Lightweight high-entropy alloy spherical powder, preparation method and application thereof

By combining mechanical alloying and vertical long-tube melting and solidification processes with laser melting deposition, the problems of satellite powder and oxide inclusions in the preparation of alloy spherical powders have been solved, realizing the low-cost preparation of high-quality alloy powders and the application of high-hardness coating materials, which are suitable for aerospace and automotive/shipbuilding industries.

CN115815585BActive Publication Date: 2025-11-11XI AN JIAOTONG UNIV
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Patent Information

Application Number
CN202211610794.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-14
Publication Date
2025-11-11
Estimated Expiration
2042-12-14

AI Technical Summary

Technical Problem

Existing technologies for preparing alloy spherical powders for metal laser 3D printing suffer from the problem of satellite powder and oxide inclusions, making it difficult to achieve low-cost, high-quality, small-batch flexible preparation of dedicated alloy spherical powders.

Method used

By employing mechanical alloying technology combined with appropriate alloying element types and relative contents, and through vibratory bar mill alloying and vertical long tube melting and solidification processes, single-phase body-centered cubic solid solution high-entropy alloy powder was prepared, and a high-entropy alloy coating was manufactured using laser melting deposition process.

Benefits of technology

A low-cost, high-quality alloy spherical powder was successfully prepared. The coating material exhibits excellent corrosion resistance and a 2-3 times increase in hardness, making it suitable for aerospace and automotive/shipbuilding industries.

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Abstract

The application relates to a light-weight high-entropy alloy spherical powder and a preparation method and application thereof, raw materials are prepared according to mass fractions, namely A1: parts, Fe: parts, Cr: parts, Mn: parts and Ti: parts; the light-weight high-entropy alloy spherical powder is obtained by combining the high-entropy alloy with a mechanical alloying technology and then combining a falling tube melting double-link process; the aluminum element is solid-solved through mechanical alloying, the powder melting point reaches 1350K, and the light-weight high-entropy alloy can be widely applied to the high-temperature alloy field; the light-weight high-entropy alloy spherical powder is subjected to 3D printing to prepare a high-entropy alloy coating, the hardness of the high-entropy alloy coating can reach 680HV, the corrosion resistance is excellent compared with a Q235 base plate, the hardness is improved by 2-3 times, and the light-weight high-entropy alloy is expected to be applied to important fields such as the aerospace and shipbuilding industries.
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Description

Technical Field

[0001] This invention belongs to the field of high-entropy alloy materials technology, specifically relating to a lightweight high-entropy alloy spherical powder, its preparation method, and its application. Background Technology

[0002] The flexible preparation of low-cost, high-quality, small-batch specialized alloy spherical powders represents the pinnacle of metal laser 3D printing; to a certain extent, mastering this technology means mastering the future of metal laser 3D printing. Existing mature powder preparation methods have significant drawbacks. For example, the melting and atomization method for preparing spherical powder can produce satellite powder particles, and plasma rotating electrode powder preparation is prone to oxide inclusions.

[0003] For example, the patent application number: CN202011213632.8, entitled "Application of a discharge plasma modification method in the treatment of spherical / quasi-spherical metal powders prepared by atomization", uses the atomization method, which will produce adverse consequences such as quasi-spherical powder and hollow spherical powder. Summary of the Invention

[0004] To overcome the shortcomings of the prior art, the present invention aims to provide a lightweight high-entropy alloy spherical powder, its preparation method, and its applications. By selecting appropriate alloying elements and their relative contents, high-entropy alloys are combined with mechanical alloying technology to achieve solid solution of aluminum through mechanical alloying. The powder has a melting point of 1350K and can be widely used in the field of high-temperature alloys. After 3D printing, a high-entropy alloy coating can be obtained with a hardness of 680HV. This lightweight high-entropy alloy is expected to be applied in important fields such as aerospace and automotive / shipbuilding industries.

[0005] To achieve the above objectives, the preparation technology adopted in this invention is as follows:

[0006] A lightweight high-entropy alloy spherical powder, the particle size of which is By weight parts: A1: Fe: Cr: Mn: Ti:

[0007] The preparation method of the above-mentioned lightweight high-entropy alloy includes the following steps:

[0008] (1) By weight parts: A1: Fe: Cr: Mn: Ti: The above granularity is After the powders are mixed evenly, they are placed into a rod mill jar and vacuumed to 1×10⁻⁶. -1 —1×10-2 Pa, fill with argon gas, repeat this process at least twice, then evacuate again and press in n-heptane, wherein the mass fraction ratio of n-heptane to powder is 1:(2-4), and finally purge with argon gas until the tank is full;

[0009] (2) The alloy powder is alloyed in a vibratory rod mill for 2-3 hours, and the mill jar is evacuated to 1×10⁻⁶. -1 a. Pour industrial alcohol into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder is 10:(3-4). Continue grinding for 10-12 minutes, and then take out the mixture of alloy powder and alcohol.

[0010] (3) Let the extracted mixture stand for 15 to 25 hours and filter out the supernatant. Place it in a vacuum drying oven, where the vacuum of the drying oven is always maintained at 0.1 to 0.12 Pa and the temperature is maintained at 60℃ to 65℃. Dry for 8 to 10 hours to obtain high-entropy alloy powder. Finally, vacuum seal the powder for storage.

[0011] (4) Turn on the power of the vertical heating furnace and set the heating process: the heating rate is 5℃ / min-10℃ / min during the heating process from 50℃ to 1650℃. After reaching the set temperature, keep it warm for 120-180 minutes. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder and use the nozzle to feed out the powder. The actual powder feeding rate of the powder feeder is 2g / min-2.4g / min. At the same time, argon gas is introduced as a protective gas.

[0012] (5) The powder is melted and solidified through a vertical long tube and falls into the bottom collection device. After all the powder has fallen into the collection device, the protective gas argon is continued to be introduced and the cooling circulation device is turned on. After the powder temperature drops to room temperature, the collection device is removed to obtain lightweight high-entropy alloy spherical powder.

[0013] Based on the above-mentioned application of a lightweight high-entropy alloy, the prepared lightweight high-entropy alloy spherical powder is loaded into the annular powder feeder of a selected laser melting 3D printer. The high-entropy alloy powder is transported under argon protection. The parameters of the coaxial powder feeding 3D printer are set as follows: laser power 700-1000W, powder supply speed 1.6-3g / min, scanning speed 50%-70%. The 3D printer is adjusted to execute the NH-1 command to print the high-entropy alloy coating. Finally, a lightweight high-entropy alloy coating is obtained on the substrate.

[0014] Compared with the prior art, the beneficial effects and innovations of this invention are as follows:

[0015] (1) A novel AlFeCrMnTi alloy composition was designed. By mechanically alloying metals (aluminum powder, manganese powder, chromium powder, iron powder, and titanium powder) were uniformly mixed in a certain proportion and then alloyed. After drying the alloy powder, a single-phase body-centered cubic solid solution high-entropy alloy powder was successfully prepared.

[0016] (2) By using the combined mechanical alloying and tube melting process, a feasible solution for preparing small batches of special alloy spherical powder with low cost and high quality was formed.

[0017] (3) A high-entropy alloy coating material was manufactured using laser melting deposition process. Compared with the original substrate, it has excellent corrosion resistance and its hardness is increased by 2-3 times. Attached Figure Description

[0018] Figure 1 The images show the XRD patterns of the high-entropy alloy powders in Examples 1, 2, 3, and 4.

[0019] Figure 2 SEM images of four high-entropy alloy powders with different Ti contents.

[0020] Figure 3 XRD patterns of Al4FeCrMnTix lightweight high-entropy alloy spherical powders with different Ti contents and a melting temperature of 1700℃.

[0021] Figure 4 The images show the SEM morphology of the high-entropy alloy spherical powders in Examples 1, 2, 3, and 4. Figure 4 In the diagram, (a) represents a Ti content of x = 0, (b) represents a Ti content of x = 0.25, (c) represents a Ti content of x = 0.5, and (d) represents a Ti content of x = 1.

[0022] Figure 5 The images show the XRD patterns of high-entropy alloy coatings with different Ti contents in Examples 1, 2, 3, and 4.

[0023] Figure 6 The images show SEM images of high-entropy alloy coatings with different Ti contents in Examples 1, 2, 3, and 4. In the images, (a) shows a Ti content x = 0.25, (b) shows a Ti content x = 0.5, and (c) shows a Ti content x = 1.

[0024] Figure 7 The graphs show the electrochemical performance changes of Al4FeCrMnTix high-entropy alloy laser cladding coatings with different Ti contents in Examples 1, 2, 3, and 4, where (a) is the polarization curve of the high-entropy alloy coating and (b) is the impedance diagram.

[0025] Figure 8 The images show the microhardness distribution curves of the high-entropy alloy laser cladding coatings in Examples 1, 2, 3, and 4. Detailed Implementation

[0026] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0027] Example 1

[0028] This embodiment describes a lightweight high-entropy alloy, comprising the following mass parts: Al: 39.9 parts, Fe: 20.6 parts, Cr: 19.2 parts, Mn: 20.2 parts, and Ti: 0 parts.

[0029] This embodiment describes a method for preparing a lightweight high-entropy alloy, comprising the following steps:

[0030] (1) According to the mass parts: Al: 39.9 parts, Fe: 20.6 parts, Cr: 19.2 parts, Mn: 20.2 parts, Ti: 0 parts, the powders were mixed evenly and then placed into a rod mill jar, and vacuumed to 1×10 -1 Pa, purging with argon gas, this process is repeated twice to prevent the powder from being oxidized during alloying; 100ml of n-heptane is injected to reduce the mixing entropy of the powder during high-energy rod mill grinding, and then argon gas is purged again.

[0031] The total weight of the powder is 300g;

[0032] (2) The powder was alloyed in a vibratory rod mill for 2 hours, and the mill jar was evacuated to 1×10⁻⁶. -1 Pa, industrial alcohol is introduced into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder is 10:3. After grinding for 10 minutes, the mixture of high entropy alloy powder and alcohol is taken out.

[0033] (3) The mixture obtained in step [1] was allowed to stand for 15 hours and the supernatant was filtered off. It was then placed in a vacuum drying oven, where the vacuum was maintained at 0.1 Pa and the temperature at 60°C for 8 hours to obtain high-entropy alloy powder. Finally, the powder was vacuum-sealed and stored. The XRD pattern of the powder is shown below. Figure 1 As shown, the SEM image is as follows Figure 2 As shown, the powder is in the form of flakes.

[0034] (4) Turn on the power of the vertical heating furnace and set the heating process: 5℃ / min during the heating process from 50℃ to 1650℃. After reaching the set temperature, keep it warm for 120 minutes. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder, turn on the controller, and the actual powder feeding rate of the powder feeder is 2g / min. At the same time, argon gas is introduced as a protective gas.

[0035] (5) The powder is melted and solidified through a vertical long tube and falls into a bottom collecting device. The powder is then removed, ultimately yielding ultrafine spherical alloy powder. The XRD pattern of the spherical powder is shown below. Figure 3As shown, the spherical powder is fully alloyed, forming a solid solution with a single body-centered cubic phase structure. The SEM image of the powder is shown below. Figure 4 As shown, the sphericity exceeds 95%.

[0036] Based on the aforementioned application of a lightweight high-entropy alloy, this embodiment selects Q235 steel as the base material. Large Q235 steel plates are cut into 150mm × 90mm × 12mm rectangular steel pieces using wire cutting equipment. The steel surface is then sanded to remove oxides, cleaned with alcohol, and dried.

[0037] The prepared lightweight high-entropy alloy spherical powder is loaded into the annular powder feeder of the selected laser melting 3D printer. Argon gas is introduced to provide a protective atmosphere and blow out the powder. The power switch and protective atmosphere valve of the powder feeder are turned on to fill the container with protective gas to prevent powder oxidation. The laser condenser circulating water system is turned on. When the water temperature rises to room temperature, the laser is turned on for positioning and the scanning path is set. The high-entropy alloy powder is transported under argon protection, and the laser cladding coating is printed.

[0038] The printer's processing precision is 1mm. The parameters of the coaxial powder-feed 3D printer were set as follows: laser power 1000W, powder supply speed 1.6g / min, scanning speed 60%. The 3D printer was debugged to execute the NH-1 command to print a 30×15mm high-entropy alloy coating. Finally, a 4mm lightweight high-entropy alloy coating was obtained on the Q235 steel plate. After the coating printing was completed, the laser power was turned off, powder feeding was stopped, and the protective gas valve was closed. After the printed specimen cooled, samples were taken for processing, and XRD patterns were analyzed for phase structure. Figure 5 As shown, the microstructure is as follows Figure 6 As shown. Electrochemical performance characterization is as follows. Figure 7 As shown, the polarization curves and impedance diagrams of the alloy demonstrate the excellent performance of the alloy coating. Figure 8 As shown, the microhardness distribution curve of the high-entropy alloy laser cladding coating is shown. In this case, the alloy hardness can reach 400 HV.

[0039] Example 2

[0040] This embodiment describes a lightweight high-entropy alloy, comprising the following mass parts: Al: 38.2 parts, Fe: 19.8 parts, Cr: 18.4 parts, Mn: 19.4 parts, and Ti: 4.2 parts.

[0041] This embodiment describes a method for preparing a lightweight high-entropy alloy, comprising the following steps:

[0042] (1) By mass parts: Al: 38.2 parts, Fe: 19.8 parts, Cr: 18.4 parts, Mn: 19.4 parts, Ti: 4.2 parts. After the powders are mixed evenly, they are placed into a rod mill jar and vacuumed to 5×10⁻⁶.-2 Pa, purging with argon gas, this process is repeated twice to prevent powder oxidation during alloying; 75ml of n-heptane is injected to reduce the mixing entropy of the powder during high-energy rod mill grinding, and then argon gas is introduced again. The total weight of the powder is 300g;

[0043] (2) The powder was alloyed in a vibratory rod mill for 2.5 hours, and the mill jar was evacuated to 1×

[0044] 10 -1 Pa, industrial alcohol was introduced into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder was 10:3.5. After grinding for 11 minutes, the mixture of high entropy alloy powder and alcohol was taken out.

[0045] (3) The mixture obtained in step [number] was allowed to stand for 20 hours and the supernatant was filtered off. It was then placed in a vacuum drying oven, where the vacuum was maintained at 0.11 Pa and the temperature at 65°C for 9 hours to obtain high-entropy alloy powder. Finally, the powder was vacuum-sealed and stored. The XRD pattern of the powder is shown below. Figure 1 As shown, the SEM image is as follows Figure 2 As shown, the powder is in the form of flakes.

[0046] (4) Turn on the power of the vertical heating furnace and set the heating process: the heating rate is 6℃ / min during the heating process from 50℃ to 1650℃. After reaching the set temperature, keep it warm for 150 minutes. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder. The actual powder feeding rate is 2.1g / min. At the same time, argon gas is introduced as a protective gas.

[0047] (5) The powder is melted and solidified through a vertical long tube and falls into the bottom collecting device. After all the powder has fallen into the collecting device, argon gas is continuously introduced as a protective gas and the cooling circulation device is activated. After the powder temperature drops to room temperature, the collecting device is removed and the powder is taken out. The powder is sieved through sieves of different mesh sizes to remove large particles, finally obtaining ultrafine spherical alloy powder. The XRD pattern of the spherical powder is shown below. Figure 3 As shown, the spherical powder is fully alloyed, forming a solid solution with a single body-centered cubic phase structure. The SEM image of the powder is shown below. Figure 4 As shown, the sphericity exceeds 95%.

[0048] Based on the aforementioned application of a lightweight high-entropy alloy, this embodiment selects Q235 steel as the base material. Large Q235 steel plates are cut into 150mm × 90mm × 12mm rectangular steel pieces using wire cutting equipment. The steel surface is then sanded to remove oxides, cleaned with alcohol, and dried.

[0049] The prepared lightweight high-entropy alloy spherical powder is loaded into the annular powder feeder of the selected laser melting 3D printer. Argon gas is introduced to provide a protective atmosphere and blow out the powder. The power switch and protective atmosphere valve of the powder feeder are turned on to fill the container with protective gas to prevent powder oxidation. The laser condenser circulating water system is turned on. When the water temperature rises to room temperature, the laser is turned on for positioning and the scanning path is set. The high-entropy alloy powder is transported under argon protection, and the laser cladding coating is printed.

[0050] The printer's processing precision is 1mm. The parameters of the coaxial powder-feed 3D printer were set as follows: laser power 800W, powder supply speed 2g / min, scanning speed 70%. The 3D printer was debugged to execute the NH-1 command to print a 30×15mm high-entropy alloy coating. Finally, a 5mm lightweight high-entropy alloy coating was obtained on the Q235 steel plate. After the coating printing was completed, the laser power was turned off, powder feeding was stopped, and the protective gas valve was closed. After the printed specimen cooled, samples were taken for processing, and characterization analysis of phase structure, microstructure, and properties was performed. Figure 8 As shown, the microhardness distribution curve of the high-entropy alloy laser cladding coating is shown. In this case, the alloy hardness can reach 480HV.

[0051] Example 3

[0052] This embodiment describes a lightweight high-entropy alloy, comprising the following mass parts: Al: 36.6 parts, Fe: 19.0 parts, Cr: 17.6 parts, Mn: 18.6 parts, and Ti: 8.1 parts.

[0053] This embodiment describes a method for preparing a lightweight high-entropy alloy, comprising the following steps:

[0054] (1) By mass parts: Al: 36.6 parts, Fe: 19.0 parts, Cr: 17.6 parts, Mn: 18.6 parts, Ti: 8.1 parts. After the powders are mixed evenly, they are placed into a rod mill jar and vacuumed to 1×10⁻⁶. -1 Pa, purging with argon gas, this process is repeated twice to prevent powder oxidation during alloying; 150ml of n-heptane is injected to reduce the mixing entropy of the powder during high-energy rod mill grinding, and then argon gas is injected again. The total weight of the powder is 300g;

[0055] (2) The powder was alloyed in a vibratory rod mill for 2 hours, and the mill jar was evacuated to 1×10⁻⁶. -1 Pa, industrial alcohol was introduced into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder was 10:4. After grinding for 12 minutes, the mixture of high-entropy alloy powder and alcohol was removed;

[0056] (3) The mixture obtained in step [number] was allowed to stand for 25 hours and the supernatant was filtered off. It was then placed in a vacuum drying oven, where the vacuum was maintained below 0.12 Pa and the temperature was kept at 65°C for 10 hours to obtain high-entropy alloy powder. Finally, the powder was vacuum-sealed and stored. The XRD pattern of the powder is shown below. Figure 1 As shown, the SEM image is as follows Figure 2 As shown, the powder is in the form of flakes.

[0057] (4) Turn on the power of the vertical heating furnace and set the heating process: the heating rate is 9℃ / min during the heating process from 50℃ to 1650℃, and the temperature is held for 180 minutes after reaching the set temperature. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder. The actual powder feeding rate is 2.4g / min.

[0058] (5) The powder melts and solidifies through a vertical long tube and falls into a bottom collecting device. After all the powder has fallen into the collecting device, argon gas is continuously introduced as a protective gas and a cooling circulation device is activated. Once the powder temperature drops to room temperature, the collecting device is removed, and the powder is taken out. The powder is then sieved using sieves of different mesh sizes to remove large particles, ultimately obtaining ultrafine spherical alloy powder. The SEM image of the powder is shown below. Figure 4 As shown, the sphericity exceeds 95%.

[0059] Based on the aforementioned application of a lightweight high-entropy alloy, this embodiment selects Q235 steel as the base material. Large Q235 steel plates are cut into 150mm × 90mm × 12mm rectangular steel pieces using wire cutting equipment. The steel surface is then sanded to remove oxides, cleaned with alcohol, and dried.

[0060] The prepared lightweight high-entropy alloy spherical powder is loaded into the annular powder feeder of the selected laser melting 3D printer. Argon gas is introduced to provide a protective atmosphere and blow out the powder. The power switch and protective atmosphere valve of the powder feeder are turned on to fill the container with protective gas to prevent powder oxidation. The laser condenser circulating water system is turned on. When the water temperature rises to room temperature, the laser is turned on for positioning and the scanning path is set. The high-entropy alloy powder is transported under argon protection, and the laser cladding coating is printed.

[0061] (8) The printer's processing accuracy is 1mm. The parameters for coaxial powder feeding 3D printing are set as follows: laser power 900W, powder supply speed 2.6g / min, scanning speed 50%. The 3D printer is then debugged to execute the NH-1 command to print a 30×15mm high-entropy alloy coating. Finally, a 4mm lightweight high-entropy alloy coating is obtained on the Q235 steel plate. After the coating printing is complete, the laser power is turned off, powder feeding is stopped, and the protective gas valve is closed. After the printed specimen cools, samples are taken for processing, and phase structure analysis XRD patterns are performed as shown in the figure. Figure 5As shown, the microstructure is as follows Figure 6 As shown. Electrochemical performance characterization is as follows. Figure 7 As shown, the polarization curves and impedance diagrams of the alloy demonstrate the excellent performance of the alloy coating. Figure 8 The alloy shown can reach a hardness of 560 HV.

[0062] Example 4

[0063] This embodiment describes a lightweight high-entropy alloy, comprising the following mass parts: Al: 33.9 parts, Fe: 17.6 parts, Cr: 16.3 parts, Mn: 17.2 parts, Ti: 15.0 parts, totaling 300g.

[0064] This embodiment describes a method for preparing a lightweight high-entropy alloy, comprising the following steps:

[0065] (1) By mass parts: Al: 33.9 parts, Fe: 17.6 parts, Cr: 16.3 parts, Mn: 17.2 parts, Ti: 15.0 parts, total 300g. After the powders are mixed evenly, they are placed into a rod mill jar and vacuumed to 1×10⁻⁶. -1 Pa, purging with argon gas, this process is repeated twice to prevent the powder from being oxidized during alloying; press in 100ml of n-heptane to reduce the mixing entropy of the powder during high-energy rod mill grinding, and then purge with argon gas again. The total weight of the powder is 300g.

[0066] (2) The powder was alloyed in a vibratory rod mill for 3 hours, and the mill jar was evacuated to 1× 100°C.

[0067] 10 -1 Pa, industrial alcohol was introduced into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder was 10:4. After grinding for 12 minutes, the mixture of high-entropy alloy powder and alcohol was removed;

[0068] (3) The mixture obtained in the step is left to stand for 25 hours and the supernatant is filtered off. It is then placed in a vacuum drying oven, where the vacuum of the drying oven is always kept below 0.12 Pa and the temperature is kept at 60°C. The mixture is kept at this temperature for 10 hours to obtain high-entropy alloy powder. Finally, the powder is vacuum-sealed and stored.

[0069] (4) Turn on the power of the vertical heating furnace and set the heating process: the heating rate is 10℃ / min during the heating process from 50℃ to 1600℃. After reaching the set temperature, keep it at that temperature for 180 minutes. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder, turn on the controller, and the actual powder feeding rate is 2.4g / min. At the same time, argon gas is introduced as a protective gas.

[0070] (5) The powder melts and solidifies through a vertical long tube and falls into the bottom collection device. After all the powder has fallen into the collection device, the protective gas argon is continued to be introduced and the cooling circulation device is turned on. After the powder temperature drops to room temperature, the collection device is removed and the powder is taken out. The powder is screened with sieves of different mesh sizes to remove large particles, and finally ultrafine spherical alloy powder is obtained.

[0071] Based on the aforementioned application of a lightweight high-entropy alloy, this embodiment selects Q235 steel as the base material. Large Q235 steel plates are cut into 150mm × 90mm × 12mm rectangular steel pieces using wire cutting equipment. The steel surface is then sanded to remove oxides, cleaned with alcohol, and dried.

[0072] The prepared lightweight high-entropy alloy spherical powder is loaded into the annular powder feeder of the selected laser melting 3D printer. Argon gas is introduced to provide a protective atmosphere and blow out the powder. The power switch and protective atmosphere valve of the powder feeder are turned on to fill the container with protective gas to prevent powder oxidation. The laser condenser circulating water system is turned on. When the water temperature rises to room temperature, the laser is turned on for positioning and the scanning path is set. The high-entropy alloy powder is transported under argon protection, and the laser cladding coating is printed.

[0073] The printer's processing precision is 1mm. The coaxial powder feeding 3D printing parameters were set as follows: laser power 900W, powder supply speed 3g / min, scanning speed 70%. The 3D printer was debugged to execute the NH-1 command to print a 30×15mm high-entropy alloy coating. Finally, a 4.8mm lightweight high-entropy alloy coating was obtained on the Q235 steel plate. After the coating printing was completed, the laser power was turned off, powder feeding was stopped, and the protective gas valve was closed. After the printed specimen cooled, samples were taken for processing, and XRD patterns were analyzed for phase structure. Figure 5 As shown, the microstructure is as follows Figure 6 As shown. Electrochemical performance characterization is as follows. Figure 7 As shown, the polarization curves and impedance diagrams of the alloy demonstrate the excellent performance of the alloy coating. Figure 8 As shown, the microhardness distribution curve of the high-entropy alloy laser cladding coating is shown. In this case, the alloy hardness can reach 680HV.

[0074] The above description is only the result of preferred implementation of the present invention. It should be noted that those skilled in the art can make several modifications and improvements without departing from the inventive concept of the present invention, and these all fall within the protection scope of the present invention.

Claims

1. A method for preparing a lightweight high-entropy alloy, characterized in that, Includes the following steps: (1) According to the following mass parts: Al: 29.4-41.3 parts, Fe: 15.3-20.6 parts, Cr: 14.2-19.2 parts, Mn: 14.9-20.2 parts, Ti: 0-26.1 parts, the above powder with a particle size of 50-100 μm is mixed evenly, loaded into a rod mill jar, and vacuumed to 1×10 -1 ~1×10 -2 Pa, the argon gas filling process is repeated twice, and then the vacuum is drawn again to press in n-heptane, wherein the mass fraction ratio of n-heptane to powder is 1:2-4, and finally argon gas is introduced until the tank is full; (2) The alloy powder is alloyed in a vibratory rod mill for 2-3 hours, and the mill jar is evacuated to 1 × 10⁻⁶. -2 Pa, industrial alcohol is introduced into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder is 10:(3-4), and grinding is continued for 10-12 minutes. Then the mixture of alloy powder and alcohol is taken out. (3) Let the extracted mixture stand for 15 to 25 hours and filter out the supernatant. Place it in a vacuum drying oven, where the vacuum of the drying oven is always maintained at 0.1 to 0.12 Pa and the temperature is maintained at 60°C to 65°C. Dry for 8 to 10 hours to obtain high-entropy alloy powder. Finally, vacuum seal the powder for storage. (4) Turn on the power of the vertical heating furnace and set the heating process: during the heating process from 50℃ to 1650℃, the heating rate is 5℃ / min~10℃ / min. After reaching the set temperature, keep it warm for 120~180 minutes. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder and use the nozzle to feed out the powder. The actual powder feeding rate of the powder feeder is 2g / min~2.4g / min. At the same time, the protective gas argon is introduced. (5) The powder is melted and solidified through a vertical long tube and falls into the bottom collection device. After all the powder has fallen into the collection device, the protective gas argon is continued to be introduced and the cooling circulation device is turned on. After the powder temperature drops to room temperature, the collection device is removed to obtain lightweight high-entropy alloy spherical powder.

2. The method for preparing a lightweight high-entropy alloy according to claim 1, characterized in that, Includes the following steps: (1) According to the following mass parts: Al: 33.9 parts, Fe: 17.6 parts, Cr: 16.3 parts, Mn: 17.2 parts, Ti: 15.0 parts, mix the above powders with a particle size of 50-100 μm evenly, put them into a rod mill jar, and evacuate to 1×10 -1 Pa, the argon gas filling process is repeated twice, and then the vacuum is drawn again to press in n-heptane, wherein the mass fraction ratio of n-heptane to powder is 1:3, and finally argon gas is introduced until the tank is full; (2) The alloy powder was alloyed in a vibratory rod mill for 3 hours, and the mill jar was evacuated to 1 × 10⁻⁶. -2 Pa, industrial alcohol is introduced into the rod mill jar, wherein the mass fraction ratio of industrial alcohol to metal powder is 10:

4. After grinding for 12 minutes, the mixture of alloy powder and alcohol is taken out. (3) The mixture was left to stand for 25 hours and the supernatant was filtered off. It was then placed in a vacuum drying oven, where the vacuum was always maintained at 0.12 Pa and the temperature was maintained at 60°C. The mixture was dried for 10 hours to obtain high-entropy alloy powder. Finally, the powder was vacuum-sealed and stored. (4) Turn on the power of the vertical heating furnace and set the heating process: the heating rate is 10℃ / min during the heating process from 50℃ to 1650℃. After reaching the set temperature, keep it warm for 180 minutes. Load the mechanically alloyed high-entropy powder obtained in step (3) into the powder feeder and use the nozzle to feed the powder. The actual powder feeding rate of the powder feeder is 2.4g / min. At the same time, the protective gas argon is introduced. (5) The powder is melted and solidified through a vertical long tube and falls into the bottom collection device. After all the powder has fallen into the collection device, the protective gas argon is continued to be introduced and the cooling circulation device is turned on. After the powder temperature drops to room temperature, the collection device is removed to obtain lightweight high-entropy alloy spherical powder.

Citation Information

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