JOM, Vol. 67, No.

10, 2015
DOI: 10.1007/s11837-015-1563-9
Ó 2015 The Minerals, Metals & Materials Society

Fracture Toughness and Fatigue Crack Growth Behavior

of As-Cast High-Entropy Alloys

MOHSEN SEIFI ,1,4 DONGYUE LI,2 ZHANG YONG,2 PETER K. LIAW,3

and JOHN J. LEWANDOWSKI1

1.—Department of Materials Science and Engineering, Case Western Reserve University, Clev-
eland, OH, USA. 2.—State Key Laboratory for Advanced Metals and Materials, University of
Science and Technology, Beijing, People’s Republic of China. 3.—Department of Materials Science
and Engineering, The University of Tennessee, Knoxville, TN, USA. 4.—e-mail: mohsen.seifi@
case.edu

The fracture toughness and fatigue crack growth behavior of two as-vacuum arc
cast high-entropy alloys (HEAs) (Al0.2CrFeNiTi0.2 and AlCrFeNi2Cu) were
determined. A microstructure examination of both HEA alloys revealed a two-
phase structure consisting of body-centered cubic (bcc) and face-centered cubic
(fcc) phases. The notched and fatigue precracked toughness values were in the
range of those reported in the literature for two-phase alloys but significantly less
than recent reports on a single phase fcc-HEA that was deformation processed.
Fatigue crack growth experiments revealed high fatigue thresholds that de-
creased significantly with an increase in load ratio, while Paris law slopes exhib-
ited metallic-like behavior at low R with significant increases at high R. Fracture
surface examinations revealed combinations of brittle and ductile/dimpled regions
at overload, with some evidence of fatigue striations in the Paris law regime.

In that regard, recent work14 has documented the

INTRODUCTION
High-entropy alloys (HEAs) are a relatively new
class of materials that typically combine five principal
elements or more and are known to exhibit a number
of unique combinations of flow and fracture behavior.
Their combination of high-temperature strength, high
tensile strength, and increased wear resistance have
generated interest in their possible use for a wide
range of functional and structural applications.1–5
Additionally, a recent review has also revealed excel-
lent corrosion resistance in some HEA systems.6
Various processing techniques have been used to
manufacture these alloys, including mechanical
alloying, arc melting, and magnetic levitation, while
various additive manufacturing techniques are also
being explored.7–9 While initial evaluations of
mechanical performance have focused on compres-
sion, tension, and hardness, a more complete assess-
ment of their potential for structural applications
requires the documentation of their damage tolerance
and fatigue behavior. Some preliminary information
is available for fatigue properties,10 but none exists for
fatigue-crack-growth behavior, and only limited
reports on fracture toughness of HEAs exist.11–13
microstructure and high compression strength of
AlxCrFeNiTi0.25 alloys, with fracture strengths
exceeding 1800 MPa and yield strengths in excess of
1300 MPa.14 In particular, when x = 0.5 in AlxCrFe-
NiTi0.25, the fracture strength and plastic strain at
failure achieved their maximum values of 3474 MPa
and 40%, respectively.14 Other work by Stephanov
et al.15 on AlxNbTiVZr revealed yield strength varia-
tions between 960 MPa and 1330 MPa with changes
in Al concentration from x = 0 to x = 1.5. The present
work was conducted to determine the fracture tough-
ness and fatigue-crack-growth behavior of Al0.2CrFe-
NiTi0.2 and AlCrFeNi2Cu alloys to provide a more
complete characterization of microstructure/property
relationships in these particular HEA materials.
MATERIALS AND METHODS
Two high-entropy alloys with nominal composition
of AlxCrFeNiTi0.2 (x molar ratio, x = 0.2) and AlxCr-
FeNi2Cu (x = 1) were manufactured by a magnetic
vacuum levitation melting (VLM) (Fig. 1), using pure
elements with a purity higher than 99.6%, followed
by drop casting into a cylindrical mold. Bend bar
samples were then machined into dimensions of

2288 (Published online August 26, 2015)

Fracture Toughness and Fatigue Crack Growth Behavior of As-Cast High-Entropy Alloys
3 mm 9 5 mm 9 47 mm. The as-cast microstruc-
tures were characterized using x-ray diffraction
(XRD) as well as scanning electron microscopy (SEM)
equipped with an energy-dispersive (EDX) x-ray
spectrometer. The hardness was measured by a
Melting metal Water-cooling
crucible
Induction coil
Fig. 1. Schematic of VLM process.
Fig. 2. X-ray diffraction patterns of Al0.2CrFeNiTi0.2 and AlCrFeNi2
Cu HEAs.
Fig. 3. SEM images of (a) Al0.2CrFeNiTi0.2 and (b) AlCrFeNi2Cu showing dendritic and interdendritic structures.
2289
HXD-1000TM Vickers microhardness tester with a
load of 500 g and a dwell time of 15 s. Fracture
toughness was determined in three-point bending
using single-edge notch (SEN) samples tested on a
Model 810 MTS servohydraulic machine in general
accordance with ASTM E399 standard.16 The speci-
mens were first notched using a slow-speed diamond
wire saw to introduce notch root radius of about 75–
100 lm and then fatigue precracked to a crack depth/
sample width (i.e., a/W) of 0.45–0.55 in accordance
with the standard. The notched toughness tests using
this same notch radius placed to a/W = 0.5 were also
tested. All toughness tests were conducted to failure
at a displacement rate of 0.25 mm/min.
Fatigue crack growth tests were performed at a
cyclic frequency of 20 Hz in room temperature air
with relative humidity of 40% in accordance with
ASTM E647 standard (Ref. 17) in the LT orientation.
A direct current potential drop technique was used to
monitor and control crack growth. Fracture Tech-
nology Associates (FTATM) software was used to
monitor crack growth continuously in both the fati-
gue and fracture toughness tests in order to also
comply with existing ASTM requirements. In all
cases, 1 A current input was used with voltage drop
amplified by 10 K gain. Fatigue crack growth tests at
load ratios R = 0.1, 0.3, and 0.7 were started at a low
stress intensity range DK, using constant cyclic
loading to produce rising DK conditions until catas-
trophic fracture. The Paris law slope and fatigue
overload Kc was calculated for multiple tests con-
ducted in this manner.
SEM of fractured samples was conducted on a FEI
Quanta 200 three-dimensional microscope (FEI
Company, Hillsboro, OR) utilizing secondary elec-
tron imaging (SE) operated at 20 keV.
RESULTS
Microstructures
The XRD patterns obtained for Al0.2CrFeNiTi0.2
and AlCrFeNi2Cu alloys in the as-cast condition
shown in Fig. 2 revealed a multiphase material, in
2290 Seifi, Li, Yong, Liaw, and Lewandowski

contrast to some HEAs.2,3,10–14 The two main phases and Ti. In contrast, the matrix in AlCrFeNi2Cu is
identified possess face-centered-cubic (fcc) and body- enriched in Al, Ni, and Cu, whereas particles are
centered-cubic (bcc) structures. There are minor enriched in Fe and Cr.
unidentified peaks at small angles and the structure Vickers microhardness results for both alloys are
corresponding to those peaks are being determined shown in Fig. 4 with Al0.2CrFeNiTi0.2 exhibiting a
by a TEM study as part of future work. hardness of 510 ± 7.7 and AlCrFeNi2Cu with
The SEM micrographs of the as-cast Al0.2CrFe- 320.9 ± 7.8.
NiTi0.2, and AlCrFeNi2Cu alloys shown in Fig. 3a
and b, respectively, reveal a cast dendritic structure Mechanical Properties
with interdendritic regions that also possess some
Table II provides the fracture toughness and
microstructural features. The chemical composi-
Rockwell C hardness for the present alloys, whereas
tions of both regions were analyzed by EDX and
Fig. 5 summarizes the effects of changing test
shown in Table I. The matrix in Al0.2CrFeNiTi0.2 is
temperature and notch root radius on the tough-
enriched in Cr and Fe, whereas the particles and
ness. Both alloys exhibited load versus displace-
small, elongated precipitates are enriched in Al, Ni,
ment traces at room temperature in the toughness
tests and the AlCrFeNi2Cu exhibited a higher
toughness but lower strength than Al0.2CrFeNiTi0.2.
Table I. Chemical compositions (in wt.%) in the Toughness testing at 200°C induced more plasticity
AlCrFeNi2Cu and Al0.2CrFeNiTi0.2 (i.e., nonlinear load versus displacement trace) and
slightly improved the toughness (Fig. 5). Table II
Alloy Al Cr Fe Ni Ti Cu provides a comparison of the present data with the
AlCrFeNi2Cu data obtained on other HEAs11,13 and a high
Gray 19.67 1.82 8.12 52.04 – 18.34 toughness bulk metallic glass (BMG).18
White 7.87 15.66 22.46 38.63 – 15.38
Al0.2CrFeNiTi0.2
Gray 0.68 38.64 45.22 14.43 1.03 –
White 2.93 20.25 33.89 37.47 5.47 –

Fig. 5. Effect of changes in notch root radius and test temperature

Fig. 4. Vickers microhardness results. on the fracture toughness of HEA alloys.

Table II. Summary of fracture toughness results of current study and other recent works

Thickness, Span, Fracture pffiffiffiffiffi

Alloy B (mm) S (mm) toughness, Kq (MPa m) Rockwell C
(HEA)
AlCrFeNi2Cu 3 20 40, 41, 42, 45 36 ± 1
AlCrFeNi2Cu(HEA)a 3 20 46, 47 NA
Al0.2CrFeNiTi(HEA)
0.2 3 20 32, 35 46 ± 1
FeCoNiCrCuTiMoAlSiB(HEA)
0.5 NA NA 51 (Ref. 13) NA
Al23Cr23Co15Cu8Fe15Ni(HEA)
15 3 24 5 (Ref. 11) NA
Zr61Ti2Cu25Al(BMG)
12 3 24 106 (Ref. 18) NA
a
Test was performed at 200°C.
Fracture Toughness and Fatigue Crack Growth Behavior of As-Cast High-Entropy Alloys 2291

Table III. Summary of fatigue crack growth results at different load ratios for data shown in Fig. 6

Fatigue overload
pffiffiffiffiffi Paris Threshold
pffiffiffiffiffi
Alloy R (load ratio) Kc (MPa m) slope (m) (MPa m)
AlCrFeNi2Cu 0.1 56 3.4 17
AlCrFeNi2Cu 0.3 36 6.5 5
AlCrFeNi2Cu 0.7 32 14.5 7
Al0.2CrFeNiTi0.2 0.1 30 4.9 16
Al0.2CrFeNiTi0.2 0.3 23 5.3 7
Al0.2CrFeNiTi0.2 0.7 21 25.8 5

Table III summarizes the fatigue-crack-growth

results and includes DKth, Paris law slope and Kmax
at failure at various load ratios (i.e., R = 0.1, 0.3 and
0.7). Both alloys showed a load ratio effect on DKth,
whereby increases in R shifted the whole fatigue
crack growth curve to the left as shown in Fig. 6.
These increases in R produced significant reduc-
tions in DKth and increases in Paris law slope,
somewhat similar to a recent report on an as-cast c-
TiAl,19 but much greater than what was reported in
as-deposited Ti-6Al-4V (Ref. 20) prepared by elec-
tron beam processing.
Both visual and SEM analyses of fracture sur-
faces revealed macroscopically (and microscopically)
rough surfaces for both HEAs. The high magnifica-
tion image in Fig. 7a illustrates fatigue striations on
the fracture surface of the tougher AlCrFeNi2Cu
alloy in the Paris law regime, while isolated ductile/
dimple-like features are evident in the overload
region, as shown in Fig. 7b, interspersed with more
brittle regions as shown in Fig. 7c and d. Figure 7c
and d illustrate the large-scale roughness of the
fracture surface in addition to revealing the combi-
nation of ductile features as well as faceted brittle
regions that appear in the overload region of this
tougher HEA, in comparison to the stronger and
more brittle Al0.2CrFeNiTi0.2 shown in Fig. 6.
The less tough Al0.2CrFeNiTi0.2 exhibited fewer
ductile regions in the overload region and larger-
scale brittle features in both the fatigue and over-
load region as shown in Figs. 8 and 9. Some ductile/
dimple-like features are evident in Fig. 8d, but
these were relatively few in extent and small in size,
with a typical size of only 3–5 lm. Fracture tough-
ness experiments on this more brittle material
similarly revealed a fracture surface dominated by
large-scale brittle features (Fig. 9), with isolated
ductile features. Fig. 6. Fatigue crack growth behavior of (a) AlCrFeNi2Cu and (b)
Al0.2CrFeNiTi0.2.
DISCUSSION
While many of the HEA systems recently
reviewed2 and experimentally evaluated12 have a Al0.2CrFeNiTi0.2 and AlCrFeNi2Cu presently tested
single phase, there are a number of examples of exhibit a combination of bcc and fcc regions that
multiphase HEA systems.2 These may possess very produce levels of strength/toughness that approach/
different combinations of properties, depending on exceed the HEA systems listed in Table II but are
the crystal structure of the phases as well as their far below that of a deformation-processed single fcc
size, volume fraction, and distribution. The present phase HEA that exhibits very high toughness12
work illustrates that the as-cast microstructures in along with fracture surface features that are 100%
2292
Fig. 7. SEM images of AlCrFeNi2Cu HEA alloy tested in fatigue: (a) fatigue striation features, (b) ductile/dimple-like features, and (c and d) brittle
and ductile/dimple features.
ductile/dimpled fracture. An examination of the
present fracture surfaces reveals combinations of
brittle and ductile/dimpled features that roughly
correspond to the size and volume fraction of the
bcc and fcc microstructural constituents, respec-
tively. At room temperature, both materials exhibit
linear load versus displacement traces in the
toughness tests in addition to the brittle fracture of
the bcc constituent. Increasing the test tempera-
ture to 200°C increases the toughness, while pro-
ducing a nonlinear load versus displacement trace
although the fracture surface features appeared
similar to those of the room-temperature tests in
that there appeared to be similar combinations of
ductile/dimpled and brittle fracture. This is not
uncommon in either single-phase bcc metals (e.g.,
Nb),21,22 ferritic steels,23 or ductile-phase tough-
ened composites containing a combination of bcc
Seifi, Li, Yong, Liaw, and Lewandowski
and non-bcc phases.24 In those cases, changes to
the load versus displacement traces and toughness
were obtained along with significant changes to the
fracture surface details due to the additional
plasticity required to reach stresses sufficient to
trigger brittle (i.e. cleavage) fracture in the bcc
metal/alloy21–23 or composite24 containing a bcc
phase. Future work will examine the effects of
testing at higher temperatures in order to induce a
brittle-to-ductile transition in the bcc constituent
in order to determine its effect on toughness of
these two-phase HEA alloys. The effects of chang-
ing the notch root radius on toughness are similar
to that exhibited by many crystalline metallic
systems, unlike that exhibited in some bulk
metallic glasses25 where relatively minor changes
in the notch root radius produce extreme increases
in the load-carrying capability.
Fracture Toughness and Fatigue Crack Growth Behavior of As-Cast High-Entropy Alloys
Fig. 8. SEM images of Al0.2CrFeNiTi0.2 tested in fatigue: (a) brittle features, (b and c) higher magnification of faceted regions, and (d) isolated
ductile/dimple-like features.
The preliminary fatigue-crack growth rate data
obtained on the Al0.2CrFeNiTi0.2 and AlCrFeNi2Cu
presently tested exhibit characteristics that are
similar to that exhibited by some metallic alloys,26,27
intermetallics,19 and metal matrix composite sys-
tems,28,29 where metallic-like Paris slopes at low R
(e.g., 3–5) significantly increase (e.g., to>10) with an
increase in R. In those systems,19,26–29 the increase in
Paris slope with increasing R coincided with an
increase in static modes of brittle failure (e.g., inter-
granular or cleavage failure) in the Paris regime,
thereby increasing the rate of crack growth in that
regime and elevating the Paris law slope. The com-
binations of brittle and ductile/dimpled features
present on the fracture surfaces of the presently
tested materials suggest that a similar mechanism
may contribute to the significantly higher fatigue-
crack growth rates and higher Paris law slopes
2293
obtained at higher R. Future work will examine the
influence of changing the test temperature in order to
induce more ductile behavior of the bcc constituent,
as test temperature should have a significant effect
on the fatigue-crack growth rate (and Paris law
slope). Despite the predominance of brittle fracture in
the fatigue regime, isolated areas of fatigue striations
(cf. Fig. 7a) were observed, indicating that some
regions of the fatigue-fracture surface did fail in a
locally ductile (i.e., striation-controlled) manner.
The fatigue threshold similarly revealed a rela-
tively large effect of changes in the load ratio R with
relatively high fatigue thresholds at low R and sig-
nificant reductions in thresholds with increasing R.
This trend likely results from the large surface
roughness producing significant levels of fatigue-
crack closure at low values of R, as shown in many
other works.
2294 Seifi, Li, Yong, Liaw, and Lewandowski

Fig. 9. SEM images of AlCrFeNi2Cu after toughness test (a and b) reveals brittle features and some isolated ductile regions.

Whereas the present work was conducted on as- exhibited high fatigue thresholds that decreased
cast materials, future work should also focus on significantly with an increase in R, while Paris
deformation-processed versions of these (and other) law slopes exhibited metallic-like values (e.g.,
HEA materials. Deformation processing is known to 3–5) at low R with significant increases at high
produce significant effects on the mechanical R. Fracture-surface examinations revealed com-
behavior of cast composite systems, whether the binations of brittle and ductile/dimpled regions
matrix is metallic30 or intermetallic31 due to various in the overload region, with limited observations
beneficial microstructural changes that are pro- of fatigue striations in the Paris law regime.
duced in the system under investigation.
ACKNOWLEDGEMENTS
CONCLUSION
This work was partially supported by the Arthur
P. Armington Professorship (J.J.L.), while mechan-
ical characterization was performed in the Ad-
1. Al0.2CrFeNiTi0.2 and AlCrFeNi2Cu HEA alloys
vanced Manufacturing and Mechanical Reliability
produced via arc casting exhibited a combina-
Center (AMMRC) at CWRU. ZY would like to thank
tion of bcc and fcc phases.
the financial support of the National Science Foun-
2. The notched and fatigue precracked toughness
dation of China (Nos. 51471025 and 51210105006),
values of these two-phase as-cast HEA alloys
111 Project (B07003), and the Program for Chang-
were in the range of those reported in the
jiang Scholars and the Innovative Research Team of
literature, although significantly less than those
the University. PKL would like to acknowledge the
reported for a deformation-processed single fcc
support of the Department of Energy (DOE), Office
phase HEA.
of Fossil Energy, National Energy Technology Lab-
3. Fracture-surface examinations of the toughness
oratory (DE-FE-0008855, DE-FE-0024054, and DE-
tests revealed a combination of ductile/dimpled
FE-0011194), the Army Research Office (W911NF-
and brittle features that roughly corresponded
13-1-0438), and the National Science Foundation
to the fcc and bcc phases, respectively, in both
(CMMI-1100080) with the program managers, Mr.
HEA alloys presently tested. While both systems
V. Cedro, Mr. R. Dunst, Dr. J. Mullen, Dr. D.M.
exhibited linear load versus displacement traces
Stepp, and Dr. C. Cooper.
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