Intermetallics 39 (2013) 74e78

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Intermetallics
journal homepage: www.elsevier.com/locate/intermet

Tensile properties of high- and medium-entropy alloys

A. Gali a, b, E.P. George a, b, *
a
Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA
b
Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996, USA

a r t i c l e i n f o a b s t r a c t

Article history: Equiatomic, face-centered-cubic, high- and medium-entropy alloys were arc melted, hot-rolled to pro-
Received 11 March 2013 duce recrystallized sheets, and tensile tested. The alloys having the compositions CrMnFeCoNi and
Accepted 25 March 2013 CrFeCoNi exhibited a strong temperature-dependent decrease in strength with increasing temperature
Available online 18 April 2013
from
196  C to 1000  C, and a relatively weak strain-rate dependence (at 10
3 and 10
1 s
1). Ductility
did not vary inversely with yield strength; rather, when strength doubled as the test temperature was
Keywords:
decreased from room temperature to
196  C, elongation to fracture increased by a factor of 1.5 to >60%.
B. Yield stress
A high degree of work hardening, possibly due to deformation-induced nanotwinning, postpones the
B. Solid-solution hardening
B. Brittleness and ductility
onset of necking and may be the reason for the ductility increase.
B. Work-hardening 2013 Elsevier Ltd. All rights reserved.
D. Microstructure
F. Mechanical testing

1. Introduction While the above concepts can, in principle, explain why some multi-
element alloys are single-phase solid solutions [2,13,14,16,17,19,20],
Recently, there has been considerable interest in multi-element, most of the so-called high-entropy alloys reported in the literature
equiatomic alloys and their derivatives e.g.[1e20], that are often contain multiple phases [e.g.,4-12,15]. The reason for this is that
referred to in the literature as high-entropy alloys. In ideal solid congurational entropy cannot usually overcome the other driving
solutions, the congurational entropy, DSconf
RSniln(ni), where forces of phase stability, such as enthalpy and non-congurational
ni is the atomic fraction of the ith element and R is the gas constant, entropy, which often have stronger inuences [19]. Additionally, in
increases with the number of alloying elements. It has been hy- alloys consisting of multiple phases, the congurational entropy is
pothesized that, when the number of alloying elements increases actually lower than that implied by the equation above for a single-
beyond ve, the contribution of congurational entropy to the total phase ideal solid solution [19]. Therefore, to study the mechanical
free energy becomes signicant enough that it can overcome the properties of high-entropy alloys, it is important that truly single-phase
enthalpies of compound formation and phase separation, thereby solid solution alloys be investigated.
stabilizing the solid solution state relative to multi-phase micro- Here we investigate the equiatomic, FCC-structured quinary alloy
structures [1]. Based on this logic, a high-entropy alloy was dened (CrMnFeCoNi), rst reported by Cantor et al. [2] and later conrmed to
as one with at least ve major elements whose individual atomic consist of a single solid-solution phase [19,20]. For comparison with
concentrations are between 5 and 35% [1,7]. Alloys based on one this high-entropy alloy, we investigated a medium-entropy quater-
principal metallic element were classied as low-entropy alloys nary alloy (CrFeCoNi) that is comprised of the same elements as the
and those comprised of two to four principal elements as medium- Cantor alloy minus the Mn; this quaternary alloy is also single-phase
entropy alloys [7]. In all such multi-element alloys, the congura- FCC [17]. The tensile properties of neither of these alloys have so far
tional entropy is obviously maximized when the alloying elements been published. We report here our initial ndings on the micro-
are present in equal atomic concentrations [1]; consequently, much structure and tensile behavior of these alloys, which were produced
of the high-entropy alloy research has tended to focus on alloys by arc melting, drop casting and hot rolling, as described below.
consisting of multiple principal elements in roughly equal
proportions. 2. Materials and methods

* Corresponding author. Materials Science and Technology Division, Oak Ridge

Starting from the pure (>99.9% purity) constituent elements in
National Laboratory, Oak Ridge, TN 37831, USA. Tel.: 1 865 574 5085. bulk form, two alloys having the equiatomic compositions
E-mail address: georgeep@ornl.gov (E.P. George). CrMnFeCoNi (HE-1) and CrFeCoNi (HE-4) were produced by arc

0966-9795/$ e see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.intermet.2013.03.018
 A. Gali, E.P. George / Intermetallics 39 (2013) 74e78 75

melting under argon atmosphere. The arc-melted buttons were patterns in a Scintag diffractometer and (b) determine their melting
ipped and remelted ve times to promote thorough mixing and to points in a NETZSCH 404 C differential scanning calorimeter.
allow the regions in contact with the water-cooled copper hearth to From the rolled sheets, dog-bone shaped specimens with gage
become fully incorporated in the melt. After the fth remelt, the sections of 10 mm  2.5 mm  0.63 mm were cut by EDM with their
arc-melted buttons were drop cast into a rectangular copper mold long axes parallel to the rolling direction. They were subsequently
measuring 127 mm  25.4 mm  12.7 mm. Weight losses after ground through 1200 grit SiC paper, and stress relieved at 900  C
melting and casting were w1% and <0.1% for the HE-1 and HE-4 for 1 h in vacuum. Tensile tests were performed on a screw-driven
alloys, respectively. Since there was negligible weight loss in the Instron machine at engineering strain rates of approximately 10
3
alloy without Mn, it was assumed that the entire weight loss in HE- and 10
1 s
1 at temperatures from
196  C to 1000  C. The cryo-
1 was due to evaporation of Mn (consistent with its much higher genic tests were performed with the specimens completely
vapor pressure). To compensate for this weight loss, we added an immersed in liquid nitrogen; tests at room temperature and higher
extra gram of Mn per 100 g of raw materials. were performed in vacuum. Prior to testing, seven, roughly equally
The drop-cast bars exhibited dendritic segregation; therefore, spaced Vickers indents were made on the gage sections using a
they were rst annealed at 1000  C for 24 h in vacuum to ho- micro-hardness tester and a 300-g load. The distance between
mogenize their compositions. After homogenization, the alloys adjacent indents was measured before and after the tensile tests
were clad with stainless steel sheet and hot rolled to break down and averaged for each specimen to get the uniform elongation to
their cast structures and obtain a recrystallized microstructure. The fracture (the two indents on either side of the fracture plane were
purpose of the cladding was to minimize heat loss to the unheated excluded from the measurements). Occasionally, all the indents
rolls during the rolling operation. Before the rst rolling pass, the could not be located after testing; in those cases, the total change in
clad bars were pre-heated at 1000  C for 1 h; between all subse- specimen length divided by the gage length was used as a measure
quent passes, reheating to 1000  C was done for w15 min. For the of ductility (implicitly assuming that all the deformation occurred
rst ve rolling passes, a 10% reduction in thickness per pass was in the gage section). Fracture surfaces of the tensile tested speci-
used; after that, a 20% reduction in thickness per pass was used for mens were examined either in an XL30 or Hitachi S4800 FEG
all subsequent passes until a nal sheet thickness of w1 mm was scanning electron microscope.
reached. Therefore, starting from the initial thickness of the drop-
cast bar (12.7 mm), the total reduction in thickness after rolling 3. Results and discussion
was w92%.
To evaluate the microstructures of the alloys, transverse sections Backscattered electron images of the cast and homogenized
were cut by electric discharge machining (EDM) from the homog- microstructures are shown in Fig. 1 (a) and (b). Both alloys are
enized bars and hot-rolled sheets. The sections were mounted in essentially single-phase; however, HE-1 contains isolated dark
epoxy, ground through 600 grit SiC paper, and polished using particles that are not present in the HE-4 alloy. Energy dispersive X-
Vibromet machines, rst with 0.3 mm Al2O3 and then in a suspen- ray spectroscopy was performed on these particles. Oxygen, chro-
sion of colloidal silica having a particle size of 60 nm. The polished mium and manganese peaks were detected, which leads to the
samples were examined in an XL30 FEG scanning electron micro- conclusion that the particles are oxides. Since they were absent in
scope (SEM) in the backscattered electron mode. Specimens from the Mn-free HE-4 alloy, the oxygen contamination is likely associ-
the homogenized bars were also used to (a) obtain x-ray diffraction ated with the Mn, but whether it was introduced through the raw

Fig. 1. Backscattered electron images of (a) CrMnFeCoNi (HE-1), (b) CrFeCoNi (HE-4) after casting and homogenization, and (c) CrMnFeCoNi (HE-1), (d) CrFeCoNi (HE-4) after hot
rolling.
76 A. Gali, E.P. George / Intermetallics 39 (2013) 74e78

materials or during one of the subsequent processing steps is not similar behavior over the ranges investigated: strong temperature
known. Regardless, because of their tiny volume fraction, they did dependence and weak strain-rate dependence. The temperature
not signicantly inuence mechanical properties as shown below. dependence is strongest at low and high temperatures with a
X-ray diffraction patterns were obtained from the two alloys in smaller slope in between. Both alloys exhibit somewhat higher
the homogenized condition. All the peaks could be indexed as FCC. strengths at the higher strain rate, especially at temperatures below
There were no peaks corresponding to the oxide particles in HE-1, w600  C. At intermediate temperatures, the slope is less steep at
consistent with their low volume fraction. The melting point the slower strain rate, but in neither case does yielding appear to be
ranges, as determined by differential scanning calorimetry, were truly athermal, although additional experiments at intermediate
determined to be 1280e1349  C and 1422e1462  C, for the HE-1 temperatures are warranted to obtain better statistics. The larger
and HE-4 alloys, respectively, indicating that the addition of Mn grain size of HE-1 relative to HE-4 (35 vs. 14 mm) appears not to
to the quaternary depresses the melting point and increases the have a signicant effect.
gap between the solidus and liquidus. The above temperature dependence of yield strength is not
Fig. 1 (c) and (d) show the microstructures of the two alloys after usually observed in pure FCC metals; however, it is known to occur
hot rolling. The microstructures are fully recrystallized indicating in binary solid-solution alloys [22e29]. In pure FCC metals, the
that dynamic recrystallization occurred during the hot rolling. athermal portion of the yield stress versus temperature curve is
Grain sizes of the roughly equiaxed grains were measured using the large compared to the thermal part, unlike in BCC metals where the
linear intercept method on a plane perpendicular to the rolling opposite is the case. Since the athermal region is where thermal
direction in the through-thickness (short-transverse) direction and activation can overcome barriers to dislocation motion, these bar-
found to be approximately 32 mm and 11 mm for the HE-1 and HE-4 riers are believed to be weak in pure FCC metals and easily over-
alloys, respectively. The larger grain size of the HE-1 alloy may be at come by thermal uctuations even at cryogenic temperatures.
least partly due to the higher homologous temperature (w0.81 Tm) Solute atoms can increase signicantly the thermal part of the yield
at which it was hot rolled compared to the HE-4 alloy (w0.75 Tm). stress, as seen in Fig. 2 for the quinary and quaternary alloys, and
Grain sizes were also measured after the rolled sheets were reported earlier for binary FCC alloys. Thus, solute atoms introduce
annealed for 1 h at temperatures of 600e1000  C. No change in obstacles to dislocation motion that are not as easily overcome by
grain size was observed up to 800  C; only at temperatures of thermal activation. However, the nature and strength of these ob-
900  C and higher was grain growth observed. These results are stacles may be different in relatively dilute binaries compared to
consistent with the notion that the alloys recrystallized during the the equiatomic quinary/quaternary alloys investigated here. In bi-
hot rolling operation. To relieve any residual stresses in the rolled nary FCC alloys, the transition between the thermal and athermal
sheets, they were annealed for 1 h at 900  C prior to tensile testing. regions often occurs at relatively low temperatures, e.g., at around
The grain sizes after this stress-relief heat treatment were room temperature in CueZn binaries [23], which implies barrier
approximately 35 and 14 mm for the HE-1 and HE-4 alloys, strengths on the order of kT at room temperature, namely, 0.025 eV.
respectively (slightly larger than in the as-rolled state, 32 and By contrast, the thermal regions in Fig. 2 extend to signicantly
11 mm). higher temperatures, implying the presence of relatively strong
Numerous annealing twins are visible in both alloys after obstacles in our HE-1 and HE-4 alloys. Some of this difference may
recrystallization [Fig. 1 (c) and (d)]. Since annealing twins are be due to the shorter distance between atoms of different kinds in
commonly found in recrystallized FCC metals and solid solution multi-element equiatomic alloys compared to more dilute solid
alloys with relatively low stacking fault energies [21], it is reason- solutions. That is, as dislocations move in the HE-1 and HE-4 alloys,
able to conclude that our HE-1 and HE-4 alloys have low stacking they encounter obstacles over lengths scales that are fractions of a
fault energies. unit cell in dimension (as opposed to distances of a few unit cells in
Fig. 2 (a) and (b) show the temperature dependencies of the 0.2% more dilute alloys). In addition, the disparate alloying elements in
offset yield strengths of HE-1 and HE-4 tensile tested at strain rates HE-1 and HE-4, although they are substitutional in nature, could
of 10
3 and 10
1 s
1, respectively. The two alloys show broadly possibly introduce tetragonal distortions that offer more resistance

Fig. 2. Temperature dependencies of the 0.2% offset yield strengths of the CrMnFeCoNi (HE-1) and CrFeCoNi (HE-4) alloys tensile tested at engineering strain rates of 10
3 s
1 (a),
and 10
1 s
1 (b).
 A. Gali, E.P. George / Intermetallics 39 (2013) 74e78 77

consistent with the decreasing work hardening rates with

increasing temperature seen on the stressestrain curves.
Fig. 4 (a) shows the tensile ductilities of HE-1 and HE-4 as a
function of temperature for an engineering strain rate of 10
3 s
1.
Surprisingly, ductility does not show an inverse dependence on
strength; rather, both strength [Fig. 2 (a) and (b)] and ductility
[Fig. 4(a)] increase with decreasing temperature. Between room
temperature and liquid nitrogen temperature, as the yield strength
doubles, the elongation to fracture increases by a factor of 1.5 (to
values in excess of 60%). As can be seen in the low-magnication
fractograph on the left [Fig. 4 (b)], the fracture surface of HE-4
tested at
196  C exhibits almost no necking (HE-1 showed
similar behavior). This, combined with the high work hardening
implicit in Fig. 3, suggests that the large elongations at cryogenic
temperatures are the result of the necking instability being post-
poned to higher strains. When fracture nally occurs, it is by
dimpled rupture (ductile transgranular) as shown in the higher
magnication fractograph on the left [Fig. 4 (c)]. At elevated tem-
peratures, the fracture mode is again dimpled rupture [Fig. 4 (d)]
but the fracture surface exhibits signicant necking [Fig. 4 (e)]. The
Fig. 3. Comparison of the temperature dependencies of the ultimate tensile strength
lower ductilities at elevated temperatures are likely the result of an
and yield strength for the two alloys and strain rates investigated in this study. The
circles represent the HE-1 alloy and the squares the HE-4 alloy; for each, the lled earlier onset of the necking instability, which in turn is related to
symbols are for 10
3 s
1 strain rate and the open symbols for 10
1 s
1. To rst order, the lower work hardening seen at elevated temperatures (Fig. 3).
the small variations between the two alloys and strain rates are ignored, so only one A possible reason for the high degree of work hardening at low
dashed curve is drawn (as a guide to the eye) through each data set. temperatures is deformation-induced twinning. Nanoscale twins
were recently observed in TEM specimens prepared from another
to dislocation motion [30]. Clearly, further investigations are batch of the HE-1 alloy tensile tested at
196  C to a strain of w20%
needed to understand the nature of these obstacles and how they [31]. While slip is the usual deformation mode in most FCC metals,
might be different in the binary and higher-order alloys. twinning can occur at low temperatures in low-stacking-fault-
Fig. 3 compares the ultimate tensile strengths of the two alloys energy metals and is sometimes associated with serrations on the
with their yield strengths. The dashed lines through the data points stressestrain curves [32]. For a given temperature and strain rate,
are merely visual aids; for the sake of simplicity, we have drawn the magnitude of the serrations depends on stacking-fault energy
only one line each through all of the yield and ultimate strengths [33]: the lower its value the smaller the serrations. In our alloys, the
(implicitly ignoring any differences between the two alloys and stressestrain curves did not exhibit any serrations at room tem-
strain rates). There is signicant work hardening at low tempera- perature or below. This could be because our specimens were
tures as evidenced by the large difference between the yield and polycrystalline (so twinning might occur in multiple grains simul-
ultimate strengths (this is clearly seen on the stressestrain curves taneously making load-drops harder to detect) or the stacking-fault
which are not shown here). While both the yield and ultimate energies of our alloys are low enough to make the serrations
strengths show strong temperature dependence, the latter de- disappear. Additional work is needed to distinguish between these
creases more rapidly with increasing temperature. This is two possibilities.

Fig. 4. (a) Temperature dependence of the tensile ductilities of CrMnFeCoNi (HE-1) and CrFeCoNi (HE-4) tested at an engineering strain rate of 10
3 s
1. Also shown are fractographs
of specimens tested at
196  C (b, c) and 400  C (d, e). The dashed outlines of the fracture surfaces show that there is less thickness reduction (necking) at
196  C (b) than at
400  C (e).
78 A. Gali, E.P. George / Intermetallics 39 (2013) 74e78

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