Powder Metallurgy

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High-entropy alloy CoCrFeMnNi produced by

powder metallurgy

Nadine Eißmann, Burghardt Klöden , Thomas Weißgärber & Bernd Kieback

To cite this article: Nadine Eißmann, Burghardt Klöden , Thomas Weißgärber & Bernd Kieback
(2017) High-entropy alloy CoCrFeMnNi produced by powder metallurgy, Powder Metallurgy, 60:3,
184-197, DOI: 10.1080/00325899.2017.1318480

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POWDER METALLURGY, 2017
VOL. 60, NO. 3, 184–197
https://doi.org/10.1080/00325899.2017.1318480

High-entropy alloy CoCrFeMnNi produced by powder metallurgy

Nadine Eißmanna, Burghardt Klöden b
, Thomas Weißgärberb and Bernd Kiebackb
a
Technische Universität Dresden, Faculty of Mechanical Science and Engineering, Institute of Materials Science Dresden, Germany;
b
Fraunhofer Institute for Manufacturing Technology and Advanced Materials IFAM, Branch Lab Dresden Dresden, Germany

ABSTRACT ARTICLE HISTORY

Lately high-entropy alloys (HEAs) have been the topic of extensive research, as these materials Received 8 December 2016
are promising candidates for many challenging applications, as for example tools, moulds and Accepted 7 April 2017
functional coatings. In contrast to conventional alloys, HEAs consist of five or more principal
KEYWORDS
elements, each having a concentration between 5 and 35 at.-%. Against expectations, HEAs High-entropy alloy; single
show a rather simple microstructure consisting preferentially of cubic phases. Due to this phase; powder metallurgy;
microstructure, HEAs show promising properties, e.g. in terms of high-temperature stability, pressureless sintering; spark
high strength and ductility. Within this research, a single-phase CoCrFeMnNi HEA was plasma sintering; gas
produced by powder metallurgy (PM). In contrast to conventional metallurgy, PM offers a lot atomisation; selective
of advantages, e.g. good material efficiency and high shape complexity. Gas atomised electron beam melting;
powder was used and selected PM methods are presented (e.g. pressureless sintering, spark dilatometry
plasma sintering, additive manufacturing (EBM)). The process methods were evaluated by
characterising the material properties (density, microstructure, mechanical properties) of the
compacted and sintered samples.

Introduction alloys was ascribed to the high mixing entropy ΔSmix.

The following equation shows, that with increasing
Beside the well-known bulk metallic glasses a new
number of elements the mixing entropy ΔSmix rises
group of materials, so-called high-entropy alloys
(R gas constant, xi atomic percentage of the i-th
(HEAs), have become part of extensive research in
element):
the last decade. In contrast to conventional alloys,
HEAs consist of at least five principal elements, each

n
with a content of 5–35 at.-%. Surprisingly, the high DSmix = R xi ln xi (1)
number of involved components in HEAs does not i−1

lead to the creation of a multitude of complex and

brittle phases as expected from ternary phase diagrams
and conventional metallurgy. Instead, simple cubic
solid solutions are formed preferentially. Due to the
high content of different elements, it cannot be distin-
guished between solvent and solute. All elements need
to be considered as solved, see Figure 1 [1–3].
Exceptional properties (some are listed in Table 1)
as for example (high temperature) strength, corrosion
and wear resistance result from the unique microstruc-
ture [2–4]. For that reason, HEAs are considered as an
extraordinary alternative to conventional alloys.
The reasons for these special microstructures and
resulting exceptional properties can be seen in the so-
called ‘core effects’ [3,6,7] – namely, the high entropy,
the sluggish diffusion and the lattice distortion. In the
following, these effects shall be explained shortly.
Core effects
High entropy effect
As the name implies, the crucial impact on stability
of solid solutions and resulting properties of these
Furthermore, the increased mixing entropy ΔSmix
decreases the Gibbs free energy of mixing ΔGmix and
therefore stabilises the solid solution phase against
the intermetallic compounds:
DGmix = DHmix − TDSmix (2)
Further examinations showed that a high mixing
entropy ΔSmix is not always sufficient to stabilise the
solid solution phase, as also intermetallic phases were
detected in some HEAs [4]. The following three state-
ments should apply, if the mixing entropy ΔSmix would
be the crucial thermodynamic parameter to stabilise
the solid solution phases [8]:
(i) The higher the number of included elements, the
more likely is the formation of simple solid sol-
utions due to high entropy.
(ii) The elements included in the HEA should not
have stronger binding forces or big differences
in atomic radius.
(iii) Near equimolar solutions are preferred to non-
equimolar ones.

CONTACT Burghardt Klöden burghardt.kloeden@ifam-dd.fraunhofer.de

© 2017 Institute of Materials, Minerals and Mining Published by Taylor & Francis on behalf of the Institute
 POWDER METALLURGY 185

Figure 1. Crystal structure of HEAs [2]. (a) body-centred cubic

(bcc): five components. (b) face-centered cubic (fcc): five
components.

In the literature [9–11] it is clearly shown, that the

mixing entropy ΔSmix is not the only thermodynamic
parameter that decides if solid solution phases are
formed in HEAs. Considering the rules for the for-
mation of conventional alloys, as for example the
Hume Rothery Rule [4] for solid solution formation
or the Rule of Inoue [12] for the formation of metallic
glasses, some additional parameters could be taken into
account. Examinations showed that especially the mix-
ing enthalpy ΔHmix and the atom size difference δ have
a significant impact on solid solution formation in
HEAs [13]. The results of Ye et al. [5] regarding the
impact of these thermodynamic parameters on phase
formation are shown in Figure 2.
Single solid solutions are formed for HEAs with
−15 kJ mol−1 < ΔHmix < 5 kJ mol−1 and 0 < δ < 5%.
For multiphase HEAs an atomic size difference up to
8% is tolerated. Depending on the publication the
values slightly vary [14].
Sluggish diffusion effect
In the literature, the diffusion of atoms in HEAs is
described as sluggish compared to conventional alloys
[15]. The reason is most likely the high number of con-
tained elements. As already mentioned, a differen-
tiation between matrix and solved elements is not
possible. Therefore, the diffusion in HEAs considerably
differs from the process in conventional alloys, as all
elements have to be regarded as solved. A vacancy as
the basis for the mobility of atoms in HEAs is sur-
rounded by different elements (see Figure 3). Due to
the strongly varying bond configuration and hence
the large fluctuations of lattice potential energy (LPE)
between different lattice sites, the atoms and vacancies
Figure 2. Influence of mixing enthalpy ΔHmix (kJ mol−1) and
the atom size difference δ (%) on phase formation [5].
can be captured at preferred lattice sites with low LPE.
Furthermore, the diffusion coefficients are different for
all elements. This is why the slowest element is likely to
be crucial for the diffusion process [16,17].
Tsai et al. [16] analysed for the first time the diffu-
sion characteristics of a CoCrFeMn0.5Ni HEA and
gave a detailed description of the diffusion process in
HEAs as well as characteristic values for diffusion coef-
ficients and activation energies.
The sluggish diffusion affects all diffusion-con-
trolled processes, as for example phase formation and
grain growth. It results in stable nano-precipitations
and metastable phases, slower grain growth and
increased recrystallisation temperature. Furthermore,
the creep resistance could be improved by the sluggish
diffusion effect [17]. However, the slow diffusion could
be a problem for the sintering process.
Lattice distortion effect
Likewise, a consequence of the high number of con-
tained elements are the resulting lattice distortions.
Every atom is surrounded by different kinds of other
atoms and the different atomic sizes cause lattice dis-
tortions. This effect can be also detected in conven-
tional alloys, but due to the fact, that in conventional
alloys the matrix atoms are most likely surrounded
by the same kind of atoms, it is clearly more distinct
in HEAs, shown in Figure 4.
The lattice distortions affect both properties as well
as the influence of temperature on these properties.

Table 1. Selected properties for some HEAs compared to conventional alloys [5].
CoCrFeMnNi
Properties AlLiMg0.5ScTi1.5 Low-density refractory HEAs (−196°C) Al-alloys Ti-alloys Steel alloys
Density (g cm−3) 2.7 6.3–6.7 … 2.6–2.9 4.3–5.1 7.8
Hardness (HV) 5.9 3–4.7 … 0.2–1.8 0.5–3.8 1.5–4.8
Yield strength (GPa) 2.0 1.0–1.6 0.7 0.1–0.6 0.2–1.3 0.5–1.6
Specific strength (GPa g−1 cm3) 0.74 0.16–0.24 … <0.24 <0.31 <0.21
Fracture toughness (MPa m1/2) … … 200–300 23–45 55–115 50–154
Note: Best values are shown in bold.
186 N. EIßMANN ET AL.
Figure 3. Diffusion in HEAs is inhibited due to strongly varying
atom size.
Due to the solid solution strengthening in the heavily
distorted lattice, the strength as well as the hardness
increase considerably in HEAs. The MoNbTaVW
alloy for example has a hardness of approximately
530 HV [18], whereas the hardness calculated by the
rule of mixture is only roughly one-third of that
value. Moreover, this effect reduces the electrical and
Figure 4. Lattice distortion for elements, conventional alloys
and HEAs [15].
thermal conductivities due to the increased electron
and phonon scattering. The influence of temperature
on the last properties is expected to be rather small,
because the lattice distortions caused by thermal
vibrations are rather small compared to the severe lat-
tice distortions caused by composition.
Manufacturing of HEAs
To date, HEAs are preferentially produced via conven-
tional metallurgy, as for example, arc melting or induc-
tion melting [9,16,19]. This kind of production results
predominantly in a dendritic microstructure [20] and
for homogenisation, extensive thermal treatments are
necessary [20–23]. Furthermore, the machining needed
for the production of final parts could be difficult
because of the high hardness of the alloys. Therefore,
powder metallurgy could be a suitable alternative.
The processes described in literature predominantly
are mechanical alloying [24–26] for powder production
and spark plasma sintering (SPS) for compaction
[27–29]. With milling times up to 60 h [30,31] mech-
anical alloying is a very time-consuming method.
Hence, this production route is not yet capable for
industrial applications. With SPS no net shape parts
can be produced. Also different additive manufacturing
methods (laser engineered net shaping, selective laser
melting, selective electron beam melting) [32–34] and
methods for coatings and layer deposition [35–38]
are described in the literature.
In this publication powder metallurgy processes will
be examined. Instead of time-consuming mechanical
alloying, inert gas atomisation is used to generate a
spherical and homogeneous powder. Furthermore,
the suitability of SPS and pressureless sintering of
HEA-powders will be determined and presented.
Since die compaction of the alloyed powders is difficult
and would result in low densities, more promising
seems metal injection moulding (MIM) as shaping pro-
cess. Because good mechanical properties require
intensive densification by sintering, the sinterability
of fine HEA powders is studied in this paper. In
addition, additive manufacturing by selective electron
beam melting (SEBM) was done on the coarse particle
fraction and first results will be presented.
Material groups and classification
Considering 13 potential elements as components,
7099 different equimolar HEAs containing of 5 up to
13 components are possible [6]. This number shows
that countless different HEAs could be considered, if
non-equimolar HEAs are taken into account addition-
ally. An attempt to classify this huge world of HEAs
into material groups is pictured in Figure 5.
Fundamentally, HEAs can be classified by their
microstructure. The main difference between the alloys
 POWDER METALLURGY 187

Figure 5. Classification of HEAs [9,11,18,39–47].

can be seen in the formation of cubic or hexagonal Materials and methods

phases. HEAs with cubic phases can be classified in sev-
The CoCrFeMnNi HEA powder was produced by gas
eral further groups that will be described in the following.
atomisation at Fraunhofer Umsicht branch lab Sulz-
AlCoCrCuFeNi and its derivatives was one of the
bach Rosenberg. During the process, the materials
first HEAs that was under intensive examination
were inductively melted and subsequently atomised
[45,48–50]. Especially the influence of aluminium con-
by compressed argon. The resulting powder was split
tent on microstructure and properties was determined
by sieving in five fractions: <32 μm, 32–45 μm, 45–
[45,49,51–53]. Numerous further HEAs were deduced
63 μm, 63–160 μm and 160–355 μm. The smallest
from this alloy, as for example CoCrCuFeNi, Al2-
three fractions were subsequently used for pressureless
CoCrCuFeNixTi and Al2CrCuFeNi2 [54–56]. CoCr-
sintering and the powder fraction with a particle size of
FeMnNi [9,11,57–59] could also be considered as
63–160 μm was used for SPS. Further experiments
derivative of AlCoCrCuFeNi, but due to the high num-
were done with SEBM using the fraction of 63–160 μm.
ber of publications, it is academically highly relevant,
SPS was carried out using the systems HDP 5 and
and that is why it is listed in a separate materials
HDP 250 by FCT Systeme GmbH. A graphite mould
group in this publication. HEAs consisting predomi-
with a diameter of 20 mm was used. To protect the
nantly of refractory elements belong to the group of
tool, an additional graphite foil was used between the
refractory HEAs that gathered more attention over
die and the powder as well as between the powder
the past few years. These alloys seem to be appropriate
and the punches. To avoid a chemical reaction
especially for high temperature applications [18,42,43].
(especially carbide formation) a second foil, made of
All other HEAs with cubic phases that could not be
tungsten, was used between powder and graphite foil.
arranged in one of these material groups are combined
Due to the application of two foils, the pressing tool
in the last group, namely ‘other HEAs’. Considerably
needed to be adapted so that the motion of the punches
less HEAs show a hexagonal structure, see Figure 5.
in the mould would not be impeded. During the SPS
The HEA chosen for this publication was an equi-
process, the starting pressure was approximately
molar CoCrFeMnNi alloy. It shows a single phase
13 MPa. Simultaneously the die was heated up to
with a face centred cubic structure – independent of
1000°C and the pressure was increased to 55 MPa.
the exact composition. CoCrFeMnNi as well as
After holding at this temperature and pressure for 10
CoCrFeMn0.5Ni [16] as well as Co5Cr2Fe40Mn27Ni26
min the temperature as well as the pressure were
[11] show the same crystal structure, therefore it is
reduced to room temperature and normal pressure.
already considered in the literature as a ‘model alloy’
Furthermore, SPS specimens for mechanical testing
[3]. However, current investigations prove the for-
with a diameter of 30 and 60 mm were successfully
mation of an intermetallic σ phase during extensive
produced at two different temperatures 1000 and
heat treatment [58]. After a holding time of 500 h at
1200°C.
700°C the intermetallic phase can be detected at the
Pressureless sintering of loose powder was carried
grain boundary (size approximately 5 μm). Moreover,
out in molybdenum crucibles using a Xerion tube fur-
this phase solves again during a heat treatment at
nace. A heating rate of 10 K min−1, argon atmosphere
1000°C. In this paper all sintering processes were con-
and titanium sponge as getter were used. A holding
ducted at higher temperatures. Therefore, a homo-
time of 30 min up to 4 h and a sintering temperature
geneous solid solution is considered to govern the
of 1000°C up to 1200°C were applied. It is pointed
densification mechanisms during sintering.
188 N. EIßMANN ET AL.
Figure 6. Geometry of tensile specimens.
out that the pressureless sintering was done on non-
compacted powder samples, i.e. without binder, in
order to study the sintering behaviour of the lose pow-
der. The shrinkage behaviour was investigated using a
horizontal push rod dilatometer (Netzsch DIL 402E) at
a temperature of 1200°C for 4 h. Instead of using a tita-
nium getter, an atmosphere mixed of argon and hydro-
gen (5 vol.-%) was applied to avoid oxidation. The
cylindrical samples for dilatometry were produced by
sedimentation and subsequent drying of a suspension
of the smallest powder fraction (<32 μm) in a water
based binder in a suitable aluminium mould.
SEBM was carried out in a dedicated machine
(Arcam A2X). Cuboid samples with dimensions of
(10 × 10 × 20) mm³ were manufactured at a process
temperature of ca. 750°C in a build space with an
area of (100 × 100) mm².
The crystal structure was identified with X-ray dif-
fraction (XRD) using Bruker’s D8 Advance with Cu-
Kα radiation (λ = 0.154 nm). The powder particle size
was analysed using a Laser particle size analyser LA-
960 (HORIBA). The chemical composition of the pow-
ders and compacted samples was determined by Zeiss
EVO 50 scanning electron microscope (SEM) equipped
with secondary electron, backscatter electron and
energy-dispersive X-ray spectroscopy (EDX) detectors.
Metallographic preparation was accomplished by sev-
eral grinding (SiC-grinding paper) and polishing
steps (polishing with diamond and oxide suspensions).
The density of the samples was calculated by measuring
Figure 7. (a) SEM-picture and (b) XRD patterns of argon atomised powder.
mass and volume or by Archimedes’ principle. Further-
more, the powder density was analysed using a gas
comparison pycnometer (Accupyc 1330, Micromeri-
tics). The impurity content was measured with TCH
600 and CS 230 by LECO. In these devices, the carbon
and sulphur contents were detected by infrared absorp-
tion of carbon oxides and sulphur oxides. Oxygen was
likewise measured by infrared absorption. Nitrogen
was instead measured by thermal conductivity
measurement. Simultaneous thermogravimetry-differ-
ential thermal analysis (STA) was realised using
Netzsch STA 449 F3 Jupiter and differential scanning
calorimetry (DSC) using Netzsch STA 449 C Jupiter.
Mechanical properties were analysed during tensile
tests as well as hardness and elastic moduli measure-
ments for SPS samples. Tensile properties were tested
using Universal Testing Machine Zwick 1476. Standard
DIN EN 6892-1 were applied during testing. The geo-
metry of the tensile specimens is pictured in Figure 6.
The elongation was measured using a video extens-
ometer (Limess VE RTSS) and the strain rate was
0.2 mm min−1. Three specimens sintered at a tempera-
ture of 1200°C and six specimens sintered at a tempera-
ture of 1000°C were tested. The Vickers hardness (HV
5) of the sintered samples (sintering temperature of
1000°C) was measured on polished surfaces using
EMCOTest 4M (EMCO). Elastic moduli were analysed
using resonant frequency damping analysis.
Results and discussion
Powder characteristics
The atomised powder is shown in Figure 7(a). As
expected, the powder has a nearly spherical particle
shape. The voids detected in the particles result from
atomisation process and can therefore be regarded as
gas porosity. Consequently, the powder density of
7.83 g cm−3 is slightly below the theoretical value of
8 g cm−3. In Table 2 the analysed composition is dis-
played. It can be clearly seen, that the generated com-
position is very close to the equimolar composition
aimed for the highest entropy.
 POWDER METALLURGY 189

Table 2. Chemical composition of atomised powder pictured in Table 4. Carbon, sulphur, nitrogen and oxygen content of the
Figure 7(a). initial powder and selected fractions.
At.-% Co Cr Fe Mn Ni Fraction C (m-%) S (m-%) N (m-%) O (m-%)
Atomised powder 19.8 20.2 19.7 20.2 20.1 Initial powder 0.022 0.007 0.016 0.062
He et al. [60] 19.3 21.3 19.4 20.7 19.3 <32 μm … … 0.016 0.134
Nominal 20.0 20.0 20.0 20.0 20.0 32–45 μm … … 0.018 0.090
>160 μm … … 0.014 0.045

well. The carbon, sulphur and nitrogen contents are

negligible and therefore not analysed for the fractions.
The oxygen content of the initial powder is reasonable.
Due to the larger surface area, the oxygen content of
the smallest fraction is considerably higher than that
of the larger fractions and the initial powder.

Processing
Spark plasma sintering
The microstructure of the samples after SPS at 1000°C
are shown in Figure 9(a), which shows a single phase
microstructure without any visible precipitations. The
varying shades of grey are a sign for different grain
Figure 8. Particle size of five fractions. orientations, not for different phases. Although no pre-
cise measurements have been made jet, the grain size
can be estimated from Figure 9(a) at about 25 μm.
The diffractogram of the resulting powder, pre-
Only a small amount of porosity was detected. These
sented in Figure 7(b), resembles literature values, as
results are also supported by XRD. Figure 9(b) presents
for example He et al. [60], Liu et al. [57] and Zaddach
the diffractogram for the SPS samples compared to the
et al. [61]. Detected distinct and small peaks show that
powder. No obvious difference could be detected
by argon gas atomisation a single-phase powder with
between powder and SPS sample.
a face-centred cubic crystal structure was produced.
The composition of the sintered samples was
For the subsequent choice of the sintering tempera-
detected by EDX-analysis. The results are listed in
ture, the melting range of the powder was analysed
Table 5. The change in values for atomised powders
by the DSC-method in a temperature range from
and SPS sample is negligible. As the composition of
1290 to 1330°C.
the consolidated sample is close to the nominal compo-
For further examinations, the powder was divided in
sition, it can be assumed that a consolidation by SPS
five fractions as described in the section ‘Materials and
does not lead to the formation of additional phases
methods’. The particle sizes of the resulting fractions
or precipitations.
compared to initial powder are displayed in Figure 8.
The element distribution, presented in Figure 10,
Sieving of powder led to fractions with clearly different
shows a homogeneous and single phase microstructure
mean diameters (listed in Table 3). The overlap of the
and supports the results of the SEM and XRD analysis.
particle sizes is caused by the sieving process. The
All elements are distributed equally and no second
spherical powders easily plug the mesh, inhibiting a
phases could be detected.
perfect sieving process. To avoid plugging, the sieves
The density of the resulting SPS samples and some
were regularly purged by water and compressed air.
properties are listed in Table 6. The results are in line
The carbon, sulphur, nitrogen and oxygen contents
with the literature values and only insignificant under-
of the atomised powders are listed in Table 4. More-
match the theoretical density.
over, the values for selected fractions are listed as

Pressureless sintering
The resulting densities after various sintering exper-
Table 3. Results of particle size analyses.
iments are summarised for three fractions (<32, 32–
Mean diameter d50
Fraction (μm) 45 and 45–63 μm) in Figure 11. Since loose powders
Initial powder 89.0 were used, the initial densities correspond to the appar-
<32 μm 13.5 ent densities of the powder bed. The following appar-
32–45 μm
45–63 μm
22.7
42.6
ent densities are reached: 4.3 g cm−³ (53.8%),
63–160 μm 85.9 4.5 g cm−³ and 4.5 g cm−³ (56.3%) for the three frac-
>160 μm 263.1 tions (from fine to coarser powder). The starting
190 N. EIßMANN ET AL.

Figure 9. (a) SEM-picture and (b) XRD-analysis of SPS-sample.

Table 5. Composition of SPS sample compared to atomised time to 4 h results in a considerably higher density
powder and literature. only for the coarsest fraction. The increase for both
At.-% Co Cr Fe Mn Ni powder fractions <32 and 32–45 μm is only marginal.
Atomised powder 19.8 20.2 19.7 20.2 20.1 Probably only an increase in temperature could further
SPS sample 20.1 20.3 20.0 19.7 19.9
He et al. [60] 19.3 21.3 19.4 20.7 19.3 raise the density. Moreover, the smallest particle frac-
Nominal 20.0 20.0 20.0 20.0 20.0 tion shows again the highest densities (Figure 11(a)).
The microstructure of the sintered powder fraction
<32 μm for 30 min and 4 h at 1200°C is pictured in
densities are clearly lower than the powder density in Figure 12. An obvious decrease in porosity was
MIM feedstock would be. Nevertheless, a first picture detected. The optical analysis of porosity for all three
of the sintering behaviour of non-compacted HEA fractions led to similar densities during density
powder could be obtained. The densities after sintering measurement using Archimedes’ principle, which is
at temperatures of 1000 and 1200°C for a holding time why the values are not listed separately. The micro-
of 30 min are listed in Figure 11(a). As expected, the structures in Figure 12 are a result of densification
density rises with increasing temperature. Further- from the loose powder state. The inhomogeneity of
more, the finest powder fraction shows always the pore sizes resulting from non-ideal packing in the start-
highest densities due to the well-known fact that the ing condition is clearly visible. This might be one
sintering activity is higher for smaller particles. Figure reason why higher densities were not observed. A
11(b) shows the influence of the holding time on den- more homogeneous packing of particles, which is typi-
sity. As expected, the longer the holding time, the cal after MIM-feedstock preparation, should avoid this
higher the resulting density is. An increase in holding problem. The observed shrinkage during sintering is a
time to 2 h results in a considerably higher density clear indication that sintering to nearly full density
for all three fractions. Instead, an increase in holding during MIM should be possible.

Figure 10. EDX mapping of SPS sample.

 POWDER METALLURGY 191

Table 6. Selected properties of SPS samples compared to dilatometer analysis and the resulting density of
literature and theoretical calculated values (rule of mixture 6.4 g cm−3 only slightly undermatches the one of the
RoM). sintered loose powder. To analyse the shrinkage of
SPS Literature Theoretical
sample Deviation value value (RoM) HEAs in more detail further dilatometer analyses are
Density (g cm−3) 7.87 0.09 7.85 [62] 8.0 required. The influence of temperature will be exam-
Relative density 0.98 0.01 0.98 1.0 ined to determine the activation energies for diffusion.
Vickers hardness 169 2 144 [63] …
(HV 5)
These results will be compared to literature values for
Elastic modulus (GPa) 198 26 203 [64] … conventional alloys to classify the diffusion behaviour
of HEAs with regard to sintering. From literature it is
already known, that higher activation energies for dif-
Dilatometry fusion in HEAs lead to lower diffusion coefficients, i.e.
The shrinkage behaviour of HEAs was studied by dilat- to slower sintering. An increase of sintering tempera-
ometer analysis. The sample was obtained by a careful ture is still possible up to the melting point of 1290°C
sedimentation of the fine powder to obtain a more and would lead to faster diffusion. Furthermore,
homogeneous particle packing. A remaining small bin- studies should be made to even higher temperatures
der content in the dried samples gave a stable sample to evaluate if supersolidus sintering is possible. Theor-
and allowed to perform dilatometry without pre-sinter- etical studies [65] showed that segregation of elements
ing. First results (particle fraction <32 μm) are shown caused by the different partial diffusion coefficients will
in Figure 13. The shrinkage starts at a temperature of not be a problem in sintering of HEAs.
1017°C and slows down during the holding time of
4 h. Altogether, a considerable shrinkage of 11.9% Selective electron beam melting
could be detected. The microstructure of the samples after processing by
The densities of the starting and sintered sedimen- SEBM shows a single phase microstructure without
tation sample compared to sintered loose powder are any visible precipitations. These results are supported
listed in Table 7. The density clearly increases during by XRD. Figure 14 presents the diffractogram for the

Figure 11. Densities of sintered loose powders for various fractions for different (a) sintering temperatures (t = 30 min) and for (b)
different holding times (T = 1200°C).

Figure 12. Microstructure of sintered powder fraction (<32 μm, 1200°C) for (a) 30 min and (b) 4 h.
192 N. EIßMANN ET AL.

Table 8. The change in values for atomised powders

and the SEBM sample is negligible apart from Mn,
which is reduced by about 2 at.-%. This is due to the
evaporation of this element under the process con-
ditions of the SEBM process. As this decrease is equal-
led by a slight increase of all other elements, it can be
assumed that processing by SEBM does not lead to
the formation of additional phases or precipitations.
The element distribution, presented in Figure 15,
shows a homogeneous and single phase microstructure
and supports the results of the SEM and XRD analysis.
All elements are distributed equally and no second
phases were detected.
Figure 13. Results of dilatometer analysis of sedimentation
samples (<32 μm).
Classification and comparison of selected
powder metallurgic methods
Table 7. Densities of sedimentation sample compared to The results, presented previously, show that powder
sintered loose powder and theoretical density. metallurgy is a suitable method for HEA production.
Density (g cm−3) Relative density (%)
The gas atomisation of the HEA melt leads to homo-
Bulk density (fraction <32 μm) 4.3 54
Sedimentation samples 4.4 56
geneous and single-phase powders. The solidification
Sedimentation samples after DIL 6.4 81 of small droplets guarantees that a homogeneous distri-
Theoretical density 8.0 100 bution of the components is achieved before sintering.
Even if segregation during crystallisation would hap-
pen due to the complexity of the multicomponent
alloy, it would lead to de-mixing within the small
dimensions of individual particles. Therefore, the
alloy can be homogenised easily during sintering.
This is a clear advantage of the powder metallurgy
approach compared to casting technology. Moreover,
atomisation is a suitable process to produce an indust-
rially relevant amount of powder at reasonable costs.
This is also a crucial advantage over other PM-methods
for powder production, as for example mechanical
alloying, which leads to considerably smaller amounts
of powder in a distinctly higher amount of time and
is therefore problematic for future industrial pro-
duction. However, it can be an approach, if it is not
Figure 14. XRD-analysis of SEBM sample.
possible to use atomisation.
Three different methods for densification were
SEBM samples compared to the powder one. Apart tested within this assignment. SPS is a time-saving
from slight differences in the height of the peaks, no method to generate homogeneous and single-phase
obvious difference could be detected between powder HEA-samples. No negative change in microstructure
and SEBM sample. Only a small amount of porosity could be detected. Due to the short process time, no
(approximately 3%) could be detected. Therefore, the distinct grain growth is expected. Since SPS is a
density of SEBM samples is comparable to the SPS pressure assisted densification method, also other PM
samples. techniques, e.g. hot pressing or hot isostatic pressing,
The composition of the sintered samples was should be suitable to produce HEA materials from
detected by EDX-analysis. The results are listed in pre-alloyed powders in big quantities and with large
dimensions. However, the possibilities to obtain net
shape parts are limited in these techniques.
Table 8. Composition of SEBM sample compared to atomised The pressureless sintering process in this paper was
powder and literature. tested to evaluate the possibility of net shape parts pro-
At.-% Cr Mn Fe Co Ni
duction from non-compacted powders, e.g. by the
Powder 20.2 20.2 19.7 19.8 20.1
SEBM 20.4 18.7 20.1 20.3 20.5
MIM process. Higher sintering temperatures are
He et al. [60] 21.3 20.7 19.4 19.3 19.3 required to achieve dense samples. The long process
Nominal 20 20 20 20 20 time for sintering in our experiments should be
 POWDER METALLURGY 193

Figure 15. EDX mapping of SEBM sample.

shortened if higher temperatures are used. If this will
have an influence on grain growth, has to be evaluated
in further experiments. The preliminary results indi-
cate that MIM could be applied in a subsequent stage
to produce net shape parts of HEA from fine powders.
Die compaction, which is frequently used in powder
metallurgy for low cost production of precision parts,
is not an alternative for HEAs because of the high
solid solution hardening in the pre-alloyed powders.
The use of powder mixtures with better densification
behaviour during pressing is questionable since swel-
ling effects are expected during sintering and the hom-
ogeneity as a prerequisite for the absence of
intermetallic phases is difficult to obtain by diffusion
at sintering temperatures.
Selective electron melting generates dense and single
phase HEA-samples. Due to the numerous advantages
of this method, it is highly suitable for production of
complex HEA-parts. A further optimisation of proces-
sing parameters as well as adjustment of powder com-
position (increase of manganese content to compensate
the evaporation during processing) could improve den-
sity and composition of the resulting parts.
considerably higher elongation at fracture. Possible
reasons could be the decrease in internal stresses,
grain growth or a proceeding homogenisation during
the process. Further examinations are required to
explain this effect in detail. The exact values are listed
in Table 9. The listed deviations indicate that the mech-
anical properties of this material are reproducible inde-
pendent of the position of the tensile specimen in the
SPS sample. Accordingly, a rather homogenous micro-
structure within the SPS samples was achieved. Fur-
thermore, the determined elastic modulus matches
the results of resonance-frequency-damping analysis
very well, see Table 6.
The observed tensile strength of CoCrFeMnNi is in
the range of conventional steels (see Figure 17). All
mechanical analyses indicate that CoCrFeMnNi is a
material with high ductility and medium strength.

Mechanical properties
The mechanical properties of this HEA were tested on
SPS samples. Hardness values and elastic properties are
already listed in Table 6. The listed literature value is
smaller than the experimental value. According to lit-
erature the hardness value strongly depends on the Figure 16. Results of tensile tests for two different sintering
manufacturing process, due to which varying values temperatures (1000 and 1200°C).
can be found [9,20,61,62]. The elastic modulus is
approximately in the range of conventional steel and
matches literature values. The results of tensile tests Table 9. Summary tensile properties and their deviations.
Elastic Yield Tensile Elongation at
are presented in Figure 16. SPS modulus strength strength fracture
Using the tensile test, the influence of SPS-tempera- temperature GPa MPa MPa %
ture was evaluated. Increasing the sintering tempera- 1000 °C 161 ± 16 312 ± 9 613 ± 13 27 ± 2
ture results in a slightly smaller tensile strength and a 1200 °C 194 ± 77 237 ± 3 571 ± 4 37 ± 5
194 N. EIßMANN ET AL.
Figure 17. Scheme for tensile properties of selected materials
compared to experimental results for CoCrFeMnNi HEA
[11,20,60,66–94].
Conclusion
The HEA CoCrFeMnNi has been successfully pro-
duced by different powder metallurgic routes. The
powder was produced by argon gas atomisation. The
resulting spherical powder with nearly ideal equimolar
composition was subsequently divided in five fractions.
Selected fractions were afterwards compacted by two
different methods: SPS and pressureless sintering.
After SPS dense and homogeneous samples are gained.
No change in composition compared to initial powder
could be detected. The sample showed a single phase
microstructure with fcc structure. The density was
determined by Archimedes’ principle to be up to 98%
of theoretical value. Pressureless sintering led to
samples with a maximum density of 87% for the finest
fraction. With further increase of sintering temperature
and improvements in the initial particle arrangement,
e.g. by feedstock technique, an increase in density
should be reached. These examinations as well as the
description of shrinkage behaviour as a function of
temperature and particle size are part of further
research. With SEBM densities up to 97% were
reached. Further optimisation of the process par-
ameters should lead to further improvements with
respect to density. Similarly to the other technologies,
a single-phase microstructure was achieved, even
though ca. 2 at.-% of Mn are lost due to evaporation
in the SEBM process.
Selected mechanical properties were analysed using
SPS samples. The achieved hardness was approxi-
mately 169 HV 5 and the elastic modulus 198 GPa.
The tensile strength ranges from 571 to 613 MPa and
the fracture strain from 27 to 37% depending on the
sintering temperature.
Altogether, powder metallurgy offers a lot of advan-
tages for HEA production, as for example the lack of
time-consuming heat treatment to achieve a homo-
geneous microstructure. Especially gas atomisation is
a highly capable powder production method for future
industrial applications. SPS is highly capable to pro-
duce dense and homogeneous HEAs. The first results
in pressureless sintering are promising and especially
the prospect of using MIM is highly interesting for
further industrial applications. Additive manufacturing
shows considerable advantages for production of com-
plex HEA-parts and should be investigated in detail.
Furthermore, the potential of more methods should
be classified by additional research.
Disclosure statement
No potential conflict of interest was reported by the authors.
Notes on contributors
Nadine Eißmann studied Materials Science at the Tech-
nische Universität Dresden from October 2008 to March
2014. Since April 2014 she has been a PhD student at the
Technische Universität Dresden; Institute of Materials
Science.
Burghardt Klöden studied Physics at the Technische Uni-
versität Dresden and University of Sheffield from October
1996 to September 2002. From October 2002 to October
2006 he was a PhD student and obtained his PhD covering
the topic of “severe plastic deformation by high-pressure tor-
sion of NiAl” at the Technische Universität Dresden; Insti-
tute of Structural Physics. During the period from
February 2006 to September 2016 he was a research fellow
at the Fraunhofer Institute for Manufacturing Technology
and Advanced Materials IFAM, Branch Lab Dresden. Since
September 2016 he has been group manager for “additive
manufacturing – electron beam melting” at the Fraunhofer
Institute for Manufacturing and Advanced Materials
IFAM, Branch Lab Dresden.
Thomas Weißgärber studied Materials Science at the Tech-
nische Universität Dresden from September 1989 to July
1994. From August 1994 to July 1997 he was a PhD student
at the Technische Universität Dresden; Institute of Materials
Science and obtained his PhD covering the topic of “manu-
facturing, microstructure and properties of dispersions
strengthened copper”. From August 1997 to June 1999 he
was a research fellow at the Fraunhofer Institute for Manu-
facturing Technology and Advanced Materials IFAM,
Branch Lab Dresden. From July 1999 to March 2001 he
was the group manager for “composite materials” at the
Fraunhofer Institute for Manufacturing and Advanced
Materials IFAM, Branch Lab Dresden. Since April 2001 he
has been the Head of the Department of “Sintered and Com-
posite Materials” at the Fraunhofer Institute for Manufactur-
ing and Advanced Materials IFAM, Branch Lab Dresden.
Since 2009 he is also the Deputy Director of Fraunhofer
IFAM Dresden.
Bernd Kieback studied Physics from 1971 to 1976 at the
State University Charkiw, Ukraine. From 1976 to 1982 he
did his PhD in Materials Science at TU Dresden. During
1985–1990 he worked as the Head of the research group
on hard materials composites, ZFW Dresden.
From 1987 to 1990 he was also Head of the Department
of Tool Materials, ZFW Dresden. In 1991 he was Director of
the Institute for Power Metallurgy and Composite Materials
in the Institute for Solid State Physics and Materials Research

Dresden (ZFW). From 1992 to the present he has been the
Director of the Dresden Branch of the Fraunhofer Institute
Manufacturing and Advanced Materials (IFAM). From
1993 to the present he has also been Full Professor (C4)
and Head of the Chair Powder Metallurgy, Sintered and
Composite Materials, TU Dresden. From 2008 to 2011 he
was Director of the Institute for Materials Science (IfWW)
TU Dresden.
ORCID
Burghardt Klöden http://orcid.org/0000-0003-1919-6894
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