Method for synthesizing metal alloy material
The preparation of spherical metal alloy materials by hydrothermal reaction solves the problems of uneven composition and high cost in traditional methods, and realizes the preparation of metal alloy materials with low cost and low energy consumption, which is suitable for consumer electronics, shipbuilding and aerospace fields.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- BEIJING TANTALUM & TITANIUM PRECISION TECHNOLOGY CO LTD
- Filing Date
- 2026-01-23
- Publication Date
- 2026-04-10
AI Technical Summary
Existing methods for preparing metal alloy materials are difficult to achieve compositional uniformity and microstructure control under mild conditions, and are also costly, have poor repeatability, and are difficult to apply on a large scale.
Spherical metal alloy materials were prepared by uniformly mixing solvent, surfactant, metal salt and reducing agent and then carrying out hydrothermal reaction, followed by separation, washing and drying.
The mass production of various metal alloy materials was achieved under mild conditions, resulting in low cost, reduced emissions of waste, and uniform microstructure, making them suitable for consumer electronics, shipbuilding, and aerospace applications.
Smart Images
Figure CN121820685A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of metal alloy materials, and specifically relates to a method for synthesizing metal alloy materials. Background Technology
[0002] Precise control of the composition and uniformity of the microstructure of metallic alloys are crucial for their application in high-end manufacturing. Traditional preparation methods, such as melting and mechanical alloying, are prone to problems such as compositional segregation and uneven grain size, and are energy-intensive, complex, and difficult to control precisely on the composition and morphology of the alloy. In recent years, liquid-phase chemical synthesis has provided a new approach for alloy preparation, but it still has significant limitations. For example, differences in reduction kinetics between multiple metal ions can easily lead to phase separation, making it difficult to obtain a homogeneous solid solution. Insufficient control of nucleation and growth during synthesis often results in particle agglomeration, wide size distribution, and irregular morphology, affecting subsequent processing performance. In addition, existing methods often rely on noble metal catalysts, high temperature and pressure, or complex organic ligands, which are costly and have poor reproducibility, restricting their large-scale application. Therefore, developing a method for synthesizing metallic alloys under mild conditions is of significant scientific importance. Summary of the Invention
[0003] The technical problem to be solved by this invention is how to synthesize metal alloy materials under mild conditions.
[0004] The present invention solves the above-mentioned technical problems through the following technical means: This invention provides a method for synthesizing metal alloy materials. A solvent, surfactant, first metal salt, second metal salt, and reducing agent are mixed evenly in a mass ratio of 20:0.0001~0.00001:0.5:0.5:0.04 to obtain a metal salt precursor solution. The metal salt precursor solution is placed in a reaction vessel for hydrothermal reaction, followed by separation, washing, and drying to obtain the metal alloy material.
[0005] Beneficial effects: This invention achieves the synthesis of metal alloy materials through hydrothermal reaction of metal salt precursor solution, and obtains metal alloy materials with spherical microstructure under mild conditions. The metal alloy materials can be used in consumer electronics, shipbuilding and aerospace fields.
[0006] Preferably, the first metal salt is an iron salt; the second metal salt is a cobalt salt or a nickel salt.
[0007] Preferably, the temperature of the hydrothermal reaction is 100~150℃.
[0008] Preferably, the hydrothermal reaction time is 360~730 min.
[0009] Preferably, the solvent includes one or more of dimethylformamide and dimethylacetamide.
[0010] Preferably, the surfactant is one or more of hexadecyltrimethylammonium bromide, sodium hexadecyl sulfonate, and polyvinylpyrrolidone.
[0011] Preferably, the reducing agent is one or more of ascorbic acid, sodium borohydride, and hydrazine hydrate.
[0012] Preferably, the mixing method includes one of stirring, ultrasonication, or vibration.
[0013] Preferably, the separation method is filtration or centrifugation.
[0014] Preferably, the washing reagent includes one or more of N,N-dimethylformamide and ethanol.
[0015] Preferred drying conditions: vacuum drying at 60°C for 8-24 hours.
[0016] The beneficial effects of this invention are: The method of the present invention can realize the preparation of a variety of metal alloy materials. The method is low-cost, mild, and can be mass-produced. The solution medium can be recycled and reused, effectively reducing the discharge of waste gas, wastewater, and solid waste. Attached Figure Description
[0017] Figure 1 This is a scanning electron microscope image of the iron-nickel alloy material of Example 1 of the present invention; Figure 2 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 2 of the present invention; Figure 3 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 3 of the present invention; Figure 4 This is a scanning electron microscope image of the iron-cobalt alloy material in Example 4 of the present invention; Figure 5 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 5 of the present invention; Figure 6 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 6 of the present invention; Figure 7 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 7 of the present invention; Figure 8 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 7 of the present invention; Figure 9 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 8 of the present invention; Figure 10 This is a scanning electron microscope image of the iron-cobalt alloy material of Example 10 of the present invention; Figure 11 This is a scanning electron microscope image of the iron-cobalt alloy material of Comparative Example 1 of the present invention; Figure 12 This is a scanning electron microscope image of the iron-cobalt alloy material of Comparative Example 2 of the present invention. Detailed Implementation
[0018] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0019] Unless otherwise specified, all test materials and reagents used in the following examples are commercially available.
[0020] Unless otherwise specified in the embodiments, the techniques or conditions described in the literature in this field or in accordance with the product manual may be followed.
[0021] Example 1 This embodiment provides a method for synthesizing metallic alloy materials, specifically iron-nickel alloy materials, including the following steps: (1) Dimethylformamide, sodium dodecyl sulfate, ferric chloride, nickel chloride and ascorbic acid are mixed in a mass ratio of 20:0.00001:0.5:0.5:0.04 and ultrasonicated until uniformly dispersed to obtain a metal salt precursor solution.
[0022] (2) Then the metal salt precursor solution was placed in a hydrothermal reactor for hydrothermal reaction. The reaction temperature was controlled at 120℃ and the reaction time was 720 min. Finally, the product was obtained.
[0023] (3) The product is placed on a microporous filter membrane (pore size of 0.22 μm) and filtered and separated by negative pressure to obtain powder. Ethanol is used as washing liquid to wash the powder at least 5 times. The washed powder is then vacuum dried at 60°C for 12 h to obtain the iron-nickel alloy material.
[0024] The microstructure of the iron-nickel alloy material prepared in this embodiment is as follows: Figure 1 As shown, the microstructure of the iron-nickel alloy material is a spherical structure with uniform particle size. The iron-nickel alloy material can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0025] Example 2 This embodiment provides a method for synthesizing metallic alloy materials, specifically iron-cobalt alloy materials, including the following steps: (1) Dimethylformamide, sodium dodecyl sulfate, ferric nitrate, cobalt nitrate and ascorbic acid are mixed in a mass ratio of 20:0.00001:0.5:0.5:0.04 and ultrasonicated until uniformly dispersed to obtain a metal salt precursor solution.
[0026] (2) Then the metal salt precursor solution was placed in a hydrothermal reactor for hydrothermal reaction. The reaction temperature was controlled at 120℃ and the reaction time was 720 min. Finally, the product was obtained.
[0027] (3) The product is placed on a microporous filter membrane (pore size of 0.22 μm) and filtered and separated by negative pressure to obtain powder. Ethanol is used as washing liquid to wash the powder at least 5 times. The washed powder is then vacuum dried at 60°C for 12 h to obtain iron-cobalt alloy material.
[0028] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 2 As shown, the microstructure of the iron-cobalt alloy material is a spherical structure with uniform particle size. The iron-cobalt alloy material can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0029] Example 3 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Embodiment 2 is that dimethylformamide is replaced with dimethylacetamide, while all other aspects remain the same.
[0030] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 3 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0031] Example 4 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Example 2 is that sodium dodecyl sulfonate is replaced with hexadecyltrimethylammonium bromide, while all other aspects remain the same.
[0032] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 4 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0033] Example 5 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Embodiment 2 is that sodium hexadecyl sulfonate is replaced with polyvinylpyrrolidone, while all other aspects remain the same.
[0034] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 5 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0035] Example 6 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Embodiment 2 is that ascorbic acid is replaced with sodium borohydride, while all other aspects remain the same.
[0036] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 6 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0037] Example 7 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Embodiment 2 is that ascorbic acid is replaced with hydrazine hydrate, while all other aspects are the same.
[0038] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 7 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0039] Example 8 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Embodiment 2 is that the reaction temperature of 120°C is replaced with 100°C, while all other aspects remain the same.
[0040] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 8 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0041] Example 9 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Embodiment 2 is that the reaction temperature of 120°C is replaced with 150°C, while all other aspects remain the same.
[0042] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 9 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0043] Example 10 This embodiment provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this embodiment and Example 2 is that dimethylformamide, sodium dodecyl sulfate, ferric nitrate, cobalt nitrate, and ascorbic acid are mixed in a mass ratio of 20:0.0001:0.5:0.5:0.04, while all other aspects remain the same.
[0044] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 10 As shown, the microstructure of the iron-cobalt alloy material is spherical, and it can be used in consumer electronics, shipbuilding, aerospace and other fields.
[0045] Comparative Example 1 This comparative example provides a method for synthesizing metallic alloy materials, specifically iron-cobalt alloy materials, including the following steps: (1) Mix dimethylformamide, sodium dodecyl sulfate, ferric nitrate, cobalt nitrate and ascorbic acid in a mass ratio of 20:0.002:0.5:0.5:0.04 and sonicate until uniformly dispersed to obtain a metal salt precursor solution.
[0046] (2) Then the metal salt precursor solution was placed in a hydrothermal reactor for hydrothermal reaction. The reaction temperature was controlled at 120℃ and the reaction time was 720 min. Finally, the product was obtained.
[0047] (3) The product is placed on a microporous filter membrane (pore size of 0.22 μm) and filtered and separated by negative pressure to obtain powder. Ethanol is used as washing liquid to wash the powder at least 5 times. The washed powder is then vacuum dried at 60°C for 12 h to obtain the iron-nickel alloy material.
[0048] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 11 As shown, the addition of excessive surfactants to the metal salt precursor solution prevented the iron-cobalt alloy material from forming a spherical microstructure.
[0049] Comparative Example 2 This comparative example provides a method for synthesizing metal alloy materials, specifically iron-cobalt alloy materials. The difference between this comparative example and Example 2 is that no surfactant was added in step (1), while all other aspects are the same.
[0050] The microstructure of the iron-cobalt alloy material prepared in this embodiment is as follows: Figure 12 As shown, the lack of surfactant in the metal salt precursor solution prevents the formation of spherical microstructures in the cobalt-nickel alloy material.
[0051] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for synthesizing metallic alloy materials, characterized in that, Includes the following steps: Solvent, surfactant, first metal salt, second metal salt and reducing agent are mixed evenly in a mass ratio of 20:0.0001~0.00001:0.5:0.5:0.04 to obtain a metal salt precursor solution. The metal salt precursor solution is placed in a reaction vessel for hydrothermal reaction, and then separated, washed and dried to obtain metal alloy material.
2. The method for synthesizing metallic alloy materials according to claim 1, characterized in that, The first metal salt is an iron salt, and the second metal salt is a cobalt salt or a nickel salt.
3. In the method for synthesizing metal alloy materials according to claim 1, the hydrothermal reaction temperature is 100~150℃; the hydrothermal reaction time is 360~730min.
4. The method for synthesizing metal alloy materials according to claim 1, wherein the solvent includes one or more of dimethylformamide and dimethylacetamide.
5. In the method for synthesizing metal alloy materials according to claim 1, the surfactant is one or more of hexadecyltrimethylammonium bromide, sodium hexadecyl sulfonate, and polyvinylpyrrolidone.
6. The method for synthesizing metal alloy materials according to claim 1, wherein the reducing agent is one or more of ascorbic acid, sodium borohydride, and hydrazine hydrate.
7. The method for synthesizing metallic alloy materials according to claim 1, wherein the mixing method includes one of stirring, ultrasonication, or vibration.
8. The method for synthesizing metal alloy materials according to claim 1, wherein the separation method is filtration or centrifugation.
9. The method for synthesizing metal alloy materials according to claim 1, wherein the washing reagent includes one or more of N,N-dimethylformamide and ethanol.
10. The method for synthesizing metal alloy materials according to claim 1, wherein the drying conditions are: vacuum drying at 60°C for 8-24 hours.