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Article

Study on Mechanical Properties and Microstructure of FeCoCrNi/Al Composites via Cryorolling

by
Kaiguang Luo
1,2,
Yuze Wu
1,2,
Yun Zhang
1,2,*,
Gang Lei
1,2 and
Hailiang Yu
1,2,3
1
State Key Laboratory of High Performance Complex Manufacturing, Central South University, Changsha 410083, China
2
College of Mechanical and Electrical Engineering, Central South University, Changsha 410083, China
3
Light Alloys Research Institute, Central South University, Changsha 410083, China
*
Author to whom correspondence should be addressed.
Metals 2022, 12(4), 625; https://doi.org/10.3390/met12040625
Submission received: 21 February 2022 / Revised: 25 March 2022 / Accepted: 2 April 2022 / Published: 4 April 2022
(This article belongs to the Special Issue Microstructure and Properties of Rolled Alloys)
Browse Figures
Versions Notes

Abstract

:
Aluminum matrix composites (AMCs) reinforced by 1.5 and 3 wt% FeCoCrNi high-entropy alloy particles (HEAp) were obtained by a stir casting process. The AMCs strip was further prepared by room temperature rolling (RTR, 298 K) and cryorolling (CR, 77 K). The mechanical properties of the AMCs produced by RTR and CR were studied. The effect of a microstructure on mechanical properties of composites was analyzed by scanning electron microscopy (SEM). The results show that CR can greatly improve the mechanical properties of the HEAp/AMCs. Under 30% rolling reduction, the ultimate tensile strength (UTS) of the RTR 1.5 wt% HEAp/AMCs was 120.3 MPa, but it increased to 139.7 MPa in CR composites. Due to the volume shrinkage effect, the bonding ability of CR HEAp/AMCs reinforcement with Al matrix was stronger, exhibiting higher mechanical properties.

1. Introduction

Aluminum matrix composites (AMCs) have many advantages, such as high specific strength and good wear resistance, that have attracted them more attention in recent years [1,2,3,4]. According to the reinforcement shape, AMCs mainly include continuous-fiber, whisker, and particle-reinforced composites [5,6,7]. Particle-reinforced aluminum matrix composites have become the most widely studied AMCs because of the advantages of the simple preparation process and low manufacturing cost [8,9,10]. Particle reinforcements mainly include ceramics and metals [11,12]. Although ceramic particles have a high strength, they are difficult to deform. As a result, after the AMCs are prepared, the secondary processing becomes difficult. Therefore, metal particles with a high strength become a potential research focus.
Alaneme et al. [13] studied aluminum matrix composites reinforced with CuZnAl, steel, nickel, and SiC particles. Compared with the SiC-reinforced AMCs, the metal particles-reinforced AMCs have better mechanical properties. In recent years, a new type of alloy, high-entropy alloy (HEA), has gradually entered the field of vision [14,15,16]. High-entropy alloys are also known as multi-principal or multi-component alloys [17]. HEAs have many advantages, such as a high strength and good plasticity, so they are paid more attention to in material science and engineering [18]. The addition of HEAp to AMCs as reinforcement particles has attracted extensive attention. Liu et al. [19] prepared AMCs reinforced with AlCoCrFeNi HEAp by spark plasma sintering technology. With the increase of sintering temperature, the strength and elongation of the AMCs were significantly increased. Praveen et al. [20] prepared AA2024 AMCs reinforced with HEAp. Mechanical properties such as ultimate tensile strength (UTS) and Young’s modulus were improved. Wang et al. [21] prepared aluminum matrix composites reinforced by Al3CoCrFeNi HEAp through the powder metallurgy process. After hot extrusion, the average grain size reached about 70 nm.
FeCoCrNi high-entropy alloy was one of the most widely studied HEAs [22]. It has a good strength and plasticity at room temperature and shows more excellent mechanical properties at a low temperature [23,24,25] (77 K). Many HEAs. such as FeCoCrNiMn and AlCoCrFeNi, were developed based on FeCoCrNi [26,27,28]. In this study, FeCoCrNi HEAp was used as a reinforcement to prepare AMCs. In order to better understand the relationship between the mechanical properties and microstructure of HEAp/AMCs in the cryorolling process, the mechanical properties of HEAp/AMCs were studied in room temperature rolling (RTR) and cryorolling (CR) under different deformation. The effect of rolling deformation on the microstructure of HEAp/AMCs under a cryogenic environment (77 K) was discussed in this paper.

2. Materials and Methods

Commercial FeCoCrNi HEAps were selected as the reinforcement of the AMCs, and the matrix was high purity aluminum. The FeCoCrNi HEAp and Al alloy ingot were bought from Beijing Yanbang New Material Technology Co., Ltd. (Beijing, China). The Al alloy was high-purity aluminum; its chemical composition was 99.99Al-0.005Cu-0.003Fe-0.002Si. The preparation processes of the HEAps were as follows: A certain amount of five-metal elements was weighed into the induction heating furnace at 1873 K with a 573 K superheat temperature. They were sprayed into fog beads by a high-pressure inert gas flow with a pressure of 4.5 MPa. The cylindrical AMCs ingot with HEAp mass fractions of 0, 1.5, and 3% was obtained by a stir casting process at a 1073 K temperature. The AMCs ingot was hot extruded at 713 K to obtain a composite sheet with a thickness of 3.3 mm. Then the composites were prepared by room temperature rolling (RTR) and cryorolling (CR). The deformation temperature of RTR was 298 K, and that of CR was 77 K. The working roll diameter in the rolling process was 80 mm, and the rolling speed was 1 m/min. Before each cryorolling of the AMCs sheets, the composite material plate was cooled in the liquid nitrogen tank for 5 min so that the HEAp/AMCs sheet was fully cooled. When the deformation of HEAp/AMCs reached 30%, 60%, and 90%, the samples of HEAp/AMCs were retained to test their mechanical properties and microstructure.
The microhardness of the HEAp/AMCs was measured by a Vickers microhardness tester (HXD-2000TMC/LCD 181101X, Shanghai Taiming Optical Instrument Co., Ltd., Shanghai, China) at the indenting head load of 1 N and a holding time of 15 s. The microhardness of each sample was randomly tested 5 times. Then, 800–2000 mesh sandpaper was used to polish the surface of the samples before microhardness testing. The samples were then polished with a polishing cloth and diamond polishing paste. The size of microhardness test samples was 10 mm × 12 mm with a rectangular shape. The strain rate of the quasi-static tensile test was 1 × 10−3 s−1, and the material in the same state was repeated three times. A scanning electron microscope (TESCAN MIRA3 LMU, Zeiss Sigma 300, Shanghai, China) equipped with energy dispersive spectrometer (EDS, Zeiss Sigma 300, Shanghai, China) was used to detect the morphology, microstructure, and element distribution of HEAp and HEAp/AMCs.

3. Results and Discussion

3.1. Morphology and Element Distribution of HEAp

The morphology of FeCoCrNi HEAp was shown in Figure 1a. It can be seen from the figure that the HEAp has a good morphology and relatively uniform particle size distribution. The size of HEAp was quantitatively analyzed, and the results were shown in Figure 1b. The average particle size of FeCoCrNi HEAp was 3.9 μm.
Figure 2a shows secondary electron images of HEAp. EDS analysis was performed on HEAp in this region. Figure 2b–e shows the distribution results of the Ni, Co, Cr, and Fe elements, respectively. These elements were relatively uniformly distributed in HEAp, and no obvious element segregation phenomenon was found. A further quantitative analysis of elements in HEAp was carried out, and the results were shown in Figure 2f. The interpolation table in Figure 2f shows the mass percentage and atomic percentage results of the elements in FeCoCrNi HEAs. FeCoCrNi HEA was composed of four elements. The main proportion for each element was Cr-26.56%, Fe-25.05%, Co-24.77%, and Ni-23.61%, which indicated that FeCoCrNi HEA conformed to the nominal ratio of equal atomic ratio [29,30]. Figure 2g,h were SEM images of 1.5 wt% and 3 wt% HEAp/AMCs before rolling deformation, respectively. Figure 2g shows that the HEAp reinforcement was evenly distributed in the aluminum alloy matrix. However, due to the relatively small amount of additive, there were some regions without reinforcement in the Al matrix. When the mass fraction of HEAp reached 3 wt%, the Al matrix was almost full of reinforcement (Figure 2h).

3.2. Mechanical Properties of HEAp/AMC

Figure 3 shows the mechanical properties of initial composites without rolling deformation. It was obvious in Figure 3a that without the addition of HEAp, the microhardness of aluminum alloy was only 25.4 HV. When 1.5 wt% HEAp was added, the microhardness of the AMCs was evidently increased to 38.1 HV, which increased by 50%. With the mass fraction of HEAp reacheding 3%, the microhardness of the AMCs was further improved to 58.7 HV. Compared with pure aluminum, the microhardness of 3 wt% HEAp/AMCs increased by 131%. The results indicated that HEAp had a significant strengthening effect to improve the microhardness of aluminum alloy. It was further verified by a quasistatic tensile test. Figure 3b shows the stress–strain curves of HEAp/AMCs. The UTS and elongation of pure aluminum were 33.4 MPa and 33.2%, respectively. However, the UTS of 1.5 wt% HEAp/AMCs was 80.3 MPa, which was 140% higher than that of pure aluminum. At the same time, its elongation was 23%, indicating a good toughness. When the mass fraction of HEAp was further increased to 3%, the UTS of the AMCs was increased to 111 MPa, which was 232% higher than that of pure aluminum. Thus, the UTS of the HEAp/AMCs were greatly improved by adding 3 wt% HEAp. Meanwhile, a relatively high elongation (14.6%) was exhibited in HEAp/AMCs.
Two deformation processes, room temperature rolling (RTR) and cryorolling (CR), were carried out for the HEAp/AMCs. Figure 4 shows the microhardness of 1.5 wt% (Figure 4a) and 3 wt% HEAp (Figure 4b) AMCs deformed by two different rolling processes. It can be seen from the statistical results that the microhardness of the HEAp/AMCs has been improved in different degrees after rolling deformation. The microhardness of the composites obtained by CR was generally higher than that obtained by RTR. For 1.5 wt% HEAp/AMCs after 30% deformation by RTR, its microhardness increased from 38.1 HV to 46.3 HV, increasing by 21.5%. Under the same deformation, the microhardness of the CR HEAp/AMCs was 50.9 HV. Comparing the values in RTR and CR composites, the microhardness of the HEAp/AMCs was increased by 33.6% after CR. Similarly, when the rolling reduction ratio reached 60%, the microhardness of the CR HEAp/AMCs was still remarkably higher than that of the RTR. A further deformation was performed to verify the improvement of mechanical properties on HEAp/AMCs by the CR process. The results show that when the rolling deformation reached 90%, the microhardness of the RTR HEAp/AMCs was 54.8 HV, while it was 61.8 HV after CR. The microhardness of the rolled HEAp/AMCs was 43.8% (RTR) and 62.2% (CR), higher than that of the initial undeformed ones, respectively. Compared with RTR, CR greatly improves the microhardness of the HEAp/AMCs [31].
Figure 5a,b shows the stress–strain curves of 1.5 wt% and 3 wt% HEAp/AMCs under different rolling processes. For a more intuitive comparison, Figure 5c,d show the UTS histograms of HEAp/AMCs. It can be seen from Figure 5 that the UTS of the HEAp/AMCs was improved to varying degrees after RTR and CR. The UTS of the CR HEAp/AMCs was generally higher than that of RTR. Taking 1.5 wt% HEAp/AMCs as an example, the UTS of the RTR HEAp/AMCs was increased by 49.8% (120.3 MPa) under 30% deformation, while the CR ones was improved by 49.8% (139.7 MPa). The elongation of the RTR and CR HEAp/AMCs was 12.6% and 12.1%, respectively, which indicated that the UTS of the HEAp/AMCs can be obviously improved by CR without significantly reducing the elongation. Under 60% deformation, the UTS of the RTR HEAp/AMCs was 148.4 MPa; it was further improved to 161.9 MPa under the CR process. After RTR, the UTS of the HEAp/AMCs was increased by 84.8%, while that of CR HEAp/AMCs was increased by 101.6%. Further, when the rolling reduction was increased to 90%, the HEAp/AMCs exhibited an UTS of 162.5 MPa and 181.2 MPa, respectively, for the RTR and CR samples. It can be concluded that, under different rolling reduction ratios, the CR process can greatly improve the mechanical properties of HEAp/AMCs.

3.3. Microstructure Analysis of HEAp/AMCs

Figure 6 shows the tensile fracture morphology of 1.5 wt% HEAp/AMCs after RTR and CR. From Figure 5, we can see that under 30% deformation, the RTR and CR HEAp/AMCs show a good toughness. As shown in Figure 6a,d, a large number of dimples were observed in the tensile fracture of HEAp/AMCs obtained by different rolling processes. At room temperature, a small number of dimples with a large individual area was presented in the fracture surface [32]. However, a larger density of smaller dimples was observed in CR HEAp/AMCs, indicating a good elongation. Several cleavage planes with local small areas were observed in RTR HEAp/AMCs. The formation of the cleavage plane was disadvantageous to the elongation of the AMCs, which implied that the elongation of the HEAp/AMCs would decrease after RTR [33,34]. However, no obvious cleavage plane was observed on the fracture surface of the CR HEAp/AMCs. Compared with Figure 6a,d, the debonding of HEAp was observed in RTR samples, while HEAp showed a better bonding ability after CR. Attributed to the volume shrinkage of HEA and aluminum alloy during CR, a difference in coefficient thermal expansion between HEAp reinforcement and aluminum alloy matrix was exhibited in the rolling process [31,35,36]. Under the condition of a cryogenic environment, the ratio of volume shrinkage will be different [37,38]. The coefficient thermal expansion of HEAp was small, as well as was the corresponding volume shrinkage effect [38]. Aluminum alloy will have a more obvious volume shrinkage, being more firmly coated with HEAp [37]. Macroscopically, the bonding ability of HEAp with an aluminum alloy matrix was stronger after cryorolling. The deformation behavior of HEAp during CR deformation (77 K) was quite different from RTR. In the cryogenic environment, dislocation recovery and annihilation were inhibited. Additionally, with the increase of rolling deformation, the deformations of HEAp and aluminum alloy matrix were quite different. The larger elastic modulus of the HEAp led to the slow deformation accumulation, so the dislocation caused by rolling deformation accumulated around the HEAp. Therefore, after CR, the HEAp/AMCs will accumulate more deformation dislocations around the HEAp, which was manifested as a higher tensile strength in macroscopic mechanical properties. In addition, higher density dislocations gathered around HEAp, resulting in a higher stress concentration, which led to the crushing and further refining of HEAp. The smaller HEAp produced by CR will further pin the dislocation and accumulate a higher dislocation density. Therefore, during the tensile process, the tendency of HEAp/AMCs fracture was delayed. At room temperature, the deformation temperature was higher, and the dislocation density could not be accumulated efficiently. When rolled at room temperature, there was no volume shrinkage effect in the HEAp/AMCs. As a result, the deformation of HEAp was not coordinated with the aluminum alloy matrix, and shear action occurred between the aluminum alloy matrix and HEAp. Due to the shear force, the interface between the aluminum alloy matrix and HEAp was destroyed, resulting in a debonding phenomenon, which was not conducive to the further improvement of mechanical properties. Figure 6b,e show the fracture morphologies of RTR and CR HEAp/AMCs after 60% deformation, respectively. The width of the RTR HEAp/AMCs was 255 μm, and the reduction of the area was 80.4%. After CR, the tensile fracture width of the HEAp/AMCs was 304 μm, and the calculated reduction of the area was 76.6%. This further proved that the CR process maintained a good elongation of the composites on the premise of improving the UTS of the HEAp/AMCs. Figure 6c,f show the fracture morphologies of HEAp/AMCs after 90% deformation. Under a larger deformation, the composites still had an appropriate elongation and a considerable number of dimples.
Figure 7 shows the tensile fracture morphology of 3 wt% HEAp/AMCs after RTR and CR. Dimples were observed on the surface of tensile fractures, indicating that the composites still had a considerable toughness after deformation [39,40]. It was noteworthy that the debonding of HEAp was observed in the tensile surface of RTR (Figure 7b) rather than the CR HEAp/AMCs. The results show that the CR bonding ability of HEAp reinforcement and matrix after cryorolling was better than that in RTR [41]. The debonding of HEAp in the RTR HEAp/AMCs would evidently decrease the strengthening effect of HEAp. Thus, the UTS of RTR HEAp/AMCs was lower than that in the CR samples.
Figure 8 shows the tensile fracture morphology of the 3 wt% HEAp/AMCs after the rolling deformation reached 60% and 90%. It can be seen that a large number of dimples still existed in the fracture of the AMCs even after the deformation reached 90%. Therefore, the HEAp/AMCs still had a good elongation under large deformation.

4. Conclusions

(1)
In this study, the mechanical properties of the HEAp/AMCs were greatly improved by adding FeCoCrNi HEAp. The UTS increased from 33.4 MPa (pure Al) to 111 MPa (3 wt% HEAp/AMCs). Then, HEAp/AMCs sheets were prepared by RTR and CR processes. The UTS of the RTR 1.5 wt% HEAp/AMCs was 120.3 MPa under 30% reduction, and that of the CR was 139.7 MPa. Furthermore, the elongations of the RTR and CR 1.5 wt% HEAp/AMCs were 12.6% and 12.1%, respectively. The UTS of CR HEAp/AMCs was increased by 16.1% compared with RTR. After rolling deformation, the elongation of HEAp/AMCs did not decrease sharply. This was one of the advantages of HEAp as a reinforcement of AMCs.
(2)
Debonding between HEAp and aluminum alloy matrix occurred in the HEAp/AMCs after RTR. However, no obvious debonding phenomenon was observed in CR due to the volume shrinkage effect. The bonding ability between the HEAp reinforcement and aluminum alloy matrix was remarkably improved by the CR process. HEAp/AMCs with higher mechanical properties can be obtained via the CR process.

Author Contributions

Conceptualization, K.L. and H.Y.; methodology, K.L. and Y.Z.; validation, K.L., Y.W., Y.Z., G.L. and H.Y.; formal analysis, K.L. and Y.Z.; investigation, K.L. and Y.W.; resources, H.Y.; data curation, K.L. and G.L.; writing—original draft preparation, K.L. and Y.Z.; writing—review and editing, K.L., Y.Z. and H.Y.; visualization, G.L.; supervision, H.Y.; project administration, H.Y.; funding acquisition, H.Y. and Y.Z. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the National Key Research and Development Program (Grant No. 2019YFB2006500), the High-tech Industry Technology Innovation Leading Plan of Hunan Province (Grant No. 2020GK2032), the Natural Science Foundation of Hunan Province (Grant No. 2021JJ40774), the Science and Technology Innovation Program of Hunan Province (Grant No. 2020RC2002), the Innovation Driven Program of Central South University (Grant No. 2019CX006), and the Research Fund of the Key Laboratory of the High Performance Complex Manufacturing at Central South University.

Institutional Review Board Statement

No ethical approval was required.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. (a) SEM images of HEAp morphology. (b) Statistical diagram of particle size distribution of high entropy alloy.
Figure 1. (a) SEM images of HEAp morphology. (b) Statistical diagram of particle size distribution of high entropy alloy.
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Figure 2. (a) SEM image of HEAp; EDS diagram results of (b) Ni, (c) Co, (d) Cr, and (e) Fe element distribution; and (f) Cr, Fe, Co, and Ni quantitative results of EDS elements in HEAp. (g,h) SEM images of 1.5 wt% and 3 wt% HEAp/AMCs before rolling deformation.
Figure 2. (a) SEM image of HEAp; EDS diagram results of (b) Ni, (c) Co, (d) Cr, and (e) Fe element distribution; and (f) Cr, Fe, Co, and Ni quantitative results of EDS elements in HEAp. (g,h) SEM images of 1.5 wt% and 3 wt% HEAp/AMCs before rolling deformation.
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Figure 3. Mechanical properties of the composites in the initial state. (a) Vickers microhardness. (b) stress–strain curves.
Figure 3. Mechanical properties of the composites in the initial state. (a) Vickers microhardness. (b) stress–strain curves.
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Figure 4. Microhardness of the AMCs after RTR and CR with (a) 1.5 wt% HEAp, (b) 3 wt% HEAp.
Figure 4. Microhardness of the AMCs after RTR and CR with (a) 1.5 wt% HEAp, (b) 3 wt% HEAp.
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Figure 5. Tensile stress–strain curves of the AMCs after RTR and CR with (a) 1.5 wt% HEAp and (b) 3 wt% HEAp. UTS histogram of (c) 1.5 wt% HEAp and (d) 3 wt% HEAp.
Figure 5. Tensile stress–strain curves of the AMCs after RTR and CR with (a) 1.5 wt% HEAp and (b) 3 wt% HEAp. UTS histogram of (c) 1.5 wt% HEAp and (d) 3 wt% HEAp.
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Figure 6. SEM images of RTR 1.5 wt% HEAp/AMCs at (a) 30%, (b) 60%, and (c) 90%. CR 1.5 wt% HEAp/AMCs at (d) 30%, (e) 60%, and (f) 90% rolling reduction-ratios fracture morphologies.
Figure 6. SEM images of RTR 1.5 wt% HEAp/AMCs at (a) 30%, (b) 60%, and (c) 90%. CR 1.5 wt% HEAp/AMCs at (d) 30%, (e) 60%, and (f) 90% rolling reduction-ratios fracture morphologies.
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Figure 7. Fracture morphologies of RTR 3 wt% HEAp/AMCs (a,b). CR 3 wt% HEAp/AMCs (c,d) at 30% rolling reduction ratios.
Figure 7. Fracture morphologies of RTR 3 wt% HEAp/AMCs (a,b). CR 3 wt% HEAp/AMCs (c,d) at 30% rolling reduction ratios.
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Figure 8. (a,b) Fracture morphologies of RTR. (c,d) CR 3 wt% HEAp/AMCs at 60% and 90% rolling reduction ratios.
Figure 8. (a,b) Fracture morphologies of RTR. (c,d) CR 3 wt% HEAp/AMCs at 60% and 90% rolling reduction ratios.
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Luo, K.; Wu, Y.; Zhang, Y.; Lei, G.; Yu, H. Study on Mechanical Properties and Microstructure of FeCoCrNi/Al Composites via Cryorolling. Metals 2022, 12, 625. https://doi.org/10.3390/met12040625

AMA Style

Luo K, Wu Y, Zhang Y, Lei G, Yu H. Study on Mechanical Properties and Microstructure of FeCoCrNi/Al Composites via Cryorolling. Metals. 2022; 12(4):625. https://doi.org/10.3390/met12040625

Chicago/Turabian Style

Luo, Kaiguang, Yuze Wu, Yun Zhang, Gang Lei, and Hailiang Yu. 2022. "Study on Mechanical Properties and Microstructure of FeCoCrNi/Al Composites via Cryorolling" Metals 12, no. 4: 625. https://doi.org/10.3390/met12040625

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