CN113684425B - High-performance iron-based medium-entropy alloy and heat treatment method thereof - Google Patents
High-performance iron-based medium-entropy alloy and heat treatment method thereof Download PDFInfo
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- CN113684425B CN113684425B CN202111014152.3A CN202111014152A CN113684425B CN 113684425 B CN113684425 B CN 113684425B CN 202111014152 A CN202111014152 A CN 202111014152A CN 113684425 B CN113684425 B CN 113684425B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
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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
Abstract
The invention discloses a high-performance iron-based medium-entropy alloy and a preparation method thereof, and relates to the technical field of metal materials. The alloy comprises the following components in percentage by mole: al: 12-20 at%, Cr: 8-12 at%, Fe: 35-55 at%, Ni: 25-45 at%. The invention defines the phase selection rule of the iron-based medium entropy alloy, and can realize scientific guidance and performance prediction on the alloy component design by utilizing the rule.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a high-performance iron-based medium-entropy alloy and a heat treatment method thereof.
Background
High-performance alloys as important structural materials play an irreplaceable role in both civil and defense industries. The strength and plasticity of the alloy are the main manifestations of its mechanical properties, so improving the strength and plasticity is an important goal of alloy design. The medium-entropy alloy takes a plurality of elements as a matrix, has wide component design space, and is a novel structural material. The medium-entropy alloy has excellent mechanical properties such as high strength, high hardness, high wear resistance, high corrosion resistance and the like, and shows wide prospects in theoretical research and industrial application. The Co-free iron-based medium entropy alloy has lower cost and thus has greater application prospect.
The conventional entropy alloy in various nickel-iron bases lacks a system for researching the components of the alloy, lacks effective regulation and control on the performance of the alloy, and cannot provide practical guidance for the practical application of the alloy. Also, the existing high-entropy alloy balances the strong plasticity of the alloy mainly by regulating the components to form a dual-phase structure of FCC + BCC, and emphasizes the cast state on the performance of the alloy. The high-entropy alloy contains high-content expensive Co and Ni elements, and has high application cost. The iron-based medium entropy alloy has good balance in cost and performance, however, the change of components has great influence on the mechanical property of the iron-based medium entropy alloy, systematic research is lacked, the function of various alloy elements in a phase selection process is unclear, and the determination of the alloy components lacks scientificity and systematicness, so that the performance of the alloy has great randomness. Therefore, the alloy elements and the content thereof are properly selected, the phase evolution and the organization rule of the alloy are determined, and the improvement of the mechanical property of the alloy is an important problem of alloy design.
Disclosure of Invention
In order to solve the problems, the invention provides a high-performance iron-based medium-entropy alloy and a heat treatment method thereof
The invention aims to provide a high-performance iron-based medium-entropy alloy which comprises the following components in percentage by mole:
Al：12-20at％，Cr：8-12at％，Fe：35-55at％，Ni：25-45at％。
preferably, the composition comprises the following components in percentage by mole: al: 15-17 at%, Cr: 10at%, Fe: 36-49 at%, Ni: 26 to 36 at%.
Preferably, the composition also comprises the following components in percentage by mole: mo: 0-3at%, W: 0 to 2at%, Mn: 0 to 5at%, Ti: 0-3at%, C: 0 to 0.2 at%.
The second purpose of the invention is to provide a heat treatment method of a high-performance iron-based medium-entropy alloy, which comprises the following steps:
after a certain amount of deformation is applied to the as-cast intermediate entropy alloy ingot, preserving heat at 1100-1250 ℃ for 15-30 min, and then quenching to obtain an intermediate entropy alloy ingot subjected to first heat treatment;
and (3) after a certain amount of deformation is applied to the medium-entropy alloy ingot subjected to the first heat treatment, preserving the heat at 1100-1250 ℃ for 15-30 min, and then quenching to obtain the heat-treated high-performance iron-based medium-entropy alloy.
Preferably, the deformation amount is 20 to 40%.
Preferably, the as-cast medium-entropy alloy ingot is prepared by the following steps:
under the condition of inert atmosphere, raw materials of alloy components Al, Cr, Fe, Ni, Mo, W, Mn, Ti and C which are weighed according to the mole percentage of elements are smelted in a vacuum induction smelting furnace or a vacuum arc smelting furnace, and after the smelting is finished and the components are completely cooled, an alloy ingot is obtained; and then casting the alloy melt into a mould to obtain the as-cast medium-entropy alloy ingot.
More preferably, the temperature during smelting is 1500-1650 ℃.
Preferably, the heat treatment temperature is 1150-1250 ℃, and the heat preservation time is 15-600 min.
Preferably, the deformation is applied by cold rolling.
Compared with the prior art, the invention has the following beneficial effects:
the invention realizes the change of the composition of the as-cast alloy phase by adjusting the components, determines the effect of each alloy element on phase selection by an orthogonal test method, and defines the phase selection rule of the entropy alloy in the iron base for the first time. The research shows that the increase of the Al element content can increase the volume fraction of the B2 phase, the increase of the Ni element content can increase the volume fraction of the FCC phase, and meanwhile, the increase of the Cr and Fe contents can promote the formation of the BCC phase. Scientific guidance and performance prediction on alloy component design can be realized by utilizing the rule.
The cast alloy has high yield strength which is about 1.1GPa, and after the thermal mechanical treatment, the strength of the alloy is reduced to some extent, but the plasticity is greatly improved. Through a thermal mechanical treatment method, the strong plasticity of the alloy is balanced, and iron-based medium entropy alloy materials with different properties can be obtained by combining the design of components.
The heat treatment process provided by the invention has the advantages of low cost and simple process, and can further regulate and improve the performance of the iron-based medium entropy alloy.
Drawings
FIG. 1 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 1.
FIG. 2 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 1.
FIG. 3 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 2.
FIG. 4 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 2.
FIG. 5 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 3.
FIG. 6 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 3.
FIG. 7 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 4.
FIG. 8 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 4.
Detailed Description
The present invention is described in detail below with reference to the attached drawings and specific embodiments so that those skilled in the art can better understand the present invention and can implement the present invention, but the present invention is not limited by the examples.
A high-performance iron-based medium-entropy alloy comprises the following components in percentage by mole:
Al：12-20at％，Cr：8-12at％，Fe：35-55at％，Ni：25-45at％，Mo：0-3at％，W：0-2at％，Mn：0-1at％，C：0-0.02at％。
the Al, Cr, Fe and Ni raw materials used in the following examples were all industrial grade pure raw materials having a purity of 99 wt% or more.
Example 1
A high-performance iron-based medium-entropy alloy comprises the following components in percentage by mole:
Al：17at％，Cr：10at％，Fe：47at％，Ni：26at％。
a heat treatment method of a high-performance iron-based medium-entropy alloy comprises the following steps:
s1, ultrasonic cleaning: removing oxide skin on the surface of elements from Al, Cr, Fe and Ni alloy raw materials by using a mechanical grinding method, then placing the raw materials into different containers, adding alcohol solution, carrying out ultrasonic cleaning, taking out the raw materials, and blowing alcohol to dry to obtain the raw materials subjected to ultrasonic treatment;
s2, batching: respectively weighing S1 according to the mole percentage of the elements to obtain Al: 3.5767g, Cr: 4.0545g, Fe: 20.4677g, Ni: 11.9010g of raw materials and mixing;
s3: smelting: placing the mixed raw materials of S2 into a crucible of a vacuum non-consumable arc furnace, closing a furnace door, and vacuumizing to 3 multiplied by 10-3Back flushing high-purity argon to 0.06MPa after Pa; after arcing, firstly smelting a titanium ingot to absorb oxygen remaining in the furnace, then smelting the mixed raw material in S2, and simultaneously starting electromagnetic stirring, wherein the smelting current is 180A, the stirring current is 1A, the smelting temperature is 1600 ℃, and the smelting time is 2 min; after the sample is melted and completely cooled, turning over the sample, repeatedly melting for 4 times, keeping the alloy in a liquid state for 8min each time to uniformly mix the elements, and casting the alloy melt into a mold after the melting is finished to obtain an as-cast medium-entropy alloy ingot;
s4, after the cold rolling thickness deformation of the medium-entropy alloy ingot is about 30%, keeping the temperature at 1200 ℃ for 20min, and then quenching to obtain the medium-entropy alloy ingot subjected to the first heat treatment;
and (3) after the medium-entropy alloy ingot subjected to the first heat treatment is subjected to cold rolling to the thickness deformation of about 30%, keeping the temperature at 1200 ℃ for 20min, and then quenching to obtain the heat-treated high-performance iron-based medium-entropy alloy.
Example 2
A high-performance iron-based medium-entropy alloy comprises the following components in percentage by mole: al: 17at%, Cr: 10at%, Fe: 36at%, Ni: 36at%, Mo: 1 at%.
Example 3
A high-performance iron-based medium-entropy alloy comprises the following components in percentage by mole: al: 17at%, Cr: 10at%, Fe: 36at%, Ni: 36at%, Mo: 0.5 at%, W: 0.5 at%.
Example 4
A high-performance iron-based medium-entropy alloy comprises the following components in percentage by mole: al: 15 at%, Cr: 10at%, Fe: 49at%, Ni: 26 at%.
Example 5
A high-performance iron-based medium-entropy alloy comprises the following components in percentage by mole: al: 17at%, Cr: 10at%, Fe: 36at%, Ni: 35 at%, Mo: 0.5 at%, W: 0.5 at%, Mn: 0.5 at%, Ti: 0.49 at%, C: 0.01 at%.
The heat treatment method of the high-performance iron-based intermediate entropy alloy of examples 2 to 5 is basically the same as that of example 1, except that the raw material ratio is changed to the ratio of each example.
In order to illustrate various performances of the high-performance iron-based medium-entropy alloy and the heat treatment method provided by the invention, the cast-state medium-entropy alloy ingots and the heat-treated high-performance iron-based medium-entropy alloy provided by the embodiments 1 to 4 are subjected to related performance tests, and the related performance tests are shown in the figures 1 to 8.
Fig. 1 is a microstructure picture of an as-cast medium-entropy alloy ingot and a heat-treated high-performance iron-based medium-entropy alloy provided in example 1.
Wherein, fig. 1(a1) and fig. 1(a2) are microstructure pictures of as-cast medium-entropy alloy ingots under different magnifications;
FIGS. 1(b1) and 1(b2) are heat treated high performance iron-based entropy alloy microstructures at different magnifications;
FIGS. 1(a1) and 1(a2) are the as-cast structures of example 1, and it can be seen that the alloy consists of a fine amplitude modulated structure comprising BCC and B2. FIGS. 1(b1) and 1(b2) show the structure of example 1 after the thermomechanical treatment described, and it can be seen that the alloy is transformed into a homogeneous two-phase equiaxed structure.
FIG. 2 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 1.
As can be seen from FIG. 2, the as-cast alloy provided by the present invention has a very high yield strength of about 1.1 GPa. After the thermomechanical treatment, the strength of the alloy is reduced to some extent, but the plasticity is greatly improved. Through the thermal mechanical treatment method, the strong plasticity of the alloy is balanced, and the iron-based medium entropy alloy materials with different properties can be obtained by combining the design of components.
FIG. 3 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 2.
Wherein, fig. 3(a1) and fig. 3(a2) are as-cast medium entropy alloy ingot microstructure pictures under different magnifications;
FIGS. 3(b1) and 3(b2) are heat treated high performance iron-based entropy alloy microstructures at different magnifications;
FIGS. 3(a1) and 3(a2) show the as-cast structure of example 2, and it can be seen that the alloy is composed of a fine amplitude-modulated structure containing FCC and B2. Fig. 3(b1) and 3(b2) show the structure of example 2 after the thermomechanical treatment, and it can be seen that the alloy is transformed into a homogeneous two-phase equiaxed structure.
FIG. 4 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 2.
As can be seen from FIG. 4, the as-cast alloy provided by the present invention has a very high fracture strength of about 1.2 GPa. After the thermal mechanical treatment, the strength of the alloy is reduced to some extent, and the plasticity is improved to a certain extent. By the thermomechanical treatment method, the strength and the plasticity of the alloy are balanced, and the iron-based medium entropy alloy materials with different properties can be obtained by combining the design of components.
FIG. 5 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 3.
Wherein, fig. 5(a1) and 5(a2) are as-cast medium entropy alloy ingot microstructure pictures under different magnifications;
FIGS. 5(b1) and 5(b2) are heat treated high performance iron-based entropy alloy microstructures at different magnifications;
FIGS. 5(a1) and 5(a2) show the as-cast structure of example 3, and it can be seen that the alloy is composed of a fine amplitude-modulated structure containing FCC and B2. FIGS. 5(b1) and 5(b2) show the structure of example 3 after the thermomechanical treatment, and it can be seen that the alloy is transformed into a homogeneous two-phase equiaxed structure.
FIG. 6 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 3.
As can be seen from FIG. 6, the as-cast alloy provided by the present invention has a very high fracture strength of about 1.1 GPa. After the thermomechanical treatment, the strength of the alloy is reduced, but the plasticity is greatly improved. By the thermomechanical treatment method, the strength and the plasticity of the alloy are balanced, and the iron-based medium entropy alloy materials with different properties can be obtained by combining the design of components.
FIG. 7 is a microstructure photograph of an as-cast intermediate entropy alloy ingot and a heat treated high performance iron-based intermediate entropy alloy provided in example 4.
Wherein, FIGS. 7(a1) and 7(a2) are as-cast microstructure pictures of the medium entropy alloy ingot at different magnifications;
FIGS. 7(b1) and 7(b2) are heat treated high performance iron-based entropy alloy microstructures at different magnifications;
FIGS. 7(a1) and 7(a2) are the as-cast structures of example 4, and it can be seen that the alloy consists of a fine amplitude modulated structure comprising BCC and B2. FIGS. 7(b1) and 7(b2) show the structure of example 4 after the thermomechanical treatment, and it can be seen that the alloy transforms into a homogeneous two-phase equiaxed structure.
FIG. 8 is a stress-strain curve at room temperature for the as-cast mid-entropy alloy ingot and the heat-treated high performance iron-based mid-entropy alloy provided in example 4.
As can be seen from FIG. 8, the as-cast alloy provided by the present invention has a very high fracture strength of about 1.3 GPa. After the thermomechanical treatment, the strength of the alloy is reduced, but the plasticity is greatly improved. Through the thermal mechanical treatment method, the strong plasticity of the alloy is balanced, and the iron-based medium entropy alloy materials with different properties can be obtained by combining the design of components.
In conclusion, the invention realizes the change of the composition of the as-cast alloy phase by adjusting the components, determines the effect of each alloy element on phase selection by an orthogonal test method, and defines the phase selection rule of the iron-based intermediate entropy alloy for the first time. The research shows that the increase of Al element content can increase the volume fraction of B2 phase, while the increase of Ni element content can increase the volume fraction of FCC phase, and at the same time, the increase of Cr and Fe content has the promotion effect on the formation of BCC phase. Scientific guidance and performance prediction on alloy component design can be realized by utilizing the rule.
The heat treatment process provided by the invention has the advantages of low cost and simple process, and can further regulate and improve the performance of the iron-based medium entropy alloy.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (5)
1. A high-performance iron-based medium-entropy alloy is characterized by comprising the following components in percentage by mole:
Al：12-20at%，Cr：8-12at%，Fe：35-55at%，Ni：25-45at%，Mo：0-3at%，W：0-2at%，Mn：0-5at%，Ti：0-3at%，C：0-0.2at%；
the heat treatment method of the high-performance iron-based medium entropy alloy comprises the following steps:
after a certain amount of deformation is applied to the as-cast intermediate entropy alloy ingot, preserving heat at 1100-1250 ℃ for 15-30 min, and then quenching to obtain an intermediate entropy alloy ingot subjected to first heat treatment;
after a certain amount of deformation is applied to the medium-entropy alloy ingot subjected to the first heat treatment, keeping the temperature at 1100-1250 ℃ for 15-30 min, and then quenching to obtain the heat-treated high-performance iron-based medium-entropy alloy;
the deformation amount is 20-40%.
2. The high performance iron-based entropy alloy of claim 1, consisting of, in mole percent: al: 15-17 at%, Cr: 10at%, Fe: 36-49 at%, Ni: 26-36 at%, Mo: 0-3at%, W: 0-2at%, Mn: 0 to 5at%, Ti: 0-3at%, C: 0 to 0.2 at%.
3. The high-performance iron-based entropy alloy according to claim 1, wherein the as-cast entropy alloy ingot is prepared by the following steps:
under the condition of inert atmosphere, raw materials of alloy components Al, Cr, Fe, Ni, Mo, W, Mn, Ti and C which are weighed according to the mole percentage of elements are smelted in a vacuum induction smelting furnace or a vacuum electric arc, and after the smelting is finished, the alloy melt is cast into a mold, so that the as-cast intermediate-entropy alloy ingot is obtained.
4. The high-performance iron-based medium entropy alloy according to claim 3, wherein a temperature during melting is 1500-1650 ℃.
5. The high-performance iron-based medium entropy alloy of claim 1, wherein the deformation is applied by cold rolling.
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| PCT/CN2022/114978 WO2023030171A1 (en) | 2021-08-31 | 2022-08-26 | High-performance iron-based medium-entropy alloy, heat treatment method therefor and application thereof |
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| CN114774785B (en) * | 2022-04-11 | 2023-01-17 | 郑州大学 | Iron-based medium-entropy alloy |
| CN115627405B (en) * | 2022-10-21 | 2024-02-27 | 中国科学院金属研究所 | Liquid lead bismuth corrosion-resistant high-entropy alloy and preparation method thereof |
| CN115786793B (en) * | 2022-11-18 | 2023-12-08 | 广州大学 | Light medium-entropy alloy with excellent mechanical properties and preparation method thereof |
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| US20200109467A1 (en) * | 2018-10-04 | 2020-04-09 | City University Of Hong Kong | High entropy alloy structure and a method of preparing the same |
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