High Entropy Amorphous Alloys

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This entry is adapted from the peer-reviewed paper 10.3390/ma17020453

High entropy amorphous alloys (HEAAs) are materials that have received much attention in recent years. They exhibit many unique properties; however, research on their composition design method has not been deep enough.

high entropy alloy amorphous alloy bulk metallic glass glass-forming ability

1. Introduction

Material innovation has become one of the most important driving forces for promoting human civilization progress, as well as promoting the development of technology and industrial upgrading. Amorphous alloys and high entropy alloys are two types of high-performance materials that have developed rapidly in the past several decades. Since its first report in 1960 ^[1], amorphous alloys have undergone significant development and have now expanded to dozens of material systems. Inoue et al. developed a copper mold casting method that greatly reduced fabrication costs ^[2]^[3]. Peker and Johnson designed a very famous amorphous alloy, Zr_41.2Ti_13.8Cu_12.5Ni₁₀Be_22.5, which was also called Vit1 since it possesses very good glass-forming ability (GFA) ^[4]. Vit1 played an important role in promoting the industrialization of amorphous alloys. Inoue presented a long review of amorphous alloys, and it got more than 5600 citations ^[5]. After entering the 21st century, more and more amorphous alloys were developed, such as Cu–Zr–Ti–Sn ^[6], Ni–Nb–Sn ^[7], Pt–Co–Ni–Cu–P ^[8], Zr–Al–Co ^[9], Zr–Cu–Al ^[10], Cu–Zr–Ag ^[11], etc.

One of the main challenges in developing amorphous alloys is how to improve its GFA. Li et al. found that similar atom substitution may be an effective way ^[12]^[13]. Santos et al. proposed a topological instability (λ) criterion to evaluate GFA in an Ni–Nb–Zr system ^[14]. Zhang et al. developed the Ti_32.8Zr_30.2Ni_5.3Cu₉Be_22.7 quinary bulk amorphous alloy; it possesses good GFA and its critical diameter exceeds 50 mm ^[15]. Nishiyama et al. prepared the world’s biggest glassy alloy, namely the Pd_42.5Cu₃₀Ni_7.5P₂₀ cylindrical glassy alloy sample. Its diameter was 80 mm and it was obtained by fluxing and water quenching method ^[16]. Apart from experiments, several parameters were proposed for evaluating the GFA of an alloy, such as T_rg ^[17], ΔT_x ^[18], γ ^[19], etc. The atomic simulation method was also applied to enhance the GFA of Ni–Nb–Ti amorphous alloys by Li et al. ^[20]. Amorphous alloys possess outstanding performance, such as high strength, high hardness, good corrosion resistance, and wear resistance, etc. As a result, amorphous alloys are used as low-loss power transformers, precise forming parts, micro-electro-mechanical system components, etc.

The concept of a high entropy alloy (HEA) has received widespread attention from the material research community since its first report in 2004 ^[21]. High entropy alloys usually contain five or more elements while the concentration of each element was in the range between 5% and 35%. In other words, the configurational entropy of high entropy alloy should be greater than 1.5 R, in which R represents the ideal gas constant (8.314 J/(mol·K)). For alloys containing five elements with equal atomic concentration, the configurational entropy reaches 1.61 R. In this sense, they are called high entropy alloys. In thermodynamics, entropy is a parameter characterizing the degree of disorder in a system. The degree of disorder increases as the number of constituent elements increases. Unlike traditional alloys that are based on one or two principle elements with other elements as minor additions, high entropy alloys belong to multicomponent, non-principle element alloy systems. Due to its breakthrough in traditional alloy design concepts, a new door for material research has opened up, making thousands of material combinations possible. As indicated by calculation, an array choice including 13 mutually miscible metallic elements enables 7099 high entropy alloy systems with 5 to 13 elements in equal molar ratios ^[21]. It provides a wide range of space and possibilities for developing new alloys.

Cantor et al. developed a series of multicomponent alloys. It was found that the total number of phases is always well below the maximum equilibrium number allowed by the Gibbs phase rule. Among them, a Fe₂₀Cr₂₀Mn₂₀Ni₂₀Co₂₀ alloy possesses an FCC structure ^[22]. This alloy was called “Cantor alloy”, and it was intensively studied by other researchers. For example, Gludovatz et al. found that the Cantor alloy possesses exceptional damage tolerance with tensile strengths above 1 GPa and fracture toughness values exceeding 200 MPa·m^1/2; it is fracture resistant for cryogenic application ^[23]. Shahmir et al. provided an overview on microstructural engineering of the Cantor alloy in the past twenty years ^[24]. Zhang et al. proposed that phase formation of HEA can be separated by mixing enthalpy ΔH_mix and atomic-size difference δ, it provides important guidance in designing HEAs with desired phases and microstructure ^[25]. Yamabe-Mitarai et al. studied the stability of Ti-containing high-entropy alloys, it was found that strengths of the BCC HEAs were greater than those of the HCP HEAs at 873 K, they were also greater than that of the commercial Ti alloy TIMETAL 834, indicating that BCC HEAs may be applied at elevated temperatures ^[26]. Uporov et al. found that ScGdTbDyHo HEA possesses good magnetocaloric properties and it can be influenced by the synthesis route ^[27]. Most HEAs were prepared by casting method; recently it was found that additive manufacturing characterized by net-shape processing is suitable for elevating the properties of HEAs ^[28]^[29]^[30]. Overall, great progress has been made in phase forming rules, composition design, processing, and application of HEA under various circumstances; they may be potential materials applied in many fields, such as heat-resistant and wear-resistant coatings, magnetic materials, and extreme high/low-temperature materials, etc.

Many factors could affect the phase formation of HEAs. In most cases, HEAs form solid solutions (especially BCC, FCC, and HCP) or intermetallics. However, under certain conditions, an amorphous structure could also be formed; this is high entropy amorphous alloy (HEAA). HEAAs possess both the long-range disordered atomic structure stacking characteristics of amorphous alloys and compositional complex characteristics in high entropy alloys. They are a new type of multiple component-disordered alloy. In other words, HEAA comprises five or more elements with an atomic ratio of each element between 5% and 35%, while it possesses an amorphous structure at room temperature. From a scientific research perspective, HEAAs provide a model material connecting amorphous alloys and high entropy alloys; it is helpful for intensive research on the amorphous forming rule of amorphous alloys and the phase evolution mechanism of high entropy alloys. From an industrial application perspective, due to complicated composition and structural characteristics, HEAAs exhibit a series of unique physical, chemical, and mechanical properties; they may be applied on certain specific occasions.

So far, positive progress has been achieved and dozens of HEAAs have been developed. The first batch of HEAAs was reported in 2002 by Ma et al., namely Ti₂₀Zr₂₀Hf₂₀Cu₂₀M₂₀ (M = Fe, Co, Ni) alloys. Among them, the Ti₂₀Zr₂₀Hf₂₀Cu₂₀Ni₂₀ alloy can form bulk metallic glass (BMG) with a critical diameter of 1.5 mm. They were called multicomponent glassy alloys or non-base glassy alloys at that time ^[31]. Later in 2011, the research work continued. Zhao et al. prepared a Zn₂₀Ca₂₀Sr₂₀Yb₂₀(Li_0.55Mg_0.45)₂₀ BMG and it possesses homogeneous flow behavior at room temperature ^[32]. Takeuchi et al. developed the Pd₂₀Pt₂₀Cu₂₀Ni₂₀P₂₀ alloy, its critical diameter reaches 10 mm and the concept of high entropy bulk metallic glass (HE-BMG) was proposed ^[33]. Li et al. developed CaMgZnSrYb HE-BMG with good biodegradable properties ^[34]. Later, Yao’s group developed a series of Ti–Zr–(Hf)–Cu–Ni–Be HE-BMGs with good GFA ^[35]^[36]^[37]^[38]; the composition design method will be discussed in detail later. Kim et al. developed Er–Gd–Y–Al–Co HE-BMGs and found that the relation between the fragility and elastic properties of these alloys is quite different from traditional BMGs ^[39]. Xu et al. developed Fe₂₅Co₂₅Ni₂₅ (P, C, B, Si)₂₅ HE-BMGs with good magnetic properties ^[40]. Huo et al. developed a denary HE-BMG with a large magnetocaloric effect ^[41]. Bizhanova et al. developed quinary Zr₃₁Ti₂₇Be₂₆Cu₁₀M₆ (M = Ag, Al, Ni, V, Cr, and Fe) and senary Zr₂₈Ti₂₄Be₂₃Cu₉Ni₁₀N₆ (N = V, Cr, Fe, Ag, and Al) alloys with critical diameters of 6–15 mm ^[42]. Inoue et al. found that Fe₄₃Cr₁₆Mo₁₆C₁₅B₁₀ HE-BMG and Zr–Al–(TM1, TM2) pseudo-HE-BMG can confer useful heat resistance at elevated temperatures ^[43]. Wada et al. developed septenary Zr–Hf–Ti–Al–Co–Ni–Cu high-entropy bulk metallic glasses with centimeter-scale glass-forming ability ^[44]. Panahi et al. studied the glass forming range of (FeCoCrNi)–(B,Si) HEAAs, the crystallization process, and the influence of Si element on the microstructure was elucidated ^[45]. Szyba et al. studied structural and electrochemical properties of resorbable Ca₃₂Mg₁₂Zn₃₈Yb_18–xB_x (x = 1, 2, 3) metallic glasses in Ringer’s solution; it was found that the HEAA had significantly higher corrosion resistance than CaMgZn alloys ^[46]. Law et al. compared the magnetocaloric properties of amorphous and crystalline HEAs; it was found that the magneto-entropy change of HEAAs was generally larger than its crystalline counterpart, while the transition temperature was relatively lower ^[47]. Calin et al. found that Ti–Zr–Nb–Hf–Si HEAAs exhibit excellent corrosion properties in simulated body fluids. Moreover, its weak paramagnetic nature and superior radiopacity offer compatibility with medical diagnostic imaging systems ^[48]. Jalali et al. studied the thermal and deformation behavior of Zr₃₃Hf₈Ti₆Cu₃₂Ni₁₀Co₅Al₆ HE-BMG; the correlation between fragility, structural relaxation enthalpy, diffusion, free volume and deformation behavior was discussed compared with the Cu–Zr–Al prototype BMG ^[49]^[50]. Jia et al. created a nanosponge-like architecture from PdPtCuNiP HEAA; it possesses outstanding hydrogen evolution reaction activity ^[51]. Makarov et al. studied temperature dependencies of enthalpy change in the initial (as-quenched) and relaxed (aged) HE-BMGs; the calculated results agreed with interstitialcy theory ^[52]. Alvi et al. reported that a thin film of HfMoNbTaTiVWZr HEAA showed thermal stability up to 750 °C, and it can resist Ar-ion irradiation ^[53].

2. Composition Design of HEAAs

2.1. Designing HEAA Based on Quinary Bulk Metallic Glasses

It is well known that the key point for preparing amorphous alloys is avoiding crystallization of high-temperature alloy melt during the cooling process. When an amorphous alloy could be obtained at a low cooling rate, or the critical size for obtaining an amorphous metallic sample is large, the alloy is recognized as possessing good or large glass-forming ability (GFA). Among traditional amorphous alloys, Zr_41.2Ti_13.8Cu_12.5Ni₁₀Be_22.5 (Vit1) ^[4] and Ti_32.8Zr_30.2Ni_5.3Cu₉Be_22.7 ^[15] quinary bulk amorphous alloys possess good GFA and a critical diameter over 50 mm. It implies that the five elements, Ti, Zr, Cu, Ni, and Be, are structural and chemically compatible to form bulk metallic glasses. So it is reasonable to suppose that the Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ high entropy alloy may possess good glass-forming ability and a big glassy sample might be made.

Figure 1 shows the composition design approach of the Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ HEAA. An equal-atomic Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ high entropy alloy was designed from quinary BMGs with good GFA. The Ø3 mm Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ rod sample was prepared by the copper mold casting technique. Its XRD spectra was shown in Figure 2a. No sharp diffraction peak corresponding to the crystalline phase was observed in the Ø3 mm Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ sample, indicating that this alloy possesses a fully amorphous structure. However, the critical diameter of the Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ BMG sample is only 3 mm, much smaller than that of Zr_41.2Ti_13.8Cu_12.5Ni₁₀Be_22.5 (Vit1) and Ti_32.8Zr_30.2Ni_5.3Cu₉Be_22.7 BMGs. The glass transition temperature (T_g), initial crystallization temperature (T_x), melting temperature (T_m), and liquidus temperature (T_l) are marked with arrows in Figure 3. T_g, T_x, T_m, and T_l are measured to be 683 K, 729 K, 1076 K, and 1161 K, respectively. This high-entropy BMG possesses a high compressive fracture strength of 2315 MPa for Ø3 mm × 6 mm sample, higher than that of Vit1 alloy, which is attributed to high entropy effect as well as high Ni content (Figure 4) ^[35]. In a uniaxial compressive experiment, it breaks in a brittle manner without plasticity. The present result provides a successful example of HEAA composition design by selecting five elements from quinary BMG with good GFA, despite the fact that the GFA of the designed high-entropy BMG is not large enough. Then, further study for improving the GFA of the high-entropy amorphous alloys is important and necessary.

Figure 1. Composition design approach for Ti–(Zr, Hf, Nb)–Cu–Ni–Be HEAAs.

Figure 2. XRD patterns of Ø3 mm Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ rod sample (a) as-cast, (b) annealed.

Figure 3. DSC curve of Ø3 mm Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ sample. Inset shows melting behavior.

Figure 4. Stress–strain curve of Ø3 mm × 6 mm Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ sample. Inset shows fracture morphology after compression.

2.2. Designing HEAAs by Similar Element Substitution/Addition

Similar element substitution/addition was proved to be an effective composition design method in traditional bulk metallic glasses ^[12]^[13], so it is reasonable to suppose that it may still work in HEAA. Hf and Zr are members of the same group in the periodic table of elements; they also possess similar atomic radii and chemical properties. Then Hf was used to replace the Zr element in Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ HE-BMG. Therefore, a Ti₂₀Hf₂₀Cu₂₀Ni₂₀Be₂₀ alloy was designed. It possesses an amorphous structure and its critical diameter is 2 mm, as shown in Figure 5 ^[54]. Moreover, Nb and Zr are also very close in the periodic table of elements, so Hf and Nb were added to the Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ HE-BMG as a sixth alloying element, respectively. Accordingly, Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 with a critical diameter of 1.5 mm (Figure 5) ^[54] and Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 with a critical diameter of 15 mm (Figure 6a,b) ^[36] were designed and developed. Surprisingly, the Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 senary HE-BMG possesses a critical size 10 times that of Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 HE-BMG, and it refreshes our cognition about GFA in an equal-atomic high entropy alloy system. Before this alloy, the largest HE-BMG with an equal-atomic concentration is the Pd₂₀Pt₂₀Cu₂₀Ni₂₀P₂₀ alloy, and its critical diameter is 10 mm by fluxing method ^[33]. The composition design approach for the Ti₂₀Hf₂₀Cu₂₀Ni₂₀Be₂₀ alloy, Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 alloy and Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 alloy is also demonstrated in Figure 1.

Figure 5. XRD patterns of Ø2 mm Ti₂₀Hf₂₀Cu₂₀Ni₂₀Be₂₀ and Ø1.5 mm Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 sample.

Figure 6. (a) XRD spectra of the Ø12 mm, Ø15 mm and Ø20 mm rod samples of Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 alloy. (b) The HRTEM image of the Ø15 mm glassy rod (inset: SAED pattern). (c) The DSC curve and (d) stress–strain curve of a Ø3 mm × 6 mm glassy sample (inset: SEM image).

For Ti₂₀Hf₂₀Cu₂₀Ni₂₀Be₂₀ alloy, T_g, T_x, T_m, and T_l are measured to be 717 K, 760 K, 1095 K, and 1220 K, respectively (Figure 7). Its compressive fracture strength is 2425 MPa for Ø2 mm × 4 mm sample, and it also breaks without plasticity (Figure 8) ^[54]. For Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 alloy, T_g, T_x, T_m, and T_l are measured to be 684 K, 739 K, 1066 K, and 1218 K, respectively (Figure 7). Its yield strength, fracture strength, and plasticity are 2330 MPa, 2450 MPa, and 0.5% for the Ø1.5 mm × 3 mm sample, respectively (Figure 8) ^[54]. For the Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 alloy, T_g, T_x, T_m, and T_l are measured to be 681 K, 751 K, 1019 K, and 1100 K, respectively (Figure 6c). Its yield strength, fracture strength, and plasticity are 1943 MPa, 2064 MPa, and 0.6% for the Ø3 mm × 6 mm sample, respectively (Figure 6d) ^[36]. These alloys possess high thermal stability and high strength; the relationship between the high entropy effect and properties will be discussed later.

Figure 7. DSC curves of Ø2 mm Ti₂₀Hf₂₀Cu₂₀Ni₂₀Be₂₀ and Ø1.5 mm Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 sample.

Figure 8. Stress–strain curves of Ø2 mm × 4 mm Ti₂₀Hf₂₀Cu₂₀Ni₂₀Be₂₀ and Ø1.5 mm × 3 mm Ti_16.7Zr_16.7Nb_16.7Cu_16.7Ni_16.7Be_16.7 sample.

The fracture surface morphology of Ti₂₀Zr₂₀Cu₂₀Ni₂₀Be₂₀ was shown as an inset in Figure 4. The nanowave structure is observed on the fracture surface. This is consistent with its brittle failure feature. In contrast, a typical vein pattern has been observed for the Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 alloy (inset in Figure 6d); it also coincides with its plastic deformation behavior. The fracture surface morphology is in agreement with compression experiment results ^[35]^[36].

Stimulated by the Ti_16.7Zr_16.7Hf_16.7Cu_16.7Ni_16.7Be_16.7 alloy with good GFA (critical diameter reaches 15 mm), the Ti–Zr–Hf–Cu–Ni–Be alloys with varied Cu/Ni ratio have been studied since Cu and Ni are also very close in the periodic table of elements, and the atomic radius difference is very small. Experimental results show that a series of Ti₂₀Zr₂₀Hf₂₀Be₂₀(Cu(Cu_20–_xNi_x) (x = 0, 2.5, 5, 7.5, 10, 12.5, 15, 17.5, 20) HE-BMGs with critical diameters of 12–30 mm were designed and developed (Figure 9) ^[37]^[38].

Figure 9. XRD patterns of Ti₂₀Zr₂₀Hf₂₀Be₂₀(Cu_20–_xNi_x) (x = 0, 2.5, 5, 7.5, 10, 12.5, 15, 17.5, 20) HE-BMGs.

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Hongyu Ding

Qi Zhang

Kefu Yao

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