Flower-like FeCoNiMnPt high-entropy magnetic alloy powder and preparation method thereof

The preparation of flower-like FeCoNiMnPt high-entropy magnetic alloy powder by hydrothermal method solves the problems of complex preparation process, high cost and low magnetic performance in the prior art, and realizes the preparation of high-performance powder with simple process, low cost and high production efficiency.

CN119794366AActive Publication Date: 2025-04-11WUHAN UNIV OF SCI & TECH

Patent Information

Application Number
CN202411985649.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-31
Publication Date
2025-04-11
Estimated Expiration
2044-12-31

AI Technical Summary

Technical Problem

The existing high-entropy magnetic alloy powder preparation technology has problems such as high cost, complex preparation process, and easy introduction of impurities. The prepared powder has a small specific surface area and a low saturation magnetization.

Method used

The flower-like FeCoNiMnPt high-entropy magnetic alloy powder was prepared by hydrothermal method. By dissolving metal precursors and other additives in oleamine, ultrasonic dispersion and high pressure reaction were carried out, and powders with large specific surface area and high saturation magnetization were prepared by combining hydrothermal conditions and inert gas heat treatment.

Benefits of technology

It realizes the preparation of high-entropy magnetic alloy powder with simple process, low cost and high production efficiency. The product has a large specific surface area and high saturation magnetization, which is suitable for large-scale production.

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Abstract

The invention relates to flower-like FeCoNiMnPt high-entropy magnetic alloy powder and a preparation method of the flower-like FeCoNiMnPt high-entropy magnetic alloy powder. According to the technical scheme, the preparation method comprises the following steps: respectively dissolving ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at equal concentration, and carrying out ultrasonic dispersion to obtain a solution A; respectively dissolving octadecyl trimethyl ammonium bromide and glucose in the solution A at equal concentration, carrying out ultrasonic dispersion, adding the obtained solution B into a sealed container, putting the sealed container into a high-pressure reaction kettle, putting the high-pressure reaction kettle into a hydrothermal oven, carrying out heat preservation and cooling, and taking out the sealed container; the obtained solution C is subjected to centrifugal treatment, washing, drying and cooling, and magnetic alloy powder is obtained; and placing the crucible filled with the magnetic alloy powder in a tubular atmosphere furnace, preserving heat at 450-650 DEG C, and cooling to obtain the flower-like FeCoNiMnPt high-entropy magnetic alloy powder. The preparation method is simple in process, low in cost and high in production efficiency, and the prepared product is large in specific surface area and high in saturation magnetization.
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Description

Technical Field

[0001] The present invention belongs to the technical field of high entropy magnetic alloy powders, and specifically relates to a flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. Background Art

[0002] High entropy magnetic alloys are alloys composed of five or more elements in equiatomic ratios or near equiatomic ratios. The alloys are widely used in aerospace, automotive, catalyst, biomedical and other fields due to their excellent magnetic properties. Since the current preparation process of high entropy magnetic alloy powders is complex and has a small specific surface area, the small specific surface area is not conducive to enhancing magnetic properties such as magnetic anisotropy, coercive force and saturation magnetization. Therefore, the development of high entropy magnetic alloy powders with high specific surface area has attracted people's attention.

[0003] The patented technology of "A FeCoNiMo high entropy alloy powder oxygen evolution catalyst and its preparation method" (CN114150330A) first places Fe, Co, Ni and Mo metal blocks into a vacuum arc melting furnace, and performs multiple smelting under a protective atmosphere to obtain a FeCoNiMo alloy ingot with uniform composition; then the alloy ingot is placed in a vacuum induction melting gas atomization powder making equipment to melt the alloy, and when the alloy liquid flows into the atomization chamber for gas atomization dispersion, alloy powder is obtained after cooling, and finally the powder is graded and screened. Although the FeCoNiMo high entropy alloy powder product is obtained, the cost is high and the preparation process is complicated.

[0004] The patented technology of "Method for preparing high entropy alloy type electrocatalytic oxygen evolution reaction catalyst by high energy ball milling" (CN110079824B) is to mix magnetic metal powders in an equal atomic mass ratio or a near atomic mass ratio, and use a high energy ball mill to obtain a uniformly dispersed two-phase metal solid solution flaky powder after a long period of ball milling. However, there is a serious cold welding phenomenon between the powder and the ball mill jar and the grinding balls, which is easy to introduce impurities, resulting in low saturation magnetization intensity.

[0005] The patented technology of "A preparation method and application of a high entropy alloy catalyst" (CN117696071A) uses an aqueous solution to prepare a colloidal polymer nanoplate precursor, then weighs five or more different metal salts and dissolves them in a solvent, adds them dropwise to the precursor and grinds them, and finally calcines and cools them to obtain a high entropy magnetic alloy. The powder prepared by this method has a small specific surface area.

[0006] In summary, the existing preparation technology of high entropy magnetic alloy powder has problems such as high cost, complex preparation process, and easy introduction of impurities. In addition, the prepared high entropy magnetic alloy powder has a small specific surface area and low saturation magnetization intensity. Summary of the invention

[0007] The present invention aims to overcome the shortcomings of the prior art and aims to provide a method for preparing flower-shaped FeCoNiMnPt high entropy magnetic alloy powder with simple process, low cost and high production efficiency. The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared by the method has a large specific surface area and a high saturation magnetization intensity.

[0008] To achieve the above purpose, the specific steps of the technical solution adopted by the present invention are:

[0009] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.002-0.01 mol / L, respectively, and perform ultrasonic dispersion at room temperature for 40-80 min to obtain solution A.

[0010] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.004-0.02 mol / L, respectively, and perform ultrasonic dispersion for 20-40 min at room temperature to obtain a solution B.

[0011] Step 3, according to the solution B accounting for 40-70% of the volume of the sealed container, the solution B is added into the sealed container; the sealed container is then placed into a high-pressure reactor, and then the high-pressure reactor is placed in a hydrothermal oven, kept warm at 140-240° C. for 6-18 hours, and naturally cooled to room temperature; the sealed container in the high-pressure reactor is taken out to obtain solution C.

[0012] Step 4: centrifuge the solution C at 3000-8000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 3-4 times; dry it at 50-60° C. for 6-12 hours, and cool it naturally to obtain magnetic alloy powder.

[0013] Step 5, placing the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 450-650° C. at a rate of 2-10° C. in an inert gas, keeping the temperature for 2-4 hours, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0014] The purity of the iron acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate is ≥98%.

[0015] The purity of the oleylamine is 80-90%.

[0016] The purity of the octadecyltrimethylammonium bromide is ≥98%.

[0017] The purity of the glucose is ≥98%.

[0018] The material of the sealed container is polytetrafluoroethylene.

[0019] The inert gas is argon or nitrogen.

[0020] Due to the adoption of the above technical solution, the present invention has the following positive effects compared with the prior art:

[0021] 1. The present invention adds the prepared solution B into a sealed container, places it in a high-pressure reactor, puts it into a hydrothermal oven, keeps it warm, cools it naturally, centrifuges it, washes it, dries it, and heat-treats it under inert gas conditions to obtain a flower-shaped FeCoNiMnPt high-entropy magnetic alloy powder. The raw materials used in the present invention are easy to obtain, do not require complex and expensive equipment, have low production costs, and have a simple preparation process.

[0022] 2. The present invention adopts a hydrothermal method and selects oleylamine with a long-chain alkyl structure as a solvent. Its amino group (-NH2) coordinates with the metal precursor to stabilize the metal ions and prevent premature reduction to form an alloy with uneven composition. In a closed container, the temperature rises and the pressure increases, and octadecyltrimethylammonium bromide self-assembles and aggregates to form a flower-shaped template. Its positively charged trimethylammonium group interacts electrostatically with the metal ions in the solution, promoting the enrichment of metal ions on the template surface. Glucose has reducing properties and slowly reduces metal ions to alloys. Finally, the stability of the flower-like structure is improved by heat treatment to prevent deformation or collapse. The flower-like structure is composed of multiple sheet structures, which can significantly increase the specific surface area; the magnetic grains are arranged in a specific direction, and when the magnetization direction is consistent with the easy magnetization direction of the grains, the magnetization is more likely to reach saturation. The components contain a large amount of magnetic elements such as iron, cobalt and nickel, which improve the saturation magnetization intensity of the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder. After detection, the saturation magnetization intensity is 128.3-138.2emu / g. Therefore, the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared by the present invention has a large specific surface area and a high saturation magnetization intensity.

[0023] 3. The present invention can control the output of high entropy magnetic alloy powder by changing the size of the closed container, which is suitable for large-scale production. By changing the reaction temperature and time, the production speed of high entropy magnetic alloy powder can be increased, so the production efficiency of the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared by the present invention is high.

[0024] Therefore, the present invention has the characteristics of simple process, low cost and high production efficiency, and the prepared flower-shaped FeCoNiMnPt high-entropy magnetic alloy powder has a large specific surface area and a high saturation magnetization intensity. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1This is an XRD diagram of a flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared by the present invention;

[0026] Figure 2 for Figure 1 SEM image of flower-shaped FeCoNiMnPt high entropy magnetic alloy powder shown;

[0027] Figure 3 for Figure 1 VSM diagram of flower-shaped FeCoNiMnPt high entropy magnetic alloy powder shown. DETAILED DESCRIPTION

[0028] The present invention is further described below in conjunction with the accompanying drawings and specific implementation methods, but is not intended to limit the scope of protection thereof.

[0029] A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. The specific method described in this specific embodiment comprises the following steps:

[0030] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.002-0.01 mol / L, respectively, and perform ultrasonic dispersion at room temperature for 40-80 min to obtain solution A.

[0031] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.004-0.02 mol / L, respectively, and perform ultrasonic dispersion for 20-40 min at room temperature to obtain a solution B.

[0032] Step 3, according to the solution B accounting for 40-70% of the volume of the sealed container, the solution B is added into the sealed container; the sealed container is then placed into a high-pressure reactor, and then the high-pressure reactor is placed in a hydrothermal oven, kept warm at 140-240° C. for 6-18 hours, and naturally cooled to room temperature; the sealed container in the high-pressure reactor is taken out to obtain solution C.

[0033] Step 4: centrifuge the solution C at 3000-8000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 3-4 times; dry it at 50-60° C. for 6-12 hours, and cool it naturally to obtain magnetic alloy powder.

[0034] Step 5, placing the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 450-650° C. at a rate of 2-10° C. in an inert gas, keeping the temperature for 2-4 hours, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0035] The inert gas is argon or nitrogen.

[0036] In this specific implementation mode:

[0037] The purity of the iron acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate is ≥ 98%;

[0038] The purity of the oleylamine is 80-90%;

[0039] The purity of the octadecyltrimethylammonium bromide is ≥98%;

[0040] The purity of the glucose is ≥98%;

[0041] The material of the sealed container is polytetrafluoroethylene.

[0042] This will not be described in detail in the embodiments.

[0043] Example 1

[0044] A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. The specific method described in this embodiment comprises the following steps:

[0045] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.006 mol / L, and perform ultrasonic dispersion for 60 min at room temperature to obtain solution A.

[0046] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.01 mol / L, respectively, and perform ultrasonic dispersion for 30 min at room temperature to obtain a solution B.

[0047] Step 3, according to the solution B accounting for 60% of the volume of the sealed container, the solution B is added into the sealed container; then the sealed container is placed in a high-pressure reactor, and then the high-pressure reactor is placed in a hydrothermal oven, kept warm at 200° C. for 12 hours, and naturally cooled to room temperature; take out the sealed container in the high-pressure reactor to obtain solution C.

[0048] Step 4: centrifuge the solution C at 6000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 3 times; dry it at 55° C. for 9 hours, and cool it naturally to obtain magnetic alloy powder.

[0049] Step 5, putting the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 550° C. at a rate of 6° C. in an inert gas, keeping warm for 3 hours, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0050] The inert gas is argon.

[0051] The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in this embodiment was tested and the saturation magnetization intensity was 138.2emu / g.

[0052] Example 2

[0053] A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. The specific method described in this embodiment comprises the following steps:

[0054] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.002 mol / L, and perform ultrasonic dispersion at room temperature for 40 min to obtain solution A.

[0055] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.004 mol / L, respectively, and perform ultrasonic dispersion for 20 min at room temperature to obtain a solution B.

[0056] Step 3, adding the solution B into the sealed container according to the solution B accounting for 40% of the volume of the sealed container; then placing the sealed container into a high-pressure reactor, and then placing the high-pressure reactor in a hydrothermal oven, keeping warm at 140° C. for 6 hours, and naturally cooling to room temperature; taking out the sealed container in the high-pressure reactor to obtain solution C.

[0057] Step 4: centrifuge the solution C at 3000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 3 times; dry it at 50° C. for 6 hours, and cool it naturally to obtain magnetic alloy powder.

[0058] Step 5, putting the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 450° C. at a rate of 2° C. in an inert gas, keeping the temperature for 2 h, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0059] The inert gas is nitrogen.

[0060] The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in this embodiment was tested and the saturation magnetization intensity was 135.6emu / g.

[0061] Example 3

[0062] A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. The specific method described in this embodiment comprises the following steps:

[0063] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.004 mol / L, and perform ultrasonic dispersion at room temperature for 50 min to obtain solution A.

[0064] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.008 mol / L, respectively, and perform ultrasonic dispersion for 25 min at room temperature to obtain a solution B.

[0065] Step 3, according to the solution B accounting for 50% of the volume of the sealed container, the solution B is added into the sealed container; then the sealed container is placed in a high-pressure reactor, and then the high-pressure reactor is placed in a hydrothermal oven, kept warm at 180° C. for 9 hours, and naturally cooled to room temperature; take out the sealed container in the high-pressure reactor to obtain solution C.

[0066] Step 4: centrifuge the solution C at 5000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 3 times; dry it at 53° C. for 8 hours, and cool it naturally to obtain magnetic alloy powder.

[0067] Step 5, putting the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 500° C. at a rate of 4° C. in an inert gas, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0068] The inert gas is nitrogen.

[0069] The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in this embodiment was tested and the saturation magnetization intensity was 133.4emu / g.

[0070] Example 4

[0071] A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. The specific method described in this embodiment comprises the following steps:

[0072] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.01 mol / L, and perform ultrasonic dispersion at room temperature for 80 min to obtain solution A.

[0073] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.02 mol / L, respectively, and perform ultrasonic dispersion for 40 min at room temperature to obtain a solution B.

[0074] Step 3, according to the solution B accounting for 70% of the volume of the sealed container, the solution B is added into the sealed container; then the sealed container is placed in a high-pressure reactor, and then the high-pressure reactor is placed in a hydrothermal oven, kept warm at 240° C. for 18 hours, and naturally cooled to room temperature; take out the sealed container in the high-pressure reactor to obtain solution C.

[0075] Step 4: centrifuge the solution C at 8000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 4 times; dry it at 60° C. for 12 hours, and cool it naturally to obtain magnetic alloy powder.

[0076] Step 5, putting the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 650° C. at a rate of 10° C. in an inert gas, keeping warm for 4 hours, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0077] The inert gas is argon.

[0078] The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in this embodiment was tested and the saturation magnetization intensity was 132.8emu / g.

[0079] Example 5

[0080] A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder and a preparation method thereof. The specific method described in this embodiment comprises the following steps:

[0081] Step 1: dissolve ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.008 mol / L, and perform ultrasonic dispersion for 70 min at room temperature to obtain solution A.

[0082] Step 2: Dissolve octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.015 mol / L, respectively, and perform ultrasonic dispersion for 35 min at room temperature to obtain a solution B.

[0083] Step 3, according to the solution B accounting for 65% of the volume of the sealed container, the solution B is added into the sealed container; then the sealed container is placed in a high-pressure reactor, and then the high-pressure reactor is placed in a hydrothermal oven, kept warm at 220° C. for 15 hours, and naturally cooled to room temperature; take out the sealed container in the high-pressure reactor to obtain solution C.

[0084] Step 4: centrifuge the solution C at 7000 r / min and room temperature, wash it alternately with deionized water and anhydrous ethanol for 4 times; dry it at 58° C. for 10 hours, and cool it naturally to obtain magnetic alloy powder.

[0085] Step 5: Place the magnetic alloy powder into a crucible, place the crucible in a tubular atmosphere furnace, heat the mixture to 600° C. at a rate of 8° C. in an inert gas, keep the mixture for 3 h, and cool the mixture naturally to room temperature to obtain a flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

[0086] The inert gas is argon.

[0087] The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in this embodiment was tested and the saturation magnetization intensity was 128.3emu / g.

[0088] Compared with the prior art, this specific implementation has the following positive effects:

[0089] 1. In this specific embodiment, the prepared solution B is added to a sealed container, placed in a high-pressure reactor, placed in a hydrothermal oven, kept warm, naturally cooled, centrifuged, washed, dried, and heat-treated under inert gas conditions to obtain a flower-shaped FeCoNiMnPt high-entropy magnetic alloy powder. The raw materials used in this specific embodiment are easy to obtain, do not require complex and expensive equipment, have low production costs, and have a simple preparation process.

[0090] 2. This specific embodiment adopts a hydrothermal method, and selects oleylamine with a long-chain alkyl structure as a solvent. Its amino group (-NH2) coordinates with the metal precursor to stabilize the metal ions and prevent premature reduction to form an alloy with uneven composition. In a closed container, the temperature rises, the pressure increases, and octadecyl trimethyl ammonium bromide self-assembles and aggregates to form a flower-shaped template. Its positively charged trimethyl ammonium group interacts electrostatically with the metal ions in the solution, promoting the enrichment of metal ions on the template surface. Glucose has reducing properties, slowly reducing metal ions to alloys, and finally improving the stability of the flower-like structure through heat treatment to prevent deformation or collapse. The flower-like structure is composed of multiple sheet structures, which can significantly increase the specific surface area; the magnetic grains are arranged in a specific direction, and when the magnetization direction is consistent with the easy magnetization direction of the grains, the magnetization is more likely to reach saturation. And the components have a large amount of magnetic elements such as iron, cobalt and nickel, which improves the saturation magnetization intensity of the flower-like FeCoNiMnPt high entropy magnetic alloy powder.

[0091] The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in this specific embodiment is shown in the accompanying drawings. Figure 1 The XRD pattern of the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared in Example 1; Figure 2 for Figure 1 SEM image of flower-shaped FeCoNiMnPt high entropy magnetic alloy powder shown; Figure 3 for Figure 1 The VSM diagram of the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder is shown in Figure 1. Figure 1 It can be seen that the flower-like FeCoNiMnPt high entropy magnetic alloy powder has two physical structures: face-centered cubic and body-centered cubic. The formation of body-centered cubic structure is beneficial to the improvement of magnetic properties. Figure 2 It can be seen that the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder is formed by combining multiple flakes together to form a flower-shaped structure, with uniform particle size and large specific surface area. Figure 3 It can be seen that the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder exhibits typical soft magnetic material properties. Since the components contain a large amount of magnetic elements and the magnetic grains on the flower-shaped structure are arranged in a specific direction, the prepared flower-shaped FeCoNiMnPt high entropy magnetic alloy powder is tested to have a saturation magnetization of 128.3 to 138.2emu / g. Therefore, this specific embodiment has a large specific surface area and a high saturation magnetization.

[0092] 3. This specific embodiment can control the output of high entropy magnetic alloy powder by changing the size of the closed container, and is suitable for large-scale production. By changing the reaction temperature and time, the production speed of the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder can be increased, so the production efficiency of the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder prepared by this specific embodiment is high. Therefore, this specific embodiment has the characteristics of simple process, low cost and high production efficiency, and the prepared flower-shaped FeCoNiMnPt high entropy magnetic alloy powder has a large specific surface area and a high saturation magnetization.

Claims

1. A method for preparing flower-shaped FeCoNiMnPt high entropy magnetic alloy powder, characterized in that: The specific steps of the preparation method are: Step 1, dissolving ferric acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate in oleylamine at a concentration of 0.002-0.01 mol / L, respectively, and dispersing by ultrasonication at room temperature for 40-80 min to obtain solution A; Step 2, dissolving octadecyltrimethylammonium bromide and glucose in the solution A at a concentration of 0.004-0.02 mol / L, respectively, and ultrasonically dispersing for 20-40 min at room temperature to obtain a solution B; Step 3, adding the solution B into the sealed container according to the solution B accounting for 40-70% of the volume of the sealed container; then placing the sealed container into a high-pressure reactor, and then placing the high-pressure reactor in a hydrothermal oven, keeping the temperature at 140-240° C. for 6-18 hours, and naturally cooling to room temperature; taking out the sealed container in the high-pressure reactor to obtain solution C; Step 4, centrifuging the solution C at 3000-8000 r / min and room temperature, washing with deionized water and anhydrous ethanol alternately for 3-4 times; drying at 50-60° C. for 6-12 hours, and cooling naturally to obtain magnetic alloy powder; Step 5, placing the magnetic alloy powder into a crucible, placing the crucible in a tubular atmosphere furnace, heating to 450-650° C. at a rate of 2-10° C. in an inert gas, keeping the temperature for 2-4 hours, and naturally cooling to room temperature to obtain flower-shaped FeCoNiMnPt high entropy magnetic alloy powder.

2. The method for preparing flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to claim 1, characterized in that: The purity of the iron acetylacetonate, cobalt acetylacetonate, nickel acetylacetonate, manganese acetylacetonate and platinum acetylacetonate is ≥98%.

3. The method for preparing the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to claim 1, characterized in that: The purity of the oleylamine is 80-90%.

4. The method for preparing the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to claim 1, characterized in that: The purity of the octadecyltrimethylammonium bromide is ≥98%.

5. The method for preparing flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to claim 1, characterized in that: The purity of the glucose is ≥98%.

6. The method for preparing flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to claim 1, characterized in that: The material of the sealed container is polytetrafluoroethylene.

7. The method for preparing flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to claim 1, characterized in that: The inert gas is argon or nitrogen.

8. A flower-shaped FeCoNiMnPt high entropy magnetic alloy powder, characterized in that The flower-shaped FeCoNiMnPt high entropy magnetic alloy powder is prepared by the method for preparing the flower-shaped FeCoNiMnPt high entropy magnetic alloy powder according to any one of claims 1 to 7.

Citation Information

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