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Analysis of mechanical properties and corrosion resistance of FeCoNiCrMn high entropy alloys

FeCoNiCrMn high-entropy alloy is one of the most excellent single-phase high-entropy alloys and has become a hot research topic in the current field. The crystal structure, mechanical properties and corrosion resistance of the prepared FeCoNiCrMn high-entropy alloys were tested and analyzed by using X-ray diffractometer, hardness tester, universal testing machine, electrochemical workstation and scanning electron microscope, etc. The sintering of FeCoNiCrMn high-entropy alloy powder was carried out by discharge plasma sintering. The results of the mechanical properties tests showed that the elongation of the alloy increased from 45.2% to 48.1% as the sintering pressure increased from 30 MPa to 50 MPa. Electrochemical test results show that the FeCoNiCrMn high-entropy alloy has lower corrosion potential and higher corrosion current density than 1Cr18Ni9Ti stainless steel in 3.5 wt.% NaCl solution and 0.5 mol/L H2SO4 solution, and the corrosion type is mainly pitting corrosion. in 0.5 mol/L H2SO4 solution.

What is high entropy alloy?

High-entropy alloys (HEA for short) are alloys formed by five or more metals in equal or approximately equal amounts, where the so-called entropy, a parameter that thermodynamically represents the degree of disorder, the greater the disorder of a system, the greater the entropy. And because high-entropy alloys have many desirable properties, they are valued in engineering. In the past, the materials industry has not developed towards more main element alloys probably because the traditional alloying ratio is still based on the concept of “one metal element is the main element”, according to the configuration of different metal compositions and ratios, using specific process methods, and can get the demand for alloy materials, for example, steel materials are mainly iron, adding carbon to get carbon steel. When the carbon content exceeds a certain percentage, it can become cast iron, and if other elements are added, different alloy steels with different properties can be obtained.
However, the so-called high entropy alloy is an alloy material using multiple major elements, where each major element has a high atomic percentage, but not more than 35%, so no one element can account for more than half of the proportion, giving full play to the effect of high chaos of multiple elements, by the random dispersion of atoms of each element to inhibit the generation of brittle compounds, which can make the material stronger toughness.
Compared with traditional alloys, high entropy alloys bring new concepts to alloy design and have more excellent properties. Through proper alloy formulation design, the combination of properties such as high hardness, high work hardening, high temperature softening resistance, high temperature oxidation resistance, corrosion resistance, and high resistivity can be obtained, and the properties are better than those of traditional alloys, and the applications are varied, such as: tools, molds, and knives with high hardness and wear, temperature, and corrosion resistance. Golf head striking surface, oil pressure air rod, steel pipe and roller hard surface; high frequency transformer, motor core, magnetic shield, magnetic head, disk, magnetic disc, high frequency soft magnetic film and horn; chemical plant, ship corrosion resistant high strength material; turbine blade, welding material, heat exchanger and high temperature furnace material; ultra-high building refractory skeleton; and microelectromechanical materials.
However, in addition to the mechanical, physical, and chemical properties of high-entropy alloys as new state alloys will continue to be explored by research, challenges related to basic theory will also arise, such as the generation of different phase systems in the process stages of high-entropy alloys. In addition, high-entropy alloys have a considerable number of combinations, although only a few combinations of systems can be shown to be functional. However, it becomes difficult to identify useful alloy components using conventional alloy detection methods, and an efficient high-throughput discrimination technique is needed for alloy screening, and further research is also needed on how to control the mechanisms of phase changes in the formation of individual atoms in high-entropy alloys.
Since researchers proposed the concept of multi-principal element high-entropy alloys in 2004, high-entropy alloys have continued to attract extensive attention from many scholars [1]. Studies have shown that high-entropy alloys are mainly composed of five or more main elements, which are combined to form alloy solid solutions according to the equimolar ratio or nearly equimolar ratio, and this technique breaks the traditional concept of designing alloys with a single element as the main element and provides a new idea for the design of new alloys. It was found that high-entropy alloys prefer to form simple disordered solid solutions rather than complex phases such as intermetallic compounds, due to the high mixing entropy of high-entropy alloys, which inhibits the generation of intermetallic compounds [2,3,4]. Compared with conventional alloys, high-entropy alloys have significant advantages and can achieve excellent properties through composition modulation and process design, such as high strength, high hardness, good wear resistance, oxidation resistance, corrosion and irradiation resistance, and excellent low-temperature mechanical properties [5,6,7,8,9,10,11,12]. Therefore, high-entropy alloys are a new class of alloy materials with great potential for development.
As a new alloy system, high entropy alloys involve many alloying elements in their composition design, and Fe, Co, Ni, Cr and Mn belong to the same period in the periodic table and are close to each other. The combination of these five elements in equal atomic ratios can form facecentered cubic (FCC) structured high-entropy alloys with excellent mechanical properties at room and low temperatures, in which Co, Cr and Ni can form dense oxide films at high temperatures, which can significantly improve the corrosion resistance of the alloys while having better plastic toughness [13]. Currently, researchers have prepared FeCoNiCrMn high-entropy alloys by melting and laser cladding processes and studied their mechanical properties and corrosion resistance. For example, Gludovatz et al [14] prepared FeCoNiCrMn high-entropy alloy with isoatomic ratio by vacuum arc melting method and systematically studied the variation of mechanical properties of the alloy with temperature. 1280 MPa and 70%, respectively; Luo et al [15] prepared FeCoNiCrMn high-entropy alloy by vacuum induction melting technique and studied its corrosion resistance in 0.1 mol/L H2SO4 solution, showing that the alloy exhibited good passivation ability and the main components of its passivation film were hydroxides of Cr, Fe and Ni and oxides of Mn and Co. In addition, related studies have shown that the conventional casting method to prepare FeCoNiCrMn high-entropy alloys undergoes a transition from liquid phase to solid phase during solidification and inevitably produces composition segregation, which affects the organization and properties of the alloy [16], while the alloy prepared by the powder metallurgy process has a uniform composition and small grain size, which is a more ideal method to prepare high-performance high-entropy alloys [17]. The alloy prepared by the powder metallurgical process is a more ideal method for the preparation of high performance high entropy alloys because of its uniform composition and fine grain size [17]. Based on this, this study prepared FeCoNiCrMn high-entropy alloy specimens by powder metallurgical process, investigated the effect of different sintering pressure on the mechanical properties of FeCoNiCrMn high-entropy alloy, analyzed the electrochemical corrosion behavior of FeCoNiCrMn high-entropy alloy in different media, and compared it with 1Cr18Ni9Ti austenitic stainless steel which has excellent corrosion resistance. It was compared with 1Cr18Ni9Ti austenitic stainless steel, which has excellent corrosion resistance, to provide relevant reference data for the further application of FeCoNiCrMn high-entropy alloy.

Experiment

Materials and apparatus

Materials
Materials used in the experiment include: aerosolized FeCoNiCrMn high-entropy alloy powder, particle size of 15-53μm, purchased from Jiangsu Willary New Materials Technology Co.
Apparatus
The instruments used in the experiment include: LABOX-350 discharge plasma sintering system (Sinterland, Japan): DX-2700B X-ray diffractometer (Liaoning Dandong Haoyuan Instrument Co., Ltd.); InspectF50 scanning electron microscope (FEI, USA); MHVD-50AP Vickers hardness tester (Shanghai Juijing Precision Instrument Manufacturing Ltd.); ETM-105D type universal testing machine (Shenzhen Wanxiao Test Equipment Co., Ltd.); CH-I660E type electrochemical workstation (Shanghai Chenhua Instruments Co., Ltd.); ME-104/02 type electronic balance (Mettler-Toledo Instruments (Shanghai) Co. (Kunshan Ultrasonic Instruments Co., Ltd.).

Specimen preparation

The preparation steps of FeCoNiCrMn high-entropy alloy specimens were as follows: 25 g of high-entropy alloy powder was weighed into a graphite mold and compacted. Then the graphite mold was placed into the sparkplasmasintering (SPS) system with sintering pressures of 30 MPa and 50 MPa, sintering temperature of 1000°C, and heating rate of 100°C/min. Cylindrical specimens with a diameter of 20 mm and a height of 10 mm were prepared.

Specimen characterization and performance testing

Testing and characterization
In the testing and characterization of the prepared high-entropy alloy specimens, the density of the specimens was tested by Archimedes’ drainage method; the crystal structure of the specimens was tested by X-ray diffraction (XRD) instrument with the following conditions: CuKα radiation, anode target voltage of 40 kV, target current of 30 mA, step angle of 0.03°, sampling time The scanning electron microscope (SEM) was used to observe the tensile fracture and the surface morphology of the specimen after corrosion.
Mechanical properties testing
The mechanical properties of high-entropy alloy specimens were tested using a universal testing machine for tensile testing, the original pitch of the tensile specimen was 5mm, the cross-sectional area was 1.5mm×1mm, and the tensile rate was 0.2mm/min. At the same time, the hardness of the specimens was determined using a Vickers hardness tester, the test loading force was 5kN, and the loading time was 15s.
Corrosion resistance test
The corrosion resistance of the prepared FeCoNiCrMn high-entropy alloy was tested using an electrochemical workstation. Before the test, the FeCoNiCrMn high-entropy alloy and 1Cr18Ni9Ti stainless steel prepared with 30MPa sintering pressure were cut into 10mm×10mm×5mm specimens, and the surface of the specimens were polished smoothly with 240#~2000# SiC sandpaper and polished with diamond abrasive paste until there were no obvious scratches. Then the specimen is connected to the wire and use epoxy resin to seal the non-test surface, leaving an area of 1 cm2 to be measured. The corrosion media used for the test were 3.5 wt.% NaCl solution and 0.5 mol/L H2SO4 solution. Test using the three-electrode method to connect the electrode, the specimen as the working electrode, saturated calomelelectrode (SCE) as the reference electrode, platinum electrode as the counter electrode, the dynamic potential scan rate of 1mV / s. According to the polarization curve, the corrosion potential of the high-entropy alloy specimens and stainless steel specimens (Ecorr), pitting potential ( Epit), passivation interval (ΔEp) and corrosion current density (Icorr) and other electrochemical parameters. After the polarization curve test was completed, the corroded surface of the specimen was cleaned with an ultrasonic cleaner, and then the specimen was characterized by SEM.

Results and analysis

XRD analysis

The XRD patterns of the original powder of aerosolized FeCoNiCrMn high-entropy alloy and the specimens of high-entropy alloy sintered and formed by SPS system under different pressures are shown in Fig. 1. By comparison, it can be seen that although the XRD diffraction intensities and widths of the original powder of the high entropy alloy and the specimen of the high entropy alloy are different, the positions of the diffraction peaks of both are basically the same, and their crystal structures are FCC structures. According to the XRD pattern, the lattice constant of the original high-entropy alloy powder is 3.5901, while the lattice constants of the high-entropy alloy specimens sintered at 30 MPa and 50 MPa are 3.5994 and 3.5993, respectively. The This indicates that the lattice constants of the prepared high-entropy alloys did not change significantly with the increase of sintering pressure.
20220616212421 25388 - Analysis of mechanical properties and corrosion resistance of FeCoNiCrMn high entropy alloys
Fig. 1 XRD patterns of the high-entropy alloy specimens
2.2 Analysis of mechanical properties
In the test, the tensile properties of the high entropy alloy specimens prepared by sintering at different pressures were tested at room temperature, and the test results are shown in Table 1 and Fig. 2.
Table.1 Properties of high entropy alloy specimens prepared under different sintering pressures

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Figure.2 Room temperature tensile stress-strain curves of high entropy alloy specimens
From Table 1, it can be seen that the densities of the high-entropy alloy specimens are 97.9% and 99.3%, respectively, and there is a significant increase in the densities, which is due to the increase in sintering pressure that can accelerate the diffusion of elements between the alloy powders and promote the increase in the densities [18]. Also, it can be seen that there is no significant change in the hardness of the specimens, indicating that the increase in sintering pressure has no significant effect on the hardness of the high-entropy alloy. In addition, it can be seen from Fig. 2 that the yield strength of the specimen decreases with the increase of sintering pressure from 30 MPa to 50 MPa, from 424 MPa to 397 MPa, but its plastic deformation capacity still increases, the elongation increases from 45.2% to 48.1%, and the fracture strength also increases from 593 MPa to 634 MPa.This indicates that with the increase of sintering pressure, the The diffusion drive of the alloy powder was increased, thus facilitating the diffusion of elements and migration of grain boundaries, thus promoting the growth of grains in the alloy [19]. As a result, the yield strength of the alloy decreases, but at the same time, the denseness of the alloy increases with the increase of the sintering pressure, i.e., the organization of the alloy is denser, the pores are reduced, and the defects between the crack sources and the powder are reduced, which leads to the improvement of the plasticity and fracture strength of the material.
The tensile fracture morphology of the high-entropy alloy specimens prepared by sintering at different pressures was observed, and the results are shown in Figure 3. It is observed that there are a large number of tough nests on the fracture surface of the specimens, and most of them contain second-phase masses. This indicates that the fracture mode is ductile fracture. The overall morphology of the fracture shows that the fracture surface of the high-entropy alloy specimen prepared by sintering at 50 MPa pressure is less porous. The reduction of pores increases the densities of the materials and reduces the crack sources, so the higher the densities, the higher the strength and elongation of the materials. At the same time, the size of the tough nests on the tensile fracture surface of the high-entropy alloy specimens prepared at 50 MPa sintering pressure also slightly increased, and the larger the size of the tough nests, the better the plasticity of the characterized material under the same tensile conditions [20].
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Figure.3 Tensile fracture morphology of the high-entropy alloy specimens

Electrochemical corrosion analysis

Polarization curve test
The dynamic potential polarization curves of FeCoNiCrMn high-entropy alloy specimens and 1Cr18Ni9Ti stainless steel specimens in 3.5 wt.% NaCl solution and 0.5 mol/L H2SO4 solution are shown in Figure 4, and the corresponding electrochemical parameters are shown in Table 2.
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Figure.4 Kinetic potential polarization curves of the specimens
Table.2 Electrochemical performance parameters of the specimens in different media
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From Fig. 4(a), it can be seen that the kinetic potential polarization curves of both the high-entropy alloy specimens and the stainless steel specimens exhibit obvious activation-passivation behavior. As can be seen from Table 2, the corrosion potential of the high-entropy alloy specimen in 3.5 wt.% NaCl solution is lower than that of the stainless steel specimen, the corrosion current density is higher than that of the stainless steel specimen, the passivation interval of the high-entropy alloy specimen (ΔEp=0.22 V) is close to one-third of that of the stainless steel specimen (ΔEp=0.59 V), and the pitting potential of the high-entropy alloy specimen (Epit=-0.12 V) is much lower than that of the The pitting potential of the high-entropy alloy specimen (Epit=-0.12V) was much lower than that of the stainless steel specimen (Epit=0.31V). The lower Epit of the high-entropy alloy specimens indicates a higher susceptibility to pitting in chloride solutions, which is caused by the fact that the passivation film of the high-entropy alloy contains less Cr ions than that of the stainless steel [21,22,23,24]. Also, the presence of large amounts of Mn in high-entropy alloys can make Epit lower. Studies in the related literature have shown that the addition of Mn to the Ni matrix promotes the formation of defects, reduces the vacancy migration energy, and provides more favorable areas for the formation of etch pits [25]. In addition, the corrosion behavior of metals is also closely related to the stability of the passivation layer, and the passivation layer of FeCoNiCrMn high-entropy alloy contains a large number of point defects, such as oxygen vacancies and metal cation vacancies, which facilitate the migration of metal ions during corrosion [26], thus making the corrosion resistance of the alloy worse.
As can be seen from Figure 4(b), in the 0.5 mol/L H2SO4 solution, both specimens showed obvious passivation, and the maximum anodic current density in the activation zone of the high-entropy alloy specimen (Icrit = 1.985 × 10-3) was much higher than that of the stainless steel specimen (Icrit = 3.859 × 10-5), with the increase of potential, the current density then decreased, and the high-entropy alloy specimens and stainless steel specimens both enter the passivation zone.
In addition, it can be seen from Table 2, the corrosion potential of the high-entropy alloy specimen is lower than that of the stainless steel specimen, and the corrosion current density is higher than that of the stainless steel specimen. This indicates that the FeCoNiCrMn high-entropy alloy has a poor resistance to uniform corrosion. However, because the △Ep of the high-entropy alloy specimen is significantly larger than that of the stainless steel specimen, and the dimensional passivation current density of the high-entropy alloy specimen (Ip=9.528×10-6) is lower than that of the stainless steel specimen (Ip=1.498×10-5), indicating that the passivation film formed by the high-entropy alloy specimen is not easily pierced, and the rate of fracture and dissolution is also slower, indicating that the high-entropy alloy has a stronger ability to resist high-potential corrosion than stainless steel.
Corrosion surface morphology

The surface morphology of the high entropy alloy specimens prepared in this study is shown in Figure 5 after the polarization curve measurement in the two corrosive media.

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Figure.5 Surface morphology of the specimens after corrosion in different media
Figure 5 surface morphology of the specimens after corrosion in different media download the original figure
Figure 5 shows that there are a large number of pits on the surface of the high entropy alloy specimen after corrosion, which indicates that pitting has occurred in the two corrosive media. Due to the presence of a large amount of Cl- in the 3.5 wt.% NaCl solution, and the strong penetration of Cl-, the occlusion cell effect occurs during the corrosion process [27], which leads to an accelerated corrosion rate after the passivation film of the high-entropy alloy specimen is broken through. The pitting pits of the high-entropy alloy specimens in 0.5 mol/L H2SO4 solution are larger and more numerous. This indicates that pitting corrosion occurs rapidly after the passivation film of the high-entropy alloy specimen is pierced due to the high potential.

Conclusion

In this study, cylindrical specimens of FeCoNiCrMn high-entropy alloy were prepared by discharge plasma sintering process, and the effects of sintering pressure on the densities, phase composition and mechanical properties of the high-entropy alloy, as well as the corrosion resistance of the high-entropy alloy in different corrosive media were investigated, and the following conclusions were drawn:

  • 1) With the increase of the sintering pressure from 30 MPa to 50 MPa, the densities of the prepared FeCoNiCrMn high-entropy alloy specimens increased from 97.9% to 99.3%, the yield strength decreased from 424 MPa to 397 MPa, the elongation increased from 45.2% to 48.1%, and the fracture strength increased from 593 MPa to 634 MPa.
  • 2) The corrosion types of the prepared FeCoNiCrMn high-entropy alloy specimens in 3.5 wt.% NaCl solution and 0.5 mol/L H2SO4 solution were mainly pitting corrosion. In 3.5 wt.% NaCl solution, the FeCoNiCrMn high-entropy alloy has lower corrosion potential and higher corrosion current density compared with 1Cr18Ni9Ti stainless steel, while its pitting corrosion potential is also lower, indicating that the corrosion resistance of the high-entropy alloy is poorer in the Cl- environment.
    3) In 0.5 mol/L H2SO4 solution, the prepared FeCoNiCrMn high-entropy alloy specimens have lower corrosion potential and higher corrosion current density, indicating that the high-entropy alloy has a poorer ability to resist uniform corrosion at low potential, but due to the large passivation interval of the high-entropy alloy, the dimensional passivation current density is lower, indicating that the passivation film formed by the high-entropy alloy is more stable and has a better ability to resist corrosion at high potential The passivation film formed by the high entropy alloy is more stable and more resistant to corrosion at high potentials.
    Authors: Liu Jia, an Xuguang, Kong Qingquan, Shu Ming, wuxiaoqiang, luoyuanqi, Zhang Jing
  • 3) In 0.5 mol/L H2SO4 solution, the prepared FeCoNiCrMn high-entropy alloy specimens have lower corrosion potential and higher corrosion current density, indicating that the high-entropy alloy has a poorer ability to resist uniform corrosion at low potential, but due to the large passivation interval of the high-entropy alloy, the dimensional passivation current density is lower, indicating that the passivation film formed by the high-entropy alloy is more stable and has a better ability to resist corrosion at high potential The passivation film formed by the high entropy alloy is more stable and more resistant to corrosion at high potentials.
    Authors: Liu Jia, an Xuguang, Kong Qingquan, Shu Ming, wuxiaoqiang, luoyuanqi, Zhang Jing

Authors: Liu Jia, an Xuguang, Kong Qingquan, Shu Ming, wuxiaoqiang, luoyuanqi, Zhang Jing

Source: China High Entropy Alloy Manufacturer: www.epowermetals.com

(Yaang Pipe Industry is a leading manufacturer and supplier of nickel alloy and stainless steel products, including Super Duplex Stainless Steel Flanges, Stainless Steel Flanges, Stainless Steel Pipe Fittings, Stainless Steel Pipe. Yaang products are widely used in Shipbuilding, Nuclear power, Marine engineering, Petroleum, Chemical, Mining, Sewage treatment, Natural gas and Pressure vessels and other industries.)

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