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Article history:
Received 10 September 2014
Received in revised form 5 March 2015
Accepted 7 March 2015
Available online xxx
Keywords:
AlSi coating
Hot stamping
Galling
Elevated temperature
a b s t r a c t
The usage of the hot stamping process is of great importance due to the high demands for production of
ultra-high strength steels (UHSS). An Al-Si coating is normally applied to the steel to prevent decarburisation and scaling during heating and to improve the corrosion resistance of the nal component. During
heating, the Al and the Si from the coating combine with the Fe from the steel substrate to form hard
intermetallic phases. Little is known about the inuence of the heating conditions on the tribological
behaviour of the Al-Si coating during interaction with tool steels. The present work investigated different heat treatment parameters and the inuence they had on the microstructure of the coating and the
galling behaviour. With low alloying temperatures (700 C), severe galling occurred and increasing the
alloying temperature to 900 C resulted in almost negligible material transfer. The reduction in galling
was associated to the development of Fe2 Al5 and FeAl2 at the surface.
2015 Elsevier B.V. All rights reserved.
1. Introduction
In the hot stamping process an Al-Si coating is commonly
applied on the ultra-high strength steel (UHSS) sheets. This coating gives good corrosion protection and has good paintability and
weldability as has been reported by Suehiro et al. (2003) in their
studies.
The Fe-Al-Si system is known for its complexity as it can form
an extensive amount of phases that are stable at various ranges of
temperatures and composition as highlighted in different studies.
Krendelsberger et al. (2007) studied this system and the challenge involved for the analysis and identication of different phases
as temperature increases through power diffraction, nonetheless,
they were able to conrm the existence of different ternary phases
reported in the open literature as well as the invariant temperatures of the reactions. Gupta (2003) carried out an analysis of the
Al-Fe-Si system with the aim of conrming which phases can be
encountered at different temperatures. Gupta was able to conrm
the existence of nine intermetallic phases despite the small differences in chemical composition. In a later study, Maitra and Gupta
(2003) found that the binary phases (Fe-Al) form solid layers. They
also stated that ternary phases such as 1 and 5 can crystallise
directly from liquid during cooling or by the occurrence of invariant
reactions.
In the case of the Al-Si coated UHSS in the hot stamping process,
when exposed to high temperatures, the Al-Si coating undergoes
microstructural changes due to the formation of intermetallics as
highlighted by Fan and De Cooman (2012) in their review. These
intermetallic phases have also been observed and studied by other
authors; Hardell et al. (2010) pointed out the formation of such
intermetallic layers and the morphological changes that it causes
on the surface of the coating. This was also conrmed by Borsetto
et al. (2009) as they observed that increasing the holding time
affects the chemical distribution of the constituents through the
coating as well as the morphology of the surface. These changes in
the chemistry of the coating are related to the formation of intermetallic phases, these intermetallics are formed by inter-diffusion
of Al, Si and the Fe from the steel substrate. When exposed to
high temperature (over 577 C), the Al-Si coating melts. This allows
the Fe from the substrate to diffuse quickly through the coating
towards the surface. The increased concentration of Fe in the coating causes the formation of intermetallic phases and the coating
solidies. As the intermetallics are formed, hardness of the coating
is increased and the coating becomes brittle. A multi layered structure after exposure to elevated temperatures has been observed by
Grigorieva et al. (2011). They reported up to ve layers (i.e. phases)
that can be found within the Al-Si coating; however, this number is
reduced with increased temperature and time. Furthermore, in the
study by Suehiro et al. (2003), it was stated that if enough time and
temperature is given, the coating homogenises into a single layer.
Veit et al. (2011) showed that even with the use of fast heating
process, the multi-layered structure of the coating is still formed.
http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
0924-0136/ 2015 Elsevier B.V. All rights reserved.
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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As mentioned before, the changes of the coating at high temperatures are not limited to the phase transformations; morphological
changes of the surface have also been reported in the studies done
by Hardell et al. (2010) in the form of nodules at the surface after
exposure to high temperature and also an increase in the average surface roughness. Borsetto et al. (2009) also observed the
increased roughness of heated specimens and also showed that
with long holding times, the roughness continues to increase. Veit
et al. (2011) suggested that the formation of such nodules is caused
by the melting of the unalloyed Al situated at the outermost layer
of the coating.
Several authors have addressed the tribological behaviour of
the Al-Si coated UHSS and reported occurrence of material transfer when it interacts with different tool steels with and without
coatings. The wear behaviour of tool steels with and without
coatings sliding against Al-Si coated UHSS has been investigated by
Kondratiuk and Kuhn (2011) and found that severe adhesive wear
can occur when coatings such as AlCrN or TiAlN are used. Azushima
et al. (2012) observed that under lubricated conditions friction
can be controlled to a steady level and suggests that wear can be
reduced. Pelcastre et al. (2012) studied the occurrence of material
transfer or galling on the tool steel surface and concluded that wear
fragments coming from the Al-Si coated UHSS accumulate within
surface defects or valleys of the surface of the tool and generate
material built up. The occurrence of adhesion was also observed by
Pelcastre et al. in untreated tool steels (2011); however, this adhesive tendency was magnied when certain PVD coatings were used
(Pelcastre et al., 2013), however, the use of oxidised plasma nitrided
tool steel reduced considerably the occurrence of galling. Hou et al.
(2010) observed that die corners are sites where severe material
transfer occurs and suggested that this was due to the increased
contact pressure and temperature at these regions.
It is clear that the heating conditions have a signicant effect on
the resulting microstructure and morphology of the coating, but
equally important is the fact that the existing phases also affect the
tribological response. The effect of the changes of surface roughness of the Al-Si coating has not yet been thoroughly studied and
its impact on galling or friction is not well understood. It has been
observed that the temperature, to which the coating is exposed to,
has an effect on material transfer and friction. For instance, in a
study by Kondratiuk and Kuhn (2011), they suggested that at temperatures around 920 C material transfer was reduced compared
to lower temperatures when Al-Si was sliding against tool steel.
In the study done by Borsetto et al. (2009) the authors observed
a reduced coefcient of friction between the Al-Si coating and a
hardened hot work tool steel at 700 C in a pin-on-disc conguration. However, it is not yet clear the reason for the above mentioned
cases.
In the actual forming process, the coating undergoes heating
during the austenitisation of the steel (930 C). Upon exiting the
furnace, the work-piece cools down to around 750 C before it gets
into contact with the forming tools. Even though it is acknowledged
that the heating history of the coating has an inuence on the tribological response, the correlation between the microstructure of
the coating and the tribological response still lacks understanding.
In this work, two temperatures (700 C and 900 C) were chosen for the investigations with a given soaking time for alloying
of the coating. From a fundamental point of view, the selected
temperatures allow the formation and evolution of typical phases
encountered in the forming process and others that are not often
seen in the process but that are also typical in the Al-Si-Fe system.
Even though the microstructural evolution of the Al-Si-Fe system
has been studied, as described in the review done by Fan and De
Cooman (2012), there is still lack of understanding concerning the
tribological behaviour of most of the phases that form in this system, and in the particular case, in the Al-Si coated UHSS.
Table 1
Test conditions to analyse inuence of alloying time.
Temperature ( C)
700
900
0
0
4
4
20
20
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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Table 2
Test parameters.
Test parameters
Value
Normal load
Nominal contact pressure
Temperature
Stroke length
Frequency
Duration
31 N
10 MPa
700 and 900 C
4 mm
12.5 Hz
30 s
(tool steel) specimen was kept separated from the lower disc (Al-Si
coated UHSS) during heating. Once the desired temperature was
reached, the lower specimen was retained at that temperature for
a given time while still separated from the upper specimen. The
holding times used for the tribological tests were 0, 4 and 20 min.
When the holding time had elapsed, the pin was loaded against
the disc and the test was started. On completion of the test, both
specimens were left to cool in air and then removed and analysed.
Repeat tests for all conditions were carried out with new specimens,
tool steel pin and work-piece disc, in order to assess repeatability
of the galling mechanisms.
The conditions used for the tests carried out in this work are
presented in Table 2. These parameters were selected based on
conditions in the forming operation.
2.4. Preparation of the Al-Si coating surface
To account for the inuence of the surface of the Al-Si coating,
the specimens were heated at 900 C for 4 min and then quenched
in water at 0 C. The specimens were subsequently ground using
#600 grit SiC abrasive paper and grinding was performed in random directions to avoid creating a dened orientation of the surface
lay. After the surface preparation, the specimens were reheated to
900 C and the tribological experiments were carried out. It was
initially intended to grind the specimens before any heat treatment. However, the thickness of the coating was severely reduced
due to the low hardness of the coating. The obtained surfaces after
grinding are shown in Fig. 2.
A reduction of the surface roughness Sa from 3.2 m to 1.2 m
was observed (the surface roughness was measured by means of
a Wyko 1100NT 3D optical interferometer). It is important to note
that the coating has a high waviness after the hot dip aluminising process which is one of the reasons for its high roughness.
This means that the thickness of the coating is not uniform and
it changes from one point to another. This type of structure persists
after heating and this could be observed when grinding the specimen as patches of at (ground) and rough (not ground) surface
(Fig. 2(c)).
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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Fig. 2. Surface morphology of the Al-Si coating: (a) as-delivered, (b) after 900 C treatment and (c) after 900 C treatment and ground with 600 grit size abrasive paper for
30 s.
Fig. 3. Phases present on the Al-Si coating: (a) as-delivered and (b) after exposure to 900 C for 4 min.
Fig. 4. Structure of the coating for all the conditions used. (a)(c) show 0, 4 and 20 min at 700 C and (d)(f) show 0, 4 and 20 min at 900 C.
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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Fig. 5. Evolution of the coefcient of friction from tests at (a) 700 C and (b) 900 C.
The wear mechanisms present on the tool steel specimen surfaces were analysed by means of SEM. The analysis focused mainly
on the material transfer mechanisms from the Al-Si coated steel
onto the tool steel.
Fig. 6 shows the material transfer observed after the tribological
tests. A strong dependence between the material transfer (galling)
and the heating conditions was observed. Severe galling occurred
at 700 C for all of the soaking times. From Fig. 6(a) and (c) it is clear
that thick lumps were developed on the surface of the tool specimens with 0 and 20 min soaking time. The test with 4 min soaking
time showed severe material transfer but a more uniform transfer layer (Fig. 6(b)). The uniform layer correlates with the observed
friction curve from Fig. 5(a), as 4 min soaking time resulted in a
more stable coefcient of friction. Formation of lumps is normally
associated with unstable and high coefcient of friction.
Tests carried out at 900 C underwent severe galling only when
0 min soaking time was used. Increasing the soaking time signicantly reduced the occurrence of material transfer. The amount of
transferred material did not change noticeably upon increasing the
soaking time from 4 min to 20 min. This behaviour also correlates
with the observed friction behaviour (Fig. 5(b)), as 4 and 20 min
resulted in a stable coefcient of friction.
3.2.1. Correlation between the phases of the coating and the
tribological response
It is known that the intermetallic formation in the coating starts
at around 570 C. In their work, Suehiro et al. (2003) observed that
Fig. 6. Tool steel specimen after tribological test at 700 C with soaking time of (a) 0 min, (b) 4 min, and (c) 20 min, and at 900 C with soaking time of (d) 0 min, (e) 4 min and
(f) 20 min.
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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Fig. 7. Cross section of the coating after the tribological tests. (a) 700 C and 0 min soaking time, (b) 900 C and 0 min soaking time and (c) 900 C and 4 min soaking time.
Fig. 9. Evolution of the coefcient of friction from tests at 900 C with and without
grinding.
Fig. 8. Evolution of the coefcient of friction from tests at 900 C with 4 min soaking time: (a) without cooling after soaking time and (b) with quenching after soaking time.
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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Fig. 10. Protective oxide layers developed on the surface of the Al-Si coated steel: (a) ground specimen and (b) as-delivered specimen.
Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009
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Please cite this article in press as: Pelcastre, L., et al., Inuence of microstructural evolution of Al-Si coated UHSS on its tribological
behaviour against tool steel at elevated temperatures. J. Mater. Process. Tech. (2015), http://dx.doi.org/10.1016/j.jmatprotec.2015.03.009