metals
Article
Influence of Stress Relief Annealing Parameters on Mechanical
Properties and Decomposition of Eutectic Si Network of L-PBF
Additive Manufactured Alloy AlSi10Mg
Ludmila Růžičková 1, * , Jana Sobotová 1 , Libor Beránek 2 , Lukáš Pelikán 2 and Jan Šimota 2
Citation: Růžičková, L.; Sobotová, J.;
Beránek, L.; Pelikán, L.; Šimota, J.
Influence of Stress Relief Annealing
Parameters on Mechanical Properties
and Decomposition of Eutectic Si
Network of L-PBF Additive
Manufactured Alloy AlSi10Mg.
Metals 2022, 12, 1497. https://
doi.org/10.3390/met12091497
Academic Editor: Paolo Ferro
Received: 2 August 2022
Accepted: 5 September 2022
Published: 9 September 2022
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Attribution (CC BY) license (https://
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4.0/).
Metals 2022, 12, 1497. https://doi.org/10.3390/met12091497
1 Faculty of Mechanical Engineering, Czech Technical University in Prague, Karlovo náměstí 13,
121 35 Praha, Czech Republic
2 Faculty of Mechanical Engineering, Czech Technical University in Prague, Technická 4,
166 07 Praha, Czech Republic
* Correspondence: ludmila.ruzickova@fs.cvut.cz
Abstract: This paper evaluates the effect of stress-relieving heat treatment on the AlSi10Mg alloy
prepared by additive manufacturing using the Laser Powder Bed Fusion (L-PBF) with print parame-
ters: 370 W, 1400 m/s, and 50 µm. The as-built state and four different annealing modes (240 ◦ C/2 h,
240 ◦ C/6 h, 300 ◦ C/2 h, and 300 ◦ C/2 h/water-quenched) are investigated. To determine the effect
of the annealing mode on the mechanical properties of the L-PBF AlSi10Mg alloy, heat-treated sam-
ples were compared with the as-built state and with each other. The mechanical properties of the
samples were determined by tensile and hardness tests. The strength in the as-built state is 488 MPa,
depending on the method of heat treatment, the strength values range from 296 MPa to 417 MPa,
and the HV10 hardness values are in accordance with the measured strength values. Furthermore,
the microstructure of the samples was investigated by scanning electron microscopy (SEM) analysis,
which was then linked to the measured mechanical properties. The composition of the microstructure
of the alloy and its influence on the mechanical properties were determined by energy dispersive
spectroscopy (EDS) analysis. Furthermore, the differences between the individual heat treatments in
comparison with the as-built state were analyzed and the phenomenon of decomposition of the silicon
network after reaching specific temperatures was discussed and confirmed. The paper evaluates
the effect of dwelling time on stress relief annealing. It was found that if annealing at intermediate
temperatures of 240 and 300 ◦ C is applied, changes in structure and mechanical properties are more
temperature- than dwell-time-dependent.
Keywords: additive manufacturing; AlSi10Mg; laser beam powder bed fusion; selective laser melting;
microstructure; mechanical properties; eutectic Si network; heat treatment
1. Introduction
Aluminum alloys are the most common and widely used non-ferrous casting ma-
terials [1]. High-quality castings with suitable mechanical properties are produced by
high-pressure casting, which is considered the best casting method for aluminum alloys
among the available casting methods [2–4]. Specific casting structure and properties are
well described [5]. In contrast, aluminum alloy components produced by 3D printing using
L-PBF technology have a completely different microstructure than cast alloys and thus
different properties [2]. By 3D printing these components, comparable or better mechanical
properties can be achieved than by high-pressure casting technology [6]. The heat treatment
process and its effect on mechanical properties and microstructure is also well known and
described for aluminum casting alloys. For casted aluminum alloys, typical heat treatment
(HT) is solution annealing followed by artificial aging (T6) [2,7], which generally leads to
an increase in strength properties compared to the as-cast state. In contrast, it was found
that the use of T6 heat treatment in the case of the 3D printed AlSi10Mg alloy leads to a
https://www.mdpi.com/journal/metals
Metals 2022, 12, 1497 2 of 14

significant decrease in strength characteristics compared to the as-built state; this fact is
given by a different structure of the Laser Beam Powder Bed Fusion (L-PBF) parts in the
comparison with casted ones [7–9]. For components after 3D printing, stress relieving is
usually used [7,10], but it is not yet entirely clear which parameters of mentioned heat
treatment are suitable for the final application of the material thus prepared and processed.
The L-PBF process is based on the melting of small volumes of powder by a high-
energy source, in this case, a laser. Unlike casting, L-PBF is characterized by an extremely
high solidification rate which has been reported to be of the order of 103 –105 K/s [11,12].
The layered structure of the printed part when the melting pools overlap brings another
phenomenon—cycles of reheating and cooling of already solidified material caused by
printing of adjacent or overlapping layers. These facts have a significant effect on the
metallurgy of the material, which among other things has the following impacts:
• Supersaturated solid solutions and residual stresses are formed and occur in the alloy
during the printing, primarily because of the high cooling rate.
• Heat treatment of previously solidified material subsequently causes local phase
transformations and precipitation.
Heat treatment of L-PBF aluminum alloys should be considered as a separate issue.
From the differences discussed above, it follows that the same heat treatment procedures
cannot be applied to printed alloys as for cast ones expecting the same results in the change
in microstructure and the associated change in mechanical properties.
The currently used HT of L-PBF additive manufactured AlSi10Mg can be divided
into three categories according to the used temperature, specifically, low-, intermediate-,
and high-temperature annealing, each with a different effect on the final microstructure.
Annealing at low temperatures can be classified as an HT up to 200 ◦ C equal to direct
aging (T5). Stress relief annealing as an intermediate-temperature HT up to 350 ◦ C, and
high-temperature HT as solution annealing up to 550 ◦ C, which can be also followed by
direct aging (T5).
HT is applied to (i) relieve stress caused by the nature of the L-PBF production process,
as previously discussed mainly by the high cooling rate and cyclic reheating of already
solidified material, and (ii) to alter the mechanical properties of the alloy.
This article focuses on intermediate-temperature annealing. This research aims to
determine how the heat treatment parameters, such as temperature, dwell time, and cooling
rate, influence the mechanical properties and microstructure of the L-PBF AlSi10Mg alloy.
HT parameters recommended by a powder manufacturer [13] and the studied literature
were used and modified to develop a comprehensive view of the issue of annealing at
intermediate temperatures.
This work evaluates modes of intermediate-temperature heat treatment (stress reliev-
ing), within one build cycle, to better compare the direct effect of HT on the as-built state
and its properties and microstructure. In the available literature are papers that evaluate
mainly HT at 300 ◦ C/2 h in various combinations, such as a comparison with low- and high-
temperature annealing [7], low-temperature HT, and hot isostatic pressing (HIP) [14], or after
stress relieving (SR) compared to SR + HIP [15]. Another evaluated HT is 300 ◦ C/2 h/water-
quenched, and in these papers, the HT is usually evaluated in comparison with solution
annealing (high-temperature HT) [16] or also followed by artificial aging (equal to T6) [17].
Several papers only evaluate intermediate-temperature HT, namely Tang and Pistorius [10],
who evaluate only the mode of 300 ◦ C/2 h and its effect on porosity oxides and fatigue
resistance. Wang et al. [18] studied 300 ◦ C compared to 270 ◦ C and 330 ◦ C and the effect of
building orientation and heat treatment on the anisotropic tensile properties, and Rosenthal
et al. [19] compared 300 ◦ C to the manufacturer’s recommendation and gravity and high-
pressure casting. Patakham et al. [20] evaluated melt pool boundary characteristics and Si
morphologies on mechanical properties and fracture behavior after HT 270 ◦ C/1.5 h.
This paper studies (a) 240 ◦ C/6 h as the manufacturer’s recommendation [13], a modi-
fied version (b) 240 ◦ C/2 h in order to find out whether the annealing time can be shortened
to make the process more efficient, and further (c) 300 ◦ C/2 h and (d) 300 ◦ C/2 h/WQ and
 Metals 2022, 12, 1497 3 of 14

their influence on mechanical and other properties. The as-built state is used to study the
influence of individual HT modes. Although the effect of HT on the structure and proper-
ties of the L-PBF AlSi10Mg alloy has been previously studied, this specific combination
of printing parameters and HT modes, and specifically the modes of HT 240 ◦ C/6 h and
240 ◦ C/2 h, have not been studied in the available literature.

2. Materials and Methods

AlSi10Mg powder CL 31AL by Concept Laser GmbH with the nominal composition
given in the following Table 1 was used.

Table 1. Chemical composition of AlSi10Mg powder by Concept Laser GmbH in wt. % [13].

Si Mg Fe Mn Ti Cu Zn C Ni Pb Sn Al
9.0–11.0 0.20–0.45 0–0.55 0–0.45 0–0.15 0–0.10 0–0.10 0–0.05 0–0.05 0–0.05 0–0.05 Bal.

The manufacturer guarantees a particle size distribution in the material sheet: 99.9%
up to 45 µm, 89.1% up to 38 µm. SEM image of the used powder is in Figure 1. In terms of
size distribution, the powder is highly heterogeneous. The scanning electron microscopy
(SEM) analysis in Figure 1 shows that considerably larger particles (up to 70 µm) are
present in the powder than guaranteed by the manufacturer. It can be a combination of
several powder grains melted together, or an incorrectly set up production process. The
imperfect spheroidization of the powder particles is also clear from the figure. All these
facts, in combination with the printing parameters, can affect the resulting mechanical
properties
Metals 2022, 12, x FOR PEER REVIEW of the printed material. However, the occurrence of elements controlled by
energy-dispersive spectroscopy (EDS) analysis corresponds to the chemical composition
given by the material sheet.

Figure1. 1. SEM
Figure SEMimage
imageofofused
usedAlSi10Mg
AlSi10Mg powder;
powder; particles
particles significantly
significantly larger
larger than 45than
µm 45 μm
lighted.
are highlighted.

Table 3. List of heat treatment modes of L-PBF AlSi10Mg used in the experiment.

Identification of the Sample Group Description of the Heat Treatmen

AB (as-built) With no further heat treatment after pri
Metals 2022, 12, 1497 4 of 14

For the additive manufacture of AlSi10Mg L-PBF technology was used. Samples were
printed in a Concept Laser M2 machine in the Z axis in a protective nitrogen atmosphere
with the printing parameters given in Table 2. The parameters that were chosen are the
optimal and used settings for the given printer and powder based on previous experience
at the given workplace.

Table 2. Printing parameters used for AlSi10Mg L-PBF samples.

Power (W) Speed (mm/s) Layer Thickness (µm) Spot Size (µm)
Skin 200 800 25 190
Core 370 1400 50 190
Support 200 1600 50 50

The samples were divided into groups of 5 and heat treated at several temperatures;
5 samples were left in an as-built state. The individual modes of heat treatment and
the method of cooling are listed in Table 3. All annealing temperatures were reached in
1 h, after dwelling at temperature cooling in different media followed, including furnace
(furnace-cooled, FC), air (air-cooled, AC), and water (water-quenched, WQ).

Table 3. List of heat treatment modes of L-PBF AlSi10Mg used in the experiment.

Identification of the Sample Group Description of the Heat Treatment

AB (as-built) With no further heat treatment after printing
T 240 ◦ C/6 h; FC to 100 ◦ C then AC
Z 240 ◦ C/2 h; FC to 100 ◦ C then AC
E 300 ◦ C/2 h; WQ
P 300 C/2 h; FC to 100 ◦ C then AC
◦

All samples were machined at Slovtos S 280 CNC to the precise shape for the tensile
test (short test rod: d = 8 mm, d1 = M12, Lo = 40 mm, Lt = 77 mm) according to the standard
(ISO 6892-1).
A tensile test was performed on all samples according to the ISO 6892-1 standard on
the universal testing machine INSTRON 5582 with a maximum load force of 100 kN and
the applied crossbar speed of 5 mm/min.
Samples for metallographic analysis in the cross-section and longitudinal section were
cut from the threaded heads of the tensile test specimens.
To reveal the microstructure, the samples were prepared through a standard metal-
lography procedure (including mechanical grinding and polishing) and etched in Keller’s
reagent (2.5% HNO3 ; 1.5% HCl; 1.0% HF; 95.0% distilled water).
Metallographic analysis was performed on the samples using optical microscope Carl
Zeiss Jena Neophot 32 and scanning electron microscope JEOL JSM-7600F) and subse-
quently the analysis of chemical composition by EDS using the Oxford X-Max detector
50 mm2 .

3. Results and Discussion

3.1. Mechanical Properties and Microstructure of the As-Built State
Although the structure of the L-PBF AlSi10Mg alloy in the as-built state has already
been described in the available literature, it should be noted that the resulting structure is
affected by several parameters (powder, printing parameters, printing direction, etc.). For
this reason, analyzing the structure and properties in the as-built state for each experiment
is always necessary.
Several phenomena cause the high strength of the as-built AlSi10Mg alloy:
• Hall–Petch reinforcement—grain boundary strengthening pile-up of dislocations at
the cell boundaries (fine Si network) which further inhibits dislocation motion and
considerably contributes to the high strength of as-built AlSi10Mg [21,22].
 Metals 2022, 12, 1497 5 of 14

• Orowan strengthening in the as-built condition upon the dislocations is pinned by

the eutectic Si phase at cell boundaries, the bend around eutectic Al phases, and the
Orowan looping mode is activated. Dislocations glide through the cell boundary, thus
highly strengthening the alloy. A large number of new dislocations are initiated by
this mechanism, which increases the alloy’s strain hardening ability [8,23].
• Strengthening induced by localized shear stress: nano-sized Si particles and Si precipi-
tates in the matrix [24].
• Dislocation strengthening hardening by dislocation interactions (pre-existing disloca-
tion network) [25].
• Solid solution strengthening: supersaturated solid solution of Si in an aluminum
matrix. Due to the fast cooling rate, the equilibrium solubility is higher; for the L-PBF
AlSi10Mg the solubility of Si was measured [26] to be approximately in the range
of 1–3%. Authors [22] calculated the solubility of Si atoms in the Al matrix to be
8.89 at. %.
Table 4 shows the measured mechanical properties of as-built parts in comparison
with casted specimens [6]. After the heat treatment, T6, of a conventionally produced alloy,
which further increases the mechanical properties of the manufactured part, the mechanical
properties such as ultimate tensile strength (UTS) and hardness are lower compared to the
as-built state.

Table 4. Mechanical properties evaluated through the tensile test of L-PBF AlSi10Mg in the as-built
state in comparison with casted AlSi10Mg.

Ref. UTS (MPa) HV10

As-built This paper 486 ± 1 128 ± 2
Conventional cast and aged [6] 300–317 86
High-pressure die casting, as-cast [6] 300–350 95–105
High-pressure die casting, T6 [6] 330–365 130–133

als 2022, 12, x FOR PEER REVIEW
By establishing a suitable heat treatment for printed parts, significantly better me-
chanical properties may be achieved than for casted parts, in addition to the possibility of
complex geometries that 3D printing allows.
In the as-built state typical microstructure (Figure 2) of the L-PBF, parts were found and
observed. The transverse cross-section consists of rounded and elongated melting pools 6 of
displaying the laser scanning strategy. The longitudinal cross-section view is comprised of
solidified melt pools with a half-cylindrical shape.

FigureFigure
2. Optical microscopy
2. Optical microscopyimage
image ofofrepresentative
representative microstructure
microstructure ofAlSi10Mg
of L-PBF L-PBF AlSi10Mg
alloy in thealloy in
(a) transverse and (b) longitudinal cross-sections, as-built
(a) transverse and (b) longitudinal cross-sections, as-built state. state.

Figure 3 shows a magnified SEM image of the melt pool boundary, which consists
the heat-affected zone (HAZ) and coarse cellular microstructure that gradually chang
into the fine cellular microstructure of the melt pool. The upper melt pool is overlappi
 Figure 2. Optical microscopy image of representative microstructure of L-PBF AlSi10Mg
Metals 2022, 12, 1497 (a) transverse and (b) longitudinal cross-sections, as-built state. 6 of 14

Figure 3 shows a magnified SEM image of the melt pool boundary, which
the heat-affected
Figure 3 shows azone (HAZ)
magnified SEMandimagecoarse cellular
of the melt microstructure
pool boundary, that of
which consists gradual
the heat-affected zone (HAZ) and coarse cellular microstructure that gradually changes
into the fine cellular microstructure of the melt pool. The upper melt pool is ov
into the fine cellular microstructure of the melt pool. The upper melt pool is overlapping
the adjacent
the adjacent melt
melt pool’s
pool’s boundary;
boundary; therefore,
therefore, no coarse
no coarse cellular cellular ismicrostructure
microstructure visible.

Figure 3. SEM image of an as-built sample of L-PBF AlSi10Mg alloy in transverse cross-section,
Figure 3. SEM image of an as-built sample of L-PBF AlSi10Mg alloy in transverse cr
showing microstructure at the melt pool boundaries.
showing microstructure at the melt pool boundaries.
Metals 2022, 12, x FOR PEER REVIEW
At a smaller scale (Figure 4), a typical fine microstructure of the supersaturated solid
solution
At of
a the α-Al phase
smaller scaleand Si continuous
(Figure networkfine
4), a typical can microstructure
be observed. of the supersatu
solution of the α-Al phase and Si continuous network can be observed.
The discussed composition of the microstructure is documented and con
EDS analysis in Figure 5. The elements found in the alloy correspond to the chem
position. The structure contains nano-sized particles of Si formed by a high co
which is one of the contributors to the strengthening of AlSi10Mg alloys produ
L-PBF [27]. Solid solution strengthening contributes to the increased hardnes
PBF specimen. The structure consists of a supersaturated α-Al matrix with dis
surrounded by a fibrous Si-enriched eutectic network which forms the cellula
of L-PBF AlSi10Mg alloys. Very fine Si particles are observable in the matrix
assumed that, according to the literature [28–30], these are nano-sized Si particle
phases.

Figure
Figure 4. SEM
4. SEM analysis
analysis of the microstructure
of the microstructure of as-built
of as-built L-PBF L-PBF
AlSi10Mg AlSi10Mg
sample sample
in the transverse in th
cross-section.
cross-section.
Metals 2022, 12, 1497 7 of 14

The discussed composition of the microstructure is documented and confirmed by

EDS analysis in Figure 5. The elements found in the alloy correspond to the chemical
composition. The structure contains nano-sized particles of Si formed by a high cooling
rate, which is one of the contributors to the strengthening of AlSi10Mg alloys produced by
the L-PBF [27]. Solid solution strengthening contributes to the increased hardness of the
L-PBF specimen. The structure consists of a supersaturated α-Al matrix with dispersed Mg
surrounded by a fibrous Si-enriched eutectic network which forms the cellular structure of
L-PBF
Figure 4. AlSi10Mg alloys.
SEM analysis Verymicrostructure
of the fine Si particlesofare observable
as-built inAlSi10Mg
L-PBF the matrix.sample
It can be
inassumed
the transverse
that, according to the literature [28–30], these are nano-sized Si particles or Mg2 Si phases.
cross-section.

Figure 5. EDS
Figure analysis
5. EDS of the
analysis chemical
of the composition
chemical compositionofofas-built
as-builtL-PBF
L-PBFAlSi10Mg
AlSi10Mg sample
sample in
in the
the trans-
verse cross-section.
transverse cross-section.

The studied structure of the as-built state corresponds to the available literature. The
The studied structure of the as-built state corresponds to the available literature. The
mechanical properties of the L-PBF AlSi10Mg alloy in the as-built state evaluated in this
mechanical properties of the L-PBF AlSi10Mg alloy in the as-built state evaluated in this
work when compared to other authors (Table 5) with similar printing parameters for
work when
better comparedand
comparability to other authors
informative (Table
value 5) with
generally similar
differ fromprinting parameters
each other. for bet-
Mechanical
terproperties
comparability and informative value generally differ from each other. Mechanical
such as values of yield strength (YS) and ultimate tensile strength (UTS) obtained
properties such
in this work areas
onevalues
of the of yieldcompared
highest strength to(YS)
the and
otherultimate tensile the
papers. Because strength (UTS) ob-
mechanical
tained in thisofwork
properties are one
the as-built offor
state theAlSi10Mg
highest differ
compared to the
even with otherprinting
similar papers.parameters,
Because the
it me-
is more accurate to compare individual heat treatments with each other and the
chanical properties of the as-built state for AlSi10Mg differ even with similar printing pa- as-built
state within
rameters, it isthe framework
more accurateofto one build cycle.
compare individual heat treatments with each other and
the3.2.
as-built stateProperties
Mechanical within theandframework
Microstructureofofone build cycle.
Intermediate-Temperature Annealing Treatments
of L-PBF AlSi10Mg
Stress relief annealing is used to reduce the accumulated stress in the material caused
by the L-PBF process and its previously discussed specifics. The chosen heat treatment for
this paper ranges from 240 to 300 ◦ C and is accompanied by several peculiarities, which
are discussed later in this work. In the following Table 6 are mechanical properties of the
L-PBF AlSi10Mg alloy treated by individual stress relief annealing modes. The values were
determined by tensile and hardness tests and are compared to the as-built state as default
and reference value.
 Metals 2022, 12, 1497 8 of 14

Table 5. Mechanical properties of evaluated as-built state L-PBF AlSi10Mg in comparison with
other papers.

UTS (MPa) YS (MPa) Printing Parameters L-PBF Machine Ref.

Power 370 W, speed 1400 mm/s, layer thickness 50 µm,
488 ± 1 264 ± 10 Concept Laser M2 This paper
spot size 190 µm
Power 370 W, speed 1300 mm/s, layer thickness 30 µm,
386 ± 10 235 ± 5 EOS M290 [30]
spot size 100 µm
396 196 Power 370 W, speed 1300 mm/s, layer thickness 30 µm - [31]
404 ± 4 268 ± 12 Power 370 W, speed 1300 mm/s, layer thickness 30 µm EOS M290 [32]
476 220 Power 380 W, layer thickness 30 µm EOSINT M 280 [16]
Power 370 W, speed 1500 mm/s, layer thickness 30 µm,
349 ± 6 224 ± 6 Concept X-line 1000R [33]
spot size 100 µm
Power 400 W, speed 1000 mm/s, layer thickness 30 µm,
384 ± 16 241 ± 10 EOSINT M 280 [15]
spot size 100–150 µm

Table 6. Mechanical properties of L-PBF AlSi10Mg at different stress relief annealing modes compared
to an as-built state.

Group Description of the Heat Treatment YS (MPa) UTS (MPa) HV 10

AB As-built 264 ± 10 488 ± 1 128 ± 2
T 240 ◦ C/6 h; FC to 100 ◦ C then AC 258 ± 8 415 ± 3 114 ± 1
Z 240 ◦ C/2 h; FC to 100 ◦ C then AC 259 ± 3 417 ± 2 115 ± 1
P 300 ◦ C/2 h; FC to 100 ◦ C then AC 195 ± 8 296 ± 5 86 ± 2
E 300 ◦ C/2 h; WQ 231 ± 6 354 ± 4 102 ± 1

Metals 2022, 12, x FOR PEER REVIEW 9 of 14

For a visual comparison of as-built and individual heat treatment modes, the values
of strength characteristics are plotted on a graph (Figure 6) below.

Figure 6. Graph summarizing mechanical properties of as-built and heat-treated L-PBF ASi10Mg
Figure 6. Graph summarizing mechanical properties of as-built and heat-treated L-PBF ASi10Mg
within one build cycle.
within one build cycle.

Table 7 compares the measured properties in this work with the available literature.
The described trend applies to all compared authors, and thus with stress relieving at 240
°C there is a smaller decrease in mechanical properties, in contrast to 300 °C, where there
is a significant decrease in mechanical properties. The results obtained in this work are in
Metals 2022, 12, 1497 9 of 14

Based on the achieved results, it can be stated that in general stress relieving applied on
L-PBF AlSi10Mg samples reduces mechanical properties compared to as-built conditions.
At the annealing temperature of 240 ◦ C, there are no significant differences in the mechanical
properties between modes T and Z. Thus, it can be stated that dwell time at 240 ◦ C does
not affect the monitored properties; in both cases, there was a decrease in strength of the
as-built state by approximately 15%. It can be seen from Figure 6 that at annealing at 300 ◦ C
the decrease is greater compared to as-built state than at 240 ◦ C, and a smaller decrease
occurs in mode E of 28% and in mode P of 39%. Thus, it can be stated that the cooling
rate from the temperature of 300 ◦ C influences the strength characteristics. When cooled
rapidly in water, the strength is 16% greater than when cooled slowly in an oven.
Table 7 compares the measured properties in this work with the available literature.
The described trend applies to all compared authors, and thus with stress relieving at
240 ◦ C there is a smaller decrease in mechanical properties, in contrast to 300 ◦ C, where
there is a significant decrease in mechanical properties. The results obtained in this work
are in good agreement with the available literature, although the values differ, which may
be due to different printing parameters. However, it is important to emphasize that no
article was found in the literature review that evaluated the T and Z annealing modes for
the AlSi10Mg alloy.

Table 7. Comparison of mechanical properties of L-PBF AlSi10Mg after annealing at T, Z, E, and P

modes; results of this work compared to the same annealing modes in the available literature.

Heat Treatment YS (MPa) UTS (MPa) Ref.

Mode T
As-built 264 ± 10 488 ± 1
This paper
240 ◦ C/6 h/ FC 258 ± 8 415 ± 3
Mode Z
As-built 264 ± 10 488 ± 1
This paper
240 ◦ C/2 h/ FC 259 ± 3 417 ± 2
Comparison of mode
E
As-built 264 ± 10 488 ± 1
This paper
300 ◦ C/2 h/WQ 231 ± 6 354 ± 4
As-built 220 476
[16]
300 ◦ C/2 h/WQ 175 290
As-built 270 446
[17]
300 ◦ C/2 h/WQ 169 273
Comparison of mode
P
As-built 264 ± 10 488 ± 1
This paper
300 ◦ C/2 h/ FC 195 ± 8 296 ± 5
As-built 241 ± 10 384 ± 16
[15]
300 ◦ C/2 h/ FC 205 ± 8 253 ± 18
As-built 319 ± 3 477 ± 5
[34]
300 ◦ C/2 h/ FC 266 ± 4 369 ± 4
Metals 2022, 12, 1497 10 of 14

Even when comparing similar printing parameters, such as this paper and [15,16],
the as-built UTS values can also differ, as discussed earlier. This can be seen in Table 7
from the comparison of this paper and [15], where the UTS in the as-built state is 384 MPa,
whereas in this paper the UTS is 488 MPa. If the results of [16] and this work are compared,
both experiments achieved comparable values in the as-built state. After applying the
heat treatment 300 ◦ C/2 h/WQ (mode E), the strength values differ between this paper
(UTS = 354 MPa) and [16] (UTS = 290 MPa).
For 240 ◦ C/6 h (mode T) and 240 ◦ C/2 h (mode Z), no data were found for comparison
from the available researched literature, and for mode E (300 ◦ C/2 h/WQ) the values
of the strength characteristics published in this paper are higher than in [16,17]. On
the contrary, in mode P (300 ◦ C/2 h/FC) this work achieves a comparable strength in
the as-built state with paper [34], but strength after stress relieving varies considerably.
Paper [34] achieves high strength values for the stress reliving of 300 ◦ C/2 h/FC (mode P),
where significant disintegration and coarsening of the Si network due to long temperature
exposure during cooling in the furnace occurs. The values in [34] are comparable with
UTS after heat treatment 300 ◦ C/2 h/WQ (mode E) in this paper, where the samples are
water-quenched, and thus higher strength characteristics are preserved than in the mode P
that is furnace-cooled.
It can be observed that individual results of different experiments cannot be easily
compared with each other. Rather, it is possible to study the trend and influence that a
given heat treatment has on the as-built state.
Figure 7 documents the microstructure of the as-built state and individual heat treat-
ments. Although a comparison of Figure 7a–c seems to show a continuous Si network in
the structure of these states, subtle differences can be seen from a more detailed analysis
at higher magnification in Figure 8. After annealing at 240 ◦ C, there is a slight disruption
in the continuity of the Si network. This phenomenon is more pronounced in the case of
annealing at 240 ◦ C/6 h. It could be assumed that this disruption of the continuity of the Si
network will affect the mechanical properties. However, this assumption does not apply to
the results of Figure 6, because the strength in the T and Z states do not differ from each
other. It can be assumed that it is caused by the fact that during annealing at 240 ◦ C/6 h
other phase transformations are happening in the structure, which may have a reciprocal
effect. An exothermic peak evaluated by differential scanning calorimetry (DSC) is reported
in [35] with a maximum temperature at 241 ◦ C, which is related to precipitation of Mg2 Si,
which is one of the strengthening mechanisms, and so this fragmentation process will not
change the resulting mechanical properties because these two effects work reciprocally.
The decomposition of the Si network is evident in Figures 7 and 8d,e. For P and E
samples, the network breakdown occurs, with the decomposition being more pronounced
in the case of the P mode. The SEM results for the P and E modes are in good agreement
with the mechanical results. In general, decomposition of the Si network leads to a decrease
in strength characteristics, but when water-quenched (mode E, Figures 7e and 8e) the rate
of decomposition of the Si network is lower than when cooled in a furnace. Accordingly,
the paper [35] states that at a temperature of 294 ◦ C it is characteristic of this alloy that the
Si network decomposes, and the spheroidization and coarsening of the Si particles occur.
The slow cooling rate significantly influences and supports the kinetics of these processes.
Metals 2022, 12, x FOR PEER REVIEW
Metals 2022, 12, 1497 11 of 14

Figure 7. SEM analysis of the microstructure of (a) as-built and (b–e) stress relief annealed L-PBF
Figure 7.samples
AlSi10Mg SEM inanalysis
the transverse cross-sections.
of the microstructure of (a) as-built and (b–e) stress reli
nealed L-PBF AlSi10Mg samples in the transverse cross-sections.
Metals 2022, 12, x FOR PEER REVIEW 1
Metals 2022, 12, 1497 12 of 14

Figure 8.8.SEM
Figure SEManalysis of the
analysis ofmicrostructure of (a) as-built
the microstructure of (a)and (b–e) stress
as-built relief annealed
and (b–e) L-PBFannealed
stress relief
AlSi10Mg samples in the transverse cross-sections, magnification 30
AlSi10Mg samples in the transverse cross-sections, magnification 30 k. k.

4. Summary and Conclusions

4. Summary
This paperand Conclusions
summarizes the structure and mechanical properties of as-built and heat-
treated AlSi10Mg
This paper samples
summarizes prepared
the by the L-PBF
structure process
and within one
mechanical build cycle.
properties The
of as-built and
AlSi10Mg alloy was evaluated in the as-built state and after four stress-relieving modes:
treated AlSi10Mg samples prepared by the L-PBF process within one build cycl
240 ◦ C/2 h, 240 ◦ C/6 h, 300 ◦ C/2 h, and 300 ◦ C/2 h/water-quenched. The samples were
AlSi10Mg
subjected to aalloy
tensilewas
test evaluated
to determinein
thethe as-builtproperties
mechanical state andandafter
werefour stress-relieving
further analyzed m
240
using°C/2
light h,
and240 °C/6microscopy.
electron h, 300 °C/2Theh,following
and 300can°C/2 h/water-quenched. The samples
be stated:
subjected
• to a tensile
The as-built state hastest
theto determine
highest the mechanical
mechanical properties
properties compared and
to the were furthe
applied
lyzed using
heat light and
treatment: stresselectron microscopy.ofThe
relief at temperatures 240 and 300 ◦ C with
following can different
be stated:cooling
methods.
• The as-built state has the highest mechanical properties compared to the applie
treatment: stress relief at temperatures of 240 and 300 °C with different cooling
ods.
• The structure of the AlSi10Mg alloy in the as-built state consists of an aluminu
trix with finely dispersed magnesium and a continuous Si network deposited
Metals 2022, 12, 1497 13 of 14

• The structure of the AlSi10Mg alloy in the as-built state consists of an aluminum matrix
with finely dispersed magnesium and a continuous Si network deposited along the
cell boundaries.
• After annealing, the following changes occurred in the structure of the AlSi10Mg alloy:
o When annealing at 240 ◦ C, the continuity of the Si network was slightly dis-
rupted, which was more pronounced by a dwell time of 6 hours compared to
2 h. However, this phenomenon did not manifest itself in the expected decrease
in strength, probably due to the parallel precipitation of the Mg2 Si phase.
o When annealing at 300 ◦ C, the Si network decomposed, and the Si particles
were spheroidized and coarse. These effects were more pronounced when the
cooling rate from 300 ◦ C was lower. Mechanical properties of the AlSi10Mg
alloy annealed at 300 ◦ C were in good agreement with the changes in structure.
• Stress relief annealing mode T (240 ◦ C/2 h) and mode Z (240 ◦ C/6 h) achieved the
same mechanical properties, within the standard deviations.
• Stress relief annealing mode E (300 ◦ C/2 h/WQ) achieved 15% higher strength values
than mode P (300 ◦ C/2 h/FC to 100 ◦ C then AC).
• When comparing the same cooling rate but variable temperature, the annealing at
240 ◦ C (modes T—6 h, Z—2 h) showed a 15% strength decrease compared to the
as-built state when annealing at 300 ◦ C, where there was a 39% decrease. The change
in the mechanical properties of L-PBF AlSi10Mg during the intermediate temperature
annealing treatments was more temperature- than dwell-time-dependent.

Author Contributions: Conceptualization, L.R.; methodology, L.R.; investigation, L.R., L.P. and
J.Š.; writing—original draft, L.R.; project administration, L.R.; writing—review and editing, J.S.;
supervision, J.S. and L.B.; funding acquisition, J.S. and L.B.; resources, L.B. All authors have read and
agreed to the published version of the manuscript.
Funding: This work was supported by the Centre of Advanced Aerospace Technology, Project No.
CZ.02.1.01/0.0/0.0/16_019/0000826, Faculty of Mechanical Engineering, Czech Technical University
in Prague, and supported by the Grant Agency of the Czech Technical University in Prague, Grant
No. SGS22/106/OHK2/2T/12.
Data Availability Statement: Not applicable.
Acknowledgments: The authors are grateful for the support of this research.
Conflicts of Interest: The authors declare no conflict of interest.

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