CN114427060A - Fe reinforced by TiC dispersed phase50Mn25Ni10Cr15Method for medium entropy alloying - Google Patents
Fe reinforced by TiC dispersed phase50Mn25Ni10Cr15Method for medium entropy alloying 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
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
-
- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
-
- 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
-
- 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
- C21D6/005—Heat treatment of ferrous alloys containing Mn
-
- 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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
-
- 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
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
-
- 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
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
Abstract
The invention discloses a method for reinforcing Fe by utilizing TiC dispersed phase50Mn25Ni10Cr15A method of medium entropy alloying, relating to Fe50Mn25Ni10Cr15The field of intermediate entropy alloy engineering application. Strengthening Fe by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy comprises the following steps: (1) selecting FeC alloy as raw materialMn, Cr, Ni, Ti according to the expression (Fe)50Mn25Ni10Cr15)100‑x(TiC)x(x is more than 0 and less than or equal to 1.5, and x is the atomic percentage content), weighing and proportioning, smelting all the raw materials together to obtain alloy liquid, and casting and molding the alloy liquid to obtain the alloy ingot. (2) Carrying out homogenization annealing treatment on the alloy ingot; (3) rolling or forging the alloy ingot to obtain an alloy plate; (4) carrying out recrystallization annealing treatment on the alloy plate to obtain Fe with TiC dispersed phases uniformly distributed on the matrix phase of the face-centered cubic structure50Mn25Ni10Cr15And (3) medium-entropy alloy. Fe prepared by the invention50Mn25Ni10Cr15The yield strength of the medium-entropy alloy is greatly improved, and the necessary plasticity and the low-cost advantage of no Co element are retained, so that the medium-entropy alloy has important significance for developing the low-cost high-strength medium-entropy alloy.
Description
Technical Field
The invention relates to Fe50Mn25Ni10Cr15The field of application of medium-entropy alloy engineering, in particular to a method for reinforcing Fe by utilizing TiC dispersed phase50Mn25Ni10Cr15A method of medium entropy alloy.
Background
Currently, a medium/high entropy alloy of a face centered cubic structure (FCC) is widely studied due to its excellent mechanical properties at room temperature and low temperature. Through reasonable components and processing technology design, the medium/high entropy alloy shows high plasticity, high strength, good wear resistance and other properties, so that the medium/high entropy alloy has great application potential in important fields of high-energy physics, nuclear energy, aerospace and the like.
In various medium/high entropy alloy series, Co element is contained. The Co element is a strategic resource, and its reserve on the earth is very limited, so it is expensive. This indirectly increases the cost of the medium/high entropy alloy, and hinders the application of the medium/high entropy alloy in engineering. Therefore, Co-free medium entropy alloys were developed and designed.
For example, in patent publication CN 110952041B, an invention of Fe-Mn-Ni-Cr IVIn the component high-entropy alloy, Fe without Co element is developed50Mn25Ni10Cr15The medium entropy alloy greatly reduces the cost.
But Fe50Mn25Ni10Cr15The medium-entropy alloy has redundant plasticity and lower strength, and particularly has lower yield strength and yield ratio.
The yield strength is the yield limit of metal when yielding, and when the metal is acted by an external force greater than the yield strength, the metal can be permanently deformed; the metal will also recover its original shape when subjected to an external force less than the yield strength.
Yield ratio refers to the ratio of the yield strength to the tensile strength of a material. Tensile strength is the maximum load bearing capacity of a metal under static tensile conditions. A high yield ratio indicates that the material has strong deformation resistance and is not easy to generate plastic deformation.
Fe50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy are low, and the requirement of engineering application is difficult to meet, so that the medium-entropy alloy is very limited in engineering application.
Therefore, how to retain Fe50Mn25Ni10Cr15The yield strength and the yield ratio of the medium entropy alloy can be improved while the medium entropy alloy has necessary plasticity, and the medium entropy alloy is a technical problem to be solved urgently by technical personnel in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for reinforcing Fe by utilizing TiC dispersed phase50Mn25Ni10Cr15Method for intermediate entropy alloying, by which method Fe is retained50Mn25Ni10Cr15The yield strength and the yield ratio of the medium-entropy alloy can be improved while the medium-entropy alloy has necessary plasticity.
In order to achieve the purpose, the invention provides the following technical scheme:
fe enhanced by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy comprises the following steps:
(1) selectingTaking FeC alloy, Mn, Cr, Ni and Ti as raw materials, and performing reaction according to an expression (Fe)50Mn25Ni10Cr15)100-x(TiC)x(x is more than 0 and less than or equal to 1.5, and x is the atomic percentage content), weighing and proportioning, smelting all the raw materials together to obtain alloy liquid, and casting and molding the alloy liquid to obtain an alloy ingot;
(2) carrying out homogenization annealing treatment on the alloy ingot;
(3) rolling or forging the alloy ingot to obtain an alloy plate;
(4) carrying out recrystallization annealing treatment on the alloy plate to obtain Fe with TiC dispersed phases uniformly distributed on the matrix phase of the face-centered cubic structure50Mn25Ni10Cr15And (3) medium-entropy alloy.
Further, in the step (1), the purities of FeC alloy, Mn, Cr, Ni and Ti as raw materials are all more than 99.5%.
Further, in the step (1), after the raw materials of FeC alloy, Mn, Cr, Ni, and Ti are weighed, the raw materials of FeC alloy, Mn, Cr, Ni, and Ti need to be placed in absolute ethanol for ultrasonic cleaning.
Further, in the step (1), raw materials of FeC alloy, Mn, Cr, Ni and Ti are sequentially placed in a water-cooled copper crucible of a vacuum arc melting furnace in the order of melting point from low to high to be melted together.
Further, in the step (1), the raw materials of FeC alloy, Mn, Cr, Ni, and Ti need to be turned over several times during smelting.
Further, in the step (1), when the molten alloy is cast and formed, the molten alloy needs to be suction-cast into a water-cooled copper mold for solidification.
Further, in the step (2), the alloy ingot is placed in a muffle furnace for homogenization annealing, and then water quenching is carried out, wherein the homogenization annealing temperature is 900-1000 ℃, and the homogenization annealing time is 30-45 min.
Further, in the step (3), forging or rolling is performed at room temperature according to the maximum deformation amount that the alloy ingot can withstand.
Further, in the step (4), the alloy ingot is placed in a muffle furnace to be subjected to recrystallization annealing treatment, wherein the temperature of the recrystallization annealing treatment is 700-900 ℃, and the time of the recrystallization annealing treatment is 3-5 min.
Compared with the prior art, the invention has the beneficial effects that:
1. fe obtained in the background art patent50Mn25Ni10Cr15The medium entropy alloy does not contain Co element, so the cost is greatly reduced, and Fe50Mn25Ni10Cr15The medium entropy alloy has the advantage of low cost. And, Fe50Mn25Ni10Cr15The medium-entropy alloy has excellent plasticity, but low yield strength and low yield ratio.
Therefore Fe50Mn25Ni10Cr15The medium entropy alloy has excellent plasticity, lower yield strength and lower yield ratio because of Fe50Mn25Ni10Cr15The medium entropy alloy is a single-phase alloy with a face-centered cubic structure. At room temperature and low temperature, the face-centered cubic structure has more slippage, and dislocation is easy to slip in the stretching process, so that the alloy has excellent plasticity and also has lower yield strength and yield ratio.
Fe50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy are low, and the requirement of engineering application is difficult to meet, so that the medium-entropy alloy is very limited in engineering application.
In the invention, FeC alloy, Mn, Cr, Ni and Ti are smelted together in the step (1) and then cast for molding, so that TiC dispersed phase reinforced Fe can be obtained50Mn25Ni10Cr15The existence of the medium entropy alloy and TiC disperse phase can realize that TiC dispersion is opposite to Fe50Mn25Ni10Cr15The second phase of the medium entropy alloy is strengthened. When the recrystallization annealing treatment of the step (4) is further performed on the basis of the step (1), fine grain strengthening can be achieved by utilizing a TiC dispersed phase.
Second phase strengthening means that TiC is used as a dispersed phase, namely, the second phase is uniformly distributed in Fe with a face-centered cubic structure50Mn25Ni10Cr15In the medium entropy alloy, TiC dispersed phase hinders the sliding movement in the face-centered cubic structure, thereby leading Fe50Mn25Ni10Cr15The medium entropy alloy is remarkably strengthened, namely, Fe can be improved50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy can reduce the plasticity of the medium-entropy alloy, but can keep the plasticity of the medium-entropy alloy.
As is clear from the tendency of the changes of (a), (b), (c) and (d) in FIG. 2, the existence of the TiC dispersed phase can inhibit the grain boundary migration and reduce the grain growth rate, thereby inhibiting the grain growth during the recrystallization annealing treatment and refining Fe50Mn25Ni10Cr15Grains, thereby increasing grain boundaries which can block the movement of slip, thereby making Fe50Mn25Ni10Cr15The medium entropy alloy is strengthened, i.e. Fe can be increased50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy can reduce the plasticity of the medium-entropy alloy, but can keep the plasticity of the medium-entropy alloy.
In sum, with Fe50Mn25Ni10Cr15Compared with the single-phase alloy of the medium-entropy alloy, the invention utilizes TiC dispersed phase to strengthen Fe50Mn25Ni10Cr15And (3) medium-entropy alloy. On one hand, the advantages of no Co element can be maintained, the cost is saved, and the popularization and application of Fe are facilitated50Mn25Ni10Cr15Medium entropy alloy; on the other hand, it is possible to realize Fe by utilizing TiC dispersed phase50Mn25Ni10Cr15Second phase strengthening and fine grain strengthening of the medium entropy alloy to facilitate retention of Fe50Mn25Ni10Cr15While the necessary plasticity of the medium-entropy alloy is realized, the yield strength and the yield ratio of the medium-entropy alloy can be improved, and Fe is facilitated50Mn25Ni10Cr15Popularization of the medium entropy alloy in engineering application.
2. In the step (1), the invention adopts FeC alloy, Mn, Cr, Ni and Ti with the purity of more than 99.5 percent,can improve Fe50Mn25Ni10Cr15The product quality of the medium entropy alloy.
3. In the step (1), FeC alloy, Mn, Cr, Ni and Ti which are used as raw materials are placed in absolute ethyl alcohol for ultrasonic cleaning, so that oil stains and other impurities on the surface of the raw materials can be removed, and Fe can be improved conveniently50Mn25Ni10Cr15The product quality of the medium entropy alloy.
4. According to the invention, in the step (1), FeC alloy, Mn, Cr, Ni and Ti which are raw materials are sequentially placed according to the sequence of the melting points from low to high, so that the volatilization of the low-melting-point raw materials can be reduced, the raw materials can be saved, the cost can be reduced, and the resources can be saved.
5. In the step (1), the FeC alloy, Mn, Cr, Ni and Ti are turned over for multiple times, so that Fe can be increased50Mn25Ni10Cr15The component uniformity of the medium-entropy alloy is favorable for improving Fe50Mn25Ni10Cr15The product quality of the medium entropy alloy.
6. The invention can realize the homogenization of the matrix composition by arranging the step of homogenization annealing so as to lead Fe to be convenient50Mn25Ni10Cr15The mechanical property of the medium entropy alloy is more uniform, and the Fe is improved50Mn25Ni10Cr15The product quality of the medium entropy alloy.
7. In the step (3) of the present invention, the maximum deformation amount can be ensured by forging or rolling according to the maximum deformation amount that the alloy ingot can bear, and at this time, the defects such as dislocation and the like in the alloy ingot are the largest, and the finer the structure after recrystallization annealing is, thereby further improving Fe50Mn25Ni10Cr15Yield strength and yield ratio of the medium entropy alloy.
8. Compared with the prior art patent, in the step (4) of the invention, the holding time of recrystallization annealing is shorter, so that the recrystallization time is short, the obtained crystal grains are not too long, and the Fe is further refined50Mn25Ni10Cr15Medium entropy alloy grains, thereby further increasingThe grain boundary can block the sliding movement, thereby further leading the Fe50Mn25Ni10Cr15The medium entropy alloy is strengthened.
Drawings
FIG. 1 is a diagram of Fe containing 0% TiC, 0.5% TiC, 1.0% TiC, 1.5% TiC50Mn25Ni10Cr15XRD pattern of the medium entropy alloy;
FIG. 2 shows Fe with different TiC contents50Mn25Ni10Cr15An EBSD antipole map of the medium entropy alloy, wherein (a) 0% TiC, (b) 0.5% TiC, (c) 1.0% TiC, (d) 1.5%;
FIG. 3 is Fe with 0% TiC50Mn25Ni10Cr15A drawing curve of the medium entropy alloy;
FIG. 4 is Fe with 0.5% TiC50Mn25Ni10Cr15A drawing curve of the medium entropy alloy;
FIG. 5 is Fe with 1.0% TiC50Mn25Ni10Cr15A drawing curve of the medium entropy alloy;
FIG. 6 is Fe with 1.5% TiC50Mn25Ni10Cr15Drawing plots of medium entropy alloys.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
fe enhanced by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy comprises the following steps:
(1) smelting and suction casting: firstly, selecting raw materials Fe, Mn, Cr and Ni with the purity of more than 99.9 percent, and mixing the raw materials Fe, Mn, Cr and Ni according to the weight ratioAccording to the expression Fe50Mn25Ni10Cr15And weighing and proportioning. When the ingredients are weighed, the atomic ratio is converted into the weight ratio, and then the ingredients are weighed by an electronic balance.
Then, the raw materials Fe, Mn, Cr and Ni are placed in absolute ethyl alcohol for ultrasonic cleaning for 5min, and impurities such as oil stains on the surface of the raw materials are removed.
Next, the raw materials Fe, Mn, Cr, and Ni are put into a water-cooled copper crucible of a vacuum arc melting furnace, and note that the raw materials Fe, Mn, Cr, and Ni are put into the water-cooled copper crucible in order of melting point from low to high, that is, Mn, Fe, Ni, and Cr are put in order from bottom to top, and volatilization of the low-melting raw material can be reduced.
Then, the cavity of the arc melting furnace is vacuumized to 5 multiplied by 10-3Introducing inert protective gas argon of 0.05MPa after the MPa, and during smelting, turning over and smelting the raw materials Mn, Cr, Ni and Ti for 4 times to ensure the component uniformity of the alloy.
And finally, carrying out suction casting on the alloy liquid to a cylindrical water-cooled copper mold with the height of 40mm multiplied by 10mm for solidification to obtain a cylindrical alloy ingot.
(2) Homogenizing and annealing: and heating the alloy ingot in a muffle furnace at 900 ℃ for 30min, and then performing water quenching.
(3) Rolling: rolling the alloy ingot after the homogenization annealing treatment to about 2mm at room temperature, wherein the reduction is about 80%, and the calculation process of the reduction is as follows: an alloy sheet was obtained by using (10-2)/10 × 100%: 0.8 × 100%: 80%.
(4) And (3) recrystallization annealing: and (3) preserving the temperature of the alloy plate in a muffle furnace at 900 ℃ for 3min, and then performing water quenching.
Through the steps, the (Fe) can be prepared50Mn25Ni10Cr15)100(TiC)0Intermediate entropy alloys, i.e. Fe50Mn25Ni10Cr15And (3) medium-entropy alloy. Then on (Fe)50Mn25Ni10Cr15)100(TiC)0And (5) carrying out mechanical property test on the medium entropy alloy.
Using wire-electrode cutting (Fe)50Mn25Ni10Cr15)100(TiC)0The medium entropy alloy is prepared by taking a tensile sample of a clavicle shape with the thickness of 50mm multiplied by 4mm multiplied by 2mm, and polishing the sample by No. 1500 metallographic abrasive paper for brightness. The treated sample was subjected to a tensile test at a tensile rate of 0.0075 mm/min.
(Fe50Mn25Ni10Cr15)100(TiC)0The XRD pattern of the medium entropy alloy is shown as 0% TiC in figure 1, and (Fe)50Mn25Ni10Cr15)100(TiC)0The medium entropy alloy exists only in FCC (face centered cubic) phase.
(Fe50Mn25Ni10Cr15)100(TiC)0The EBSD photograph of the medium entropy alloy is shown in FIG. 2(a), and it can be seen that (Fe)50Mn25Ni10Cr15)100(TiC)0The medium entropy alloy is a single FCC phase and has coarse grains.
(Fe50Mn25Ni10Cr15)100(TiC)0The tensile curve of the medium entropy alloy is shown in FIG. 3, and it can be seen that (Fe)50Mn25Ni10Cr15)100(TiC)0The yield strength of the medium entropy alloy is 251MPa, the tensile strength is 543MPa, the elongation after fracture is about 60%, and the yield ratio is 0.46.
Example 2:
fe enhanced by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy comprises the following steps:
(1) smelting and suction casting: firstly, selecting raw material Fe with purity of more than 99.9 percent95C5Alloy, Mn, Cr, Ni, Ti. The raw materials are expressed by the expression (Fe)50Mn25Ni10Cr15)99.5(TiC)0.5And weighing and proportioning. When the ingredients are weighed, the atomic ratio is converted into the weight ratio, and then the ingredients are weighed by an electronic balance.
Then, the raw material Fe95C5Ultrasonic cleaning alloy, Mn, Cr, Ni, and Ti in anhydrous ethanol for 5min to remove impurities such as oil stain on the surface of raw material。
Then, the raw material Fe95C5Alloy, Mn, Cr, Ni, Ti were put into a water-cooled copper crucible of a vacuum arc melting furnace, and attention was paid to Fe as a raw material95C5The alloy, Mn, Cr, Ni and Ti are sequentially placed in a water-cooled copper crucible from low melting point to high melting point, namely Mn and Fe are sequentially placed from bottom to top95C5Alloy, Ti, Ni and Cr can reduce the volatilization of low-melting-point raw materials.
Then, the cavity of the arc melting furnace is vacuumized to 5 multiplied by 10-3Introducing inert protective gas argon of 0.05MPa after the MPa, and when smelting, needing to lead the raw material Fe95C5The alloy, Mn, Cr, Ni and Ti are all smelted in a forward and reverse overturning way for 4 times so as to ensure the component uniformity of the alloy.
And finally, casting the alloy liquid in a cylindrical water-cooled copper mold with the height of 40mm multiplied by 10mm for solidification to obtain a cylindrical alloy ingot.
(2) Homogenizing and annealing: and heating the alloy ingot in a muffle furnace at 900 ℃ for 30min, and then performing water quenching.
(3) Rolling: rolling the alloy ingot after the homogenizing annealing treatment to about 2.86mm at room temperature, wherein the reduction is about 71.4%, and the calculation process of the reduction is as follows: (10-2.86)/10 × 100%: 0.714 × 100%: 71.4%, to obtain an alloy sheet.
(4) And (3) recrystallization annealing: and (3) preserving the temperature of the alloy plate in a muffle furnace at 900 ℃ for 3min, and then performing water quenching.
Through the steps, the (Fe) can be prepared50Mn25Ni10Cr15)99.5(TiC)0.5And (3) medium-entropy alloy. Then on (Fe)50Mn25Ni10Cr15)99.5(TiC)0.5And (5) carrying out mechanical property test on the medium entropy alloy.
Using wire-electrode cutting (Fe)50Mn25Ni10Cr15)99.5(TiC)0.5The medium entropy alloy is prepared by taking a tensile sample of a clavicle shape with the thickness of 50mm multiplied by 4mm multiplied by 2mm, and polishing the sample by No. 1500 metallographic abrasive paper for brightness. The treated sample was subjected to a tensile test at a tensile rate of 0.0075 mm/min.
(Fe50Mn25Ni10Cr15)99.5(TiC)0.5The XRD pattern of the medium entropy alloy is shown as 0.5% TiC in figure 1, and it can be seen that the diffraction peak of the TiC phase begins to appear except for the matrix FCC phase.
(Fe50Mn25Ni10Cr15)99.5(TiC)0.5The EBSD photograph of the intermediate entropy alloy is shown in FIG. 2(b), and it can be seen that the grains of the alloy start to be significantly refined after 0.5% TiC is added.
(Fe50Mn25Ni10Cr15)99.5(TiC)0.5The tensile curve of the medium entropy alloy is shown in FIG. 4, and it can be seen that (Fe)50Mn25Ni10Cr15)99.5(TiC)0.5The yield strength of the medium entropy alloy is 452MPa, the tensile strength is 664MPa, the elongation after fracture is 46%, and the yield ratio is 0.68.
Fe prepared in example 150Mn25Ni10Cr15Medium entropy alloy comparison (Fe)50Mn25Ni10Cr15)99.5(TiC)0.5The medium-entropy alloy has better strength and plasticity. Specifically, (Fe)50Mn25Ni10Cr15)99.5(TiC)0.5The yield strength of the medium-entropy alloy is improved by 80%, the tensile strength is improved by 22.3%, the yield ratio is improved by 48%, and the strengthening effect is obvious; the elongation after fracture was excellent although it was reduced.
Example 3:
fe enhanced by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy comprises the following steps:
(1) smelting and suction casting: firstly, selecting raw material Fe with purity of more than 99.9 percent95C5Alloy, Mn, Cr, Ni and Ti, and the raw materials are expressed by the expression (Fe)50Mn25Ni10Cr15)99.0(TiC)1.0And weighing and proportioning. When the ingredients are weighed, the atomic ratio is converted into the weight ratio, and then the ingredients are weighed by an electronic balance.
Then, the raw material Fe95C5And (3) placing the alloy, Mn, Cr, Ni and Ti in absolute ethyl alcohol for ultrasonic cleaning for 5min to remove impurities such as oil stains on the surface of the raw material.
Then, Fe is added95C5Alloy, Mn, Cr, Ni and Ti are put into a water-cooled copper crucible of a vacuum arc melting furnace, and Mn and Fe are sequentially placed from bottom to top95C5Alloy, Ti, Ni and Cr can reduce the volatilization of low-melting-point raw materials.
Then, the cavity of the arc melting furnace is vacuumized to 5 multiplied by 10-3Introducing inert protective gas argon of 0.05MPa after the MPa, and when smelting, needing to lead the raw material Fe95C5The alloy, Mn, Cr, Ni and Ti are all smelted in a forward and reverse overturning way for 4 times so as to ensure the component uniformity of the alloy.
And finally, casting the alloy liquid in a cylindrical water-cooled copper mold with the height of 40mm multiplied by 10mm for solidification to obtain a cylindrical alloy ingot.
(2) Homogenizing and annealing: and heating the alloy ingot in a muffle furnace at 1000 ℃ for 45min, and then performing water quenching.
(3) Rolling: rolling the alloy ingot after the homogenizing annealing treatment to about 3.34mm at room temperature, wherein the reduction is about 66.6%, and the calculation process of the reduction is as follows: (10-3.34)/10 × 100%: 0.666 × 100%: 66.6%, to obtain an alloy sheet.
(4) And (3) recrystallization annealing: and (3) preserving the temperature of the alloy plate in a muffle furnace at 700 ℃ for 5min, and then performing water quenching.
Through the steps, the (Fe) can be prepared50Mn25Ni10Cr15)99.0(TiC)1.0And (3) medium-entropy alloy. Then on (Fe)50Mn25Ni10Cr15)99.0(TiC)1.0And (5) carrying out mechanical property test on the medium entropy alloy.
Using wire-electrode cutting (Fe)50Mn25Ni10Cr15)99.0(TiC)1.0The medium entropy alloy is prepared by taking a tensile sample of a clavicle shape with the thickness of 50mm multiplied by 4mm multiplied by 2mm, and polishing the sample by No. 1500 metallographic abrasive paper for brightness. The treated sample was subjected to a tensile test at a tensile rate of 0.0075 mm/min.
(Fe50Mn25Ni10Cr15)99.0(TiC)1.0The XRD pattern of the medium entropy alloy is shown as 1.0% TiC in figure 1, and the diffraction peak of the TiC phase is obvious except for the matrix FCC phase.
(Fe50Mn25Ni10Cr15)99.0(TiC)1.0The EBSD photograph of the medium entropy alloy is shown in fig. 2(c), and it can be seen that 1.0% TiC can make the alloy grains significantly fine and uniform in size.
(Fe50Mn25Ni10Cr15)99.0(TiC)1.0The tensile curve of the medium entropy alloy is shown in FIG. 5, and it can be seen that (Fe)50Mn25Ni10Cr15)99.0(TiC)1.0The yield strength of the medium entropy alloy is 544MPa, the tensile strength is 726MPa, the elongation after fracture is 38%, and the yield ratio is 0.75.
Fe prepared in example 150Mn25Ni10Cr15Medium entropy alloy ratio. (Fe)50Mn25Ni10Cr15)99.0(TiC)1.0The medium-entropy alloy has better strength and plasticity. Specifically, (Fe)50Mn25Ni10Cr15)99.0(TiC)1.0The yield strength of the medium entropy alloy is improved by 117%, the tensile strength is improved by 33.7%, the yield ratio is improved by 63%, and the strengthening effect is obvious. Although the elongation after fracture was reduced by about 50%, the plasticity was still excellent.
Example 4:
fe enhanced by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy comprises the following steps:
(1) smelting and suction casting: firstly, selecting raw materials of Fe95C5 alloy, Mn, Cr, Ni and Ti with the purity of more than 99.9 percent. Raw materials are expressed as (Fe)50Mn25Ni10Cr15)98.5(TiC)1.5And weighing and proportioning, converting into a weight ratio according to an atomic ratio, and weighing by using an electronic balance.
Then, the raw material Fe95C5And (3) placing the alloy, Mn, Cr, Ni and Ti in absolute ethyl alcohol for ultrasonic cleaning for 5min to remove impurities such as oil stains on the surface of the raw material.
Then, the raw material Fe95C5Alloy, Mn, Cr, Ni, Ti were put into a water-cooled copper crucible of a vacuum arc melting furnace, and attention was paid to Fe as a raw material95C5The alloy, Mn, Cr, Ni and Ti are sequentially placed in a water-cooled copper crucible from low melting point to high melting point, namely Mn and Fe are sequentially placed from bottom to top95C5Alloy, Ti, Ni and Cr can reduce the volatilization of low-melting-point raw materials.
Then, the cavity of the arc melting furnace is vacuumized to 5 multiplied by 10-3Introducing inert protective gas argon of 0.05MPa after the MPa, and when smelting, needing to lead the raw material Fe95C5The alloy, Mn, Cr, Ni and Ti are all smelted in a forward and reverse overturning way for 4 times so as to ensure the component uniformity of the alloy.
And finally, casting the alloy liquid in a cylindrical water-cooled copper mold with the height of 40mm multiplied by 10mm for solidification to obtain a cylindrical alloy ingot.
(2) Homogenizing and annealing: and heating the alloy ingot in a muffle furnace at 1000 ℃ for 30min, and then performing water quenching.
(3) Rolling: rolling the alloy ingot after the homogenizing annealing treatment to about 4.4mm at room temperature, wherein the reduction is about 56%, and the calculation process of the reduction is as follows: (10-4.4)/10 × 100%: 0.56 × 100%: 56%, to obtain an alloy sheet.
(4) And (3) recrystallization annealing: and (3) preserving the temperature of the alloy plate in a muffle furnace at 800 ℃ for 5min, and then performing water quenching.
Through the steps, the (Fe) can be prepared50Mn25Ni10Cr15)98.5(TiC)1.5And (3) medium-entropy alloy. Then on (Fe)50Mn25Ni10Cr15)98.5(TiC)1.5And (5) carrying out mechanical property test on the medium entropy alloy.
Using wire-electrode cutting (Fe)50Mn25Ni10Cr15)98.5(TiC)1.5The medium entropy alloy is prepared from 50mm × 4mm × 2mm clavicleThe tensile sample is polished to be bright by No. 1500 metallographic abrasive paper. The treated sample was subjected to a tensile test at a tensile rate of 0.0075 mm/min.
(Fe50Mn25Ni10Cr15)98.5(TiC)1.5The XRD pattern of the medium entropy alloy is shown as 1.5% TiC in figure 1, and the diffraction peak of the TiC phase is obvious except for the matrix FCC phase.
(Fe50Mn25Ni10Cr15)98.5(TiC)1.5The EBSD photograph of the medium entropy alloy is shown in FIG. 2(d), and it can be seen that 1.5% TiC is added to start to aggregate and grow, the grain refining effect is poor, but the strengthening effect is good.
(Fe50Mn25Ni10Cr15)98.5(TiC)1.5The tensile curve of the medium entropy alloy is shown in FIG. 6, and it can be seen that (Fe)50Mn25Ni10Cr15)98.5(TiC)1.5The yield strength of the medium entropy alloy is 670MPa, the tensile strength is 763MPa, the elongation after fracture is 9.6%, and the yield ratio is 0.88.
Fe prepared in example 150Mn25Ni10Cr15Medium entropy alloy ratio. (Fe)50Mn25Ni10Cr15)98.5(TiC)1.5The medium entropy alloy has good comprehensive mechanical properties of strength and plasticity. Specifically, (Fe)50Mn25Ni10Cr15)98.5(TiC)1.5The yield strength of the medium-entropy alloy is improved by 167%, the tensile strength is improved by 40.5%, the yield ratio is improved by 91%, and the strengthening effect is remarkable. Although the elongation after fracture was reduced to 10%, the plasticity was maintained.
The examples summarize:
in the first aspect, the present invention is based on Fe as shown in step (1) of examples 2 to 495C5The alloy, Mn, Cr, Ni and Ti are smelted together in a vacuum arc smelting furnace and then cast into a mold. The patent of background technology is that four raw materials of Fe, Mn, Cr and Ni are smelted together in a vacuum arc smelting furnace and then cast into a mold.
The invention can lead Fe to be95C5The alloy and Ti are subjected to a replacement reaction to generate Fe and TiC, and the components of TiC, Fe, Mn, Cr and Ni are fully smelted into a whole so as to obtain Fe with a TiC dispersed phase distributed on a matrix phase of a face-centered cubic structure50Mn25Ni10Cr15And (3) medium-entropy alloy. The TiC dispersed phase hinders the sliding movement in the face-centered cubic structure, thereby leading Fe50Mn25Ni10Cr15The medium entropy alloy is remarkably strengthened, namely, Fe can be improved50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy can reduce the plasticity of the medium-entropy alloy, but can keep the plasticity of the medium-entropy alloy.
In the second aspect, as can be seen from the step (2) in the embodiments 2 to 4, the present invention realizes the uniform annealing of the alloy ingot by heating the alloy ingot in a muffle furnace at 900-1000 ℃ for 30 to 45min and then water quenching. The prior art patent does not have a step of homogenizing annealing.
The homogenizing annealing is mainly realized by atomic diffusion at high temperature to homogenize the matrix composition so as to lead Fe to be convenient50Mn25Ni10Cr15The mechanical property of the medium entropy alloy is more uniform, and the Fe is improved50Mn25Ni10Cr15The product quality of the medium entropy alloy.
In the third aspect, as can be seen from the step (3) in the embodiments 2 to 4, the forging or rolling process is performed according to the maximum deformation amount that the alloy ingot can bear on the premise of ensuring that the alloy ingot does not crack. The maximum deformation amount which can be borne by the alloy ingot can be determined through tests, and when the first crack occurs in the alloy ingot, the maximum deformation amount which can be borne by the alloy ingot is determined. In the background art patent, a suction cast alloy sample is rolled on a rolling mill, the rolling deformation is 0.5mm or 0.6mm each time, and the final total rolling deformation is 50% of the original thickness of the sample.
Rolling or forging is a necessary step to improve the internal structure of this cast piece of the alloy ingot. Forging or rolling must be present to improve the quality of the alloy ingot. Forging or rolling with maximum deformation bearable by alloy ingotThe treatment can ensure that the deformation is maximum, the defects such as dislocation and the like in the alloy ingot are maximum, and the structure is finer after recrystallization annealing, thereby further improving the Fe content50Mn25Ni10Cr15Yield strength and yield ratio of the medium entropy alloy.
In the fourth aspect, as can be seen from the step (4) in the embodiments 2-4, the rolled alloy plate is subjected to heat preservation in an annealing furnace cavity at the temperature of 700-50Mn25Ni10Cr15And (3) medium-entropy alloy. In the patent of background technology, the rolled alloy is placed in an annealing furnace cavity with the temperature rising to 700 ℃ or 900 ℃ for heat preservation for 10 minutes, and then the alloy is taken out and quickly put into cold water to obtain Fe with refined grains50Mn25Ni10Cr15And (3) medium-entropy alloy.
The recrystallization annealing is a process of heating a workpiece subjected to cold deformation processing to a temperature higher than the recrystallization temperature, preserving heat for a certain time, and then cooling to recrystallize the workpiece, thereby eliminating work hardening.
The main effect of the step (4) of the invention is to lead the Fe with the TiC dispersed phase to appear50Mn25Ni10Cr15Medium entropy alloy for grain refinement to further improve Fe50Mn25Ni10Cr15Strength of the medium entropy alloy. Because of Fe50Mn25Ni10Cr15The medium entropy alloy has TiC dispersed phase on FCC phase matrix, so that in the step (4), existence of TiC dispersed phase can be utilized to block grain boundary migration and reduce grain growth speed, thereby blocking grain growth in the step (4) and refining Fe50Mn25Ni10Cr15Medium entropy alloy grain, thereby increasing grain boundary which can block sliding movement, thereby leading Fe50Mn25Ni10Cr15The medium entropy alloy is strengthened. In the background art patent, Fe50Mn25Ni10Cr15The medium entropy alloy only has a single phase of FCC phase, so the strengthening effect of the invention can not be achievedAnd (5) fruit.
In step (4), the present invention is different from the prior art patent in that the present invention has a shorter incubation time. The time is short, the recrystallization time is short, the obtained crystal grains are not too long, so that the crystal grains are further refined, the crystal boundary is further increased, the sliding movement can be blocked by the crystal boundary, and the Fe is further caused50Mn25Ni10Cr15The medium entropy alloy is strengthened.
In combination with the first to fourth aspects described above, Fe obtained in the background art patent50Mn25Ni10Cr15Intermediate entropy alloy, or Fe obtained in example 150Mn25Ni10Cr15The medium entropy alloy does not contain Co element, so the cost is greatly reduced, and Fe50Mn25Ni10Cr15The medium entropy alloy has the advantage of low cost.
Further, as is clear from example 1, Fe50Mn25Ni10Cr15The yield strength of the medium entropy alloy is 251MPa, the tensile strength is 543MPa, the elongation after fracture is about 60%, and the yield ratio is 0.46. That is, Fe50Mn25Ni10Cr15The medium-entropy alloy has excellent plasticity, but low yield strength and low yield ratio.
Therefore Fe50Mn25Ni10Cr15The medium entropy alloy has excellent plasticity, lower yield strength and lower yield ratio because of Fe50Mn25Ni10Cr15The medium entropy alloy is a single-phase alloy with a face-centered cubic structure. At room temperature and low temperature, the face-centered cubic structure has more slippage, and dislocation is easy to slip in the stretching process, so that the alloy has excellent plasticity and also has lower yield strength and yield ratio.
Fe50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy are low, and the requirement of engineering application is difficult to meet, so that the medium-entropy alloy is very limited in engineering application.
From examples 2 to 4, the present invention is clearBy mixing Fe in step (1)95C5The alloy, Mn, Cr, Ni and Ti are smelted together and cast to form Fe with TiC dispersed phase strengthening50Mn25Ni10Cr15The existence of the medium entropy alloy and TiC disperse phase can realize that TiC dispersion is opposite to Fe50Mn25Ni10Cr15The second phase of the medium entropy alloy is strengthened. When the recrystallization annealing treatment of the step (4) is further performed on the basis of the step (1), fine grain strengthening can be achieved by utilizing a TiC dispersed phase.
Second phase strengthening means that TiC is used as a dispersed phase, namely, the second phase is uniformly distributed in Fe with a face-centered cubic structure50Mn25Ni10Cr15In the medium entropy alloy, TiC dispersed phase hinders the sliding movement in the face-centered cubic structure, thereby leading Fe50Mn25Ni10Cr15The medium entropy alloy is remarkably strengthened, namely, Fe can be improved50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy can reduce the plasticity of the medium-entropy alloy, but can keep the plasticity of the medium-entropy alloy.
As shown in the variation trends of (a), (b), (c) and (d) in FIG. 2, the existence of the TiC dispersed phase can hinder the grain boundary migration and reduce the grain growth rate, thereby hindering the grain growth during the recrystallization annealing treatment and refining Fe50Mn25Ni10Cr15Grains, thereby increasing grain boundaries which can block the movement of slip, thereby making Fe50Mn25Ni10Cr15The medium entropy alloy is strengthened, i.e. Fe can be increased50Mn25Ni10Cr15The yield strength and yield ratio of the medium-entropy alloy can reduce the plasticity of the medium-entropy alloy, but can keep the plasticity of the medium-entropy alloy.
In sum, with Fe50Mn25Ni10Cr15Compared with the single-phase alloy of the medium-entropy alloy, the invention utilizes TiC dispersed phase to strengthen Fe50Mn25Ni10Cr15And (3) medium-entropy alloy. On one hand, the advantages of no Co element can be maintained, the cost is saved, and the popularization and application of Fe are facilitated50Mn25Ni10Cr15Medium entropy alloy; on the other hand, it is possible to realize Fe by utilizing TiC dispersed phase50Mn25Ni10Cr15Second phase strengthening and fine grain strengthening of the medium entropy alloy to facilitate retention of Fe50Mn25Ni10Cr15While the necessary plasticity of the medium-entropy alloy is realized, the yield strength and the yield ratio of the medium-entropy alloy can be improved, and Fe is facilitated50Mn25Ni10Cr15Popularization of the medium entropy alloy in engineering application.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. Fe enhanced by TiC dispersed phase50Mn25Ni10Cr15The method for preparing the medium-entropy alloy is characterized by comprising the following steps of:
(1) selecting FeC alloy, Mn, Cr, Ni and Ti as raw materials according to an expression (Fe)50Mn25Ni10Cr15)100-x(TiC)xWeighing and proportioning, wherein x is more than 0 and less than or equal to 1.5, x is the atomic percentage content, smelting all the raw materials together to obtain alloy liquid, and casting and molding the alloy liquid to obtain an alloy ingot;
(2) carrying out homogenization annealing treatment on the alloy ingot;
(3) rolling or forging the alloy ingot to obtain an alloy plate;
(4) carrying out recrystallization annealing treatment on the alloy plate to obtain Fe with TiC dispersed phases uniformly distributed on the matrix phase of the face-centered cubic structure50Mn25Ni10Cr15And (3) medium-entropy alloy.
2. A TiC dispersoid-reinforced Fe according to claim 150Mn25Ni10Cr15Method of making a medium entropy alloyCharacterized in that in the step (1), the purities of FeC alloy, Mn, Cr, Ni and Ti as raw materials are all more than 99.5%.
3. A TiC dispersoid phase reinforced Fe according to claim 250Mn25Ni10Cr15The method for preparing the medium-entropy alloy is characterized in that in the step (1), after raw materials of FeC alloy, Mn, Cr, Ni and Ti are weighed, the raw materials of FeC alloy, Mn, Cr, Ni and Ti are required to be placed in absolute ethyl alcohol for ultrasonic cleaning.
4. A TiC dispersoid-reinforced Fe according to claim 350Mn25Ni10Cr15The method for medium-entropy alloy is characterized in that in the step (1), raw materials of FeC alloy, Mn, Cr, Ni and Ti are sequentially placed in a water-cooled copper crucible of a vacuum arc melting furnace in sequence from low melting point to high melting point to be melted together.
5. A TiC dispersed phase reinforced Fe according to claim 450Mn25Ni10Cr15The method for medium-entropy alloy is characterized in that in the step (1), the FeC alloy, Mn, Cr, Ni and Ti which are raw materials need to be turned over for multiple times in a positive and negative mode during smelting.
6. A TiC dispersed phase reinforced Fe according to claim 550Mn25Ni10Cr15The method for the medium-entropy alloy is characterized in that in the step (1), when the alloy liquid is cast and formed, the alloy liquid needs to be suction-cast into a water-cooled copper mold for solidification.
7. A TiC-dispersed phase reinforced Fe according to claim 150Mn25Ni10Cr15The method for the medium-entropy alloy is characterized in that in the step (2), the alloy ingot is placed in a muffle furnace for homogenization annealing, and then water quenching is carried out, wherein the homogenization annealing temperature is 900-1000 ℃, and the homogenization annealing time is30-45min。
8. A TiC dispersoid-reinforced Fe according to claim 150Mn25Ni10Cr15The method for the medium-entropy alloy is characterized in that in the step (3), forging or rolling is carried out at room temperature according to the maximum deformation amount which can be borne by the alloy ingot.
9. A TiC dispersoid-reinforced Fe according to claim 150Mn25Ni10Cr15The method for the medium-entropy alloy is characterized in that in the step (4), the alloy ingot is placed in a muffle furnace to be subjected to recrystallization annealing treatment, the temperature of the recrystallization annealing is 700-900 ℃, and the time of the recrystallization annealing is 3-5 min.
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