the laser, stopping powder feeding, and closing a protective gas valve; after the printed test piece is cooled, sampling and processing are carried out, and the XRD (X-ray diffraction) spectrum of phase structure analysis is shown in figure 5, and the microstructure is shown in figure 6. Electrochemical properties are characterized as shown in fig. 7, and the polarization curve diagram and the impedance diagram of the alloy show that the alloy coating has excellent properties. As shown in FIG. 8, the microhardness distribution curve of the high-entropy alloy laser cladding coating can reach 400HV in the case of alloy hardness.
Example two
The light high-entropy alloy of the embodiment comprises the following components in parts by weight: al:38.2 parts of Fe:19.8 parts of Cr:18.4 parts, mn:19.4 parts of Ti:4.2 parts.
The preparation method of the light high-entropy alloy comprises the following steps:
(1) According to the mass parts: al:38.2 parts, fe:19.8 parts of Cr:18.4 parts of 1, mn:19.4 parts, ti:4.2 parts. Mixing the powders, placing into a rod mill, and vacuum-pumping to 5 × 10 -2 Pa, filling argon, and repeatedly operating the process twice to prevent the powder from being oxidized in the alloying process; 75ml of n-heptane were introduced under pressure to lower the entropy of mixing of the powders during grinding in a high-energy rod mill, and argon gas was introduced again. The total weight of the above powder is 300g;
(2) Alloying the powder for 2.5h by a vibrating rod mill, vacuumizing the rod mill tank to 1
10 -1 Pa, filling industrial alcohol into the rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10:3.5, continuously grinding for 11min, and taking out the mixture of the high-entropy alloy powder and the alcohol;
(3) Standing the mixture obtained in the step for 20h, filtering out supernatant, placing in a vacuum drying oven, wherein the vacuum of the drying oven is always kept at 0.11pa, the temperature is kept to 65 ℃, keeping the temperature and drying for 9h to obtain high-entropy alloy powder, and finally, carrying out vacuum packaging and storing on the powder. The XRD pattern of the powder is shown in FIG. 1, and the SEM image is shown in FIG. 2, so that the powder is in a lamellar shape.
(4) Turning on a power supply of the vertical heating furnace, and setting a temperature rise process: heating to 50-1650 deg.C at 6 deg.C/min, and keeping the temperature for 150 min; filling the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, wherein the actual powder feeding rate is 2.1g/min, and simultaneously introducing argon as protective gas;
(5) The powder is melted and solidified through the vertical long pipe and falls into the bottom collecting device. And when the powder completely falls into the collecting device, continuously introducing the protective gas argon and starting the cooling circulating device. And after the temperature of the powder is reduced to room temperature, taking down the collecting device and taking out the powder. And screening the powder by using sieves with different meshes to remove large particles included in the powder, and finally obtaining the superfine spherical alloy powder. The XRD pattern of the spherical powder is shown in fig. 3, and it can be seen that the spherical powder is completely alloyed to form a solid solution with a single body-centered cubic phase structure. The SEM image of the powder is shown in fig. 4, and the sphericity ratio exceeds 95%.
Based on the application of the light high-entropy alloy, in the embodiment, a Q235 steel material is used as a base material, and a large Q235 steel plate is cut into rectangular steel materials of 150mm × 90mm × 12mm by a wire cutting device. And (3) polishing the surface of the steel by using abrasive paper to remove oxides on the surface of the steel, cleaning by using alcohol and drying.
The prepared light high-entropy alloy spherical powder is filled into a ring-shaped powder feeder of a selected laser melting 3D printer, argon is introduced to provide a protective atmosphere environment, and the powder is blown out; opening a power switch and a protective atmosphere valve of the powder feeder to make protective gas fill the container to avoid powder oxidation; opening a laser condensation circulating water system, opening the laser for positioning when the water temperature is raised to the room temperature, and setting a scanning path; and conveying the high-entropy alloy powder under the protection of argon gas, and starting to print the laser cladding coating.
The machining precision of the printer is 1mm, the parameters of the coaxial powder feeding 3D printer are set to be laser power 800W, the powder supply speed is 2g/min, the scanning speed is 70%, and the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating with the thickness of 30 x 15 mm. Finally, a 5mm light high-entropy alloy coating is obtained on the Q235 steel plate. After the coating is printed, closing a power supply of the laser, stopping powder feeding, and closing a protective gas valve; and after the printed test piece is cooled, sampling and processing, and performing characterization analysis on the phase structure, the microstructure and the performance. As shown in FIG. 8, the microhardness distribution curve of the high-entropy alloy laser cladding coating can reach 480HV in the case of alloy hardness.
EXAMPLE III
The embodiment provides a light high-entropy alloy which comprises the following components in parts by weight: al:36.6 parts, fe:19.0 parts of Cr:17.6 parts, mn:18.6 parts, ti:8.1 parts.
The preparation method of the light high-entropy alloy comprises the following steps:
(1) According to the parts by mass: al:36.6 parts, fe:19.0 parts of Cr:17.6 parts, mn:18.6 parts, ti:8.1 parts. Mixing the powders, placing into a rod mill, and vacuum-pumping to 1 × 10 -1 Pa, filling argon, and repeatedly operating the process twice to prevent the powder from being oxidized in the alloying process; 150ml of n-heptane was added under pressure to reduce grinding by a high energy rod millThe entropy of mixing of the powders was determined by charging argon. The total weight of the above powder is 300g;
(2) Alloying the powder for 2h by a vibrating rod mill, vacuumizing the rod mill tank to 1 × 10 -1 Pa, filling industrial alcohol into the rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10:4. continuously grinding for 12min, and taking out the mixture of the high-entropy alloy powder and the alcohol;
(3) Standing the mixture obtained in the step for 25h, filtering out supernatant, placing in a vacuum drying oven, keeping the vacuum of the drying oven below 0.12pa all the time, keeping the temperature to 65 ℃, keeping the temperature and drying for 10h to obtain high-entropy alloy powder, and finally packaging and storing the powder in vacuum. The XRD pattern of the powder is shown in FIG. 1, and the SEM picture is shown in FIG. 2, and the powder is seen to be lamellar.
(4) Turning on a power supply of the vertical heating furnace, and setting a temperature rise process: the temperature is increased to 9 ℃/min in the process of heating to 50-1650 ℃, and is kept for 180 minutes after being increased to the set temperature. And (4) filling the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, wherein the actual powder feeding rate is 2.4g/min.
(5) The powder is melted and condensed through the vertical long pipe and falls into the bottom collecting device, when the powder completely falls into the collecting device, the argon gas as the protective gas is continuously introduced, the cooling circulating device is started, and after the temperature of the powder is reduced to the room temperature, the collecting device is taken down, and the powder is taken out. And screening the powder by using sieves with different meshes to remove large particles included in the powder, and finally obtaining the superfine spherical alloy powder. The SEM image of the powder is shown in fig. 4, and the sphericity ratio exceeds 95%.
Based on the application of the light high-entropy alloy, in the embodiment, a Q235 steel material is used as a base material, and a large Q235 steel plate is cut into rectangular steel materials of 150mm × 90mm × 12mm by a wire cutting device. And (3) polishing the surface of the steel by using abrasive paper to remove oxides on the surface of the steel, cleaning by using alcohol and drying.
The prepared light high-entropy alloy spherical powder is filled into a ring-shaped powder feeder of a selected laser melting 3D printer, argon is introduced to provide a protective atmosphere environment, and the powder is blown out; opening a power switch and a protective atmosphere valve of the powder feeder to make protective gas fill the container to avoid powder oxidation; opening a laser condensation circulating water system, opening the laser for positioning when the water temperature is raised to the room temperature, and setting a scanning path; and conveying the high-entropy alloy powder under the protection of argon gas, and starting to print the laser cladding coating.
(8) The machining precision of the printer is 1mm, the parameters of coaxial powder feeding 3D printing are set to be laser power 900W, the powder supply speed is 2.6g/min, the scanning speed is 50%, and the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating with the thickness of 30 x 15 mm. Finally, obtaining a 4mm light high-entropy alloy coating on the Q235 steel plate. After the coating is printed, closing a power supply of the laser, stopping powder feeding, and closing a protective gas valve; after the printed test piece is cooled, sampling and processing are carried out, and the XRD (X-ray diffraction) spectrum of phase structure analysis is shown in figure 5, and the microstructure is shown in figure 6. Electrochemical properties are characterized as shown in fig. 7, and the polarization curve diagram and the impedance diagram of the alloy show that the alloy coating has excellent properties. The alloy shown in FIG. 8 has a hardness of 560HV.
Example four
The light high-entropy alloy of the embodiment comprises the following components in parts by weight: al:33.9 parts, fe:17.6 parts, cr:16.3 parts, mn:17.2 parts, ti:15.0 parts, and 300g in total.
The preparation method of the light high-entropy alloy comprises the following steps:
(1) According to the mass parts: al:33.9 parts, fe:17.6 parts, cr:16.3 parts, mn:17.2 parts, ti:15.0 parts, and 300g in total. Mixing the powders, loading into rod mill, and vacuumizing to 1 × 10 -1 Pa, filling argon, and repeatedly operating the process twice to prevent the powder from being oxidized in the alloying process; pressing 100ml of n-heptane to reduce the mixing entropy of the powder when the high-energy rod mill grinds, and then filling argon, wherein the total weight of the powder is 300g;
(2) Alloying the powder for 3h by a vibrating rod mill, vacuumizing the rod mill tank to 1 function
10 -1 Pa, filling industrial alcohol into the rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10:4. continuously grinding for 12min, and taking out the mixture of the high-entropy alloy powder and the alcohol;
(3) And (3) standing the mixture obtained in the step (2) for 25h, filtering out supernatant, placing the mixture in a vacuum drying oven, keeping the vacuum of the drying oven below 0.12pa all the time, keeping the temperature to 60 ℃, keeping the temperature and drying for 10h to obtain high-entropy alloy powder, and finally packaging and storing the powder in vacuum.
(4) Turning on a power supply of the vertical heating furnace, and setting a temperature rise process: the temperature is increased to 10 ℃/min in the process of heating to 50-1600 ℃, and the temperature is maintained for 180 minutes after the temperature is increased to the set temperature. And (4) loading the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, opening a controller, and introducing protective gas argon while the actual powder feeding rate is 2.4g/min.
(5) The powder is melted and condensed by the long vertical tube and falls into the bottom collecting device. And when the powder completely falls into the collecting device, continuously introducing protective gas argon and starting a cooling circulating device, and after the temperature of the powder is reduced to the room temperature, taking down the collecting device and taking out the powder. And screening the powder by using sieves with different meshes to remove large particles included in the powder, and finally obtaining the superfine spherical alloy powder.
Based on the application of the light-weight high-entropy alloy, in the embodiment, a steel product of Q235 is selected as a base material, and a large-sized steel product of Q235 is cut into rectangular steel products of 150mm × 90mm × 12mm by a wire cutting device. And (3) polishing the surface of the steel by using abrasive paper to remove oxides on the surface of the steel, cleaning by using alcohol, and drying.
The prepared light high-entropy alloy spherical powder is filled into a ring-shaped powder feeder of a selected laser melting 3D printer, argon is introduced to provide a protective atmosphere environment, and the powder is blown out; opening a power switch and a protective atmosphere valve of the powder feeder to ensure that protective gas is filled in the container to avoid powder oxidation; opening a laser condensation circulating water system, opening the laser for positioning when the water temperature is raised to the room temperature, and setting a scanning path; and conveying the high-entropy alloy powder under the protection of argon gas, and starting to print the laser cladding coating.
The machining precision of the printer is 1mm, the parameters of coaxial powder feeding 3D printing are set to be laser power 900W, the powder supply speed is 3g/min, the scanning speed is 70%, and the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating with the thickness of 30 x 15 mm. Finally, a 4.8mm light high-entropy alloy coating is obtained on the Q235 steel plate. After the coating is printed, closing a power supply of the laser, stopping powder feeding, and closing a protective gas valve; after the printed test piece is cooled, sampling and processing are carried out, and the XRD (X-ray diffraction) spectrum of phase structure analysis is shown in figure 5, and the microstructure is shown in figure 6. Electrochemical properties are characterized as shown in fig. 7, and the polarization curve diagram and the impedance diagram of the alloy show that the alloy coating has excellent properties. As shown in FIG. 8, the microhardness distribution curve of the high-entropy alloy laser cladding coating can reach 680HV.
The above description is only a result of the preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various changes and modifications without departing from the inventive concept, and these are all within the scope of the present invention.
Claims (6)
1. The light high-entropy alloy spherical powder is characterized in that the granularity of raw materials is
According to the parts by mass: a1:
Fe：
Cr：
Mn：
Ti：
2. the light-weight high-entropy alloy spherical powder according to claim 1, characterized in that: al:33.9 parts of Fe:17.6 parts, cr:16.3 parts, mn:17.2 parts, ti:15.0 parts.
3. The preparation method of the light high-entropy alloy based on claim 1 is characterized by comprising the following steps of:
(1) The components in parts by mass: a1:
Fe：
Cr：
Mn：
Ti：
the particle size is
Mixing the powders, placing into a rod mill, and vacuumizing to 1 × 10 -1 ～1×10 -2 And Pa, filling argon for twice, vacuumizing again and pressing into n-heptane, wherein the mass fraction ratio of the n-heptane to the powder is 1:2-4, finally introducing argon until the tank body is filled with argon;
(2) Alloying the alloy powder with a vibrating rod mill for 2-3 hours, vacuumizing the rod mill tank to 1 × 10 -2 Pa, filling industrial alcohol into the rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10: (3-4), after continuously grinding for 10-12 minutes, taking out the mixture of the alloy powder and the alcohol;
(3) Standing the mixture for 15-25 hours, filtering out supernatant, and placing the mixture in a vacuum drying oven, wherein the vacuum of the drying oven is always kept to 0.1-0.12 pa, the temperature is kept to 60-65 ℃, the mixture is dried for 8-10 hours under the condition of heat preservation to obtain high-entropy alloy powder, and finally the powder is packaged and stored in vacuum;
(4) And opening a power supply of the vertical heating furnace, and setting a temperature rise process: heating to 50-1650 deg.C at 5-10 deg.C/min, heating to set temperature, and maintaining for 120-180 min; filling the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, and feeding the powder out by using a nozzle, wherein the actual powder feeding speed of the powder feeder is 2g/min-2.4g/min, and simultaneously introducing protective gas argon;
(5) The powder is melted and condensed through the vertical long pipe and falls into the bottom collecting device, the protective gas argon is continuously introduced and the cooling circulating device is started after the powder completely falls into the collecting device, and the collecting device is taken down after the temperature of the powder is reduced to the room temperature, so that the light high-entropy alloy spherical powder is obtained.
4. The preparation method of the light-weight high-entropy alloy according to claim 3, characterized by comprising the following steps:
(1) And according to the mass parts: al:33.9 parts of Fe:17.6 parts, cr:16.3 parts, mn:17.2 parts of Ti:15.0 parts of the above-mentioned material with the particle size of
Mixing the powders, placing into a rod mill, and vacuumizing to 1 × 10 -1 Pa, filling argon, repeating the process twice, vacuumizing again and pressing into n-heptane, wherein the mass fraction ratio of the n-heptane to the powder is 1:3, finally introducing argon until the tank body is filled with argon;
(2) Alloying the alloy powder for 3 hr in a vibrating rod mill, and vacuumizing the rod mill to 1 × 10 -2 Pa, filling industrial alcohol into the rod milling tank, wherein the mass fraction ratio of the industrial alcohol to the metal powder is 10:4, continuously grinding for 12 minutes, and taking out the mixture of the alloy powder and the alcohol;
(3) Standing the taken mixture for 25 hours, filtering out supernatant, placing the mixture in a vacuum drying oven, keeping the vacuum of the drying oven to be 0.12pa all the time, keeping the temperature to be 60 ℃, keeping the temperature and drying for 10 hours to obtain high-entropy alloy powder, and finally packaging and storing the powder in vacuum;
(4) And opening a power supply of the vertical heating furnace, and setting a temperature rise process: heating to 50-1650 deg.C at 10 deg.C/min, and keeping the temperature for 180 min; filling the mechanically alloyed high-entropy powder obtained in the step (3) into a powder feeder, and feeding the powder out by using a nozzle, wherein the actual powder feeding speed of the powder feeder is 2.4g/min, and simultaneously introducing argon as a protective gas;
(5) The powder is melted and condensed through the vertical long pipe and falls into the bottom collecting device, the protective gas argon is continuously introduced and the cooling circulating device is started after the powder completely falls into the collecting device, and the collecting device is taken down after the temperature of the powder is reduced to the room temperature, so that the light high-entropy alloy spherical powder is obtained.
5. The application of the light high-entropy alloy prepared based on the method in claim 3 is characterized in that the prepared light high-entropy alloy spherical powder is loaded into an annular powder feeder of a selected laser melting 3D printer, the high-entropy alloy powder is conveyed under the protection of argon, the parameters of the coaxial powder feeding 3D printer are set to be 700-1000W of laser power, the powder supply speed is 1.6-3 g/min, the scanning speed is 50% -70%, the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating, and finally the light high-entropy alloy coating is obtained on a substrate.
6. The application of the light high-entropy alloy as claimed in claim 5, wherein the prepared light high-entropy alloy spherical powder is loaded into an annular powder feeder of a selected laser melting 3D printer, the high-entropy alloy powder is conveyed under the protection of argon, the parameters of the coaxial powder feeding 3D printer are set to be laser power 900W, the powder supply speed is 13g/min, and the scanning speed is 570%, the 3D printer is debugged to execute an NH-1 instruction to print a high-entropy alloy coating, and finally the light high-entropy alloy coating is obtained on a Q235 steel plate.
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| CN116809940A (en) * | 2023-08-30 | 2023-09-29 | 吉林大学 | Multi-component shape memory high-entropy alloy for additive manufacturing and preparation method thereof |
| CN116809940B (en) * | 2023-08-30 | 2023-11-03 | 吉林大学 | Multi-component shape memory high-entropy alloy for additive manufacturing and preparation method thereof |
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