A method for homogenizing a chemically synthesized multi-component alloy

By using chemical synthesis methods for MOF materials, the problem of uneven mixing of multi-component alloying elements has been solved, achieving atomic-level uniform mixing, which improves the performance of the alloy, reduces the preparation cost, and simplifies the process.

CN117161397BActive Publication Date: 2026-01-27XI AN JIAOTONG UNIV
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Patent Information

Application Number
CN202311146809.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-06
Publication Date
2026-01-27
Estimated Expiration
2043-09-06

AI Technical Summary

Technical Problem

Existing alloying methods struggle to achieve homogenization of multi-component alloying elements, especially in high-entropy alloys. Traditional methods suffer from problems such as pollution, complex equipment, high cost, and uneven mixing.

Method used

The chemical synthesis method of MOF materials is adopted. Powder is prepared by mixing ammonium molybdate and ammonium tungstate with polyethyleneimine, followed by ultrasonic stirring and rotary evaporation. Then, hot pressing and thermal processing are carried out under vacuum conditions to achieve uniform mixing of elements at the atomic scale.

Benefits of technology

This technology enables atomic-level mixing of multiple alloying elements, improving alloy uniformity and tensile strength, reducing preparation costs and environmental pollution, and simplifying the process.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a method for homogenizing a chemical synthetic multi-component alloy, and the method comprises the following steps: dissolving ammonium molybdate and ammonium tungstate in deionized water to obtain a mixed solution of ammonium molybdate and ammonium tungstate; dissolving polyethyleneimine in deionized water to obtain a polyethyleneimine solution; adding the polyethyleneimine solution into the mixed solution of ammonium molybdate and ammonium tungstate to uniformly disperse the precipitate; completely evaporating the solvent by using a rotary evaporation method to obtain a powder; performing secondary reduction on the powder to obtain a reduced powder; sintering the reduced powder in a graphite mold; heating the sintered product to 1500-1600 DEG C by using a medium-frequency induction furnace, extruding the sintered product on a horizontal extruder, naturally cooling the sintered product, and then annealing the sintered product at 1300-1400 DEG C. Compared with solid-state mixing, the method can save a mechanical alloying process and reduce sintering forming power in solidification forming; compared with liquid-phase mixing, the method can improve the uniformity of element mixing; compared with gas-phase mixing, the method can improve material utilization, reduce preparation cost and homogenization difficulty, and has no environmental pollution.
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Description

Technical Field

[0001] This invention relates to a method for alloy homogenization, and more particularly to a method for homogenizing chemically synthesized component alloys. Background Technology

[0002] Metal alloying is a primary method for enhancing and improving the properties of metallic materials, including strength, toughness, wear resistance, corrosion resistance, oxidation resistance, and electrothermal properties. With the increasing number of alloying elements and the emergence of high-entropy alloys, the types and quantities of alloying components added have significantly increased, and the degree of homogenization of alloying elements has an increasingly significant impact on the performance of alloy materials. Currently, the preparation process of multi-component alloys is mainly divided into solid-state mixing, liquid-phase mixing, and gas-state mixing based on the element mixing method. Liquid-phase melting and casting can prepare various metallic materials, resulting in alloy grain sizes ranging from tens to hundreds of micrometers. However, it has poor adaptability for multi-element mixing with significant differences in melting point, density, and segregation. Unlike liquid-phase melting and casting, solid-phase mixing using powder metallurgy can achieve low-temperature sintering, effectively suppressing alloy compositional segregation, preventing dendrite formation and multiphase precipitation, and ultimately obtaining a block alloy with a uniform phase structure. This method is particularly suitable for alloying elements with significantly different thermal properties, thus becoming a very important alloying method. Currently, a significant portion of the components in high-entropy alloys are mixed through the preparation of pre-alloyed powders. One of the main methods for pre-alloying powders is high-energy ball milling. Essentially, this involves mixing and dissolving powders of different elements through crushing, cold welding, and re-crushing processes during high-energy ball milling. However, due to the large number of elements and the varying powder characteristics and physicochemical properties, achieving complete homogenization is extremely difficult. This limits the potential performance of high-entropy alloys. Furthermore, powders are easily contaminated during ball milling; grinding balls, container walls, milling media, and process control agents can all contaminate the sample, generating harmful impurities that affect the mechanical properties of high-entropy alloys. Gas-state mixing is the most ideal method for element mixing, significantly improving the uniformity of alloying element distribution. There are three main methods: first, metal vapor mixing, which is difficult to homogenize due to the high boiling points of general metal materials and varying deposition conditions; second, some metal fluorides, halides, and carbonyl compounds exist in gaseous form, allowing for atomic-level mixing. However, these gases require sophisticated equipment and environmental conditions, making industrial application difficult; and third, vacuum sputtering of metal targets is also a method for homogenizing different elements. However, not only are the material requirements high, but the sputtering volume is also limited, which is quite restrictive.

[0003] Multi-element metal alloys possess a variety of superior properties and have become the mainstream of modern materials. Especially with the continuous development of entropy increase, the formation of multi-element high-entropy alloys has placed higher demands on alloy homogenization. However, traditional alloying methods—casting and powder metallurgy—each have certain problems, making it very difficult to achieve homogenization of alloying elements. To achieve the goal of homogenization of alloying elements, efforts have been made to overcome the limitations of micron-sized particles in solid-solid doping and explore atomized and ionized doping methods. Industry professionals have invented various mixing methods, mainly including liquid-phase coprecipitation, chemical vapor deposition (CVD), and vacuum magnetron sputtering. Liquid-phase coprecipitation is an important chemical synthesis method. Its basic principle is to mix two or more solutions together to form a precipitate, then separate the precipitate through centrifugation, filtration, etc., and finally perform drying and sintering to obtain the desired product. Although liquid-phase coprecipitation has a simple reaction process, low cost, and is easy to promote and industrialize, the synthesized product has poor dispersibility, agglomeration, and is difficult to wash and filter. Chemical vapor deposition (CVD) is a method of synthesizing coatings or nanomaterials by reacting chemical gases or vapors on a substrate surface. It is the most widely used technique in the semiconductor industry for depositing a wide range of materials, including a broad spectrum of insulating materials, most metals, and metal alloys. Theoretically, it is quite simple: two or more gaseous raw materials are introduced into a reaction chamber, where they react chemically to form a new material, which is then deposited onto the wafer surface. The deposition of silicon nitride (Si3N4) is a good example, formed by the reaction of silane and nitrogen. CVD offers advantages such as simple equipment, convenient operation and maintenance, and high flexibility. However, its high reaction temperature, low deposition rate, difficulty in localized deposition, and the toxicity of the gas source and residual gas after the reaction, along with the thin coating thickness, limit its development. Magnetron sputtering: Magnetron sputtering is a type of physical vapor deposition (PVD). General sputtering methods can be used to prepare metals, semiconductors, insulators, and many other materials, and offer advantages such as simple equipment, easy control, large coating area, and strong adhesion. Developed in the 1970s, magnetron sputtering has achieved high speed, low temperature, and low damage. Because high-speed sputtering occurs under low pressure, it is essential to effectively increase the ionization rate of the gas. Magnetron sputtering increases the plasma density and sputtering rate by introducing a magnetic field onto the target cathode surface and using this magnetic field to confine charged particles. However, the development of magnetron sputtering is currently hampered by the target utilization rate of only 20-30%.

[0004] Metal-organic frameworks (MOFs) are the earliest microporous organic framework materials. They are novel, designable crystalline microporous materials formed through the coordination copolymerization of organic groups (pillars) with metal ions or clusters (nodes), and can therefore also be called coordination porous polymers. MOFs can be synthesized by combining one or more metal ions with one organic ligand, or by combining one metal ion with one or two organic ligands. The variety of coordination complexes of organic units is extremely rich, and the methods of combining ligands with metal ions are numerous, directly leading to the diversity of MOF materials. MOF materials not only possess high porosity but also exhibit considerable controllability in pore size and the composition of synthesized materials. However, their high surface area cannot mask their relatively poor chemical and thermal stability, which severely limits their application range, but provides a new approach for the preparation of multi-component alloy powders.

[0005] The MOF (Metal-Organic Fiber) method offers numerous advantages for the preparation of multi-component alloys. It utilizes combinations of various metal ions and organic ligands to achieve multi-component alloy preparation. This allows for flexible control over the alloy's composition and proportions, expanding the compositional space. Simultaneously, the MOF method forms a homogeneous structure through coordination interactions between metal ions and organic ligands, enabling atomic-level mixing. This promotes the uniform distribution of elements within the alloy, thereby improving its homogeneity and stability. Furthermore, the MOF method allows for control over the alloy's composition and microstructure by adjusting parameters such as synthesis conditions, ligand selection, and metal ion ratios. This enables customized alloy design to meet specific application requirements.

[0006] As previously stated, the drawbacks of existing technologies are that while liquid-phase mixing can melt refractory metals, yielding alloy grain sizes between tens and hundreds of micrometers, the high melting points of the main components and the significant differences in melting points between elements in refractory alloys make this method prone to compositional segregation, affecting alloy performance. Liquid-phase co-precipitation also suffers from poor product dispersibility, agglomeration, and difficulties in washing and filtering. A key unresolved issue in powder metallurgy is the susceptibility of alloy powders to contamination during ball milling. Grinding balls, container walls, milling media, and process control agents can all contaminate the sample, generating impurities and ultimately affecting the mechanical properties of high-entropy alloys. While gas-phase mixing can improve and repair the surface of the base alloy, enhancing corrosion resistance, wear resistance, and oxidation resistance, chemical vapor deposition (CVD) suffers from high reaction temperatures, low deposition rates, difficulty in localized deposition, and the toxicity of the gas source and residual gas after the reaction, along with thin coatings, hindering its development. Magnetron sputtering requires complex equipment, has low target utilization, and excessively high preparation costs. Summary of the Invention

[0007] The purpose of this invention is to provide a method for homogenizing chemically synthesized multi-component alloys. This method utilizes the concept of MOF material preparation and, based on the existing multi-component alloy preparation process, changes the element mixing method. Specifically, it achieves atomic-scale bonding of elements in the multi-component alloy through chemical synthesis of multi-component alloy powder, thereby achieving the purpose of alloying, reducing the particle size of alloying elements, and improving compositional uniformity.

[0008] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0009] 1) Powder preparation

[0010] First, ammonium molybdate and ammonium tungstate are mixed in a molar ratio of 3:5. Then, the mixture of ammonium molybdate and ammonium tungstate is added to deionized water in a mass ratio of 1:30 to 35 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0011] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0012] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0013] 2) Powder reduction

[0014] The powder is reduced once at 500-600℃, and then reduced a second time at 700-850℃. The powder is then passed through a 200-mesh sieve to obtain the reduced powder.

[0015] 3) Hot pressing and sintering

[0016] The reduced powder was placed in a graphite mold and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0017] 4) Heat treatment

[0018] The sintered product was heated to 1500-1600℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1300-1400℃ for 1 hour.

[0019] The purity of the ammonium molybdate and ammonium tungstate is above 99.9%.

[0020] The diameter of the graphite mold is 60mm.

[0021] The material prepared by this invention was subjected to room temperature tensile testing, and its tensile strength was 700-750 MPa, which is 14-64 MPa higher than the tensile strength of the best-performing molybdenum-tungsten alloy currently available.

[0022] Compared to solid-state mixing, this invention eliminates the mechanical alloying process and reduces sintering power during solidification; compared to liquid-phase mixing, it improves the uniformity of element mixing; compared to gas-phase mixing, it improves material utilization, reduces preparation costs and homogenization difficulty, and causes no environmental pollution. Attached Figure Description

[0023] Figure 1 Amorphous morphology of powder under an optical microscope;

[0024] Figure 2 Elemental distribution of powder under scanning electron microscopy (SEM). Detailed Implementation

[0025] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments.

[0026] Example 1:

[0027] 1) Powder preparation

[0028] First, ammonium molybdate and ammonium tungstate with a purity of 99.9% or higher are mixed at a molar ratio of 3:5. The mixture of ammonium molybdate and ammonium tungstate is then added to deionized water at a mass ratio of 1:30 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0029] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0030] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0031] like Figure 1 As shown, under a light microscope, it can be seen that the powder prepared in step 1) is amorphous and no crystalline substances similar to ammonium tungstate and ammonium molybdate were found.

[0032] Depend on Figure 2 The results also prove that the elements are evenly distributed;

[0033] 2) Powder reduction

[0034] The powder was reduced once at 500℃, and then reduced a second time at 700℃. The powder was then passed through a 200-mesh sieve to obtain the reduced powder.

[0035] 3) Hot pressing and sintering

[0036] The reduced powder was placed in a graphite mold with a diameter of 60 mm and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0037] 4) Heat treatment

[0038] The sintered product was heated to 1500℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1300℃ for 1 hour.

[0039] Example 2:

[0040] 1) Powder preparation

[0041] First, ammonium molybdate and ammonium tungstate with a purity of 99.9% or higher are mixed at a molar ratio of 3:5. The mixture of ammonium molybdate and ammonium tungstate is then added to deionized water at a mass ratio of 1:33 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0042] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0043] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0044] 2) Powder reduction

[0045] The powder was reduced once at 580℃ and then reduced a second time at 800℃. The powder was then passed through a 200-mesh sieve to obtain the reduced powder.

[0046] 3) Hot pressing and sintering

[0047] The reduced powder was placed in a graphite mold with a diameter of 60 mm and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0048] 4) Heat treatment

[0049] The sintered product was heated to 1580℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1350℃ for 1 hour.

[0050] Example 3:

[0051] 1) Powder preparation

[0052] First, ammonium molybdate and ammonium tungstate with a purity of 99.9% or higher are mixed at a molar ratio of 3:5. The mixture of ammonium molybdate and ammonium tungstate is then added to deionized water at a mass ratio of 1:35 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0053] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0054] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0055] 2) Powder reduction

[0056] The powder was reduced once at 530℃ and then reduced a second time at 750℃. The powder was then passed through a 200-mesh sieve to obtain the reduced powder.

[0057] 3) Hot pressing and sintering

[0058] The reduced powder was placed in a graphite mold with a diameter of 60 mm and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0059] 4) Heat treatment

[0060] The sintered product was heated to 1530℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1320℃ for 1 hour.

[0061] Example 4:

[0062] 1) Powder preparation

[0063] First, ammonium molybdate and ammonium tungstate with a purity of 99.9% or higher are mixed at a molar ratio of 3:5. The mixture of ammonium molybdate and ammonium tungstate is then added to deionized water at a mass ratio of 1:32 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0064] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0065] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0066] 2) Powder reduction

[0067] The powder was reduced once at 600℃ and then reduced a second time at 850℃. The powder was then passed through a 200-mesh sieve to obtain the reduced powder.

[0068] 3) Hot pressing and sintering

[0069] The reduced powder was placed in a graphite mold with a diameter of 60 mm and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0070] 4) Heat treatment

[0071] The sintered product was heated to 1600℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1400℃ for 1 hour.

[0072] Example 5:

[0073] 1) Powder preparation

[0074] First, ammonium molybdate and ammonium tungstate with a purity of 99.9% or higher are mixed at a molar ratio of 3:5. The mixture of ammonium molybdate and ammonium tungstate is then added to deionized water at a mass ratio of 1:34 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0075] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0076] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0077] 2) Powder reduction

[0078] The powder was reduced once at 550℃ and then reduced a second time at 830℃. The powder was then passed through a 200-mesh sieve to obtain the reduced powder.

[0079] 3) Hot pressing and sintering

[0080] The reduced powder was placed in a graphite mold with a diameter of 60 mm and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0081] 4) Heat treatment

[0082] The sintered product was heated to 1550℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1380℃ for 1 hour.

[0083] Example 6:

[0084] 1) Powder preparation

[0085] First, ammonium molybdate and ammonium tungstate with a purity of 99.9% or higher are mixed at a molar ratio of 3:5. The mixture of ammonium molybdate and ammonium tungstate is then added to deionized water at a mass ratio of 1:31 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate.

[0086] Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution.

[0087] Finally, after the polyethyleneimine solution was added to the ammonium tungstate and ammonium molybdate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder.

[0088] 2) Powder reduction

[0089] The powder was reduced once at 560℃ and then reduced a second time at 780℃. The powder was then passed through a 200-mesh sieve to obtain the reduced powder.

[0090] 3) Hot pressing and sintering

[0091] The reduced powder was placed in a graphite mold with a diameter of 60 mm and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace.

[0092] 4) Heat treatment

[0093] The sintered product was heated to 1570℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1360℃ for 1 hour.

[0094] This invention combines the chemical synthesis concept of MOF (Metal-Oxide-Foil) to achieve atomic mixing of multiple elements, fundamentally solving the problem of uniformity in multi-element mixing. The mixed powder can reach the nanoscale, eliminating the need for mechanical alloying and reducing the time and economic costs in the alloy preparation process. Utilizing the MOF method to achieve uniform atomic mixing of elements allows for wider application in the preparation of alloys with more elements, such as medium-entropy or high-entropy alloys. Furthermore, the material prepared by this invention exhibits a room-temperature tensile strength of 700-750 MPa, representing a 14-64 MPa increase compared to the current best-performing molybdenum-tungsten alloy.

Claims

1. A method for homogenizing chemically synthesized multi-component alloys, characterized in that... Includes the following steps: 1) Powder preparation First, ammonium molybdate and ammonium tungstate are mixed in a molar ratio of 3:

5. Then, the mixture of ammonium molybdate and ammonium tungstate is added to deionized water in a mass ratio of 1:30 to 35 and ultrasonically stirred until completely dissolved to obtain a mixed solution of ammonium molybdate and ammonium tungstate. Then, polyethyleneimine was taken at a mass ratio of 1:3 to a mixture of polyethyleneimine, ammonium molybdate, and ammonium tungstate, and the polyethyleneimine was completely dissolved in deionized water under ultrasonic stirring to obtain a polyethyleneimine solution. Finally, after the polyethyleneimine solution was added to the ammonium molybdate and ammonium tungstate mixed solution and a precipitate was obviously formed, the mixture was sonicated for 10-20 minutes to completely precipitate and disperse the precipitate evenly. Then, the solvent was completely evaporated by rotary evaporation to obtain the powder. 2) Powder reduction The powder is reduced once at 500-600℃, and then reduced a second time at 700-850℃. The powder is then passed through a 200-mesh sieve to obtain the reduced powder. 3) Hot pressing and sintering The reduced powder was placed in a graphite mold and subjected to a vacuum condition of 40 MPa <10. -3 Pa was heated from room temperature to 1200℃ at a heating rate of 10℃ / min and held for 1 hour, then heated to 1700℃ at a heating rate of 10℃ / min and held for 2.5 hours before being cooled to room temperature in the furnace. 4) Heat treatment The sintered product was heated to 1500-1600℃ in a medium-frequency induction furnace, held for 30 minutes, extruded on a horizontal extruder, and then naturally cooled before annealing at 1300-1400℃ for 1 hour.

2. The method for homogenizing chemically synthesized multi-component alloys according to claim 1, characterized in that: The purity of the ammonium molybdate and ammonium tungstate is above 99.9%.

3. The method for homogenizing chemically synthesized multi-component alloys according to claim 1, characterized in that: The diameter of the graphite mold is 60mm.

Citation Information

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