Microstructure and phase transformations in a liquid immiscible
Fe
60
Cu
20
P
10
Si
5
B
5
alloy
Krzysztof Ziewiec
a, *
, Miroslawa Wojciechowska
a
, Grzegorz Garzel
b
, Tomasz Czeppe
b
,
Artur Blachowski
c
, Krzysztof Ruebenbauer
c
a
Institute of Technology, Pedagogical University of Cracow, Podchora ˛ _ zych 2, 30 084 Krak ow, Poland
b
Institute of Metallurgy and Materials Science of Polish Academy of Sciences, Reymonta 25, 30 059 Krak ow, Poland
c
M€ ossbauer Spectroscopy Division, Institute of Physics, Pedagogical University, Podchora ˛ _ zych 2, 30 084 Krak ow, Poland
article info
Article history:
Received 20 July 2015
Received in revised form
16 September 2015
Accepted 17 October 2015
Available online xxx
Keywords:
Metallic glasses
Microstructure
Segregation
Differential scanning calorimetry
Scanning electron microscopy
M€ ossbauer spectroscopy
abstract
This work presents a study of the microstructure formed in a liquid immiscible Fe
60
Cu
20
P
10
Si
5
B
5
alloy
during moderate cooling on a copper plate and melt-spinning. The alloy ingot was re-melted on a copper
plate and observed while cooling using a mid-wave infra-red (MWIR) camera. The heating and cooling
characteristics of the melt-spun ribbon were studied using differential scanning calorimetry (DSC). The
morphology and chemical composition of the ingot as well as the melt-spun ribbon were analyzed using
scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS). The compositions of the
ingot and the ribbon were investigated using X-ray diffraction (XRD). M€ ossbauer spectroscopic mea-
surements showing the influence of adding Cu to the FeeSiePeB alloy were also analyzed.
The IR images from the MWIR camera enabled direct observation and identification of the liquid state
transformations of the alloy. The DSC trace of the melt-spun ribbon showed crystallization of the
amorphous matrix and confirmed that high temperature transformations occurred when the alloy was in
the liquid state. Observations of the microstructure of the ingot revealed crystalline surface fractal
structures formed by the Fe-rich eutectic constituent and Cu-rich fcc spherical precipitates. The
morphology of the precipitates indicated that the precipitates formed in the miscibility gap. The
microstructure of the melt-spun ribbon is composed of an amorphous Fe-rich matrix and elongated Cu-
rich fcc precipitates. The observations based on the study of the microstructure are supported by
M€ ossbauer spectroscopy.
© 2015 Elsevier Ltd. All rights reserved.
1. Introduction
Liquid immiscibility could be an interesting concept to explore
when considering the issue of controlling the microstructure of
composite materials. It is well known that liquid immiscible alloys
such as AlePb, AleBi and CuePb are potential materials for
advanced bearings in the automotive industry. There are recent
reports on the formation of two-phased glassy composites in an
NieNbeY system [1,2],YeTieAleCo system [3], AlePbeNieYeCo
system [4], iron-based FeeCueNieSieSneBeY system [5],
FeeCueNiePeSieB system [6,7] and FeeCuePeSieB [8] amor-
phous/crystalline composite. In the latter alloys, it has been shown
that the morphology of the composites can be changed by varying
the temperature prior to ejection.
Phase transformations and structure development in alloys
processed in the liquid state are important for controlling the final
microstructure and properties of the alloys, and as such, should be
better investigated and understood. Up to this time, the only re-
ports on liquid immiscibility in metal alloys were based on ther-
mocouple [9], pyrometer [10,11], differential thermal analysis (DTA)
[12] and DSC [13,14] measurements. In Ref. [8], the studies of the
Fe
60
Cu
20
P
10
Si
5
B
5
amorphous/crystalline alloy prove that its
microstructure depends on the temperature of ejection from the
crucible, and that the temperature at which the liquid separates can
be found using indirect pyrometric and DTA measurements. This
present work provides further evidence for this through direct
observation of thermal images made by a MWIR camera. These
images are verified by DSC analysis and microstructural studies
using SEM/EDS and XRD.
FeePeSieB alloys are known for their ability to form glass and
* Corresponding author.
E-mail address: kziewiec@up.krakow.pl (K. Ziewiec).
Contents lists available at ScienceDirect
Intermetallics
journal homepage: www.elsevier.com/locate/intermet
http://dx.doi.org/10.1016/j.intermet.2015.10.010
0966-9795/© 2015 Elsevier Ltd. All rights reserved.
Intermetallics 69 (2016) 47e53