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Journal of Materials Processing Technology


journal homepage: www.elsevier.com/locate/jmatprotec

Inuence of microstructural evolution of Al-Si coated UHSS on its


tribological behaviour against tool steel at elevated temperatures
Leonardo Pelcastre , Jens Hardell, Anthony Rolland, Braham Prakash
Division of Machine Elements, Lule University of Technology, Lule SE-971 87, Sweden

a r t i c l e

i n f o

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.

Corresponding author. Tel.: +46 736969813; fax: +46 920491047.


E-mail address: leonardo.pelcastre@ltu.se (L. Pelcastre).

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)

Soaking time (min)

700
900

0
0

4
4

20
20

In the forming industry, there is always a drive to modify the


heating conditions to increase productivity and reduce costs. However, little information is available concerning possible effects that
may occur as a result of the microstructural evolution of the Al-Si
coating.
This work aims to increase the understanding of the tribological
behaviour of Al-Si coated UHSS under different heating conditions.
Particular focus is given to the friction behaviour and galling mechanisms. Furthermore, the effect of the surface roughness of the Al-Si
coating on the tribological behaviour is also studied.
2. Materials and experimental methodology
2.1. Test materials and specimens
The specimens used for the tribological tests were an upper pin
of 2 mm made from a hot work, quenched and tempered tool steel.
A similar composition is normally used for tools in the actual hot
stamping process. The tool steel pin surface was polished to an
Sa value of 50 nm. The lower disc (16 mm and 1.7 mm height)
was made from Al-Si-coated UHSS which was welded onto a steel
backing plate of 24 mm and 6.3 mm height. The Al-Si coated steel
is widely used as workpiece in the hot stamping process. According
to the review done by Fan and De Cooman (2012), the boron steel is
usually aluminised by hot dipping into a molten Al alloy bath with
a composition of approximately 88% Al, 9% Si and 3% Fe in weight
percentage.
2.2. Heat treatment of the Al-Si coated boron steel
Initially, the effect of temperature on the evolution of the Al-Si
coating microstructure was considered.
For this study, three different soaking times were used for the
analysis of the microstructural evolution. Table 1 shows the times
used for each temperature. A soaking time of 0 min means that
the samples were heated up to the desired temperature and then
cooled down immediately. The coating undergoes melting when
exposed to temperatures higher than 570 C followed by solidication caused by diffusion and interaction between the constituents
of the steel substrate and the Al-Si coating. The 0 min soaking time
was selected to determine whether the presence of melted coating material could be observed and its effect on the tribological
response. A soaking time of 4 min was selected as it is close to the
duration normally used in the hot stamping process. In the study
done by Suehiro et al. (2003), it was proposed that given enough
time and temperature, the coating can develop a structure with a
single layer. The soaking time corresponding to 20 min was selected
to evaluate changes in the microstructure of the Al-Si coating (shifts
in the formed layers) and the effects on the tribological behaviour.
A schematic of the heat treatment history is shown in Fig. 1.
The heat treatment was performed in the tribometer itself to have
the same heating conditions that are normally obtained during the
tribological tests.
2.3. Tribological tests
Tribological tests were carried out using an Optimol SRV hightemperature reciprocating friction and wear tester. Before the tests,
all specimens were cleaned with ethanol and dried. The upper pin

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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To achieve a totally at surface, it needed to be ground for a


considerable amount of time which caused the removal of a great
part of the coating at some locations. Altering the thickness of the
coating has an effect on the diffusion kinetics of the constituents
and hence on the phase transformations during heating, meaning
that large variations would be obtained when comparing with other
analysis found in the literature. To avoid this, all samples were set to
be ground for the same duration (30 s), so as to reduce the surface
roughness without reducing too much the thickness of the coating. It is clear that the optimal conditions (totally smooth and at
surface) were not obtained, however, it does give a good insight to
characterise the effect of the surface topography on the tribological
behaviour.

Fig. 1. Heat treatment history for treatments at 700 C and 900 C.

3. Results and discussion


3.1. Microstructural evolution of the Al-Si coating

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)).

For the identication of the different phases, backscatter


electron microscopy coupled with EDS analysis was used. The
observations were then compared with what has been reported
in the open literature, for instance the review done by Fan and De
Cooman (2012) or the studies by Grigorieva et al. (2011) and Veit
et al. (2011). In these references, the analysis has been done mainly
by means of EDS and then the composition has been compared with
the phase diagrams of the Fe-Al-Si system. A cross section of the
coating in the as-delivered state can be seen in Fig. 3(a). The coating
is composed of two layers, an intermetallic situated at the interface
coating/steel substrate which different authors have identied as
Fe2 Al78 Si (Fan and De Cooman, 2012; Veit et al., 2011) and a mixture of unalloyed Al and Si. The coating is characterised by a very
low hardness of the Al + Si outer layer (55 HV25g ), whilst the layer
at the interface coating/steel has higher hardness (475 HV25g ).
When the coating is heated up, new phases are formed as the Fe
from the steel substrate diffuses outwards and the Al of the coating
diffuses inwards. The formation of these phases depends on the diffusion of the coating and steel constituents, thus the existing phases
depend on factors such as temperature, time and thickness of the
coating. The most common phases observed during heating of the
Al-Si coated UHSS are shown in Fig. 3(b). As mentioned before, a
multi-layered structure is obtained after heating, from bottom to
top the layers are as follows: a diffusion layer between the substrate
and the coating, a layer containing FeAl2 and/or Fe2 Al5 , an intermediate layer of Fe2 Al2 Si and a layer of Fe2 Al78 Si. In Fig. 3(b) these
phases are shown. The Fe2 Al78 Si is seldom observed as it is not
stable at the process temperatures (it has a melting point of 855 C
according to the studies done by Gupta (2003), Krendelsberger et al.
(2007) and Veit et al. (2011)).
Fig. 4 shows the coating after each of the soaking times used in
this work (0, 4 and 20 min). The temperatures used were 700 and
900 C. At 700 C, an interlayer with the appearance of a continuous thin line is formed (Fig. 4(a)). This phase is Fe2 Al2 Si and it is
characterised by a high hardness (600 HV25g ). Surrounding this
interlayer, FeAl2 and/or Fe2 Al5 are formed which also have a high
hardness (830 HV25g ) and the outer layer was unalloyed Al and
Si. Longer soaking time at 700 C allowed more diffusion of Fe and
when 4 min had elapsed, the unalloyed Al and Si layer had already
disappeared and the whole coating had transformed into intermetallic phases. Fe2 Al78 Si was formed at the outermost layer and
the Fe2 Al2 Si had shifted position towards the surface of the coating
(Fig. 4(b)). Similar microstructure was observed for longer soaking
times (Fig. 4(c)); the main difference was that the Fe2 Al78 Si layer
was thinner whilst the FeAl2 /FeAl5 layer had grown.
At 900 C, the layer with unalloyed Al and Si was not observed
for any soaking time and the Fe2 Al2 Si phase was already at the

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.

middle of the coating when 0 min soaking time was used


(Fig. 4(d)(f)) and it was present for all of the soaking times. When
20 min soaking time had elapsed, this layer shifted further outwards in the coating (Fig. 4(f)). The Fe2 Al78 Si phase was observed
only when 0 min soaking time was used. For all of the other cases,
this phase had dissolved and only layers containing Fe2 Al2 Si and
FeAl2 /Fe2 Al5 were observed (Fig. 4(e) and (f)).
In addition to the aforementioned phases, at 900 C another
layer was observed at the interface between the coating and
the steel substrate (Fig. 4(d)(f)), other authors identify it as a

diffusion layer (Fan and De Cooman, 2012). The thickness of this


layer increased with the soaking time and its hardness was in the
range of 330380 HV25g .
It is clear that the most stable phases of this system, under
the heating conditions used, are Fe2 Al5/ FeAl2 and Fe2 Al2 Si. In their
study, Suehiro et al. (2003) stated that if enough activation energy
is provided, the coating ends up with a single layer. The conditions
selected in the present study did not provide with such activation
energy or time therefore the nal state of the coating could not be
reached.

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 formation of a homogeneous coating is limited or hindered


by the diffusion of different constituents through the coating and
in the steel substrate. Initially, part of the Al + Si layer melts. This
causes a rapid diffusion of the Fe from the steel substrate and the
Fe2 Al2 Si, Fe2 Al5 and FeAl2 phases are formed. As time is increased
further, more Fe diffuses towards the surface of the coating and
the Fe2 Al78 Si is formed whilst at the same time the remaining
unalloyed Al + Si phase combines with the Fe and more Fe2 Al5 and
FeAl2 are formed. With further increase of the holding time, the
Fe2 Al78 Si phase dissolves and the constituents combine and as a
result, only Fe2 Al2 Si, Fe2 Al5 and FeAl2 remain.
3.2. Inuence of heating conditions on the tribological behaviour
and galling
Concerning the inuence of the heating conditions on the tribological behaviour, the soaking time had a signicant effect on
the friction behaviour. For the specimens heated up to 700 C,
the coefcient of friction had in general an unstable behaviour
(Fig. 5(a)). Using 4 min soaking time resulted in a lower and more
stable coefcient of friction compared to the other soaking times.
It was observed that at 900 C (Fig. 5(b)), the coefcient of friction
was unstable and large uctuations were seen with 0 min soaking
time. Once the soaking time was increased from 0 min to 4 min, a
stable coefcient of friction was observed. Comparing the coefcient of friction at 900 C after 4 and 20 min soaking time, a similar
behaviour was observed for the two soaking times.

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.

melting of the coating occurred and it solidied as the Fe from the


substrate diffused towards the surface. Initially, the kinetics for the
intermetallic formation are high due to the presence of the liquid
Al + Si phase, however, once it starts to solidify as it combines with
the Fe from the steel substrate, the diffusion rate is then drastically
reduced and the phase transformations are slowed down.
It was observed that more severe galling occurred at 700 C
compared to 900 C. The increased galling and unstable friction
behaviour at 700 C can be attributed to the absence of the harder
and more stable phases at the contacting surface formed at 900 C.
It is however not entirely clear whether all the Al-Si coating was
solidied or if part of it was still melted. From the results shown in
Fig. 6, it seems that a liquid phase only exists when 0 min soaking
time is used, and as the exposure time increases, the solid phases are
indeed formed. 700 C and 4 min soaking time showed a homogenous transfer layer on the tool steel surface, which suggests that no
liquid phase was present. Similarly, at 20 min soaking time, even
though thicker lumps were developed, it is clear that these lumps
were formed as a result of continuous accumulation of wear debris,
rather than severe smearing of a liquid or partially liquid phase. It
has to be noted that the reason for the increased severity of material transfer, going from 4 min to 20 min soaking time, is not clear
from the conducted experiments. The analysis of the microstructure and the measured properties (hardness) after the tests did not
yield any conclusive evidence to explain this behaviour. Therefore
this needs to be investigated further.
In a study by Borsetto et al. (2009), they observed low friction in a
pin-on-disc conguration at 700 C and a holding time of 3 min. The
low friction they observed may be attributed to the low hardness
of the coating at this temperature and the low shearing stresses
needed to plastically deform it.
In the present work, at 900 C, the phases with high hardness
(FeAl2 /Fe2 Al5 ) were formed after relatively short soaking time. The
observations suggest that these phases reduce adhesion during
interaction with the tool steel. Only mild galling was observed
when these phases (FeAl2 /Fe2 Al5 ) had reached the surface contrary to the severe galling observed when Fe2 Al78 Si phase was

Fig. 9. Evolution of the coefcient of friction from tests at 900 C with and without
grinding.

at the surface. This was linked to the low mechanical properties


of this phase at the testing temperatures, as it is near its melting
point (855 C). The high hardness that the coating develops once
FeAl2 /Fe2 Al5 are formed all the way to the surface, causes rapid
wear of the counter tool steel specimen, mainly through abrasive
wear, whilst the surface of the Al-Si coating is protected by an oxide
layer. The occurrence of this phenomenon has been reported by the
authors elsewhere (Pelcastre et al., 2013). The coefcient of friction initially increases but then stabilises once the glaze layers are
formed.
If the equilibrium diagrams of the Fe-Al-Si system are considered for the composition of the as-delivered Al-Si coating, for all
the temperatures used in this study, a liquid phase exists together
with a solid phase. In the forming operation as well as in the tribological tests carried out at 900 C in the present work, diffusion
of the constituents of the coating and the substrate is activated.
Thus, the chemical composition of the system changes locally as the
atoms move within the coating. This is the reason for the resulting
multi-layered structure of the coating. With the change in chemical

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.

composition, the position of the alloy in the equilibrium diagram


shifts and this allows the existence of different phases and causes
solidication of the coating.
It is clear that the friction and galling behaviour are inuenced
by the phases in the Al-Si coating as they have different properties, both physical and mechanical. Providing the system with
enough activation energy to allow diffusion is an important parameter to consider for reduction of galling. Enough diffusion is needed
in order to form the harder phases (FeAl2 /Fe2 Al5 ), which have
promoted reduced material transfer and also the most stable coefcient of friction.
As mentioned before, the increased material transfer observed
in some of the tests can be explained by the presence of melted
Al-Si coating or extremely soft phases when the tribological tests
start. In Fig. 7, cross sections of the wear scar of the Al-Si coating
after tribological tests are shown. When the test temperature was
700 C and 900 C and 0 min soaking time was used, the steel substrate and the coating underwent wear. A non-uniform tribolayer
of mixed oxidised wear debris was also observed and also a considerable amount of the Al-Si coating had been detached (Fig. 7(a)
and (b)). When the exposure time increased, the coating continued
transforming and in consequence no wear on the steel substrate
was observed. Furthermore, a protective glaze layer was formed
on top of the Al-Si coating, thus minimising the wear of the coating
itself (Fig. 7(c)).
3.3. Inuence of Al-Si coating surface roughness on frictional
behaviour and galling
As described in Section 2.4, the specimens were pre-heated to
allow the development of the hard intermetallics (900 C and 4 min
soaking time) and subsequently quenched and ground with abrasive paper. Once the surfaces were prepared, the specimens were
heated up once more and the tribological tests were performed.
This procedure had no major inuence on the frictional behaviour
compared to a test where the specimen does not undergo cooling before the tribological test. In Fig. 8, the coefcient of friction
for a specimen that had undergone heating, quenching and reheating before the tribological test is compared to one that had not
undergone an intermediate quenching. The level of the coefcient
of friction as well as the overall behaviour did not show signicant
differences. This is in agreement with the observations from the
previous section; once only FeAl2 /Fe2 Al5 and Fe2 Al2 Si are in the
coating, the structure or the existing phases of the coating do not
change unless the soaking time is signicantly long.
3.3.1. Morphological changes of the coating and its surface
Grinding the Al-Si coated UHSS after a heat treatment did not
have a considerable effect on the friction behaviour. In Fig. 9, the
coefcient of friction is shown for the specimens with and without

grinding. The friction levels as well as the stability of the coefcient


of friction were similar in both tests.
The observations from the tests suggest that the surface topography of the work-piece material is not as signicant for the
tribological performance when sliding against tool steels. Similar
behaviour was observed by Azushima et al. (2012). However, in
those studies, the tool steel was the one that was tested with different surface roughness levels. An explanation for this behaviour is
that the formation of tribo-layers (either adhered material or protective oxide layers), on either of the contacting surfaces, control
the friction behaviour and not the initial surface topography of the
test specimens. It was observed in previous studies by the authors
(Pelcastre et al., 2013), that glaze layers or protective oxide layers are formed on the surface of the Al-Si coated steels. Formation
of such layers prevents wear of the Al-Si coating and avoids prolonged direct contact between the two specimens. Furthermore,
these oxide layers also allow the occurrence of a stable, although
high, friction coefcient.
Fig. 10 shows the oxide layers formed on the ground and asdelivered Al-Si coated specimens. Clear differences between the
two types of layers formed were observed. In the case of the ground
specimen, a more continuous oxide layer was developed on top of
the plateaus formed during grinding (Fig. 2(c)). On the other hand,
the as-delivered specimen showed small patches of agglomerated
oxides randomly distributed over the wear scar.
The observations suggest that the nodules on the as-delivered
surface prevent the formation of a continuous oxide layer. It is possible that the more irregular surface of the Al-Si coating does not
allow the oxidised debris to accumulate and form a large and continuous oxide layer. However, the formation of either type of layer
protects against galling as in both cases direct contact between the
Al-Si coating and the tool steel specimen is prevented.
4. Conclusions
The evolution of the microstructure and the surface of the Al-Si
coating under different heating conditions was analysed and the tribological performance was correlated to the existing phases in the
coating. From the results, the main conclusions can be summarised
as follows:
- With enough activation energy and holding time, the Al-Si coating
reduces the number of existing phases (layers) in its structure.
- The phases at the surface of the Al-Si coating signicantly affect
the tribological response during the interaction with tool steel.
Galling is reduced when the Fe5 Al2 and FeAl2 phases are present
at the surface.
- The tribological behaviour of the coating does not change upon
cooling and reheating once the stable Fe5 Al2 and FeAl2 phases are
formed.

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

G Model
PROTEC-14326; No. of Pages 8

ARTICLE IN PRESS
L. Pelcastre et al. / Journal of Materials Processing Technology xxx (2015) xxxxxx

- Surface roughness of the Al-Si coating has a minor impact on the


galling behaviour when it interacts with uncoated tool steels.
Acknowledgements
This work has been carried out with nancial support from the
Centre for High Performance Steel at Lule University of Technology
and the authors gratefully acknowledge their support. The authors
would also like to thank Gestamp HardTech for providing test specimens for these studies and also thank them for their active interest
in this work.
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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

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