CN111733358B - High-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy and preparation method thereof - Google Patents
High-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy and a preparation method thereof, wherein the cobalt-free high-entropy alloy comprises the following components in parts by weight: ni: cr: mn: the atomic percentages of Al are respectively 30% -27.5%: 30% -27.5%: 15%: 10%: 15% -20%. The preparation process comprises the following steps: selecting five elements of Fe, Ni, Cr, Mn and Al with the purity higher than 99.9wt.% as raw materials to prepare the high-entropy alloy by smelting in a non-consumable electric arc furnace. The high-entropy alloy disclosed by the invention is uniform in structure, excellent in comprehensive mechanical property, free of expensive Co element and low in price. The yield strength of the high-entropy alloy is larger than or equal to 770MPa, the fracture strain is larger than or equal to 45%, the 3.5wt.% NaCl corrosion resistance is superior to that of stainless steel SUS304, and the application prospect is wide.
Description
Technical Field
The invention relates to the field of metal materials and preparation thereof, and provides a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy.
Background
The high-entropy alloy is a new material developed based on 'chemical disorder', mainly proposes to develop and research alloy materials from the entropy angle, and breaks through the limitation of the original alloy material elements. High entropy alloys are generally made up of five or more metals or non-metals in an equal or near equal atomic ratio. In order to search for wider fields, the definition of the high-entropy alloy is extended to the condition that the proportion of each principal element in the alloy in the system can be 5at.% to 35 at.%. Unlike conventional alloys, multi-principal element high-entropy alloys are the result of the combined action of multiple principal elements, rather than exhibiting the unique properties of a single element. Research shows that after the multi-principal-element high-entropy alloy is solidified, not only a great number of intermetallic compounds are not formed, but also a simple solid solution phase is formed. The high entropy effect, the lattice distortion effect, the delayed diffusion effect and the cocktail effect of the high entropy alloy enable the alloy to show excellent mechanical properties, good wear resistance, corrosion resistance, high temperature oxidation resistance, high resistivity, excellent magnetoelectricity and other comprehensive properties, and have wide application prospects.
FeNiCoCrMn alloys were first reported by Cantor et al. The alloy consists of a single FCC solid phase, exhibits good strength and ductility at low temperatures, but yield strength at room temperature is difficult to meet engineering practical requirements. Therefore, although researchers have made great efforts to improve the strength of the alloy, the cost is greatly increased by adding expensive Co elements in many cases.
Liuliang et Al Pair AlXAccording to the research of the CoCuFeNi alloy, the structural morphology is changed from a dendritic crystal morphology to an isometric crystal morphology along with the increase of the Al content, and the hardness of the alloy is also obviously increased; in AlXIn the CoCuFeNi alloy, Al1The CoCuFeNi alloy has the best room temperature compressibility, and the compression strength and the compression ratio are 1548 MPa and 8.9 percent respectively.
In summary, even though the currently developed alloy has excellent room temperature strength, the toughness is still low, and many expensive Co elements are contained in a large amount of research, in order to search for a new material from the viewpoint of low price and practicality, Co is selected to be replaced by another element.
Disclosure of Invention
Aiming at the problem of poor strong-plasticity matching of the existing high-entropy alloy, the invention provides a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy. In order to realize the purpose of the invention, the following technical scheme is provided:
a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy, wherein Fe: ni: cr: mn: the atomic percentages of Al are respectively Fe: 27.5% -30%, Ni: 27.5% -30%, Cr: 12% -18%, Mn: 8% -12%, Al: 15 to 20 percent.
Further, when the raw material components are as follows according to atomic percentage: fe: 30%, Ni: 30%, Cr: 15%, Mn: 10%, Al: at 15%, the alloy is of the FCC + BCC + B2 structure.
Further, when the raw material components are as follows according to atomic percentage: fe: 27.5%, Ni: 27.5%, Cr: 15%, Mn: 10%, Al: at 20%, the alloy is of BCC + B2 structure.
Wherein, the preparation method comprises the following steps:
selecting five elements of Fe, Ni, Cr, Mn and Al as raw materials for proportioning;
removing surface oxide scales of raw material metals Fe, Ni, Cr, Mn and Al, cleaning and drying;
and step three, smelting to obtain the Fe-Ni-Cr-Mn-Al high-entropy alloy.
Furthermore, in the step one, in order to avoid harmful impurities and the like in the smelting process from influencing the alloy performance, the purity of the metal raw materials is higher than 99.9 wt.%.
Further, in the third step, the raw materials obtained in the first and second steps are placed in a smelting furnace at a vacuum degree of 10-3~10-2Smelting under Pa.
(3) The specific smelting operation is as follows: according to the melting point of the alloy, Fe, Al and Mn are paved on the bottom layer of the crucible, and Cr and Ni are placed on the upper layer, so that the outer layer of the low-melting-point raw material is wrapped in the smelting process, and volatilization is reduced. Considering that Mn is volatile due to high steam pressure in the furnace, an additional 1-1.5wt.% Mn is added before evacuation. Vacuum pumping to 10 deg.C to ensure oxygen content in the vacuum furnace as low as possible-3~10-2When Pa is needed, high-purity argon (purity 99.99%) is introduced into the reactor to 0.3X 105Pa-0.5×105Pa, in order to exhaust the residual oxygen in the furnace and the gas pipe. Then vacuumized 10-3~10-2Pa, opening the molecular pump, and pumping the furnace to pressure by using the molecular pump<1×10-3After Pa, the reaction vessel was purged with argon gas to 0.3X 105Pa-0.5×105Pa, before formal smelting, oxygen absorption experiment is needed, the electrode is aligned to the middle of a crucible filled with pure Ti, the distance between the electrode and the pure Ti is about 3-5mm, and smelting is carried out for 1-2min after arc striking, so that residual oxygen is removed, and the high-entropy alloy is prevented from being oxidized during smelting. When the alloy ingot is smelted, proper magnetic stirring is required to ensure uniform heating. And then moving the electric arc to a crucible, controlling the current to be 20A-300A for smelting, opening a magnetic stirring button during smelting, performing alloy ingot turnover remelting by using a manipulator after the smelting is finished once, and repeating the operation for 5-7 times to obtain the high-strength high-toughness cobalt-free high-entropy alloy.
According to the preferable scheme of the scheme, Fe, Al and Mn are sequentially paved on the bottom layer of the crucible, Cr and Ni are sequentially placed on the outer layer, and the crucible is vacuumized to 6 x 10-2When Pa, argon gas is introduced to 0.4X 105Pa, vacuumizing, and pumping the furnace by a molecular pumpTo pressure<1×10-3After Pa, the reaction mixture was purged with argon gas to 0.5X 105Pa。
In the smelting process in the step (3), when the electric arc is moved to the high-entropy alloy raw material crucible, setting the current intensity to be 20-30A, increasing the current to 120-160A to melt the Cr and Ni of the high-entropy alloy raw material, shaking the electrode to enable the melted Cr and Ni to flow to the bottom of the crucible along the surface layer of the raw material, enabling the molten metal to wrap the Mn and Al at the bottom, adding the large current to 280-300A, and smelting for 2-2.5 minutes.
Preferably, in the smelting process in the step (3), when the electric arc is moved to the high-entropy alloy raw material crucible, the current intensity is set to be 25A, the current is rapidly increased to 150A, the smelting is carried out for 20s, then the current is increased to 280A, and the smelting is carried out for 2.5 minutes.
The technical conception of the invention is as follows: fe. High entropy alloys formed by Mn, Cr, Ni, Co and other atomic ratios are reported to have stable single-phase FCC solid solutions, while alloys with single-phase FCC structures have good plasticity and poor strength and are difficult to meet the requirements of industrial production and application. Therefore, in order to reduce the alloy cost, and to strengthen the structure by considering that the addition of Al element can promote the formation of BCC phase, Al element is used to replace high-price Co element. In Fe-Ni-Cr-Mn-Al, the atomic radius of Al element is relatively large, so that the serious lattice distortion effect is easily generated, and the alloy strength is provided. Meanwhile, the binary mixed enthalpy of Al and Ni is most negative (in the alloy system), Al-Ni intermetallic compounds, namely B2 phase, are easily formed and are dispersed in the structure, and the alloy strength is greatly improved on the basis of not seriously sacrificing the plasticity.
The high-entropy alloy is applied as a high-quality cheap structural material. By researching the influence rule of the Al content on the solidification structure and the performance of the FeNiCrMn high-entropy alloy, the Co-free high-entropy alloy with excellent performance is obtained.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy which is uniform in structure, has yield strength of more than or equal to 770MPa and fracture strain of more than or equal to 45%, has very high strength, and simultaneously shows excellent plasticityAnd (4) toughness. Self-corrosion potential E of the high-entropy alloycorrAll are greater than or equal to-0.106V, critical pitting potential EpAre all more than or equal to 0.449V. The corrosion resistance of the alloy to 3.5wt.% NaCl is higher than that of stainless steel SUS 304. Has good corrosion resistance and pitting corrosion resistance, is higher than stainless steel SUS304, and has good pitting corrosion resistance. The high-entropy alloy does not contain expensive Co, is relatively low in price, and is preferably applied to high-quality and low-price structural materials, wherein the molar ratio of Fe to Ni is 1: 1.
Drawings
FIG. 1 is an XRD spectrum of a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy.
FIG. 2 is a room temperature compressive stress strain curve of the high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy.
FIG. 3 is a polarization curve of a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy.
FIG. 4 is a metallographic structure diagram of a high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy, wherein (a) is Fe30Ni30Cr15Mn10Al15(ii) a (b) Is Fe27.5Ni27.5Cr15Mn10Al20；(c)Fe32.5Ni32.7Cr15Mn10Al10；(d)Fe25Ni25Cr15Mn10Al25。
FIG. 5 is a photograph of a back scattering microstructure of a high-strength, high-toughness, corrosion-resistant, cobalt-free and high-entropy alloy, wherein (a) and (b) are Fe30Ni30Cr15Mn10Al15(ii) a (c) And (d) is Fe27.5Ni27.5Cr15Mn10Al20(ii) a (e) And (f) Fe32.5Ni32.7Cr15Mn10Al10(ii) a (g) With (h) Fe25Ni25Cr15Mn10Al25。
Detailed Description
The structural characterization, mechanical property and electrochemical property test information of the high-entropy alloy are as follows:
(1) phase analysis: x-ray diffraction analysis was performed using a Cu ka radiation diffractometer type UltimaIV (λ =1.54 a), operating voltage and current were 40Kv and 40mA, respectively, scanning at 2 θ from 20 ° to 100 ° at a speed of 4 °/min, the results are as in fig. 1.
(2) Microstructure: the samples were observed under different magnification using a scanning electron microscope, spot and area scans were performed on different regions in combination with the energy spectrum attached to the instrument, and elemental composition was analyzed, with the results shown in fig. 4 and 5.
(3) Mechanical properties: according to the relevant requirements of the GB/T7314-2017 metal material room temperature compression test method, a room temperature compression test is carried out, and the compression loading rate of the test is 0.36 mm/min. The stress-strain curve data are the mean of two runs for each component alloy, and the results are shown in fig. 2.
(4) Electrochemical performance: the potentiometric polarization experiment was performed on potentiostat workstation PARSTAT 2263, and the samples were immersed in 3.5wt.% NaCl solution. The electrochemical test adopts a three-electrode system, a working electrode is a test sample, a reference electrode is a saturated calomel electrode, and a counter electrode is a pure platinum sheet. The scanning speed is 5mV/s, the scanning potential interval is-2V-1V, and when the current density exceeds 1mA/cm2The experiment was stopped and the scan repeated 2 times to ensure accuracy, the results are shown in figure 3.
The present invention is further illustrated by the following specific examples.
Example 1
High-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy Fe30Ni30Cr15Mn10Al15
Step one, selecting metal particles of five elements of Fe, Ni, Cr, Mn and Al as raw materials, wherein the purity of all the metal raw materials is more than 99.9 wt.%.
Step two, Fe of the alloy: ni: cr: mn: the molar ratio of Al is 30%: 30%: 15%: 10%: 15%, according to the naming characteristics of the high-entropy alloy, the atomic mol ratio of each element is converted into the percentage of the mass of each element to the total mass of the alloy, namely wt (Fe) =32.40%, wt (Ni) =34.05%, wt (Cr) =15.08%, wt (Mn) =10.63%, wt (Al) =7.84%, and the batching of each element is carried out according to the total mass of the prepared alloy.
Removing surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using a mechanical and chemical combined method, cleaning, and drying for later use, namely removing the surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using sand paper for polishing, ultrasonically cleaning by using an organic solution, and then drying for later use.
Fourthly, spreading Fe, Al and Mn on the bottom layer of the crucible, placing Cr and Ni on the outer layer, adding Mn which accounts for 1 wt% of the total mass of the Fe, Ni, Cr, Mn and Al, and vacuumizing to 10 DEG-3~10-2When Pa, argon gas is introduced to 0.4X 105Pa, then vacuuming by 6X 10-2Pa, then opening the molecular pump, pumping the furnace to the pressure of 0.8X 10 by using the molecular pump-3After Pa, the reaction mixture was purged with argon gas to 0.4X 105Pa, aligning an electrode to the middle of a crucible filled with pure Ti, keeping the distance to the pure Ti by 4mm, smelting for 1.5min after arc striking, removing residual oxygen, controlling the current to 25A, moving an electric arc to a high-entropy alloy raw material, increasing the current to 150A, smelting for 20s, melting Cr and Ni of the high-entropy alloy raw material, shaking the electrode, allowing the molten Cr and Ni to flow to the bottom of the crucible along the surface layer of the raw material, wrapping Mn and Al at the bottom by molten metal, reducing the volatilization of the raw material in the smelting process as much as possible, adding large current to 280A, smelting for 2.5 min, opening a magnetic stirring button during smelting, re-melting an alloy ingot by turning over by using a manipulator after each time of smelting, and repeating the operation for 5 times to obtain the high-toughness cobalt-free high-entropy alloy Fe with high strength and high toughness30Ni30Cr15Mn10Al15。
For Fe in example30Ni30Cr15Mn10Al15The phase analysis of the high-entropy alloy sample is carried out, and the X-ray diffraction (XRD) spectrum is shown in figure 1. From the figure, Fe can be seen30Ni30Cr15Mn10Al15The alloy has a structure of FCC + BCC + B2.
For Fe in this example30Ni30Cr15Mn10Al15The microstructure analysis of the high-entropy alloy sample was carried out, and the optical micrograph thereof is shown in FIG. 4(a), and the backscatter microstructure (BSE) photograph thereof is shown in FIGS. 5 (a-b), from which it was found that Fe30Ni30Cr15Mn10Al15The alloy is lamellar structure, and formed FCC phase and BCC phase are arranged alternately.
For Fe in this example30Ni30Cr15Mn10Al15When the high-entropy alloy sample is subjected to a room temperature compression experiment, the compression true stress-strain curve is shown in figure 2, and Fe can be known30Ni30Cr15Mn10Al15The yield strength of the alloy is 770MPa, and the fracture strain is more than 70 percent. Has good plasticity and strength.
For Fe in this example30Ni30Cr15Mn10Al15The electrochemical performance of the high-entropy alloy sample is tested, the polarization curve is shown in figure 3, and Fe can be known30Ni30Cr15Mn10Al15E of the alloycorr=-0.023V，Icorr=92.79μA/cm2，Ep= 0.585V. Studies have shown that (DOI:10.1016/j. mathhemiphys.2017.07.085), stainless steel SUS304 has a self-corrosion potential Ecorr= 0.215V, critical pitting potential Ep= 0.613V. By contrast, Fe30Ni30Cr15Mn10Al15The corrosion resistance of the alloy to NaCl of 3.5wt.% is excellent and is obviously higher than that of stainless steel SUS304, and the pitting corrosion resistance is good.
Example 2
High-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy Fe27.5Ni27.5Cr15Mn10Al20
Step one, selecting metal particles of five elements of Fe, Ni, Cr, Mn and Al as raw materials, wherein the purity of all the metal raw materials is more than 99.9 wt.%.
Step two, Fe of the alloy: ni: cr: mn: molar ratios of Al are, in order, 27.5%: 27.5%: 15%: 10%: and 20%, converting the atomic mol ratio of each element into the percentage of the mass of each element to the total mass of the alloy, namely wt (Fe) =30.60%, wt (Ni) =32.16%, wt (Cr) =15.54%, wt (Mn) =10.95% and wt (Al) =10.75%, according to the naming characteristics of the high-entropy alloy, and batching each element according to the total mass of the prepared alloy.
Removing surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using a mechanical and chemical combined method, cleaning, and drying for later use, namely removing the surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using sand paper for polishing, ultrasonically cleaning by using an organic solution, and then drying for later use.
Fourthly, spreading Fe, Al and Mn on the bottom layer of the crucible, placing Cr and Ni on the upper layer, adding Mn which accounts for 1 wt% of the total mass of the Fe, Ni, Cr, Mn and Al, and vacuumizing to 10%-3~10-2When Pa, argon gas is introduced to 0.4X 105Pa, then vacuuming by 6X 10-2Pa, then opening the molecular pump, pumping the furnace to the pressure of 0.8X 10 by using the molecular pump-3After Pa, the reaction mixture was purged with argon gas to 0.4X 105Pa, aligning an electrode to the middle of a crucible filled with pure Ti, keeping the distance to the pure Ti by 4mm, smelting for 1.5min after arc striking, removing residual oxygen, controlling the current to 25A, moving an electric arc to a high-entropy alloy raw material, increasing the current to 150A, smelting for 25s, melting Cr and Ni of the high-entropy alloy raw material, shaking the electrode, allowing the molten Cr and Ni to flow to the bottom of the crucible along the surface layer of the raw material, wrapping Mn and Al at the bottom by molten metal, reducing the volatilization of the raw material in the smelting process as much as possible, adding large current to 280A, smelting for 2.5 min, opening a magnetic stirring button during smelting, re-melting an alloy ingot by turning over by using a manipulator after each time of smelting, and repeating the operation for 6 times to obtain the high-toughness cobalt-free high-entropy alloy Fe with high toughness27.5Ni27.5Cr15Mn10Al20High entropy alloy.
For Fe in example27.5Ni27.5Cr15Mn10Al20The phase analysis of the high-entropy alloy sample is carried out, and the X-ray diffraction (XRD) spectrum is shown in figure 1. From the figure, Fe can be seen27.5Ni27.5Cr15Mn10Al20The alloy has a BCC + B2 structure.
For Fe in this example27.5Ni27.5Cr15Mn10Al20The microstructure analysis of the high-entropy alloy sample is carried out, and the optical microscope photograph is shown in FIG. 4(b), the back scattering microstructure (BSE) photograph is shown in FIG. 5 (c-d), and the image analysis shows that,Fe27.5Ni27.5Cr15Mn10Al20the alloy structure is in a non-equiaxial dendritic morphology.
For Fe in this example27.5Ni27.5Cr15Mn10Al20When the high-entropy alloy sample is subjected to a room temperature compression experiment, the compression true stress-strain curve is shown in figure 2, and Fe can be known27.5Ni27.5Cr15Mn10Al20The alloy has yield strength of 1013MPa, compressive strength of 1590MPa and fracture strain of 45 percent, has very high strength and simultaneously shows good ductility and toughness.
For Fe in this example27.5Ni27.5Cr15Mn10Al20The electrochemical performance of the high-entropy alloy sample is tested, the polarization curve is shown in figure 2, and Fe can be known27.5Ni27.5Cr15Mn10Al20E of the alloycorr=-0.106V，Icorr=99.74μA/cm2，Ep= 0.449V. Studies have shown that (DOI:10.1016/j. mathhemiphys.2017.07.085), stainless steel SUS304 has a self-corrosion potential Ecorr= 0.215V, critical pitting potential Ep= 0.613V. Comparative results, Fe27.5Ni27.5Cr15Mn10Al20The alloy has excellent 3.5wt.% NaCl corrosion resistance which is higher than stainless steel SUS304, and has good pitting corrosion resistance.
Example 3
High-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy Fe32.5Ni32.5Cr15Mn10Al10
Step one, selecting metal particles of five elements of Fe, Ni, Cr, Mn and Al as raw materials, wherein the purity of all the metal raw materials is more than 99.9 wt.%.
Step two, Fe of the alloy: ni: cr: mn: the molar ratio of Al is 32.5%: 32.5%: 15%: 10%: 10%, according to the naming characteristics of the high-entropy alloy, the atomic mol ratio of each element is converted into the percentage of the mass of each element to the total mass of the alloy, namely wt (Fe) =34.11%, wt (Ni) =35.84%, wt (Cr) =14.66%, wt (Mn) =10.32%, wt (Al) =5.07%, and the batching of each element is carried out according to the total mass of the prepared alloy.
Removing surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using a mechanical and chemical combined method, cleaning, and drying for later use, namely removing the surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using sand paper for polishing, ultrasonically cleaning by using an organic solution, and then drying for later use.
Fourthly, spreading Fe, Al and Mn on the bottom layer of the crucible, placing Cr and Ni on the outer layer, adding Mn which accounts for 1 wt% of the total mass of the Fe, Ni, Cr, Mn and Al, and vacuumizing to 10 DEG-3~10-2When Pa, argon gas is introduced to 0.4X 105Pa, then vacuuming by 6X 10-2Pa, then opening the molecular pump, pumping the furnace to the pressure of 0.8X 10 by using the molecular pump-3After Pa, the reaction mixture was purged with argon gas to 0.4X 105Pa, aligning an electrode to the middle of a crucible filled with pure Ti, keeping the distance to the pure Ti by 4mm, smelting for 1.5min after arc striking, removing residual oxygen, controlling the current to 25A, moving an electric arc to a high-entropy alloy raw material, increasing the current to 150A, smelting for 20s, melting Cr and Ni of the high-entropy alloy raw material, shaking the electrode, allowing the molten Cr and Ni to flow to the bottom of the crucible along the surface layer of the raw material, wrapping Mn and Al at the bottom by molten metal, reducing the volatilization of the raw material in the smelting process as much as possible, adding large current to 280A, smelting for 2.5 min, opening a magnetic stirring button during smelting, re-melting an alloy ingot by turning over by using a manipulator after each time of smelting, and repeating the operation for 5 times to obtain the high-toughness cobalt-free high-entropy alloy Fe with high strength and high toughness32.5Ni32.5Cr15Mn10Al10。
For Fe in example32.5Ni32.5Cr15Mn10Al10The phase analysis of the high-entropy alloy sample is carried out, and the X-ray diffraction (XRD) spectrum is shown in figure 1. From the figure, Fe can be seen32.5Ni32.5Cr15Mn10Al10The alloy is in a FCC + BCC structure.
For Fe in this example32.5Ni32.5Cr15Mn10Al10The microstructure of the high-entropy alloy sample was analyzed, and the optical micrograph thereof is shown in FIG. 4(c), and the backscattered micro-fractionThe photographs of the tissue (BSE) are shown in FIG. 5 (e-f), and Fe is found by analysis of the photographs32.5Ni32.5Cr15Mn10Al10The alloy is typically a dendritic structure.
For Fe in this example32.5Ni32.5Cr15Mn10Al10When the high-entropy alloy sample is subjected to a room temperature compression experiment, the compression true stress-strain curve is shown in figure 2, and Fe can be known32.5Ni32.5Cr15Mn10Al10The yield strength of the alloy is 280MPa, and the fracture strain is more than 70 percent. The plasticity is better, but the yield strength is far lower than 770 MPa.
For Fe in this example32.5Ni32.5Cr15Mn10Al10The electrochemical performance of the high-entropy alloy sample is tested, the polarization curve is shown in figure 3, and Fe can be known32.5Ni32.5Cr15Mn10Al10E of the alloycorr=-0.717V，Icorr=57.80μA/cm2，Ep= 0.209V. Studies have shown that (DOI:10.1016/j. mathhemiphys.2017.07.085), stainless steel SUS304 has a self-corrosion potential Ecorr= 0.215V, critical pitting potential Ep= 0.613V. By contrast, Fe32.5Ni32.5Cr15Mn10Al10The corrosion resistance of the alloy to 3.5wt.% NaCl is lower than that of stainless steel SUS304, and the pitting corrosion resistance is poor.
Example 4
High-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy Fe25Ni25Cr15Mn10Al25
Step one, selecting metal particles of five elements of Fe, Ni, Cr, Mn and Al as raw materials, wherein the purity of all the metal raw materials is more than 99.9 wt.%.
Step two, Fe of the alloy: ni: cr: mn: the molar ratio of Al is 25%: 25%: 15%: 10%: 25%, according to the naming characteristics of the high-entropy alloy, the atomic mol ratio of each element is converted into the percentage of the mass of each element to the total mass of the alloy, namely wt (Fe) =28.68%, wt (Ni) =30.15%, wt (Cr) =16.02%, wt (Mn) =11.29% and wt (Al) =13.86%, and the proportioning of each element is carried out according to the total mass of the prepared alloy.
Removing surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using a mechanical and chemical combined method, cleaning, and drying for later use, namely removing the surface oxide skin of the raw material metals Fe, Ni, Cr, Mn and Al by using sand paper for polishing, ultrasonically cleaning by using an organic solution, and then drying for later use.
Fourthly, spreading Fe, Al and Mn on the bottom layer of the crucible, placing Cr and Ni on the upper layer, adding Mn which accounts for 1 wt% of the total mass of the Fe, Ni, Cr, Mn and Al, and vacuumizing to 10%-3~10-2When Pa, argon gas is introduced to 0.4X 105Pa, then vacuuming by 6X 10-2Pa, then opening the molecular pump, pumping the furnace to the pressure of 0.8X 10 by using the molecular pump-3After Pa, the reaction mixture was purged with argon gas to 0.4X 105Pa, aligning an electrode to the middle of a crucible filled with pure Ti, keeping the distance to the pure Ti by 4mm, smelting for 1.5min after arc striking, removing residual oxygen, controlling the current to 25A, moving an electric arc to a high-entropy alloy raw material, increasing the current to 150A, smelting for 25s, melting Cr and Ni of the high-entropy alloy raw material, shaking the electrode, allowing the molten Cr and Ni to flow to the bottom of the crucible along the surface layer of the raw material, wrapping Mn and Al at the bottom by molten metal, reducing the volatilization of the raw material in the smelting process as much as possible, adding large current to 280A, smelting for 2.5 min, opening a magnetic stirring button during smelting, re-melting an alloy ingot by turning over by using a manipulator after each time of smelting, and repeating the operation for 6 times to obtain the high-toughness cobalt-free high-entropy alloy Fe with high toughness25Ni25Cr15Mn10Al25High entropy alloy.
For Fe in example25Ni25Cr15Mn10Al25The phase analysis of the high-entropy alloy sample is carried out, and the X-ray diffraction (XRD) spectrum is shown in figure 1. From the figure, Fe can be seen25Ni25Cr15Mn10Al25The alloy has a BCC + B2 structure.
For Fe in this example25Ni25Cr15Mn10Al25The microstructure of the high-entropy alloy specimen was analyzed, and the optical micrograph thereof is shown in FIG. 4(d), and the backscattering microscopic groupThe photographs of the tissue (BSE) are shown in FIG. 5 (g-h), and the analysis of the photographs reveals Fe25Ni25Cr15Mn10Al25The alloy structure is an isometric crystal structure and consists of alternating bright phases and dark phases.
For Fe in this example25Ni25Cr15Mn10Al25The compression true stress-strain curve of the high-entropy alloy sample is shown in figure 2 after room temperature compression experiment, and Fe25Ni25Cr15Mn10Al25The alloy has yield strength of 1088MPa, compressive strength of 1660MPa and breaking strain of 42 percent, has very high strength, but has slightly reduced plasticity.
For Fe in this example25Ni25Cr15Mn10Al25The electrochemical performance of the high-entropy alloy sample is tested, the polarization curve is shown in figure 2, and Fe can be known25Ni25Cr15Mn10Al25E of the alloycorr=-0.6286V，Icorr=98.05μA/cm2，EpAnd = 0.291V. Studies have shown that (DOI:10.1016/j. mathhemiphys.2017.07.085), stainless steel SUS304 has a self-corrosion potential Ecorr= 0.215V, critical pitting potential Ep= 0.613V. Comparative results, Fe25Ni25Cr15Mn10Al25The alloy has poor 3.5wt.% NaCl corrosion resistance which is lower than that of stainless steel SUS304, and meanwhile, the pitting corrosion resistance is poor.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (5)
1. The preparation method of the high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy is characterized by comprising the following steps of:
(1) selecting five elements of Fe, Ni, Cr, Mn and Al as raw materials for proportioning, wherein the raw materials comprise the following components in atomic mole percentage: fe: 27.5% -30%, Ni: 27.5% -30%, Cr: 12% -18%, Mn: 8% -12%, Al: 15-20%;
(2) removing surface oxide skin of raw material metals Fe, Ni, Cr, Mn and Al, cleaning and drying;
(3) spreading Fe, Al and Mn on the bottom layer of the crucible, placing Cr and Ni on the upper layer, adding Mn to the crucible in an amount of 1-1.5wt.% of the total mass of Fe, Ni, Cr, Mn and Al before vacuumizing, and vacuumizing to 10%-3~10-2 When Pa, argon gas is introduced to 0.3X 105 Pa-0.5×105 Pa, then vacuuming 10 percent-3~10-2 Pa, opening the molecular pump, and pumping the furnace to pressure by using the molecular pump<1×10-3After Pa, the reaction vessel was purged with argon gas to 0.3X 105 Pa-0.5×105 Pa, aligning an electrode to the middle of a crucible filled with pure Ti, keeping the distance between the electrode and the pure Ti by 3-5mm, carrying out arc striking, then smelting for 1-2min, removing residual oxygen, then moving an electric arc to the crucible, setting the current intensity to be 20-30A, rapidly increasing the current to be 160A, smelting for 10-30s, increasing the current to be 300A again, smelting for 2.5 min, opening a magnetic stirring button during smelting, carrying out alloy ingot turnover remelting by using a manipulator after finishing smelting once, and repeating the operation for 5-7 times to obtain the high-strength high-toughness cobalt-free high-entropy alloy.
2. The preparation method of the high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy as claimed in claim 1, wherein when the raw material components are as follows in atomic mole percentage: fe: 30%, Ni: 30%, Cr: 15%, Mn: 10%, Al: at 15%, the alloy is of the FCC + BCC + B2 structure.
3. The preparation method of the high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy as claimed in claim 1, wherein when the raw material components are as follows in atomic mole percentage: fe: 27.5%, Ni: 27.5%, Cr: 15%, Mn: 10%, Al: at 20%, the alloy is of BCC + B2 structure.
4. The method for preparing the high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy as claimed in claim 1, wherein Fe, Al and Mn are sequentially addedSpreading on the bottom layer of the crucible, sequentially placing Cr and Ni on the outer layer, vacuumizing to 6 × 10-2 When Pa, argon gas is introduced to 0.4X 105 Pa, vacuumizing again, and pumping the furnace to pressure by using a molecular pump<1×10-3After Pa, the reaction mixture was purged with argon gas to 0.5X 105Pa。
5. The preparation method of the high-strength high-toughness corrosion-resistant cobalt-free high-entropy alloy as claimed in claim 1, wherein in the smelting process in the step (3), when an electric arc is moved to a high-entropy alloy raw material crucible, the current intensity is set to be 25A, the electric current is rapidly increased to 150A, the alloy is smelted for 20s, the electric current is added to 280A, and the smelting is carried out for 2.5 minutes.
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