Metals and Materials International

https://doi.org/10.1007/s12540-023-01394-x

Effect of α‑Al and Si Precipitates on Microstructural Evaluation

and Corrosion Behavior of Laser Powder Bed Fusion Printed AlSi10Mg
Plates in Seawater Environment
Periyakaruppan Murugesan1,2 · V. Satheeshkumar1 · N. Jeyaprakash3 · Che‑Hua Yang4 ·
Sundara Subramanian Karuppasamy4

Received: 13 October 2022 / Accepted: 10 January 2023

© The Author(s) under exclusive licence to The Korean Institute of Metals and Materials 2023

Abstract
AlSi10Mg is a hypoeutectic alloy that has remarkable characteristics and implemented in diverse areas. Most of the
AlSi10Mg parts are fabricated via traditional processes. The AlSi10Mg parts made by these processes have coarser
microstructure, reduced mechanical behaviors, and minimum lifespan. This study is aimed at manufacturing the AlSi10Mg
parts by Laser Powder Bed Fusion (LPBF) process followed by analyzing their mechanical properties. The microstructure
evolution was examined from the micrographs of Optical Microscope (OM), Field Emission Scanning Electron Microscope
(FESEM), Electron Backscatter Diffraction (EBSD), and Transmission Electron Microscope (TEM). Tafel, Nyquist, Bode
and surface plots were used to determine the corrosion resistance and surface roughness at different intervals. FESEM
micrographs revealed the existence of bimodal equiaxed α-Al grains containing Si phase as their grain boundaries. After
solidification, the secondary precipitates (­ Mg2Si) were segregated in the printed sample which accounts for enhancing the
mechanical characteristics. More grain growth and textures were noticed along the building direction of the sample and
this direction exhibits higher hardness compared with the scanning direction. Further, TEM analysis confirmed that the
formed microstructure is rich in equiaxed α-Al with Si eutectics. Corroded X-ray Diffraction (XRD) plot showed that the
maximum intensity of M ­ gAl2O4 is observed at 25 h immersion test sample. Among the various samples, 25 h LPBF sample
provides significant resistance toward corrosion based on the values of current density, polarization resistance and average
surface roughness. This is due to the formation of stable passive film on its surface thereby providing better anti-corrosion
characteristics.

Keywords LPBF · AlSi10Mg · EBSD · TEM · Corrosion · Surface roughness

1 Introduction suitable for applications that operate in both cryogenic

and elevated temperature conditions. This alloy consists
Aluminum alloys belong to the category of emerging alloys of a significant percentage of aluminum which makes it a
that have been used in a wide range of sectors. These alloys lightweight alloy and has a major contribution to the avia-
are well known for their potential characteristics and more tion, electronics and automobile sectors [1–3]. Besides its

* N. Jeyaprakash 1
Department of Production Engineering, National Institute
prakash84gct@gmail.com
of Technology, Tiruchirappalli 620015, Tamil Nadu, India
Periyakaruppan Murugesan 2
Ordnance Factory, Tiruchirappalli 620016, Tamil Nadu, India
periyakaruppanm@ord.gov.in
3
School of Mechatronic Engineering, China University
V. Satheeshkumar
of Mining and Technology, Xuzhou 221116, China
satheeshv@nitt.edu
4
Graduate Institute of Manufacturing Technology, National
Che‑Hua Yang
Taipei University of Technology, Taipei 10608, Taiwan
chyang@ntut.edu.tw
Sundara Subramanian Karuppasamy
diwahar3@gmail.com

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lightweight, the combination of its alloying elements makes
it exhibit several properties such as high strength, better duc-
tility in lower temperatures, thermally stable, good electri-
cal conductivity, resilient, corrosion resistance and a high
strength-to-weight ratio [4, 5]. In automotive applications,
these alloys provide better advantages when compared to
steel in terms of density, thermal conductivity and crash
energy absorption [6]. These predominant characteristics
made this alloy as the first priority for fabricating parts of
heat exchangers, manifolds, cylinder heads, radiator cores,
chassis castings, chemical equipment, forgings and the food
industry [6–8].
Based on the composition of alloying elements, alu-
minum alloys are classified into two major categories as cast
and wrought aluminum alloys. Cast aluminum alloys have
nearly 10%–12% of alloying elements whereas the wrought
aluminum alloys contain 1%–2% of alloying elements [9].
Among the cast aluminum alloys, the AlSi10Mg cast alloy
is majorly employed in the aviation and automotive indus-
tries. This hypoeutectic alloy has good mechanical proper-
ties including better hardness, greater toughness and higher
strength which paved the way for aerospace and nuclear
applications [10, 11]. Most of the AlSi10Mg parts used in
applications are manufactured via traditional manufactur-
ing practices like powder metallurgy, forging, casting and
extrusion process [12]. These conventional manufacturing
practices encounter several drawbacks. In casted AlSi10Mg
parts, the cooling rate has a significant influence on the
mechanical properties of the parts. The low cooling rate is
responsible for coarser microstructure and also the exist-
ence of defects like shrinkage, slags, offsets and elemen-
tal segregation has been reported in the casted AlSi10Mg
parts. These coarser microstructures and defects affect the
mechanical properties offered by the casted parts [13]. In
the case of the high-performance Al alloys, the forming and
production of these alloys are a separate process that tends
to long process chain which consumes more time. Moreover,
the structural requirements of Al alloys have been changing
due to industrial developments and the fabrication of com-
plex and tiny AlSi10Mg parts is more challenging by means
of traditional manufacturing practices [14, 15]. Hence, time
consumption, defects, coarser microstructure, fabricating
tiny and complex shapes are considered to be the major
drawbacks of conventional manufacturing methods.
To overcome the drawbacks of conventional methods,
advanced manufacturing practices are currently employed
for making components with high accuracy. Metal Additive
Manufacturing (MAM) is one of the advanced techniques
that fabricate parts/components in a layer-by-layer fashion.
Complex parts have been built with greater dimensional
accuracy and the additive manufactured parts provide better
mechanical properties compared with the parts made by
the traditional methods [16, 17]. MAM creates parts using
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these techniques. Among them, the powder bed fusion
technique holds good for manufacturing a wide range of
components and applies to a vast range of materials [18,
19]. This fusion technique uses a high-energy power source
to melt the powders as per the prescribed CAD model of the
components. Based on the power source, the powder bed
fusion technique is classified into two categories. The high-
energy laser serves as the power source for the first category
(Laser Powder Bed Fusion, Selective Laser Sintering, Direct
Metal Laser Sintering) whereas the second category uses an
electron beam to build the components [20]. Laser Powder
Bed Fusion (LPBF) is a widely used MAM technique since
it is economic, holds good for complex shapes and applies
to a wide range of alloy powders. This fast technique can
produce high-precision parts where dimensional accuracy is
concerned. Moreover, the LPBF printed parts have a better
microstructure and offer excellent mechanical properties
than the parts made via conventional methods [21].
Particularly for AlSi10Mg alloy, the LPBF process is best
suited since it eliminates the post-processing techniques used
for improving the surface finish whereas these techniques
are unavoidable in the casting process to accomplish better
surface in components. The rapid heating and cooling rate
in the LPBF process is responsible for achieving better
microstructure and mechanical characteristics than the
casted AlSi10Mg parts [22]. Brandl et al. [23] examined the
fatigue and fracture behavior of the LPBF printed AlSi10Mg
parts. They reported that the fatigue limit and the tensile
strength had a correlation between them which enhanced the
characteristics of the alloy. Beretta et al. [24] assessed the
fatigue strength of AlSi10Mg alloy in various orientations.
They said that among the horizontal, vertical and diagonal
orientations, the specimens made by horizontal orientation
exhibit higher fatigue strength compared to the other
orientations. Zyguła et al. [25] compared the microstructure
of cast and LPBF printed AlSi10Mg parts. The LPBF
printed parts consist of better microstructure whereas the
casted parts contain coarser microstructure. Roth et al.
[26] examined the material properties of the as-cast and
LPBF printed AlSi10Mg specimens and reported that the
LPBF printed specimens exhibit better material properties
due to the obtained microstructure. Moreover, the additive
manufactured AlSi10Mg is reported to provide better
tribological properties [27]. These literatures reported that
the LPBF printed AlSi10Mg alloy exhibits better mechanical
characteristics when compared with the AlSi10Mg parts
made via traditional manufacturing practices. But however,
the microstructural evolution along with the corrosion
resistance behavior of the LPBF AlSi10Mg alloy at
different time intervals are yet to be addressed. This work
is attempted to investigate the anti-corrosion behavior of
the LPBF fabricated AlSi10Mg specimens at various time
intervals followed by investigating the microstructural
Metals and Materials International
evolution. The as-printed AlSi10Mg microstructure and
grain textures were evaluated by means of micrographs
captured by the OM, FESEM, EBSD and TEM analysis. The
microhardness of the samples fabricated in both building and
scanning directions was examined with the aid of Vickers
microhardness test. The anti-corrosion property offered by
the additive manufactured samples was investigated in terms
of polarization and impedance plots in different durations.
Moreover, the corroded morphology was analyzed using the
XRD, FESEM along with surface roughness measurement.
2 Materials and Methods
2.1 Materials
The gas atomized AlSi10Mg powder serves as the feedstock
for the powder bed used in the LPBF process. This alloy
powder has been bought from the market and the as-received
alloy powder particles were investigated using the SEM
microscope (Fig. 1a) for measuring the particle size. The
average particle size of the powder used in this process was
reported as 33.33 ± 10 μm. With the aid of EDS analysis,
the elemental composition of the elements present in the
as-received alloy powder was represented in Fig. 1b.
2.2 LPBF Process
LPBF technique serves as a unique way of fabricating
parts. It minimizes the waste and is economic among the
powder bed fusion techniques. The rapid cooling rate
followed by the solidification of the printed parts makes
this technique different from other 3D printing processes.
By optimizing the printing parameters, the parts can be
Fig. 1  FESEM image and EDS plot of as-received AlSi10Mg powder
printed in a reliable manner. Figure 2a shows the LPBF
process for printing the parts whereas the image of the
manufactured parts is represented in Fig. 2b. The LPBF
process involves a step-by-step procedure to fabricate the
components [28, 29]. These steps are detailed as below:
(i) Model slicing The parts to be fabricated are designed
using the CAD software. The CAD model of the part
is sliced so that every slice represents each layer in
the LPBF part.
(ii) Loading It involves importing the sliced 3D model
into the LPBF hardware (equipment) for starting the
printing process.
(iii) Printing Here, the high-energy laser beam is used to
melt the AlSi10Mg particles and the melted particles
are deposited according to the 3D model of the parts
to be made.
(iv) Unloading After printing, the LPBF parts were col-
lected to carry out further characterizations.
The process parameters such as the scanning (laser
travel) speed, laser power and hatch spacing will determine
the microstructure evolution in the LPBF parts. The laser
power will decide the surface finish and porosity levels.
Lower laser power results in higher porosity levels fol-
lowed by the poor surface finish. Also, it will pave the way
for uneven melting of the powder particles which could
minimize the mechanical characteristics. By increasing
the laser power with a simultaneous decrease in the laser
travel speed and hatch spacing will result in lower porosity
levels and better surface finish in the LPBF parts. Thus,
by following these steps, the LPBF AlSi10Mg parts were
fabricated by the trial and error method in the industry
and the microstructure was examined [30, 31]. The LPBF
parts having better surface finish and lower porosity levels
were preferred to carry out further characterizations and
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Fig. 2  (a) Schematic illustration

of LPBF process, and (b) LPBF
printed AlSi10Mg parts

Table 1  LPBF printing parameters Finally, the printed parts have been removed from the base
Parameter Values
plate to carry out further investigations.

Powder particle size 33 ± 10 µm 2.3 Characterization

Layer thickness 50 μm
Power 350 W The printed parts undergo an etching process for inves-
Laser beam spot size 150 μm tigating the microstructures present in it. Swab type of
Laser travel speed 1400 mm/s chemical etching was carried out with the aid of Keller’s
Printing bed temperature 150 °C reagent containing 1 ml HF, 1.5 ml HCl, 2.5 ml ­HNO3 and
Build orientation Z direction 95 ml ­H 2O. The optical and FESEM micrographs were
captured for examining the microstructures followed by
the hardness investigation in both scanning and building
the optimized process parameters were listed in Table 1. directions using the Vickers microhardness test (Wolp-
ert Wilson 402 MVD instrument). The texture formations
and orientation of grains in the LPBF printed A ­ lSi10Mg
samples were evaluated with the help of EBSD (pole and

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inverse pole figures) and TEM analysis. Moreover, the cor-
roded morphology after the corrosion test was evaluated
with the help of FESEM images.
2.4 Corrosion Analysis by 3.5% NaCl
The anti-corrosion behavior of the additive manufactured
AlSi10Mg samples at different time intervals has been
evaluated with the aid of Tafel, Nyquist and Bode plots.
The setup used for this analysis contains thee electrodes
immersed in the electrolyte solution. Here, the NaCl
crystals weighing about 3.5 g are dissolved in 96.5 ml of
deionized water which serves as the electrolyte for the test
process. This composition is same as the concentration of
Cl ions in the sea and this concentration is good enough to
provide rigorous corrosion attacks on the materials [32].
The thee-electrode setup is controlled by the software pro-
vided by Autolab Metrohm and among those electrodes,
the test sample represents the working electrode which
is sealed perfectly excluding the test surface to avert
electrolyte leakage to other surfaces. The counter elec-
trode is made by using silver chloride whereas platinum
serves as the reference electrode. First, the polarization
curves were plotted for the samples followed by Nyquist
and bode plots. The corrosion resistance offered by the
samples at various intervals was investigated by means
of current density and polarization resistance values. The
corroded morphology of the samples and the phases that
contributed to the resistance were analyzed with the help
Fig. 3  Optical micrographs of
(a) LPBF printed AlSi10Mg
sample, (b) Magnified view of
(a) representing the melt pool
boundaries, (c) FESEM image
of LPBF printed ALSi10Mg
sample containing secondary
precipitates (white spots-encir-
cled) and (d) EDS area map of
the printed sample
of SEM images with the corresponding EDS and X-ray
diffraction (XRD) (D/MAX/2200/PC Ultima IV, Regaku,
Japan) phase analysis. Furthermore, the average surface
roughness (Ra) values of the samples after the corrosion
test were measured using the OLS5000 laser microscope.
3 Results and Discussion
3.1 OM and FESEM Analysis
The as-fabricated LPBF AlSi10Mg samples undergo micro-
structural analysis to evaluate the microstructures present
in those samples. After etching with Keller’s reagent, the
microstructure was analyzed based on the images captured
from the optical and FESEM microscopes. Figure 3a and
b represent the optical microscopic images of the LPBF
printed AlSi10Mg samples at different magnifications.
From Fig. 3a it can be inferred that the printed sample con-
sists of a hierarchical microstructure in it. This is due to the
overlapping of melt pools during the LPBF process. These
overlapped pools are formed as a result of continuous raster-
ing of the laser that melts the AlSi10Mg powder particles
followed by the solidification effect which tends to the suc-
cessive layer formation along the building direction [33, 34].
On magnification (Fig. 3b), the fine dendritic structure can
be observed on the inner side of the melt pool boundary.
Also, these melt pool boundaries consist of a coarser micro-
structure. This is due to the fractional re-melting effect of
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the already deposited layer during the formation of the top

layer followed by the overlapping of the pools [35]. Hence,
the boundaries were rich in coarser microstructure whereas
fine dendrites were formed after the solidification of the melt
pool.
Figure 3c shows the FESEM image of the as-printed
AlSi10Mg sample at a magnification of 1 µm. From this
figure, it can be seen that the melt pool was rich in fine den-
dritic structure. This dendritic morphology formation is due
to the subsequent solidification effect and this fine structure
will pave the way for this alloy to exhibit better mechanical
properties [36]. Moreover, the formed dendritic morphol-
ogy was enriched with the bimodal equiaxed grains which
are larger and finer. This equiaxed grain formation is due to
the consistent heating and cooling rate of the molten melt
pool during the LPBF process [37]. The equiaxed grains are
made up of α-Al phase decorated with eutectic Si phase as
their grain boundary. This Si phase will lead to the formation
of a network-like structure throughout the printed surface
[38, 39]. Thus, finer equiaxed grains were formed during
the solidification of the melt pool whereas larger equiaxed
grains were seen near the melt pool boundaries which might Fig. 4  Schematic illustration of microstructure evolution during the
be due to the transition effect of coarser to equiaxed grains. LPBF process, (a) Molten melt pool of AlSi10Mg powder, (b) For-
After solidification, the secondary precipitates were segre- mation of α-Al grains, (c) Equiaxed α-Al grains decorated with Si
(red color) particles as grain boundaries, and (d) Secondary precipi-
gated and randomly distributed in the formed microstruc- tates ­(Mg2Si-orange color) formed in the end of solidification
ture. These precipitates were represented as white spots in
Fig. 3c. These are reported to be made of ­Mg2Si precipi-
tates and aid in enhancing the mechanical characteristics dwell time of 15 s according to the ASTM E92-17 standards
like hardness [40, 41]. Moreover, the EDS area scan has [42, 43]. Ten indentations were made in both the building
been performed on the LPBF printed sample to evaluate the and scanning direction to analyze the hardness behavior.
elements present in it. The obtained EDS scanned image is The average hardness value obtained from these profiles was
represented in Fig. 3d. It can be observed that the elemental calculated in both directions and plotted in Fig. 5b. From
peak obtained for the Al element tends to be higher than the this figure, it can be confirmed that the indentation peaks
peaks of Si, Mg, Fe and other elements. This high peak of obtained in the building direction seem to be higher than the
Al confirms that the formed microstructure is rich in the Al peaks of scanning direction indentation. The average hard-
matrix. The microstructure evolution that happens during the ness value obtained in the building direction (151.94 HV)
LPBF process is schematically illustrated in Fig. 4. This fig- is higher than that of the scanning direction value (145.94
ure describes the process of equiaxed grains formation along HV). After successive heating and cooling rate, the succes-
with the secondary precipitates from the molten melt pool sive layer formation may result in obtaining a higher average
of ­AlSi10Mg powders. Thus, the OM and SEM micrographs hardness value along the building direction. This succes-
of the LPBF printed A ­ lSi10Mg sample contains equiaxed sive layer has overlapped pools where the grain boundaries
dendrites decorated with Si precipitates along their grain were intermixed during the LPBF process. The changes in
boundaries in the Al matrix. the average microhardness value in both directions tell us
the existence of anisotropic behavior in the LPBF printed
3.2 Hardness Evaluation AlSi10Mg samples. Also, higher hardness along the build-
ing direction was reported by a few literatures. Ponnusamy
The hardness offered by the LPBF printed A­ lSi10Mg samples et al. [44] compared the hardness of LPBF printed AlSi12
in both building and scanning orientations was examined by alloy in both directions and reported that the vertical (build-
the Vickers microhardness analysis. Figure 5a represents the ing) direction has the highest hardness than the horizontal
indentation profile made along the building and scanning (scanning) direction. They concluded that a higher level of
directions whereas the inset image represents the magni- porosity has been observed in the horizontal direction which
fied view of indentation. These indentation profiles in both results in reduced hardness.
directions were made by applying the load of 0.3 kgf with a

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Fig. 5  (a) Indentation profile, and (b) Profile graph in both scanning and building direction
On the other hand, the hardness along the building direc-
tion tends to increase since this direction has a lower poros-
ity level and minimum strain rate. In addition, better grain
orientation and formation are reported in the building direc-
tion of the LPBF printed Ti–6Al–4 V alloy [45]. Here, the
building direction has better grain formation with fewer
pores and low residual stress which accounts for higher
hardness than the scanning direction. The same anisotropic
behavior was reported in the other type of materials fabri-
cated via additive manufacturing. The orientation of grains,
residual stress developed during fabrication, heat transfer,
and crystallographic textures were identified as the major
factors which effects in such anisotropic behavior in the
LPBF samples [46, 47]. These factors will result in changes
in the average microhardness value of both building and
scanning directions during the LPBF printing process [48,
49].
3.3 EBSD Analysis
Apart from the optical and FESEM micrographs, the EBSD
and TEM analyses were performed on the LPBF printed
­AlSi10Mg samples for a better understanding of the crystal-
lographic orientations present in the samples. Figure 6a–f
represents the EBSD, pole and inverse pole images captured
on the LPBF printed sample. The image quality (IQ) map
and its corresponding EBSD image was shown in Fig. 6a
and b. From this figure, it can be inferred that the micro-
structure of the as-printed AlSi10Mg is bimodal that con-
tains a combination of larger and finer equiaxed grains [50].
Larger equiaxed grains were formed near the melt pool
boundaries whereas finer equiaxed grains were noticed in
the melt pool. The color-coded standard triangle map was
shown as an inset in Fig. 6b. Here, the grains normal to
the plane < 001 > are red, < 010 > are blue, < 101 > are green
and the grains belonging to the intermediate orientations are
represented in the intermediate colors respectively. The suc-
cessive overlapping of layers paved the way for larger grains
near the pool boundaries. The α-Al bimodal equiaxed grains
surrounded Si eutectics as their boundaries which forms a
network-like structure. The optimized printing parameters,
heating and cooling rate have resulted in obtaining the
bimodal microstructure in the sample. The average grain
size was found to be 11 ± 6 μm respectively. Thus, the image
quality and EBSD maps confirmed the existence of bimodal
equiaxed grains in the LPBF printed ­AlSi10Mg sample.
Moreover, the orientation of grains in the additive man-
ufactured sample was analyzed by means of the pole and
inverse pole figures of α-Al and Si are shown in Fig. 6c–f
since the growth of grains is along the building direction
[51]. From the inverse pole figures of α-Al and Si (Fig. 6c
and d), it can be observed that the maximum intensity
obtained for the α-Al (16.67 MUD) phase whereas the Si
eutectic phase has the intensity of 2.57 MUD. The α-Al is
reported to be more intense in the z-direction. The decreas-
ing trend is observed in the intensity of formed α-Al in the
x and y-direction. The eutectic Si is intense in all direc-
tions but it is more dominant in the z-direction than in the
other direction. Hence, both the α-Al and Si grains tend to
be more intense in the z-direction which tends to be the
building direction. In the z-direction, the < 210 > plane
contains more α-Al grains textures than the other two
planes. The minimum textures of α-Al grains were reported
in < 120 > and < 001 > planes. On the other hand, the Si
grains are grown predominantly in the < 111 > plane on
the z-axis than in < 101 > and < 001 > planes. Also, the
Z-direction of α-Al and Si contains sufficient textures com-
pared to the other axes respectively. Thus, Fig. 6c and d
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Fig. 6  (a) Image quality (IQ) map, (b) EBSD image, Inverse pole figures of (c) α-Al (d) Si, Pole figures of (e) α-Al and (f) Si
confirmed that the z-direction has more grain growth
because of the grain textures and intensity in all the planes
than the x and y-direction. Further, the pole figures of α-Al
and Si are shown in Fig. 6e and f. The α-Al grain texture
is stronger in the < 1120 > plane (63.36 MUD) whereas
the other two planes < 0001 > and < 1010 > have weak
textures of α-Al grains. On the other hand, all the planes
(< 100 > , < 110 > and < 111 >) have a sufficient texture for
the Si grains. In particular, the < 111 > plane has a more
intense texture with a maximum intensity of 9.15 MUD.
Thus, the pole and inverse pole figures confirmed that the
grain growth and its textures are dominant in the building
direction of the LPBF printed AlSi10Mg.
3.4 TEM Analysis
Further, the TEM and EDS analyses were performed for
a depth understanding of the microstructure evolution and
elemental distribution in the as-fabricated LPBF AlSi10Mg
sample. The bright-field TEM image at 200 nm resolution is
shown in Fig. 7a. From this image, the formed α-Al grains
(primary Al), their eutectic boundaries, Si element and
their precipitate can be clearly visualized. Also, it is evident
that the microstructure formed after solidification contains
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equiaxed α-Al grains. The grain boundaries of these equi-
axed grains are decorated with eutectic Ai particles that form
a network-like structure. After solidification, the segregation
of ­Mg2Si precipitates (block spots) can be noticed on these
grains. The Al eutectic phase with Si elements contributed
to network-like morphology in the obtained microstructure.
Thus, from the bright field image, it is confirmed that the
LPBF printed sample exhibits equiaxed grains with Si eutec-
tics as their grain boundaries. The obtained SAED pattern
of α-Al and Si elements are shown in Fig. 7b and c which
consists of larger and tiny bright spots [52, 53]. By combin-
ing the TEM and SAED patterns, the microstructure present
in the as-printed LPBF AlSi10Mg sample can be concluded
as equiaxed Al/Si eutectics. Figure 7c shows the H-TEM
image and the corresponding FFT (inset) image at the Si
element. Crystal, amorphous structures and eutectics Si are
observed in this Fig. 7c. The lattice constant of Al starts to
decrease due to the dissolution effect of Si in the Al matrix.
This results in obtaining the solid solution of α-Al due to the
formation of Si eutectics [54]. The elemental composition of
the sample is determined by the EDS plot with color maps
as in Fig. 7d and e. From the point maps, the peak obtained
for the Al element is higher than the Si and Mg elements
which shows that the formed structure is rich in α-Al solid
Metals and Materials International
Fig. 7  (a) Bright field TEM
image representing α-Al grains
having Si as grains boundaries
with secondary precipitates
(encircled in yellow), (b) SAED
diffraction pattern containing
Al (encircled in yellow) and Si
(encircled in red), (c) HR-TEM
image, (d, e) EDS plot with
color maps
solution. Moreover, the EDS area color maps also proved
that the concentration of Al is much greater than the con-
centration of Si and Mg elements. Thus, from both maps,
Al has a higher concentration in terms of maximum peak
(point scan) and larger distribution (area scan) than the Si
and Mg elements. There is a decreasing trend (both point
and area scan) is observed in the element concentration of
Si and Mg elements which shows that the formed structure
is rich in the Al matrix.
3.5 Corrosion Plots
By using the electrolytic solution containing 3.5%wt of NaCl
crystals in 96.5 ml of DI water, the corrosion behavior of
the as-fabricated AlSi10Mg samples was examined in the
electrochemical environment at 0, 10, 25 and 66 h respec-
tively. The results were plotted as potentiodynamic polariza-
tion curves (Tafel plots) and the parameters such as current
density and electrode potential values were measured for
the samples and compared for a better understanding of the
corrosion resistance behavior. When the AlSi10Mg alloy is
exposed to corrosive media, it develops a strong and stable
passive film on its surface. This passive film is reported to be
enriched in the oxides of aluminum and silicon. These oxides
are called as native oxides which are inherently formed on
the surface during corrosion [55]. Thus, the formed oxide
film on the AlSi10Mg sample’s surface is reported to exhibit
better resistance against corrosion. The net balance chemical
reaction that takes place during the oxide film formation is
given in Eqs. (1) and (2).
4Al(s) + 6O(g) → 2Al2 O3(s) (1)
Si(s) + O2(g) → SiO2(s) (2)
During the corrosion test, the Tafel graph was plotted
for 0, 10, 25 and 66 h samples as shown in Fig. 8. It can
be observed that the oxide film formed on the surface of
all samples is continuous which resists corrosion. Also, the
current density (I, A/cm2) and potential (V) values were
calculated and listed in Table 2. The sample which has a
minimum current density value is said to provide maximum
corrosion resistance [56, 57]. On comparing the obtained
current density values of various samples, the current den-
sity value increases (0 h sample—1.51090842 × ­10–6 A/
cm2), then decreases (10 h sample—1.4143730 × ­10–6 A/
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Fig. 8  Tafel plot of LPBF AlSi10Mg samples at different intervals
Table 2  Corrosion analysis data
Duration (h) E-current (V) I-current (A/cm2)
0 −0.62188738 1.51090842 × ­10–6
10 −0.524235993 1.4143730 × ­10–6
25 −0.624462366 5.99514287 × ­10–7
66 −0.606734578 1.93726048 × ­10–6
cm2), further decreases (25 h sample—5.99514287 × ­10–7
A/cm2) and finally attained the maximum value (66 h sam-
ple—1.93726048 × ­10–6 A/cm2). The initial increase in the
current density value of the as-printed (0 h) sample is might
be due to the presence of surface irregularities which acts as
the interfacial sites [58]. These irregularities will tend to the
pores formation that will result in the reduction of corrosion
resistance. As time increases (10 and 25 h samples), there
will be a continuity in the formation of the oxide film which
corresponds to a decrease in their current density values.
After attaining a stable oxide film, at the higher interval
(66 h sample) the stable oxide film starts to rupture (fragile
patches) since it can’t withstand the potential range for a
longer time duration. Hence the current density value of the
66 h sample is the maximum among the other samples due to
the rupturing of the film into patches. Hence, among the dif-
ferent interval samples, the 25 h AlSi10Mg sample exhibits
maximum corrosion resistance due to the strong oxide film
formed on its surface with a lower current density value.
In addition, the FESEM micrographs and the EDS maps
were captured at the passive layer to analyze the film forma-
tion and elements present in it. Figure 9a, c, e and g repre-
sents the FESEM image taken at the formed layer after the
corrosion test. It can be inferred that the micrograph of 0
and 10 h LPBF (Fig. 9a and c) samples contain fewer pores
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Metals and Materials International
and the formed oxide film is not continuous. This might be
due to the effect of surface irregularities caused by the melt
pool boundaries. Moreover, the greater potential difference
between the Al and Si phase could be a reason for the forma-
tion of pits in these samples [59, 60]. On the other hand, a
compact oxide film formation is noticed on the 25 h LPBF
sample (Fig. 9e). This might be due to the presence of stable
oxide phases that could result in the continuous and com-
pact passive film on it. As discussed earlier, after attaining
the stableness, the formed film starts to rupture in the case
of the 66 h sample (Fig. 9g) thereby minimizing its corro-
sion resistance behavior. Hence, except the 25 h sample,
the other films contain more pits and fragile patches which
reduce the corrosion resistance behavior in those samples.
The fine equiaxed grain formation has resulted in continu-
ous passive film formation that resists corrosion to a greater
extent. Moreover, the EDS point and area maps at differ-
ent intervals are shown in Fig. 9b, d, f and h and the cor-
responding weight distribution of elements present at the
oxide layer is tabulated in Table 3. Both the point and area
maps of the 25 h LPBF AlSi10Mg sample revealed that it
has higher oxide content compared to the other samples.
This higher oxide content paved the way for the formation of
stable passive film on its surface which provides significant
anti-corrosion characteristics. The oxide film formed on the
LPBF AlSi10Mg sample is schematically depicted in Fig. 10
where the Al and Si ions react with the oxygen to form the
oxide film which is rich in their oxides and resists corrosion.
3.6 EIS Plots
To further evaluate the anti-corrosion behavior in terms
of the polarization resistance value, the EIS analysis was
performed on the LPBF AlSi10Mg samples at 0, 10, 25
and 66 h intervals. Both the Nyquist and bode plots were
obtained from the EIS analysis for investigating the charge
transfer resistance offered by the passive film formed on the
samples. It is found that the charge transfer reaction (elec-
trochemical reaction) is stronger than the electrode reaction.
Figure 11a represents the Nyquist plots for 0, 10, 25 and 66 h
samples respectively. These plots will decide the corrosion
resistance offered by means of semicircular arc radius. For
all samples, a single semicircular loop is obtained which
shows the continuity in the film formation. The AlSi10Mg
sample which has a higher arc radius is said to provide maxi-
mum resistance [61]. On comparing the semi-circular arc
radius of the different interval samples, the arc radius ini-
tially decreases (0 h sample), then increases (10 h sample),
reaches the maxima (25 h sample) and finally decreases to a
greater extent (66 h sample). The initial decrease in the arc
radius (0 h sample) is might be due to the effect of cavity for-
mation and unevenness in the formed filmed [62]. The 10 h
sample’s arc radius is somewhat better than the 0 h sample.
Metals and Materials International

Fig. 9  FESEM image and EDS point, area maps of LPBF AlSi10Mg sample at (a, b) 0 h, (c, d) 10 h, (e, f) 25 h and (g, h) 66 h respectively. Pits
are encircled in yellow color

13

Maximum arc radius is obtained for 25 h sample. This could
be due to the effect of continuous film formation on it and
the larger semi-circular arc radius indicates the slower kinet-
ics behind the corrosion process [63]. Also, the maximum
arc radius shows the greater electrochemical stability of the
25 h LPBF sample [64]. And, the arc radius decreases fur-
ther for the 66 h LPBF sample since the formed film on this
sample could not withstand the potential and starts to rupture
at higher intervals (66 h). Hence among the different time
periods, the 25 h LPBF AlSi10Mg sample has the maximum
arc radius and provides significant corrosion resistance when
compared with 10, 0 and 66 h samples. The corrosion resist-
ance initially increases for 0 h then decreases for 10 h fol-
lowed by a significant increase for 25 h and finally decreases
for 66 h sample. This might be due to the formation of pits
and fragile patches in 0, 10 and 66 h samples. The same
trend has been observed while investigating the bode plots
(Fig. 11b). Rather than the loop’s radius, the area covered by
the bode plot is considered as the key factor which is directly
proportional to the corrosion resistance [65]. Here also, the
25 h LPBF sample has a greater covered area which tends to
exhibit significant anti-corrosion behavior. However, there is
a decreasing trend is observed in terms of the area covered
for 0, 10 and 66 h samples. Hence, the obtained Nyquist and
bode plots showed that the 25 h LPBF AlSi10Mg sample has
a better arc radius and greater curve-covered area thereby
offering significant resistance against corrosion.
Besides the Nyquist and bode plots, the corrosion resist-
ance offered by the samples can be confirmed by means of an
equilibrium circuit. Figure 11a inset represents the equilib-
rium circuit used for calculating the parameters like solution
resistance (Rs), polarization resistance (Rp) and constant
phase element (CPE) respectively. The polarization resist-
ance value will influence the resistance offered. Higher the
Rp value, greater the resistance offered [66]. The parameters
such as Rp, Rs and CPE with their error values for the LPBF
AlSi10Mg at 0, 10, 25 and 66 h intervals were tabulated in
Table 4. Here also, the Rp value initially increases (0 h),
then decreases (10 h), attains its maximum value (25 h) and
finally decreases for 66 h sample. The Rp value obtained for
0, 10, 25 and 66 h samples are 13,133, 12,739, 36,714 and
8831.8 respectively. On comparing those values, the 25 h
sample has the highest Rp value (36,714) and this value is
nearly thrice than that of 0 h sample. Thus, the 25 h LPBF
AlSi10Mg sample exhibits better anti-corrosion character-
istics because of its higher Rp value.
3.7 XRD Analysis on the Corroded Surface
The above study confirms that the 25 h LPBF AlSi10Mg
sample possesses a higher corrosion resistance. To clarify
the formation of the corrosion product, the XRD analysis
has carried out on the corroded surface. Figure 12 shows the
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Metals and Materials International
XRD results of the LPBF AlSi10Mg sample after immersion
of 0, 10, 25 and 66 h in the NaCl solution. In 0 h immersion
time, the corrosion products formed at the surfaces are sam-
ples α-Al(OH)3 (2θ = 40.5°, 67.1° and 80.3° approximately)
and ­SiO2 (2θ = 46.7° approximately). Notably, in 10, 25 and
66 h LPBF AlSi10Mg samples, the ­MgAl2O4 component
is present at the diffraction peaks of (2θ = 33.0°, 42.7° and
58.2°, approximately. This ­MgAl2O4 component is formed
due to higher affinity to the electrochemical reactivity of Mg
element than that of remaining elements such as Al and Si
[67]. The following steps are the sequential procedure for the
formation of ­MgAl2O4 which is described below.
Mg → Mg2+ + 2e− (3)
Mg2+ + O2− → MgO (4)
MgO + Al2 O3 → MgAl2 O4 (5)
The presence of M ­ gAl2O4 corrosion product reveals
that a sufficient amount of ­Mg2Si is present in the eutectic
region. The M ­ g2Si component act as the barrier to protect
the surface from Al dissolution. The M ­ g2Si makes the cross-
link with corrosion product based on Si and Al elements
that lead to the form Mg–O–Si and Mg–O–Al bonds. It
acts as a stable corrosion-resistant layer that protects the
LPBF AlSi10Mg sample. The increase in M ­ g2Si content
produces a more stable corrosion-resistant product based
on the immersion time in the NaCl solution. The maximum
stability of the protection layer accrues at the 25 h immer-
sion test. Further increase in the immersion leads to reduce
the stability of the protection layer due to phase changes.
The reduction in the presence of the protection layer leads to
the creation of a porous structure. As a result, the exposure
of the LPBF AlSi10Mg sample to the corrosion solution is
increased. Al and Si have low binding energy that leads to
the release of the electron density of Al, Si and O. However,
Si–O–Al also protects the surface from corrosion which is
difficult to maintain the link as the difference in electron-
egativity of Si and Al is very less. Hence, Al and Si produce
the corrosive product in the Mg environment in the form of
Mg–O–Si and Mg–O–Al.
The same results were obtained for other authors. Junho
Kim et al. [68] analyzed the phases present in the oxide layer
formed on the hypoeutectic Al–Si–Mg alloy. They reported
that the passive layer was rich in the oxides of Mg, Si, Al
and the bonding energy of these oxides are measured to be
358, 799 and 501 respectively. They also reported that in the
presence of corrosive media, the binding energy of the Mg
increases whereas the binding energy of Al and Si tends to
decrease. This increased binding energy of Mg makes it to
form crosslinks with the Si and Al based corrosion product
Metals and Materials International

Table 3  The elemental Duration Element Al Si C O Fe Mg Mn Total

compositions of SLM printed
AlSi10Mg samples at various 0h Point-Weight% 76.6 9.8 8.3 4.4 0.5 0.3 – 99.90
time intervals
Area-Atomic% 71.9 7.7 6.5 13.2 – 0.6 0.2 100.10
10 h Point-Weight% 67.7 9.6 – 19.7 2.0 0.2 0.8 100.00
Area-Weight % 46.5 6.1 14.9 30.6 – 0.6 1.3 100.00
25 h Point-Weight% 54.5 0.8 4.3 39.4 – 1.0 – 100.00
Area-Weight % 32.1 6.0 4.2 54.8 2.0 0.9 – 100.00
66 h Point-Weight% 67.3 10.0 4.6 16.7 0.3 0.5 0.5 99.90
Area-Weight % 55.4 6.7 8.8 28.3 – 0.4 0.4 100.00

Fig. 10  Schematic illustra-

tion of passive (oxide) film
formation (a) LPBF printed
AlSi10Mg sample, (b) Reaction
of Al and Si ions with O ions
and (c) Passive film formed on
the LPBF AlSi10Mg sample’s
surface

Fig. 11  (a) Nyquist plot and (b) Bode plot of LPBF AlSi10Mg samples at various intervals

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Table 4  Equilibrium circuit Duration Element Rs Rp CPE

parameter values of SLM
AlSi10Mg samples at 0, 10, 25 Parameter R R Y0 N
and 66 h 2
0 h (χ = 3.4888) Value 12.96 12,739 2.4636E-06 0.86793
Estimated Error (%) 11.738 6.237 14.408 1.990
10 h (χ2 = 1.3663) Value 37.601 13,133 2.0952E-05 0.80412
Estimated Error (%) 3.804 4.431 6.903 1.450
25 h (χ2 = 0.35562) Value 28.267 36,714 3.4689E-05 0.81303
Estimated Error (%) 1.905 6.054 2.692 0.641
66 h (χ2 = 0.36661) Value 34.494 8831.8 4.3557E-05 0.74856
Estimated Error (%) 2.084 3.661 3.793 0.892

3.8 Corroded Surface Roughness

Apart from the electrochemical investigation, surface irregu-

Fig.12  XRD of passive film formed on LPBF ALSi10Mg samples at
different time intervals
namely ­MgAl2O4. The ­MgAl2O4 is formed by the combina-
tion of MgO and ­Al2O3 as represented in the above equation.
This crosslinked product is responsible for enhancing the
corrosion resistance offered by the passive layer formed on
the LPBF printed AlSi10Mg alloy. The formed M ­ gAl2O4 is
reported to act as a sole barrier that improves the corrosion
resistance. These results were obtained for Arrabal et al. [69]
and Mingo et al. [70] respectively. In addition to it, the ­SiO2
and Al(OH)3 increase the corrosion resistance by covering
the corrosion pits [71]. However, Al(OH)3, ­SiO2 are decom-
posed to ­H2O, ­O2 as it is unstable in nature which leads
to allowing the corrosive action on the LPBF AlSi10Mg
surface. Hence, the presence of Al(OH)3, ­SiO2 temperately
protects the LPBF AlSi10Mg surface. As a result, The pres-
ence of α-Al(OH)3 product in all samples is unable to protect
the surface from corrosion.
larities present on the surface of the LPBF AlSi10Mg sam-
ple after the corrosion test will also influence the corrosion
resistance characteristics offered by the sample. These tiny
irregularities are more prone to corrosion attacks than the
surface without irregularities [72]. Moreover, these irregu-
larities make the surface rough thereby minimizing the
anti-corrosion behavior. Here, for all samples, the surface
roughness was investigated with the help of the surface and
2D plot captured from the laser microscope. Figure 13a–h
shows the surface and 2D plots of 0, 10, 25 and 66 h samples
respectively. On comparing these plots, the 2D plot obtained
for 25 h sample tends to have a minimum amount of irregu-
larities than the 10, 0 and 66 h samples. These irregularities
are due to the effect of pits during corrosion. In addition, the
average surface roughness (Ra) was measured and tabulated
in Table 5. Generally, the Ra value is inversely proportional
to the corrosion resistance. Hence, a smaller Ra value will
result in a lesser corrosion rate thereby providing maximum
resistance [73, 74].
On comparing the average surface roughness value
obtained for various immersion samples, the Ra value ini-
tially increases (0 h sample—3.633 μm), then decreases
(10 h sample—3.593 μm), attaining its minimum (25 h
sample—3.554 μm) and finally reaches the maximum
value (66 h sample—3.688 μm). The initial increase in the
Ra value of the 0 h sample is might to due to the presence
of pits in its passive layer. Normally, these pits or pores
are considered as surface irregularities that are responsi-
ble for increasing the Ra value [75, 76]. The 10 h sample
shows reduced surface roughness than the 0 h sample. At
this interval, the passivation is said to be steady and thus
shows a reduced Ra value in the presence of some pits. On
the other hand, the 25 h sample has the minimum Ra value
among all the samples since its passive surface are free for
irregularities [77, 78]. The higher interval (66 h sample)
sample reported the maximum value of surface rough-
ness since the broken fragile patches act as the surface

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Metals and Materials International

Fig. 13  Surface and 2D plot of LPBF AlSi10Mg samples at (a, b) 0 h, (c, d) 10 h, (e, f) 25 h and (g, h) 66 h

13

Table 5  Average roughness Duration Roughness
value (Ra) of SLM AlSi10Mg value—Ra
samples after corrosion test (μm)
0h 3.633
10 h 3.593
25 h 3.554
66 h 3.688
irregularities which could be responsible for attaining the
maximum surface roughness value. Thus, these results are
in correlation with the electrochemical aspects (Tafel and
EIS plots). Thus, the 25 h LPBF AlSi10Mg sample pro-
vides significant resistance against corrosion.
4 Conclusion
In this work, the microstructure evolution along with the
mechanical characteristics such as hardness, corrosion
resistance, and corroded surface roughness of the LPBF
printed AlSi10Mg sample was investigated at different time
intervals. The major outcomes are summarized as follows:
1. LPBF printed AlSi10Mg microstructure contains equi-
axed α-Al grains decorated with Si as their grain bound-
aries along with the ­Mg2Si precipitates (white spots).
2. The Vickers microhardness test showed that the building
direction has a higher average hardness value (151.94
HV) than the scanning direction of the LPBF printed
sample.
3. The EBSD and inverse pole maps confirmed that the
grain growth is more in the building direction.
4. The TEM analysis has further proved the existence of
equiaxed α-Al grains along with the secondary ­(Mg2Si)
precipitates.
5. The Tafel and EIS plots showed that the 25 h LPBF
AlSi10Mg sample has better anti-corrosion characteris-
tics in terms of current density and polarization resist-
ance values due to the formation of the stable oxide film.
6. The XRD plot confirmed the formation of ­MgAl2O4
corrosion product on the LPBF AlSi10Mg surface. The
maximum intensity of ­MgAl2O4 is observed on 25 h
immersion test sample which revealed the reason for its
superior corrosion resistance. Moreover, 25 h sample
has a minimum Ra value and provides significant resist-
ance against corrosion.
In the future, the authors are focusing on analyzing
the wear-resistant characteristics and the microstructural
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Metals and Materials International
evolution happening in the LPBF AlSi10Mg samples
under various heat treatment procedures.
Data Availability The experimental datasets obtained from this research
work and then the analysed results during the current study are avail-
able from the corresponding author on reasonable request.
Declarations
Competing Interest The authors declare that they have no known com-
peting financial interests or personal relationships.
Ethical Approval This article does not contain any studies with human
participants or animals performed by any of the authors.
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