EBSD and EDS characterization

of high entropy alloys.

Introduction

EBSD

A high entropy alloy, Al8Co17Cr17Cu8Fe17Ni33, has been developed from an equiatomic AlCoCrCuFeNi alloy. Due to
its promising properties, such as high corrosion and oxidation resistance and high thermal stability, it is a candidate
for various applications at elevated temperature as, e.g., furnace parts, tools and moulds. The exploration of new
metallic systems for high temperature applications is an important challenge in todays materials science.
However, an increase of the strength of this alloy is desirable and requires further optimization. In order to improve
these mechanical properties, knowledge of the microstructure is necessary. Therefore, Al8Co17Cr17Cu8Fe17Ni33 high
entropy alloy has been studied by means of energy-dispersive X-ray spectroscopy (EDS) and electron backscatter
diffraction (EBSD).

High entropy alloys

Experimental procedure

High entropy alloys have been defined as consisting of five or

more elements, each one having a concentration between 5
and 35 at.% [1-3]. These alloys are crystalline materials which
predominantly form simple solid solutions, mainly of facecentred or body-centred cubic structures. High entropy alloys
promise an interesting combination of properties, such as
oxidation resistance, thermal stability, high strength and soft
magnetic behaviour [3, 6-9].

The Al8Co17Cr17Cu8Fe17Ni33 alloy was prepared in a vacuum

induction furnace. The alloy constituents were of 99.99%
purity. The ingots were remelted three times to achieve
a better homogenisation. Specimens for analysis were
mechanically ground and polished using an OP-U colloidal
silica suspension.

The most studied high entropy alloy is AlCoCrCuFeNi

with equiatomic composition [4, 5, 8, 10, 11]. It solidifies
dendritically within a large variation of casting conditions. The
dendrites mainly consist of two phases, an Al/Ni-rich and a Fe/
Cr-rich phase, whereas interdendritic regions are enriched in
Cu [4, 10]. It has also been found that the Fe/Cr-rich phase
decomposes into Fe-rich and Cr-rich domains. A length scale
between these domains of just a few nanometres indicates
spinodal decomposition as the formation process [8], which is
often reported for Fe-Cr systems [12, 13].
The ductile Al8Co17Cr17Cu8Fe17Ni33 alloy shows mainly two fcc
phases in transmission electron microscopy, an ordered phase
of L12 structure and a disordered fcc matrix. The ordered
phase has been found to be Ni- and Al-rich as measured by
atom probe tomography. Very few Cu-rich precipitates are
found at the grain boundaries [14].
In the present work, an Al8Co17Cr17Cu8Fe17Ni33 high entropy
alloy which had undergone cold rolling was investigated
in order to reveal the microstructural properties as well as
elemental distributions within the specimen.

The investigated samples underwent a cold rolling, with up to

70% decrease in thickness.
Elemental distribution maps by EDS and EBSD maps given in
the present work, were obtained using Oxford Instruments
X-Max 80 X-ray and NordlysNano EBSD detectors. The
acceleration voltages and beam currents applied were 15 kV
and 10nA. EDS and EBSD acquisitions, and analyses, were
performed using the AZtec software package. Evaluation of
stored EBSD patterns for strain/stress analysis within individual
grains were conducted using CrossCourt 3 (BLG Productions).

EBSD and EDS characterization

of high entropy alloys.

EBSD

Results
The scanning electron micrograph in Fig. 1 reveals a high
density of extended structural defects within individual
grains. The EBSD maps (using fcc Ni as reference) in Fig.
2 show that along linear features, the local orientation
is changed when compared with the matrix of the
Al8Co17Cr17Cu8Fe17Ni33 specimen. The distributions of the
11, 22, and 33 strain tensor components, calculated from
the EBSD data, indeed indicates that the strain is modulated
across these linear features, with peak values of about 6 %
strain.

Fig. 1: Scanning electron micrograph of Al8Co17Cr17Cu8Fe17Ni33

alloy. On the region highlighted by a white frame, EBSD and EDS
measurements (Figs. 2-4) were performed.

Fig. 2: EBSD band contrast as well as orientation-distribution maps of the region highlighted by a white frame in Fig. 1. The local orientations
are given as colors (see legend) for the x, y, and z directions.

Fig. 3: Distributions of the 11, 22, and 33 strain tensor components, as calculated from the EBSD data (same identical position as in Figs. 1
and 2) by means of the CrossCourt software.

EBSD and EDS characterization

of high entropy alloys.

EBSD
It is apparent from the elemental
distribution maps acquired (Fig. 4)

that the Al8Co17Cr17Cu8Fe17Ni33 alloy

decomposes after casting into dendrites
mainly consisting of Al/Ni/Cu-rich and
Cr/Fe/Co-rich regions, which agrees well
to previous reports [4,10]. In addition,
elemental distribution maps acquired
in cross-section show the layered
structure of the Al/Ni/Cu-rich dentrites.
Together, the distribution of the Al/Ni/
Cu-rich dendrites appears similar to the
distributions of the 11, 22, and 33 strain
tensor components.

Fig. 4: EDS elemental distribution maps calculated, using the Al-K, Ni-L, Cr-L, Fe-L, Cu-L, and
Co-L signals, acquired on the same identical position as in Figs. 1-3.

Fig. 5: Fig. 4: EDS elemental distribution maps calculated using the Al-K, Ni-L, Cr-L, Fe-L, Cu-L, and Co-L signals, acquired on a cross-section
specimen (view perpendicular to the maps in Fig. 4).

EBSD and EDS characterization

of high entropy alloys.

Conclusion

EBSD

The present work shows how correlative imaging as well as EBSD and EDS analysis in scanning electron microscopy on identical
specimen positions may reveal the microstructural properties and the elemental distributions in an Al8Co17Cr17Cu8Fe17Ni33 alloy.
The distributions of Al/Ni/Cu-rich and Cr/Fe/Co-rich were detected and correlated to the distributions of the 11, 22, and 33 strain
tensor components.

Acknowledgements
A. Manzoni, N. Wanderka, N. Schfer, D. Abou-Ras (all Helmholtz-Zentrum Berlin fr Materialien und Energie, Germany) for
providing the Ni high entropy sample and the EDS/EBSD analyses.
Special thanks are due to A. Bakai for carrying out the cold rolling experiments (Kharkov Institute of Experimental and
Theoretical Physics, Ukraine).

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