CN111676409B - Preparation method of low-density low-cost Fe-Mn-Al-C intermediate entropy alloy - Google Patents
Preparation method of low-density low-cost Fe-Mn-Al-C intermediate entropy alloy Download PDFInfo
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- CN111676409B CN111676409B CN202010530555.2A CN202010530555A CN111676409B CN 111676409 B CN111676409 B CN 111676409B CN 202010530555 A CN202010530555 A CN 202010530555A CN 111676409 B CN111676409 B CN 111676409B
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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
- 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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0075—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rods of limited length
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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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
Abstract
The invention discloses a preparation method of a low-density and low-cost Fe-Mn-Al-C entropy alloy, belonging to the field of metal materials and preparation. The alloy comprises the following chemical components in atomic percentage: 33.0-38.0% of Fe33.0%, 33.0-38.0% of Mn33.0%, 21.0-25.0% of Al0% and 4.0-7.0% of C. The preparation process of the alloy comprises the steps of removing oxide skin from metallurgical raw materials of Fe, Mn, Al and C, and cleaning by an ultrasonic wave or acid pickling method; the alloy is smelted by a non-consumable vacuum arc furnace or an induction furnace, and the medium-entropy alloy plate-shaped or rod-shaped material is obtained by a vacuum suction casting or casting method. The medium-entropy alloy has low density, high strength and high plasticity, and low cost of alloy elements, and can be used in the industrial fields of traffic, machinery, energy and the like.
Description
Technical Field
The invention relates to a preparation method of a low-density, low-cost and high-performance medium-entropy alloy, belonging to the field of metal materials and preparation thereof.
Background
Alloys can be classified as high entropy alloys (Δ S) according to their entropy of mixingmix>1.6R, R is gas constant, the same below), medium entropy alloy (1.1R)<ΔSmix<1.6R), low entropy alloy (Delta S)mix<1.1R). The traditional metal materials such as steel, aluminum alloy, titanium alloy and the like are basically low-entropy alloys. The high-entropy alloy has various main elements, is widely researched due to the excellent performance of the high-entropy alloy, and various high-entropy alloy series are developed. For example, FeCoCrNiMn series high-entropy alloy has good mechanical property at low temperature, AlCoCrCuFeNi series high-entropy alloy can obtain higher strength and corrosion resistance, and NbMoTaW series high-entropy alloy has excellent high-temperature resistance.
Although high entropy alloys have gained widespread attention, the number of high entropy alloys that can be used for engineering applications is still small, particularly less high entropy alloys that can achieve high strength and plasticity matches. For example, FeCoCrNiMn-based high-entropy alloy has excellent tensile plasticity, but generally has a low tensile strength. Recently, medium entropy alloys are receiving increasing attention and research as a potential alloy. Compared with the high-entropy alloy, the medium-entropy alloy has the advantages that the principal element number is reduced, excellent performance can be obtained through proper regulation and control of components and processes, and industrial application is easier to realize. Currently, most researches are carried out on entropy alloys in a CoCrNi system and a FeCoNi system, nanocrystalline particles are separated out on an FCC solid solution matrix through component optimization and process adjustment, the number, the form and the distribution of a nano strengthening phase are changed, and the matching of strength and plasticity is realized. However, in the current medium-entropy alloy system, elements with high cost such as Co and Ni are contained, so that the cost of the alloy is high, and the large-scale popularization and application of the alloy are not facilitated. On the other hand, for engineering structural materials, the aim of pursuing light weight and high strength is constant, and the addition of high Co and Ni contents is not beneficial to the reduction of the alloy density. However, no report is found on the low-density Fe-Mn-Al-C medium entropy alloy which does not contain Co and Ni elements at present.
Disclosure of Invention
The invention aims to solve the problem of good matching of specific strength and plasticity of a medium-entropy alloy, and provides a medium-entropy Fe-Mn-Al-C alloy with low density, high specific strength, high plasticity and low cost and a preparation method thereof so as to be beneficial to popularization and application of the alloy and greatly reduce the cost of the alloy. The method designs the low-density and low-cost medium-entropy alloy components by adding a proper amount of alloy strong plasticizing elements. By formulating a reasonable hot working and solution aging heat treatment process system, on the premise of keeping better processing performance, higher strength and plasticity are kept. Therefore, the key technology for solving the problems is selection and dosage of alloy elements, optimization of a processing and preparation process and selection of a solution aging heat treatment process.
The invention is realized by the following technical scheme:
a preparation method of a low-density low-cost Fe-Mn-Al-C intermediate entropy alloy comprises the following alloy chemical components in atomic percentage: 33.0-38.0% of Fe33.0%, 33.0-38.0% of Mn33.0%, 21.0-25.0% of Al0% and 4.0-7.0% of C.
The preparation method comprises the following steps:
1) removing surface oxide skin of raw material metal from metallurgical raw materials Fe, Mn, Al and C with purity of over 99.9% by mechanical polishing or acid washing for alloy preparation;
2) the mixture ratio is accurately weighed by converting the molar ratio into the mass ratio, the Mn raw material is additionally added by 5 percent by mass to compensate the smelting loss, and then the raw material is cleaned by absolute ethyl alcohol ultrasonic oscillation;
3) smelting the alloy, and carrying out suction casting or casting on the molten alloy melt into a mold to obtain a medium-entropy alloy plate-shaped or rod-shaped material;
4) homogenizing and solution-treating the plate-shaped or rod-shaped sample of the medium-entropy alloy.
Further, the alloy chemical composition according to the atom percentage preferred range is: 35.0-37.0% of FeC, 34.5-36.5% of MnC, 22.0-24.0% of AlC and 4.0-4.5% of C.
Further, the smelting is vacuum non-consumable electrode arc furnace smelting, and the vacuum degree value is lower than 5 multiplied by 10-2Introducing argon to the pressure in the furnace to reach 0.05 MPa; the smelting current is 100-250A, the electric arc holding time is 1-3 min, and the overturning and repeated smelting is carried out for more than 4 times so as to ensure that the components of the alloy ingot are uniform.
Further, the smelting is induction smelting, the induction heating frequency is medium frequency or high frequency, the smelting environment is atmosphere, and the melting temperature is 1450-1550 DEG C
Further, the homogenization heat treatment process comprises the following steps: the heat preservation temperature is 1000-1200 ℃, and the heat preservation time is 1-4 h;
further, the solution heat treatment process comprises the following steps: heating at 1000-1150 deg.c for 0.5-4 hr, and water quenching at normal temperature.
The alloy comprehensively considers the influence of the added elements on the density, the cost, the strength, the plasticity and the hot working performance of the alloy during component design, and the specific consideration factors are as follows:
mn: is a main element forming a gamma phase in steel, and the gamma phase region formed by Mn and Fe increases along with the increase of MnThe solid solubility of Mn in gamma phase can reach 31.5 at% at 400 ℃. From the perspective of reducing density, the 1 wt% Mn content in the alloy can reduce the density by 0.0085g/cm3The weight reduction effect was about 0.1%. Therefore, in order to have good plasticity and low density in the alloy, Mn in the alloy should be sufficiently high. However, if the Mn content in the alloy is too high, α -Mn is easily formed in the structure at room temperature and β -Mn phase is easily formed at high temperature. Comprehensively considering the mechanical property and density of the alloy, the Mn content is Mn33.0-38.0%.
Al: in the Fe-Al binary phase diagram, a wide Al composition range of an alpha-Fe solid solution region exists on the Fe side, and a face-centered cubic (gamma-Fe) -based solid solution region is closed. Therefore, Al is an element promoting the formation of alpha-Fe. Meanwhile, when the content of Al exceeds a certain limit, Fe is also formed3Al and FeAl phases. From the phase diagram of the Al-Mn binary system, Al has great solid solubility in the beta-Mn phase, or Al can promote the formation of the beta-Mn phase. The interaction of Al with Fe and Mn is comprehensively considered, and the content of Al is not easy to be too high. However, Al is an element which is very effective in reducing the density, and the density of the alloy is reduced by 0.101g/cm per 1 wt% of Al added3The weight can be reduced by about 1.3%. Therefore, the mechanical property and the density are both considered, and the content of Al is 21.0-25.0%.
C: c is the most important strengthening element in steel and also an element that lowers the density. C is an expanded austenite element, but the content of C is too high, so that continuous and network-distributed carbide is formed on the grain boundary, and the improvement of the mechanical property of the alloy is not facilitated. C is an element which enlarges alpha-Mn phase to seal beta-Mn phase region, and the density of the alloy is reduced by 0.41g/cm for every 1 wt% of C3The weight can be reduced by about 5.2%. Therefore, the mechanical property and the density are comprehensively considered, and the content of C is 4.0-7.0%.
The invention has the following beneficial effects:
1) the alloy can realize the matching of high strength and high plasticity. The addition of high Mn and C contents promotes the formation of austenite, so that the alloy takes an austenite phase as a matrix structure, and the alloy has excellent plasticity. Meanwhile, the addition of Al, Mn and C can also play a role in strengthening. Through a reasonable heat treatment process, a second phase can be further precipitated, so that the alloy is further strengthened.
2) The alloy has a low density. It is especially suitable for traffic, machinery and energy industry. Especially for equipment and devices requiring energy consumption such as automobiles, ships, gas turbines and the like, the use of the alloy will lead to weight reduction of the equipment, thereby further reducing energy consumption.
3) Compared with the existing high-entropy alloy and medium-entropy alloy, the alloy only contains Fe, Mn, Al and C elements with lower cost, so that the cost of the alloy is greatly reduced.
Drawings
FIG. 1 shows Fe as a component in example 536.4Mn36.3Al23.0C4.3Scanning electron microscope organization after alloy heat treatment;
FIG. 2 shows Fe as a component in example 536.4Mn36.3Al23.0C4.3X-ray diffraction curves of the alloy in an as-cast state and a heat treatment state;
FIG. 3 shows Fe as a component in example 536.4Mn36.3Al23.0C4.3Room temperature mechanical property curve of the alloy.
Detailed Description
Table 1 shows the alloy compositions of the examples and part of the reference alloy compositions (atomic percent). It is apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Preparing an alloy: prepared according to the compositions shown in alloys 1-9 in table 1. (1) Removing surface oxide skin of raw material metal by mechanically polishing or acid washing metallurgical raw materials Fe, Mn, Al and C with the purity of more than 99.9%; (2) converting into a mass ratio, accurately weighing and proportioning, adding 5% of Mn raw material by mass to compensate smelting loss, and ultrasonically vibrating and cleaning the raw material by absolute ethyl alcohol; (3) alloy is smelted by using a vacuum non-consumable arc furnace, and the vacuum degree value is lower than 5 multiplied by 10-3Introducing high-purity argon until the pressure in the furnace reaches 0.05 MPa; (4) melting current of 100-250A, keeping the electric arc for 1-3 min, and overturning and repeatedly smelting for more than 4 times to ensure that the components of the alloy ingot are uniform; (5) the master alloy ingot was suction-cast into a water-cooled copper mold using a vacuum suction casting apparatus to obtain a plate-like sample having a thickness of 10 mm.
Table 1 example alloy compositions
| Examples | Fe | Mn | Al | C | Mixed entropy Δ Smix |
| 1 | 35.7 | 34.5 | 24.5 | 5.3 | 1.24R |
| 2 | 35.7 | 35.0 | 24.5 | 4.8 | 1.23R |
| 3 | 35.7 | 35.5 | 24.5 | 4.3 | 1.22R |
| 4 | 36.2 | 36.0 | 23.5 | 4.3 | 1.21R |
| 5 | 36.4 | 36.3 | 23.0 | 4.3 | 1.21R |
| 6 | 36.7 | 36.5 | 22.5 | 4.3 | 1.21R |
| 7 | 36.6 | 36.4 | 22.5 | 4.5 | 1.21R |
| 8 | 36.4 | 36.3 | 22.5 | 4.8 | 1.22R |
The heat treatment process comprises the following steps: a10 mm thick plate-shaped sample is processed by linear cutting, a 2mm thick sheet-shaped sample is cut out, solution heat treatment is carried out, the heating temperature is 1050 ℃, the temperature is 1100 ℃, the heat preservation time is 0.5h, and then water quenching is carried out at normal temperature.
And (3) testing the density: the principle of alloy sample density determination is an Archimedes drainage method, the used equipment is a YTN-100L densimeter, oxide skin on the surface of a sample is ground off before testing, ultrasonic cleaning and blow-drying are carried out, and an average value is taken after at least 5 times of measurement to obtain an actually measured density value. The measured density values for the example alloys and for some of the reference alloys are listed in table 2.
Organization and phase structure: and (3) grinding the alloy sample by abrasive paper with different mesh numbers, then mechanically polishing until the surface is bright and has no scratch, and testing the metallographic structure by adopting a D/max-2500/PC X-ray diffractometer. The polished sample was etched with a 4% nital solution, and the tissue was observed and analyzed using a SUPRA55 thermal field emission scanning electron microscope. As shown in figure 1, the SEM structure of the alloy 5 is subjected to heat treatment at 1050 ℃ for 0.5h, and the structure is a dual-phase structure of an austenite matrix and a small amount of ferrite. As shown in FIG. 2, XRD curves of alloy 5 in the as-cast and heat-treated states were obtained by heat treatment at 1100 ℃ for 0.5 hour, and from the as-cast state to the heat-treated state, the two-phase structure was substantially transformed into a completely austenitic structure.
And (3) testing mechanical properties: 2mm multiplied by 3mm sheet-shaped tensile samples with the gauge length of 15mm are subjected to room temperature tensile test on a CMT4305 type electronic universal tester, and the tensile rates are unified to be 0.5 multiplied by 10-3s-1And at least 3 samples are selected for testing to obtain an engineering stress-strain curve. As an example, FIG. 3 is an engineering stress-strain curve for alloy 5, which has a tensile strength of 720.5MPa, a yield strength of 548.8MPa, an elongation of 44.7%, and a bond density value of 6.28g/cm, and is calculated to achieve a specific strength of 0.115. According to the density measurement and the engineering stress-strain curve, the density, the yield strength, the tensile strength and the specific strength of the alloy 1-10 are obtained, and the experimental results are listed in Table 2.
Table 2 results of density and mechanical property tests of alloys of examples
Claims (5)
1. A preparation method of a low-density low-cost Fe-Mn-Al-C intermediate entropy alloy is characterized in that the alloy comprises the following chemical components in atomic percentage: 33.0-38.0% of Fe33.0%, 33.0-38.0% of Mn33.0%, 21.0-25.0% of Al0%, and 4.0-7.0% of C;
the preparation method comprises the following steps:
1) removing surface oxide skin of raw material metal from metallurgical raw materials of Fe, Mn, Al and C with the purity of more than 99.9% by mechanical polishing or acid pickling for alloy preparation;
2) the mixture ratio is accurately weighed by converting the molar ratio into the mass ratio, the Mn raw material is additionally added by 5 percent by mass to compensate the smelting loss, and then the raw material is cleaned by absolute ethyl alcohol ultrasonic oscillation;
3) smelting the alloy, and carrying out suction casting or casting on the molten alloy melt into a mold to obtain a medium-entropy alloy plate-shaped or rod-shaped material;
4) homogenizing and solution-treating a plate-shaped or rod-shaped sample of the medium-entropy alloy;
the solid solution heat treatment process comprises the following steps: heating at 1000-1150 deg.c for 0.5-4 hr, and water quenching at normal temperature.
2. The method for preparing low-density and low-cost Fe-Mn-Al-C entropy alloy as claimed in claim 1, wherein the chemical composition of the alloy in atomic percentage is preferably in the range of: 35.0-37.0% of FeC, 34.5-36.5% of MnC, 22.0-24.0% of AlC and 4.0-4.5% of C.
3. The method of claim 1, wherein the melting is vacuum non-consumable arc melting with a vacuum value of less than 5 x 10-2Introducing argon to the pressure in the furnace to reach 0.05 MPa; fusion furnaceSmelting current is 100-250A, electric arc holding time is 1-3 min, and overturning and repeated smelting is carried out for more than 4 times so as to enable components of the alloy ingot to be uniform.
4. The method for preparing a low-density and low-cost Fe-Mn-Al-C entropy alloy as claimed in claim 1, wherein the melting is induction melting, the induction heating frequency is medium frequency or high frequency, the melting environment is atmospheric air, and the melting temperature is 1450 ℃ to 1550 ℃.
5. The method for preparing the low-density and low-cost Fe-Mn-Al-C entropy alloy as recited in claim 1, wherein the homogenization heat treatment process comprises: the heat preservation temperature is 1000-1200 ℃, and the heat preservation time is 1-4 h.
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