CN114892064A - FeCrCuVCo high-entropy alloy and preparation method thereof - Google Patents
FeCrCuVCo high-entropy alloy and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a FeCrCuVCo high-entropy alloy which comprises the following components in percentage by mole: 19-22% of Fe, 19-22% of Cr, 19-21% of Cu, 18-20% of V, 18-20% of Co, 0.2-0.5% of Mo and inevitable impurities. And discloses a preparation method of the FeCrCuVCo high-entropy alloy. The performance characteristics of each element are fully exerted by the limitation of the proportion of the components of the FeCrCuVCo high-entropy alloy, particularly the limitation of the contents of Fe, Cr and Cu and V, Co, and the FeCrCuVCo high-entropy alloy has the advantages of very uniform structure, excellent wear resistance and corrosion resistance, higher hardness and better toughness due to the fusion between the elements.
Description
Technical Field
The invention relates to the technical field of metal composite materials and metallurgy, in particular to a FeCrCuVCo high-entropy alloy and a preparation method of the FeCrCuVCo high-entropy alloy.
Background
Unlike conventional alloys, which consist of one main element and a plurality of trace elements, high entropy alloys are solid solutions of a plurality of elements (usually more than 4) mixed at equal or near equal ratios. Under the action of high thermodynamic entropy, atoms with different properties occupy disordered positions in the solid solution, so that serious lattice distortion is caused. The special crystal structure enables the high-entropy alloy to have excellent characteristics of high strength, strong corrosion resistance, high wear resistance and the like.
At present, the preparation of the traditional refractory high-entropy alloy is mainly based on a vacuum arc melting method. However, the melting points of the constituent elements of most high entropy alloys differ greatly. For example, V has a melting point of 1890 deg.C, while W has a melting point of 3620 deg.C, which differs by 1530 deg.C, but rather by more than V (3000 deg.C). Therefore, during the smelting preparation process of the refractory high-entropy alloy, the volatilization of low-melting-point substances is easily caused, and the composition of the formed alloy deviates from the initial setting. Meanwhile, the huge melting point difference causes that a very wide liquid-solid two-phase temperature area is often formed when refractory metals are mixed two by two, thereby causing obvious solidification time difference and forming a large number of casting defects such as shrinkage cavities, dendrites and the like, and influencing the performance and large-size forming of the refractory high-entropy alloy. Therefore, the maximum size of the existing casting-molded refractory high-entropy alloy is only 10mm multiplied by 60mm, which is far from meeting the practical application and even difficult to meet the test sample size requirement of national standard tensile property.
Powder metallurgy is a technique for converting a powder material having a certain specific particle size, shape and apparent density into a material having high strength, high precision and high performance, and its key steps include preparation of powder, shaping and subsequent sintering and heat treatment. Since the powder metallurgy technology has the advantages of low energy consumption, high material utilization rate, low cost, unique shape, high product performance and the like, the powder metallurgy technology is widely used for scientific research and industrial production of various metal materials at present. The alloy prepared by adopting the powder metallurgy process has the advantages of no component segregation, fine crystal grains, fine carbides, small heat treatment deformation, uniform hardness, good toughness and wear resistance and the like.
The invention utilizes the powder metallurgy technology to carry out hot isostatic pressing on the prepared high-entropy alloy powder, and can produce the high-entropy alloy material with excellent performance and larger specification and size.
Disclosure of Invention
The invention aims to solve the technical problem of providing a FeCrCuVCo high-entropy alloy and a preparation method thereof, wherein a metal alloy repeated melting technology is utilized, and atomization powder preparation and hot isostatic pressing sintering are adopted, so that the FeCrCuVCo high-entropy alloy has a single structure, is uniform in structure, is wear-resistant, corrosion-resistant, high in hardness and has certain toughness. In order to solve the problems, the invention provides a FeCrCuVCo high-entropy alloy, which has the technical scheme as follows:
the invention discloses a FeCrCuVCo high-entropy alloy which comprises the following components in percentage by mole: 19-22% of Fe, 19-22% of Cr, 19-21% of Cu, 18-20% of V, 18-20% of Co, 0.2-0.5% of Mo and inevitable impurities.
Furthermore, in the high-entropy alloy, the content ratio of Fe, Cr and Cu is 1:1:0.9-1, and the content ratio of V, Co is 1: 1.
The invention discloses a preparation method of FeCrCuVCo high-entropy alloy, which comprises the following steps:
step S1, electric furnace smelting: adding pure copper, pure iron, pure chromium, pure cobalt and pure vanadium into a smelting furnace in sequence according to a preset proportion, introducing argon for protection to start smelting, electromagnetically stirring for 20-30 minutes after all metals in the smelting furnace are molten, adding pure molybdenum powder with a preset content, uniformly stirring, and keeping the temperature when the smelting heating temperature is controlled to 1650-1950 ℃;
step S2, atomizing to prepare powder: directly atomizing the smelted alloy liquid when the smelted alloy liquid flows out of the smelting furnace, wherein the atomizing gas is nitrogen, and the gas pressure of an atomizing nozzle is 3-6 MPa, so that FeCrCuVCo high-entropy alloy powder is prepared;
step S3, powder wrapping and packaging: mechanically stirring FeCrCuVCo high-entropy alloy powder uniformly, filling the mixture into a sheathing die, performing static pressure preforming, vacuumizing to a vacuum degree of more than 10Pa-1Pa in a sheathing, and then welding and sealing a sheathing end cover by using an electron beam welding machine;
step S4, hot isostatic pressing sintering: and placing the sheath in a hot isostatic pressing furnace, and carrying out hot isostatic pressing sintering in vacuum or inert gas atmosphere, wherein the pressure is controlled to be 50-200 MPa, the sintering temperature is controlled to be 850-1050 ℃, and the heat preservation time is 1-5h, so that the high-entropy alloy is obtained.
Further, in step S1, the purities of pure copper, pure iron, pure chromium, pure cobalt, pure vanadium, and pure molybdenum powder are all greater than or equal to 99.9%, and the mesh number of the particle size of the pure molybdenum powder is greater than or equal to 200 mesh.
Further, in step S1, adding pure copper, pure iron, pure chromium, pure cobalt, pure vanadium, and pure molybdenum powder into the smelting furnace, smelting into an alloy melt, and casting into an alloy ingot; then melting the alloy ingot, and repeatedly melting the alloy ingot for 2-3 times to prepare powder by atomization.
Further, in step S2, the fecrcuvo high-entropy alloy powder obtained by pulverization has the following conditions: the powder sphericity rate is more than 90%, the powder oxygen content is less than 200ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 90%.
Further, in step S2, the fecrcuvo high-entropy alloy powder obtained by pulverization has the following conditions: the powder sphericity rate is more than 95%, the powder oxygen content is less than 120ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 95%.
Further, in step S3, the jacket is made of a low carbon steel plate or a pure iron plate, and the thickness of the jacket plate is 2mm to 5 mm.
The FeCrCuVCo high-entropy alloy and the preparation method thereof have the beneficial effects that:
firstly, the performance characteristics of each element are fully exerted through the proportion limitation of FeCrCuVCo high-entropy alloy components, particularly the content limitation of Fe, Cr and Cu and V, Co, and the FeCrCuVCo high-entropy alloy has the advantages of very uniform structure, excellent wear resistance and corrosion resistance, higher hardness and better toughness due to the fusion between the elements.
Secondly, by adopting atomization powder preparation and hot isostatic pressing sintering means, the structure and components of the FeCrCuVCo high-entropy alloy are more uniform while the smelting frequency is reduced, the material structure is more compact and the crystal grains are finer than the high-entropy alloy produced by the common casting process, and the comprehensive performance of the material is obviously superior to that of the high-entropy alloy produced by the common casting process.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a metallographic structure photograph of a FeCrCuVCo high-entropy alloy of the invention.
Detailed Description
In order to make the technical solutions in the embodiments of the present invention better understood and make the above objects, features, and advantages of the present invention more comprehensible, specific embodiments of the present invention are described below with reference to the accompanying drawings.
It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example one
The FeCrCuVCo high-entropy alloy of the present embodiment is composed of the following components in mole percentage: 19-22% of Fe, 19-22% of Cr, 19-21% of Cu, 18-20% of V, 18-20% of Co, 0.2-0.5% of Mo and inevitable impurities.
In a more preferred embodiment, the ratio of the contents of Fe, Cr and Cu in the high-entropy alloy is 1:1:0.9-1, and the ratio of the contents of Fe, Cr and Cu in the high-entropy alloy is 1: 1.
Example two
The preparation method of the fecrcuvo high-entropy alloy of the embodiment includes the following steps:
step S1, electric furnace smelting: adding pure copper, pure iron, pure chromium, pure cobalt and pure vanadium into a smelting furnace in sequence according to a preset proportion, introducing argon for protection to start smelting, electromagnetically stirring for 20-30 minutes after all metals in the smelting furnace are molten, adding pure molybdenum powder with a preset content, uniformly stirring, and keeping the temperature when the smelting heating temperature is controlled to 1650-1950 ℃;
step S2, atomizing to prepare powder: directly atomizing the smelted alloy liquid when the smelted alloy liquid flows out of the smelting furnace, wherein the atomizing gas is nitrogen, and the gas pressure of an atomizing nozzle is 3-6 MPa, so that FeCrCuVCo high-entropy alloy powder is prepared;
step S3, powder wrapping and packaging: mechanically stirring FeCrCuVCo high-entropy alloy powder uniformly, filling the mixture into a sheathing die, performing static pressure preforming, vacuumizing to a vacuum degree of more than 10Pa-1Pa in a sheathing, and then welding and sealing a sheathing end cover by using an electron beam welding machine;
step S4, hot isostatic pressing sintering: and placing the sheath in a hot isostatic pressing furnace, and carrying out hot isostatic pressing sintering in vacuum or inert gas atmosphere, wherein the pressure is controlled to be 50-200 MPa, the sintering temperature is controlled to be 850-1050 ℃, and the heat preservation time is 1-5h, so that the high-entropy alloy is obtained.
In a preferred embodiment, in step S1, the purities of pure copper, pure iron, pure chromium, pure cobalt, pure vanadium, and pure molybdenum powder are all greater than or equal to 99.9%, and the particle size of the pure molybdenum powder is greater than or equal to 200 mesh.
Preferably, in step S1, adding pure copper, pure iron, pure chromium, pure cobalt, pure vanadium, and pure molybdenum powder into a smelting furnace, smelting into an alloy melt, and casting into an alloy ingot; then melting the alloy ingot, and repeatedly melting the alloy ingot for 2-3 times to prepare powder by atomization.
Preferably, in step S2, the FeCrCuVCo high-entropy alloy powder obtained by pulverization has the following conditions: the powder sphericity rate is more than 90%, the powder oxygen content is less than 200ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 90%. Further preferably, in step S2, the fecrcuvo high-entropy alloy powder obtained by pulverization has the following conditions: the powder sphericity rate is more than 95%, the powder oxygen content is less than 120ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 95%.
Preferably, in step S3, the jacket is made of mild steel plate or pure iron plate, and the thickness of the jacket plate is 2mm-5 mm.
EXAMPLE III
The embodiment provides a specific implementation case of the FeCrCuVCo high-entropy alloy and the preparation method thereof:
1. smelting alloy, namely adding pure copper, pure iron, pure chromium, pure cobalt and pure vanadium into a smelting furnace in sequence, and introducing argon for protection to start smelting; the high-entropy alloy comprises the following components: 21 at.% Fe, 21 at.% Cr, 20 at.% Cu, 19 at.% V, 18.75 at.% Co, and 0.25 at.% Mo. Controlling the smelting temperature at 1750 +/-50 ℃, electromagnetically stirring for 20 minutes after metals such as Fe, Cr, V and the like in the furnace are completely molten, adding pure molybdenum powder, uniformly stirring, repeatedly smelting for 1 time after casting into ingots, uniformly stirring the alloy liquid, standing for 10 minutes, and then starting atomization and powder preparation.
2. Preparing high-speed steel alloy powder, wherein the alloy liquid is directly subjected to vacuum atomization treatment when discharged from a smelting furnace, the atomization is carried out by adopting nitrogen, and the gas pressure of an atomization nozzle is 3.8MPa, so that the high-speed steel alloy powder is prepared; the powder sphericity rate is more than 90%, the powder oxygen content is less than 200ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 90%.
3. And (3) sheath preparation: the sheath is welded by a low-carbon steel plate with the thickness of 4mm, the inner surface of the sheath needs to be mechanically polished to remove oxide skin and impurities, 5 surfaces of the sheath are well welded, and an opening at the upper end face is reserved for filling FeCrCuVCo high-entropy alloy powder.
4. Powder filling and compacting: FeCrCuVCo high-entropy alloy powder is filled into a packing box, an upper end cover plate is covered after the powder is filled, the powder is put into a pressure device, a lower end cover plate presses the powder, the unit pressure is 40MPa, the powder is pressed for 40min, and the powder is pressed tightly.
5. And (3) vacuum packaging: and transferring the cold-pressed powder casing box to a vacuumizing device, vacuumizing to remove air in the casing box to a vacuum degree of 10-2Pa, and welding and sealing the end cover plate by using an electron beam welding machine.
6. Hot isostatic pressing forming: and (3) carrying out hot isostatic pressing sintering in a hot isostatic pressing furnace in an inert gas atmosphere, controlling the atmosphere pressure to be 30MPa and the sintering temperature to be 980 ℃, and preserving heat for 2 hours to obtain the FeCrCuVCo high-entropy alloy.
7. A sample is taken for performance detection, and the alloy hardness is 63-65HRC, and the bending strength is 5100-5200 MPa.
8. After the material is made into a blade for edging, the measured sharpness is 157, the sharpness durability reaches 935, and the corrosion resistance is greatly higher than that of common 3Cr13 stainless steel.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
The embodiments of the present invention are described in detail above with reference to the drawings, but the present invention is not limited to the described embodiments. Various changes, modifications, substitutions and alterations to these embodiments will occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (8)
1. FeCrCuVCo high entropy alloy, characterized in that it consists of, in mole percentages: 19-22% of Fe, 19-22% of Cr, 19-21% of Cu, 18-20% of V, 18-20% of Co, 0.2-0.5% of Mo and inevitable impurities.
2. FeCrCuVCo high-entropy alloy as claimed in claim 1, wherein the content ratio of Fe, Cr and Cu in the high-entropy alloy is 1:1:0.9-1, and the content ratio of V, Co is 1: 1.
3. A preparation method of FeCrCuVCo high-entropy alloy is characterized by comprising the following steps:
step S1, electric furnace smelting: adding pure copper, pure iron, pure chromium, pure cobalt and pure vanadium into a smelting furnace in sequence according to a preset proportion, introducing argon for protection to start smelting, electromagnetically stirring for 20-30 minutes after all metals in the smelting furnace are molten, adding pure molybdenum powder with a preset content, uniformly stirring, and keeping the temperature when the smelting heating temperature is controlled to 1650-1950 ℃;
step S2, atomizing to prepare powder: directly atomizing the smelted alloy liquid when the smelted alloy liquid flows out of the smelting furnace, wherein the atomizing gas is nitrogen, and the gas pressure of an atomizing nozzle is 3-6 MPa, so that FeCrCuVCo high-entropy alloy powder is prepared;
step S3, powder wrapping and packaging: mechanically stirring FeCrCuVCo high-entropy alloy powder uniformly, filling the mixture into a sheathing die, performing static pressure preforming, vacuumizing to a vacuum degree of more than 10Pa-1Pa in a sheathing, and then welding and sealing a sheathing end cover by using an electron beam welding machine;
step S4, hot isostatic pressing sintering: and placing the sheath in a hot isostatic pressing furnace, and carrying out hot isostatic pressing sintering in vacuum or inert gas atmosphere, wherein the pressure is controlled to be 50-200 MPa, the sintering temperature is controlled to be 850-1050 ℃, and the heat preservation time is 1-5h, so that the high-entropy alloy is obtained.
4. The method according to claim 3, wherein in step S1, the purities of pure copper, pure iron, pure chromium, pure cobalt, pure vanadium, and pure molybdenum powder are all greater than or equal to 99.9%, and the mesh number of the particle sizes of the pure molybdenum powder is greater than or equal to 200 mesh.
5. The method according to claim 3, wherein in step S1, pure copper, pure iron, pure chromium, pure cobalt, pure vanadium and pure molybdenum powder are added into the smelting furnace to be smelted into an alloy melt, and then cast into an alloy ingot; then melting the alloy ingot, and repeatedly melting the alloy ingot for 2-3 times to prepare powder by atomization.
6. The preparation method of claim 4, wherein in step S2, the FeCrCuVCo high-entropy alloy powder obtained by pulverization has the following conditions: the powder sphericity rate is more than 90%, the powder oxygen content is less than 200ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 90%.
7. The preparation method of claim 6, wherein in step S2, the FeCrCuVCo high-entropy alloy powder obtained by pulverization has the following conditions: the powder sphericity rate is more than 95%, the powder oxygen content is less than 120ppm, and the mass percentage content of atomized powder below 100 mu m reaches more than 95%.
8. The manufacturing method according to claim 3, wherein in step S3, the jacket is made of mild steel plate or pure iron plate, and the thickness of the jacket plate is 2mm-5 mm.
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