CN117265360A - Composite precipitation strengthening type high-entropy alloy and preparation method thereof - Google Patents
Composite precipitation strengthening type high-entropy alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 129
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000005728 strengthening Methods 0.000 title claims abstract description 32
- 238000001556 precipitation Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 238000003723 Smelting Methods 0.000 claims description 36
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- 238000010438 heat treatment Methods 0.000 abstract description 15
- 239000002184 metal Substances 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 2
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- 239000010949 copper Substances 0.000 description 36
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
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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
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The invention discloses a composite precipitation strengthening type high-entropy alloy and a preparation method thereof, and belongs to the field of metal material preparation. The high-entropy alloy consists of Al, co, cr, fe, ni, cu, V and Ti elements, and has a general formula of Al a Co b Cr c Fe d Ni e Cu f V g Ti h Wherein a is more than or equal to 2 and less than or equal to 4, b is more than or equal to 16 and less than or equal to 20, c is more than or equal to 16 and less than or equal to 20, d is more than or equal to 16 and less than or equal to 20, e is more than or equal to 35 and less than or equal to 40, f is more than or equal to 0 and less than or equal to 3, g is more than or equal to 0 and less than or equal to 3, h is more than or equal to 0 and less than or equal to 3, and a+b+c+d+e+f+g+h=100. The alloy is prepared by vacuum arc melting and heat treatment, and has excellent mechanical properties. The various metal raw materials are environment-friendly, the preparation process is safer, and the industrial production can be realized.
Description
Technical Field
The invention belongs to the field of metal material preparation, and particularly relates to a composite precipitation strengthening type high-entropy alloy and a preparation method thereof.
Background
In recent years, a high-entropy alloy which is designed based on configuration entropy and is used for multi-principal element alloy design gets rid of a single principal element design yoke which takes the mixed enthalpy as the main component of the traditional alloy, and is a good trigger for cutting into the field of high-function and high-added-value special alloy materials. Among them, high entropy alloys of Face Centered Cubic (FCC) structure have attracted much attention from researchers due to many excellent properties such as good ductility and toughness, but the intrinsic properties of their crystal structure determine the low strength of such alloys, thus limiting their industrial applications.
Precipitation strengthening is an effective strengthening method. In most cases, however, precipitation strengthening increases the strength of the alloy while reducing the plasticity. How to improve both the strength and the plasticity of the alloy is still a primary problem faced by precipitation-strengthened alloys, which is largely affected by the size and characteristics of the precipitated phases. When the size of the precipitated phase is large, the strengthening mechanism may be attributed to the Orowan bypass mechanism. Although such large-sized precipitations also have good strengthening effects with respect to high entropy alloys, they generally come at the expense of the plasticity of the alloy, mainly due to the negative effects of the hard brittleness of the precipitations themselves, resulting in reduced ductility of the alloy.
How to solve the problem of high ductility while maintaining the strength of high-entropy alloy is a key problem to be solved.
Disclosure of Invention
In order to improve the strength of the high-entropy alloy and simultaneously maintain high ductility, the invention designs a nano-scale precipitated phase which has a coherent relation with a matrix, and can ensure that the strength and the plasticity of the alloy can be well combined.
A composite precipitation strengthening type high-entropy alloy is described as being composed of Al, co, cr, fe, ni, cu, V andti element, the general formula of the high-entropy alloy is Al a Co b Cr c Fe d Ni e Cu f V g Ti h Wherein a is more than or equal to 2 and less than or equal to 4, b is more than or equal to 16 and less than or equal to 20, c is more than or equal to 16 and less than or equal to 20, d is more than or equal to 16 and less than or equal to 20, e is more than or equal to 35 and less than or equal to 40, f is more than or equal to 0 and less than or equal to 3, g is more than or equal to 0 and less than or equal to 3, h is more than or equal to 0 and less than or equal to 3, and a+b+c+d+e+f+g+h=100.
As a preferable technical scheme of the invention, the composite precipitation strengthening type high-entropy alloy Al a Co b Cr c Fe d Ni e Cu f V g Ti h The alloy composition satisfies the following conditions: wherein a is more than or equal to 3 and less than or equal to 4, b is more than or equal to 17 and less than or equal to 19, c is more than or equal to 17 and less than or equal to 19, d is more than or equal to 17 and less than or equal to 39,0 is more than or equal to 37 and less than or equal to f is more than or equal to 2, g is more than or equal to 0 and less than or equal to 2, h is more than or equal to 0 and less than or equal to 2, and a+b+c+d+e+f+g+h=100.
The preparation method of the composite precipitation strengthening type high-entropy alloy comprises the following steps:
step one, taking Al, co, cr, fe, ni, cu, V, ti as a raw material, cleaning and weighing the raw material, then placing the raw material into a smelting furnace, vacuumizing, filling argon for smelting, cooling to obtain a master alloy ingot, repeatedly smelting the master alloy ingot for 3-5 times, and cooling to obtain a final high-entropy alloy ingot.
And secondly, carrying out solution treatment on the high-entropy alloy ingot for 6 hours at 1050-1150 ℃ under the protection of argon, carrying out room temperature rolling, wherein the total rolling deformation is 90%, and then carrying out annealing treatment and then air cooling or further carrying out aging treatment to obtain the high-entropy alloy.
As a preferable technical scheme of the invention, a vacuum arc melting furnace is selected in the first step to perform alloy melting.
As a preferable technical scheme of the invention, the annealing treatment process is selected in the step two, and the annealing treatment process is performed for 30min at 1000 ℃ and then air cooling is performed.
As a preferable technical scheme of the invention, in the second step, the aging treatment is selected to age at 800 ℃ for 4 hours and then air-cooled.
The composite precipitation strengthening type high-entropy alloy is prepared through component design, and researches show that the high-entropy alloy not only has tensile strength of 500-1100 MPa, but also has an elongation of 29-68%, and has great potential in practical application.
The beneficial effects achieved by the invention are as follows:
(1) The invention adopts a small amount of precipitated phase strengthening elements Ti and Cu to form a composite ordered phase.
(2) The invention adopts six elements with larger melting point difference, namely Al (600 ℃), co (1495 ℃), cr (1907 ℃), fe (1538 ℃), ni (1453 ℃), ti (1678 ℃) and Cu (1083.4 ℃), as novel high-entropy alloy materials, and finally obtains the high-entropy alloy with FCC structure.
(3) The invention separates out a large amount of coherent ordered L1 in the FCC matrix 2 The phase strengthens the alloy, obviously increases the strength of the high-entropy alloy, has the tensile strength of 1090MPa and the fracture elongation of 29 percent.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is an XRD pattern for the homogenized high entropy alloys prepared in examples 1 and 2, examples 3 and 4, examples 5, examples 6 and examples 7, according to the present invention;
FIG. 2 is a golden phase diagram of the high entropy and homogenization state prepared in examples 1 and 2, examples 3 and 4, examples 5, examples 6 and examples 7 of the present invention;
FIG. 3 is a stress-strain curve comparison of the high entropy alloys prepared in examples 1 and 2, examples 3 and 4, examples 5 and 6 of the present invention;
FIG. 4 is a plot of the hardness of the high entropy alloy prepared in example 7 of the present invention;
FIG. 5 is a stress-strain curve of the high entropy alloy prepared in example 7 of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
The tests and equipment involved in the various embodiments are as follows:
a high-vacuum non-consumable arc melting furnace, NF-800 type high-vacuum non-consumable arc melting furnace manufactured by Sichuan yang Organin materials Co., ltd.
Microstructure: metallographic observation adopts an Axio Observer D1M inverted metallographic microscope manufactured by Karl zeiss company; the metallographic specimen has the size of 4mm multiplied by 3mm multiplied by 1.2mm, the specimen is inlaid by phenolic resin, and then polished by 400# silicon carbide abrasive paper, 600# silicon carbide abrasive paper, 1000# silicon carbide abrasive paper, 1500# silicon carbide abrasive paper and 2000# silicon carbide abrasive paper in sequence, and then polished by diamond polishing paste with the granularity of 2.5 mu m.
Testing the quasi-static tensile mechanical properties: according to the standard GB/T228.1-2010, a Zwick Z020 microcomputer controlled electronic universal testing machine is adopted to carry out indoor axial quasi-static tensile test, and the strain rate is selected to be 10 -3 s -1 The test sample is a nonstandard I-shaped piece. 1.20mm thick, 30mm long, 12mm gauge length and 3mm gauge width.
Example 1
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, cu:1.9%, V:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, then placing the washed and dried metal particles into an electric oven for drying, piling the cleaned and dried metal particles into a water-cooled copper crucible from top to bottom according to the sequence from low melting point to high melting point, and vacuumizing until the vacuum degree reaches 3X 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 1 h.
Homogenizing sample Al obtained after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 XRD detection analysis is carried out, and the result is shown in figure 1, and the annealed sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of fig. 3 and table 1, the high-entropy alloy 1 prepared had a tensile strength of 578MPa and an elongation at break of 68%.
Example 2
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, cu:1.9%, V:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, and then placing the metal particles into an electric ovenThe metal particles which are cleaned and dried are piled up into a water-cooled copper crucible from top to bottom according to the sequence from the melting point to high, and then vacuumized until the vacuum degree reaches 3 multiplied by 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 1 h.
Step six, aging treatment: and (3) preserving the heat of the annealed sample at 600 ℃ for 24 hours, and taking out the sample from the furnace for air cooling to obtain the aged high-entropy alloy.
Obtaining homogenized sample Al after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Cu 1.9 V 1.9 XRD detection analysis is carried out, and the homogenized sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of FIG. 3 and Table 1, the high-entropy alloy 2 prepared had a tensile strength of 678MPa and an elongation at break of 67%.
Example 3
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, V:1.9%, ti:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, then placing the washed and dried metal particles into an electric oven for drying, piling the cleaned and dried metal particles into a water-cooled copper crucible from top to bottom according to the sequence from low melting point to high melting point, and vacuumizing until the vacuum degree reaches 3X 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 1 h.
Homogenizing sample Al obtained after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 XRD detection analysis was carried out, and the results are shown in FIG. 1, wherein the homogenized sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of fig. 3 and table 1, the prepared high-entropy alloy 3 had a tensile strength of 799MPa and an elongation at break of 55%.
Example 4
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, V:1.9%, ti:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, then placing the washed and dried metal particles into an electric oven for drying, piling the cleaned and dried metal particles into a water-cooled copper crucible from top to bottom according to the sequence from low melting point to high melting point, and vacuumizing until the vacuum degree reaches 3X 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 1 h.
Step six, aging treatment: and (3) preserving the heat of the annealed sample at 600 ℃ for 24 hours, and taking out the sample from the furnace for air cooling to obtain the aged high-entropy alloy.
Homogenizing sample Al obtained after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 V 1.9 Ti 1.9 XRD detection analysis was carried out, and the results are shown in FIG. 1, wherein the homogenized sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of fig. 3 and table 1, the prepared high-entropy alloy 4 had a tensile strength of 902MPa and an elongation at break of 50%.
Example 5
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, ti:1.9%, cu:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, then placing the washed and dried metal particles into an electric oven for drying, piling the cleaned and dried metal particles into a water-cooled copper crucible from top to bottom according to the sequence from low melting point to high melting point, and vacuumizing until the vacuum degree reaches 3X 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 1 h.
Homogenizing sample Al obtained after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 XRD detection analysis was carried out, and the results are shown in FIG. 1, wherein the homogenized sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of fig. 3 and table 1, the prepared high-entropy alloy 5 had a tensile strength of 958MPa and an elongation at break of 53%.
Example 6
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, ti:1.9%, cu:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, then placing the washed and dried metal particles into an electric oven for drying, piling the cleaned and dried metal particles into a water-cooled copper crucible from top to bottom according to the sequence from low melting point to high melting point, and vacuumizing until the vacuum degree reaches 3X 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 1 h.
Step six, aging treatment: and (3) preserving the heat of the annealed sample at 600 ℃ for 24 hours, and taking out the sample from the furnace for air cooling to obtain the aged high-entropy alloy.
Homogenizing sample Al obtained after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 XRD detection analysis is carried out, and the result is shown in figure 1, and the homogenized sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of fig. 3 and table 1, the prepared high-entropy alloy 6 had a tensile strength of 1048MPa and an elongation at break of 46%.
Example 7
A composite precipitation strengthening type high-entropy alloy comprises Al as a component 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 。
The preparation method comprises the following steps:
step one, weighing: the embodiment provides a composite precipitation strengthening type high-entropy alloy which comprises the following element components in percentage by mole: al:3.7%, co:18.5%, cr:18.5%, fe:18.5%, ni:37%, ti:1.9%, cu:1.9 percent of metal raw materials corresponding to the element components are respectively weighed according to the proportion relation, and the total mass is 100g.
Smelting: washing the weighed metal particles with alcohol, then placing the washed and dried metal particles into an electric oven for drying, piling the cleaned and dried metal particles into a water-cooled copper crucible from top to bottom according to the sequence from low melting point to high melting point, and vacuumizing until the vacuum degree reaches 3X 10 -3 After Pa, argon is filled as a smelting oxidation-preventing protective gas, then high-entropy alloy is smelted, alloy cast ingots are obtained by cooling, and then smelting is repeated for 5 times to obtain Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 A master alloy ingot.
Step three, homogenizing: al to be obtained 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 Vacuum sealing the mother alloy ingot with quartz glass, filling argon gas, placing in a heat treatment furnace, heating to 1100 deg.C at 10 deg.C/min, maintaining for 6 hr, taking out sample, air cooling to obtain homogenized Al 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 Alloy samples.
Step four, deformation treatment: and (3) carrying out multi-pass rolling on the homogenized sample at room temperature, wherein the total rolling reduction is 90%, and obtaining a rolled high-entropy alloy sample.
Step five, annealing treatment: and (3) carrying out recrystallization annealing treatment on the rolled high-entropy alloy at 1000 ℃ for 30 min.
Step six, aging treatment: and (3) preserving the heat of the annealed sample for 4 hours at 800 ℃, and taking out the sample from the furnace for air cooling to obtain the ageing-state high-entropy alloy.
Homogenizing sample Al obtained after smelting 3.7 Co 18.5 Cr 18.5 Fe 18.5 Ni 37 Ti 1.9 Cu 1.9 XRD detection analysis is carried out, and the result is shown in figure 1, and the homogenized sample mainly comprises FCC and L1 2 From the compositions, as can be seen from the tensile test results of fig. 3 and table 1, the prepared high-entropy alloy 7 had a tensile strength of 1090MPa and an elongation at break of 29%.
TABLE 1
In conclusion, the composite precipitation strengthening type high-entropy alloy and the preparation method thereof are simple and feasible, and the obtained high-entropy alloy has higher strength and better plasticity through component design and simple vacuum arc melting, has simple preparation flow and strong safety, can realize industrial production, and has great application potential in the engineering field.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A composite precipitation strengthening type high-entropy alloy is characterized in thatJin Tongshi A is Al a Co b Cr c Fe d Ni e Cu f V g Ti h Wherein a is more than or equal to 2 and less than or equal to 4, b is more than or equal to 16 and less than or equal to 20, c is more than or equal to 16 and less than or equal to 20, d is more than or equal to 16 and less than or equal to 20, e is more than or equal to 35 and less than or equal to 40, f is more than or equal to 0 and less than or equal to 3, g is more than or equal to 0 and less than or equal to 3, h is more than or equal to 0 and less than or equal to 3, and a+b+c+d+e+f+g+h=100.
2. The composite precipitation-strengthened high-entropy alloy according to claim 1, wherein a is 3.ltoreq.4, b is 17.ltoreq.19, c is 17.ltoreq.19, d is 17.ltoreq.19, e is 37.ltoreq. 39,0.ltoreq.f is 2, g is 0.ltoreq.2, h is 0.ltoreq.2, and a+b+c+d+e+f+g+h=100.
3. The method for preparing the composite precipitation strengthening type high-entropy alloy as claimed in claim 1, which is characterized by comprising the following steps:
step one, taking Al, co, cr, fe, ni, cu, V, ti as a raw material, cleaning and weighing the raw material, then placing the raw material into a smelting furnace, vacuumizing, filling argon for smelting, cooling to obtain a master alloy ingot, repeatedly smelting the master alloy ingot for 3-5 times, and cooling to obtain a final high-entropy alloy ingot;
and secondly, carrying out solution treatment on the high-entropy alloy ingot for 6 hours under the protection of argon, then carrying out room-temperature rolling, wherein the total rolling deformation is 80-90%, and then carrying out annealing treatment and then air cooling or continuous aging treatment to obtain the high-entropy alloy.
4. The method for preparing the composite precipitation-strengthened high-entropy alloy according to claim 3, wherein the method is characterized by comprising the following steps: in the first step, the smelting furnace is a vacuum arc smelting furnace.
5. The method for producing a composite precipitation-strengthened high-entropy alloy according to claim 3, wherein the temperature of the solution treatment in the second step is 1050 to 1150 ℃.
6. The method for preparing the composite precipitation-strengthened high-entropy alloy according to claim 3, wherein the method is characterized by comprising the following steps: and step two, annealing at 1000 ℃ for 30min and then air-cooling.
7. The method for preparing the composite precipitation-strengthened high-entropy alloy according to claim 3 or 6, wherein the method comprises the following steps: and step two, aging treatment is carried out for 4 hours at 800 ℃ and then air cooling is carried out.
8. The method for preparing the composite precipitation strengthening type high-entropy alloy according to claim 3, wherein the method comprises the following steps: the tensile strength of the alloy is 500-1100 MPa, and the elongation is 29-68%.
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| CN118308640B (en) * | 2024-06-05 | 2024-08-30 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | High-entropy alloy and preparation method thereof, high-entropy alloy component and preparation method thereof |
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