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Article

Impact of Temperature on the Tensile Properties of Hypereutectic High-Entropy Alloys

by
Wei Jiang
1,2,
Shuaishuai Wu
1,2,
Xuehui Yan
1,2,
Haochen Qiu
1,2,3,
Shengli Guo
1,2,3,
Baohong Zhu
1,2,3,* and
Hanjun Zhang
1,2,3
1
GRIMAT Engineering Institute Co., Ltd., Beijing 101407, China
2
China GRINM Group Corporation Limited, Beijing 100088, China
3
General Research Institute for Nonferrous Metals, Beijing 100088, China
*
Author to whom correspondence should be addressed.
Coatings 2023, 13(11), 1836; https://doi.org/10.3390/coatings13111836
Submission received: 8 October 2023 / Revised: 21 October 2023 / Accepted: 23 October 2023 / Published: 27 October 2023
(This article belongs to the Special Issue Advances in Protective Coatings: Materials, Fabrication, Corrosion and Applications)
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Abstract

:
Eutectic high-entropy alloys (EHEAs) can achieve a balance of high strength and ductility. It has been found that the mechanical properties of hypoeutectic high-entropy alloys are superior to those of EHEAs. In this work, hypereutectic Al1.1CoCrFeNi2.1 alloy was prepared, and the mechanical properties in a wide temperature range were studied. The presence of both soft ordered L12 and hard BCC (B2) phases results in a combination of ductile and brittle fracture modes. The Al1.1CoCrFeNi2.1 hypereutectic high-entropy alloy contains more primary soft L12 phases, which ensure excellent ductility. Moreover, the Orowan by-passing mechanism caused by the B2 precipitates increases in the strength of the alloy for low-temperature tensile tests (−100 °C and 23 ± 2 °C). The −100 °C test exhibits a dimple morphology and demonstrates the highest ultimate tensile strength of 1231 MPa, along with an excellent elongation of 44%. At high tensile temperatures (650 °C, 750 °C, and 850 °C), the dislocation cutting mechanism and dynamic recrystallization increase the plasticity. However, the presence of a large number of cracks near the spherical primary L12 phase significantly reduces the ductility and strength. The results show that the hypereutectic Al1.1CoCrFeNi2.1 exhibits superior plasticity and strength properties at low temperatures. The findings of the article provide a new approach to enhancing the comprehensive mechanical properties of hypereutectic alloys.

1. Introduction

Yeh et al. in 2004 [1,2,3,4,5,6], established the concept of high-entropy alloys (HEAs), which were originally defined based on the viewpoint that high-mixing entropy favors the formation of a single solid–solution phase. HEAs contain at least four principal elements with an atomic percentage of 5%–35% [7,8,9,10]. HEAs have attracted increased attention due to their desirable properties resulting from a high entropy effect, slow diffusion effect, and cocktail effect [11,12,13,14,15].
From a mechanical standpoint, it is widely acknowledged that single-phased body-centered-cubic (BCC) HEAs possess constrained ductility. Conversely, single-phase face-centered-cubic (FCC) HEAs may possess enhanced ductility but display lower strength [16,17,18,19]. Eutectic high-entropy alloys (EHEAs), which contain a mixture of soft FCC and hard BCC phases, can achieve a balance of high strength and ductility, as well as excellent castability [5,20,21,22,23,24,25]. Among the reported EHEAs, the AlCoCrFeNi2.1 alloy, with the combination of a hard phase and soft phase, which contributes to achieving excellent mechanical properties, has attracted the most attention and is considered a potential structural and functional material [26,27,28,29,30,31,32].
The AlCoCrFeNiNi2.2 hypereutectic high-entropy alloy contains more primary FCC phases. Therefore, the ductility of the AlCoCrFeNiNi2.2 hypereutectic high-entropy alloy is superior to that of the AlCoCrFeNi2.1 eutectic high-entropy alloy [33]. Moreover, it is believed that the Al atoms in AlCoCrFeNi-based alloys can lead to the formation of a B2 precipitate phase, and the precipitate guarantees the strength of the alloys [34,35,36,37]. The above advantages make it clear that there is great potential for their application in the field of structural materials. However, hypereutectic alloys, which are prepared by increasing the Al content, have been scarcely investigated. Moreover, the influence of the primary FCC phase and B2 precipitate phase on the tensile properties of hypereutectic alloys in a wide temperature range have seldom been studied. Therefore, a novel hypereutectic Al1.1CoCrFeNi2.1 high-entropy alloy is prepared. This study presents a detailed discussion of the microstructural evolution and mechanical properties of the alloy in a wide temperature range.

2. Materials and Methods

2.1. Material Processing

In this work, the as-cast Al1.1CoCrFeNi2.1 (at%) high-entropy alloy was prepared in a vacuum magnetic levitation induction furnace. The raw materials of high purity Al, Co, Cr, Fe, and Ni (>99.9 at% pure) were remelted at least 5 times in the Ar atmosphere to guarantee homogeneity.

2.2. Tensile Test

Tensile tests were conducted at −100 °C (−100-alloy), 23 ± 2 °C (room temperature, RT-alloy), and elevated temperatures of 650 °C (650-alloy), 750 °C (750-alloy), and 850 °C (850-alloy) in air with a strain rate of 10−3 s −1. Dog-bone flat samples with the size of 49 mm × 12 mm were machined from the as-cast samples. The tensile properties were evaluated using a universal testing machine with a strain rate of 0.015 mm/min prior to the yield point and 4.8 mm/min after the yield point. Three parallel samples were tested to obtain the average values of the results.

2.3. Microstructural Characterization

The phase constitution of the alloys was determined by X-ray diffraction (XRD) at 30 kV with Cu Kα radiation. The XRD measurement was conducted at a step size of 4° for a range of 40°–100°. The morphology and microstructure of the alloys were observed by scanning-electron microscopy (SEM). The chemical composition of the alloys was identified using energy dispersive X-ray spectroscopy (EDS). The grain distribution was investigated by SEM, coupled with an electron backscattered diffraction (EBSD) detector. Transmission electron microscopy (TEM) was utilized to identify the microstructure of the alloys.

3. Results

3.1. Microstructure of the As-Cast Alloy

Figure 1 shows the SEM image and XRD pattern of the hypereutectic Al1.1CoCrFeNi2.1 alloy. The eutectic structures and dendrite structures can be observed in the as-cast condition. Two phases, a white phase (lamellar phase and primary spherical phase) and black phase, exhibit a significant distinction due to the different composition and microstructure, as shown in Figure 1a. The composition of the alloy was 18.12Al-16.01Co-16.11Cr-16.07Fe-33.69Ni (at%) from the EDS results, and the alloy consisted of an FCC and BCC dual-phase from the XRD results (Figure 1b).
Combined with the elemental distributions of the alloy (Figure 2), the white phase was recognized to consist of FCC phases (lamellar and spherical) enriched in Ni, Fe, Co, and Cr elements, whereas the black phase was identified as consisting of BCC enriched in Al and Ni.
Figure 3 gives the TEM images and corresponding selected-area electron diffraction (SEAD) patterns of the as-cast hypereutectic Al1.1CoCrFeNi2.1 alloy. The main diffraction spot of the FCC phase is shown in Figure 3a. The presence of superlattice reflections at the {001} position indicates the existence of the L12-ordered structure. The nano-sized precipitates (in BCC-lamellae) had a B2 superlattice structure (inset in Figure 3b).

3.2. Microstructure of the Alloy after Tensile Tests

To further provide insight into the deformation mechanism, TEM observation of the sample after tension tests (RT-alloy and 650-alloy) was conducted and the results are shown in Figure 4 and Figure 5. As shown in Figure 4a, at room temperature, parallel dislocations appear in the FCC phases, indicating the occurrence of dislocation slip and cross slip. Meanwhile, the deformation of FCC and BCC (B2) phases is asynchronous; the BCC (B2) phase is much harder than the FCC phase. Due to the weaker deformability property of the BCC (B2) phase, shear bands and shear fractures are observed in the BCC (B2) phases due to shearing stress concentration, and a high density of dislocations piled up at the shear fracture. From the magnified TEM image of Figure 4b, numerous nano-sized B2 precipitates are uniformly dispersed in the BCC phases with sizes of about 40 nm.
From the 650 °C tensile test (650-alloy), the dislocation density is decreased obviously, and necking is observed for the BCC (B2) phases. The BCC (B2) phase undergoes softening and both FCC and BCC (B2) phases experience severe plastic deformation (Figure 5a). From the magnified TEM image of Figure 5b, numerous nano-sized B2 precipitates are uniformly dispersed in the BCC phases with sizes of about 20 nm. After the high temperature tension test, the nano-sized precipitates dissolve into the BCC phase, causing a reduction in size.
The EBSD grain distribution maps of the tensile samples for the −100-alloy and RT-alloy are shown in Figure 6. The tensile sample at −100 °C (−100-alloy) exhibits a grain distribution comparable to that of the tensile sample at room temperature (RT-alloy).
However, newly formed fine grains in the high-temperature tensile samples were observed, suggesting the occurrence of recrystallisation (Figure 7a–c). The fraction of recrystallized grains increased with increasing tensile temperatures. Recrystallization promotes the dissociation of the dislocation. Since the dissociation of the partial dislocation decreases the dislocation density and reduces the barrier to dislocation movement, the work hardening phenomenon decreases at higher temperatures, and consequently, it promotes the plastic deformation ability. In conclusion, smaller B2 precipitates and the recrystallization enhanced the collaborative deformation ability of the L12 and BCC (B2) phases, which are beneficial to the excellent plastic deformation capacity at high temperatures.

3.3. Mechanical Properties

The tensile properties of the hypereutectic Al1.1CoCrFeNi2.1 alloys are shown in Figure 8. The strain of the alloys increased with increasing tension temperatures. The −100-alloy shows the highest ultimate strength of 1238 MPa. At room temperature, the alloy (RT-alloy) shows an ultimate tensile strength of 964 MPa. At elevated temperatures, there is a significant reduction in strength. The ultimate tensile strength is 455 MPa for the 650-alloy, and 278 MPa for the 750-alloy. The 850-alloy exhibits the lowest ultimate tensile strength, with a value of 156 MPa. Although the plastic deformation capacity exhibits a rising tendency, the strain is still lower than the −100-alloy.
To determine the fracture mechanism, typical fracture features of the alloys are observed, as shown in Figure 9. The tensile fractography of the −100-alloy exhibits a large number of dimple morphologies with a minor presence of trench-like morphologies, and no cracks are observed (Figure 9a). The RT-alloy also shows a mixture of trench-like and dimples morphology (Figure 9b). Two different kinds of fracture modes can be clearly distinguished for both the RT-alloy and the −100-alloy: a ductile fracture in the L12 phase and brittle-like fracture in the BCC (B2) phase. The incompatibility of strain arising from different levels of elasticity and plasticity between the BCC (B2) and L12 phases lead to the local stress concentration. During the tension, the ductile L12 phase is stretched and then gradually becomes thinner and edged up, whereas the BCC (B2) phase deforms difficultly and forms a trench bottom. Moreover, many more dimples are observed on the fracture surface of the −100-alloy compared to the RT-alloy, indicating its superior plastic deformation ability.
However, for the high-temperature tensile tests, as shown in Figure 9c–f, although numerous dimples also appear (ductile fracture), the cracks observed near the spherical L12 phase (Figure 9f) significantly reduce the plastic deformation ability.

4. Discussion

With an increasing tensile temperature, the tensile strength decreased. However, the total elongation of the alloys shows an increasing tendency, except for the low-temperature tensile samples (−100-alloy and RT-alloy). The −100 °C test exhibits the highest ultimate tensile strength, along with an excellent elongation. The effect of the tensile temperature on the tensile properties is investigated for the hypereutectic Al1.1CoCrFeNi2.1 alloy.

4.1. Synergistic Effect of L12 and BCC (B2) Phases

It has been known from earlier studies that the FCC phase (L12 phase) is more ductile than the BCC (B2) phase [23]. It seems plausible that the dislocation in the L12 phase is easier to move than that in the BCC (B2) phase. A large number of dislocations (dislocation slip and cross slip) are observed within the L12 phase at room temperature (RT-alloy), as shown in Figure 4a. The deformation of the FCC and BCC (B2) phases is asynchronous, resulting in the fractures of the BCC (B2) phases.
The precipitates inhibit the dislocation motion and result in a strengthening effect. Figure 4b shows that the B2 precipitate phase observed during the deformation process can effectively pin the dislocations through a process known as the Orowan bypass mechanism. When the dislocations approach the precipitates, they start to curve around the non-deformable particles. Under sufficiently applied stress, dislocations may move across the precipitates, leaving behind Orowan loops around the particles (Figure 10a). Dislocation movement can be impeded by the B2 precipitates, thereby improving the strength for the −100-alloy and RT-alloy.
For the 650-alloy, dislocations are easily cut through by the smaller B2 precipitates (20 nm), resulting in dislocation slip (Figure 5b and Figure 10b). The dislocation cutting phenomenon is identified as the main mechanism for the softening of the BCC (B2) phases in the 650-alloy. Softening of the BCC (B2) phases occurs without shear fracture, and plastic deformation occurs simultaneously in the L12 and BCC (B2) phases. Therefore, the ductility increases with increasing tensile temperatures.
However, during high temperature tensile tests, the bonding strength of the spherical primary L12 and BCC (B2) phases decreases. The cracks observed near the spherical L12 phase significantly reduce the plastic deformation ability and strength. Therefore, the plastic deformation ability of the low temperature tensile tests (−100-alloy) is more outstanding than that of the high temperature tensile tests.

4.2. Dynamic Recrystallization

The alloy undergoes recrystallization during the high-temperature tensile tests. When the dislocation density and driving force reach sufficient levels in the heated, formable alloy, recrystallization takes place. This is because the accelerated diffusion rate of the grain boundaries at high temperatures leads to the continuous growth of sub-grains, ultimately forming new recrystallized grains. In general, when a high temperature collectively ensures the sufficient nucleation time and the high diffusion rate of the grain boundary, dynamic recrystallization occurs. At the same time, the phenomenon of accumulated high-density dislocations disappeare, which improves the plastic deformation ability of the high temperature tensile tests, as shown in Figure 5a.
In conclusion, the Orowan by-passing mechanism and dislocation cutting mechanism affect the dislocation slip. Besides, dynamic recrystallization in the matrix reduces the stress concentration arising from dislocation motion and increases the plastic deformation ability. For the low temperature tensile tests, the Orowan by-passing mechanism caused by the B2 precipitates increase the strength (−100-alloy and RT-alloy). At high temperatures (650-alloy, 750-alloy, and 850-alloy), the dislocation cutting mechanism and dynamic recrystallization increase the plasticity, while the cracks near the spherical L12 phase significantly reduced the plastic deformation ability.
The Al1.1CoCrFeNi2.1 hypereutectic high-entropy alloy contains more primary soft FCC phases, which ensure excellent ductility. Moreover, the interaction of the B2 phase and dislocations triggers the Orowan bypass mechanism, thereby contributing to the excellent strength of the alloy. Therefore, compared to other reported hypereutectic high entropy alloys, the alloy studied in this work demonstrates comprehensive mechanical performance advantages [5,19,23].

5. Conclusions

In summary, in this work, hypereutectic Al1.1CoCrFeNi2.1 alloys were prepared by vacuum magnetic levitation induction melting. Based on the above analysis and results, the main conclusions are as follows:
  • The alloy consisted of L12 (lamellae and spherical) and BCC (B2) phases. Numerous nano-sized coherent B2 precipitates are uniformly dispersed in the BCC phases. A ductile fracture occurs in the L12 phase, while a brittle-like fracture occurs in the BCC (B2) phase for both the −100-alloy and RT-alloy.
  • At low tensile temperatures (−100 °C and 23 ± 2 °C), the Orowan by-passing mechanism affects the dislocation slip, contributing to the excellent strength of the alloy. The −100-alloy exhibits the highest ultimate tensile strength of 1231 MPa and excellent elongation of 44%.
  • At high tensile temperatures, the presence of smaller B2 precipitates and the recrystallization resulting from crystallization enhance the collaborative deformation ability of the L12 and BCC (B2) phase. However, the cracks observed near the spherical primary L12 phase significantly reduced the plastic deformation ability and strength.

Author Contributions

Conceptualization, B.Z. and S.G.; methodology, W.J.; formal analysis, B.Z. and X.Y.; investigation, S.W. and X.Y.; data curation, S.W., H.Q. and H.Z.; writing—original draft preparation, W.J.; writing—review and editing, S.G. and H.Q.; visualization, H.Z.; supervision, B.Z.; funding acquisition, W.J. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Innovation Foundation of GRIMAT Engineering Institute (No. 57922102, No. 57922201) and Youth Fund Project of GRINM (No. 66922207).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. (a) SEM image and (b) XRD pattern of hypereutectic Al1.1CoCrFeNi2.1.
Figure 1. (a) SEM image and (b) XRD pattern of hypereutectic Al1.1CoCrFeNi2.1.
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Figure 2. Elemental distributions of the hypereutectic Al1.1CoCrFeNi2.1.
Figure 2. Elemental distributions of the hypereutectic Al1.1CoCrFeNi2.1.
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Figure 3. TEM images of Al1.1CoCrFeNi2.1: (a) SAED corresponding to the L12; (b) HRTEM image of BCC (B2).
Figure 3. TEM images of Al1.1CoCrFeNi2.1: (a) SAED corresponding to the L12; (b) HRTEM image of BCC (B2).
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Figure 4. TEM images of RT-alloy: (a) low magnification and (b) dislocation morphology around B2 phase.
Figure 4. TEM images of RT-alloy: (a) low magnification and (b) dislocation morphology around B2 phase.
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Figure 5. TEM images of 650-alloy: (a) low magnification and (b) dislocation morphology around B2 phase.
Figure 5. TEM images of 650-alloy: (a) low magnification and (b) dislocation morphology around B2 phase.
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Figure 6. EBSD grain distribution maps of (a) −100-alloy; (b) RT-alloy.
Figure 6. EBSD grain distribution maps of (a) −100-alloy; (b) RT-alloy.
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Figure 7. EBSD grain distribution maps of (a) 650-alloy; (b) 750-alloy; (c) 850-alloy.
Figure 7. EBSD grain distribution maps of (a) 650-alloy; (b) 750-alloy; (c) 850-alloy.
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Figure 8. Mechanical properties of hypereutectic Al1.1CoCrFeNi2.1 alloy at different temperatures.
Figure 8. Mechanical properties of hypereutectic Al1.1CoCrFeNi2.1 alloy at different temperatures.
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Figure 9. Fracture morphologies of (a) −100-alloy; (b) RT-alloy; (c) 650-alloy; (d) 750-alloy; (e) 850-alloy; (f) magnified spherical L12 and lamellar eutectic of 850-alloy.
Figure 9. Fracture morphologies of (a) −100-alloy; (b) RT-alloy; (c) 650-alloy; (d) 750-alloy; (e) 850-alloy; (f) magnified spherical L12 and lamellar eutectic of 850-alloy.
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Figure 10. Schematic illustration of (a) Orowan bypass mechanism and (b) dislocation cutting mechanism.
Figure 10. Schematic illustration of (a) Orowan bypass mechanism and (b) dislocation cutting mechanism.
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MDPI and ACS Style

Jiang, W.; Wu, S.; Yan, X.; Qiu, H.; Guo, S.; Zhu, B.; Zhang, H. Impact of Temperature on the Tensile Properties of Hypereutectic High-Entropy Alloys. Coatings 2023, 13, 1836. https://doi.org/10.3390/coatings13111836

AMA Style

Jiang W, Wu S, Yan X, Qiu H, Guo S, Zhu B, Zhang H. Impact of Temperature on the Tensile Properties of Hypereutectic High-Entropy Alloys. Coatings. 2023; 13(11):1836. https://doi.org/10.3390/coatings13111836

Chicago/Turabian Style

Jiang, Wei, Shuaishuai Wu, Xuehui Yan, Haochen Qiu, Shengli Guo, Baohong Zhu, and Hanjun Zhang. 2023. "Impact of Temperature on the Tensile Properties of Hypereutectic High-Entropy Alloys" Coatings 13, no. 11: 1836. https://doi.org/10.3390/coatings13111836

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