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Materials Chemistry and Physics 289 (2022) 126411

Contents lists available at ScienceDirect

Materials Chemistry and Physics


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

Recycling of additive manufactured AlSi10Mg and its effect on


mechanical properties
Mert Coşkun a, *, Kerem Can Dizdar b, Gürkan Tarakçi a, Gökhan Özer a, Derya Dispinar b, c
a
Fatih Sultan Mehmet Vakif University, Aluminium Test Training and Research Center (ALUTEAM), TR 34445, Halic Campus, Istanbul, Turkey
b
Istanbul Technical University, Metallurgical and Materials Engineering, Istanbul, Turkey
c
Foseco R&D Center, NonFerrous Metal Treatment, Enschede, Netherlands

H I G H L I G H T S

• Additive manufacturing has great advantages to produce complex shapes.


• Recycling of AM aluminum was investigated for the first time.
• Material loss due to high surface area was high in recycled AM around 17%.
• Yield and ultimate tensile strength were in acceptable range.
• Elongation at fracture was scattered with low reliability due to unmelted pools.

A R T I C L E I N F O A B S T R A C T

Keywords: Energy savings and sustainability have become the critical factors for economic development. Recycling of
AlSi10Mg aluminum has been studied for a long time. It is well known that there is a significant difference in terms of
AM energy consumption when comparing primary and secondary aluminum. Alternative production methods have
Casting
been developed and additive manufacturing (AM) of aluminum has become popular in the recent years. AM has
Recycling
Mechanical property
many advantages such as the flexibility of geometry. There are almost no design limits since the part is produced
layer by layer. In this work, for the first time, the properties of recycled AM AlSi10Mg was compared with both
AM and cast alloy. Statistical analysis was carried out to characterize the changes. It was found that yield
strength was decreased in recycled AM, whereas ultimate tensile strength values were almost the same as in the
cast alloy. For elongation at fracture, the average value for recycled AM was higher than cast alloy, however the
reliability and reproducibility was low compare to cast alloy.

1. Introduction swarf etc. That can be feed back to the main melting furnace in pro­
duction lines and plants, and (ii) old scrap is the materials that have been
Aluminum and its alloys are the most widely used alloys in auto­ discarded due to their end-of-life cycle in application use. Today, a large
motive, aerospace and transportation industries due its high mechanical amount of new aluminum products is made by recycled (or so called:
properties and low-density properties. The process of primary aluminum secondary) alloys [2]. The recycled raw materials are known to be more
production involves the electrolytic process called smelting that is the than half of the aluminum that is in use [3,4].
removal of oxygen from Al2O3. Since the reaction of Al with O2 is quite During recycling process, there are critical points such as oxide and
favorable and it lies at the very low end of the Ellingham diagram, it inclusion intrusion which decreases the quality of the product [5–11].
requires high energy and powerful electric current to break the strong Therefore, care should be taken to clean the melt as best means such
Al–O bond [1]. Therefore, the recycling of aluminum has attracted great degassing, filtration prior to cleaning the surface contaminants such as
attention since the energy required for recycling is almost 95% less than oil, lubrication, paint and coatings. Kvithyld [12–16] carried out several
the primary melting [2]. Typically, there are two categories of recycled studies to show the importance of preparation before the recycling of
aluminum: (i) new scrap is the excess alloy such as runners, feeders, any scrap and their effect on the quality of the final product. Dispinar

* Corresponding author.
E-mail address: mcoskun@fsm.edu.tr (M. Coşkun).

https://doi.org/10.1016/j.matchemphys.2022.126411
Received 21 December 2021; Received in revised form 4 April 2022; Accepted 13 June 2022
Available online 15 June 2022
0254-0584/© 2022 Elsevier B.V. All rights reserved.
M. Coşkun et al. Materials Chemistry and Physics 289 (2022) 126411

Table 2
Standard process parameters for AlSi10Mg powder.
Laser Power 370 W

Laser Scan Speed 1300 mm/s


Hatch distance 0.19 mm
Layer thickness 30 μm
Scanning strategy X-Rotated
Preheat temperature 35 ◦ C (building platform)
Atmosphere Argon
Beam offset 0.02 mm
Beam diameter 100 μm
Energy density 49,932 J/mm3
Laser type Yb (Ytterbium) fibre laser

Fig. 1. SEM microstructure of AlSi10Mg powder.

[17–24] has shown that secondary alloys can expose similar mechanical
properties and high quality casting can be achieved if bifilms are
removed from the recycled alloy.
Additionally, the control of the alloying elements also plays a sig­
nificant role in the recycling operations. Typical elements such as Mg
and Sr have the tendency to oxidize and loss to the dross [25–31].
Increased Fe content coming from the permanent molds is another issue
which may result in the formation of Fe-intermetallic phases that has the
potential to decrease the ductility of the cast alloy [32,33].
Additive manufacturing (AM) is the three-dimensional printing
processes. High density powders are joint by high density heat source.
The process has gained much attention due to its flexibility and con­
struction of complex shape [34]. The most commonly used one is called
Selective Laser Melting (SLM). The system provides the advantage of
producing very complex parts not any other process can achieve.
Metallic powders are partially melted and layer by layer the product is
produced. Currently, oxidation and poor surface roughness are few of Fig. 2. Tensile specimen positioned for production (12 mm diameter x 90
mm height).
the challenges and drawbacks of AM processing of aluminum alloys
[34]. Many works have been carried with AlSiMg alloys [35–46]. Dynin
[47] reported that mechanical properties of SLM Al10SiMg alloy had properties when recycled powders were used. The fractography of the
exceed the parts produced by conventional casting methods. Ferro [48] tensile samples were almost identical revealing similar kind of failure
found that 2.106 cycles of fatigue strength was achieved with AlSi10Mg mechanism.
alloy and lack of fusion defects were found to be the root cause of fail­ Tillova [3] had suggested that a better understanding of mechanical
ures. Bagherifard [49] reported the unmolten particles and agglomer­ property of recycled alloys has to be studied. Energy savings, environ­
ates in AlSi10Mg that resulted in lowered ductility. However, by T6 heat mental issues have led to the use of recycled materials in many appli­
treatment, spheroidization of Si had revealed an increase of 400% cations. In this, for the first time to the knowledge of the authors,
ductility. Uzan [50] reported similar findings where post processing was recycled properties of AM produced AlSi10Mg was compared with AM
the key to enhance mechanical properties. Rosenthal [51] used 300 ◦ C as and cast alloy. The loss of material during melting, microstructural
the modified T5 compare to 200 ◦ C T5 and found that tensile properties changes and tensile properties were statistically evaluated.
were increased by 64%. However, after HIP, tensile properties were
decreased. Hirata [52] also looked into the effect of HIP, and significant 2. Experimental work
decrease in yield and tensile properties were observed although micro­
structure was not changed. Liu [53] showed that primary dendrites were AlSi10Mg specimens were fabricated by Laser Powder Bed Fusion
elongated in columnar structure along the laser direction that was sur­ (LPBF) technique using the EOS M 290 metal AM system. The average
rounded by fine eutectic Si phases, and thus, inhomogeneity was grain size of the AlSi10Mg powder used for the fabrication is 47 μm. The
occurred in the microstructure. Takata [54] concluded that strength was SEM microstructure of the powder is shown in Fig. 1. The powder is
independent of microstructure but ductility was orientation related. spherical in shape and its chemical composition is given in Table 1. The
Barile [55] used recycled powders to produce AM parts from AlSi10Mg production parameters used in this study are given in Table 2.
alloy and reported that there was no significant effect on the mechanical Tensile specimens whose design has been completed and scrap parts

Table 1
Chemical composition of AlSi10Mg powder (wt %).
Si Fe Cu Mn Mg Ni Zn Pb Ti Al

9.8 0.14 0.02 <0.01 0.36 0.01 <0.01 <0.01 0.01 Rest

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M. Coşkun et al. Materials Chemistry and Physics 289 (2022) 126411

Thus, based on the values given in Table 2, the energy calculation


was found to be 49.93 J/mm3.
The tensile samples used in the study were designed in the CATIA V5
3D design program. As in Fig. 2, the tensile specimens are positioned on
the production ZX or ZY axis, the dimensions are in accordance with
ASTM E8, the length is 90 mm, and the outer diameter is 12 mm. 10
samples were produced for statistical analysis purposes.
Non-compliance with the production system design criteria, inability
to clean the dense support structure, deformation of the parts due to
temperature differences in the thermal gradient, incompatibilities that
occur during testing of different parameters are among the reasons that
cause scrap parts. In this study, besides scrap parts, support structures
were also used for recycling. Support structures are used in the LPBF to
connect the part to the building platform [57], to provide heat con­
duction, to carry the part and to prevent deformations [58]. After pro­
duction, these support structures are removed with the CNC and hand
tools and even become non-functional. It is known that approximately
Fig. 3. Recycled materials in the crucible before melting (a) AM, (b) Ingot.
50 kg of 650 kg AlSi10Mg powder, which has been used in production
for 4 years, consists of non-functional support structures and scrap parts.
The melting experiments were carried out in ICS induction furnace.
The charge was weighed and placed in A50 crucible (Fig. 3). When the
temperature was at 750 ◦ C, the dross was skimmed off and weighed.
Then, the melt was poured into resin bonded sand mould (Fig. 4) where
10 cylindrical bars were produced (Ø9 by 180 mm). The samples were
subjected to T6 heat treatment: solutionizing at 540 ◦ C for 6 h,
quenching at 80 ◦ C and 4 h of artificial aging at 160 ◦ C. Samples were
machined and subjected to tensile testing at Zwick Roell 250 kN ac­
cording to ASTM E− 8. Weibull statistical analysis and survivability plots
were used to evaluate the reliability and reproducibility of the condi­
tions where 10 samples were produced in each parameter.

Fig. 4. CAD drawing of tensile test samples produced by casting (cylinder 3. Results
dimension: 9 mm diameter, 180 mm length).
Before starting the tensile tests, samples were analyzed by X-ray
are produced by the LPBF powder bed fusion method using AlSi10Mg using YXLON MU-2000. No apparent porosity was observed in X-ray
powder. EOS M290 machine and standard process parameters in Table 1 analysis as can be seen in Fig. 5.
were used in the production of these parts. The production of the parts Microstructural analysis was carried out and the images are given in
was carried out in an Argon atmosphere in order to prevent the oxida­ Fig. 6 for ingot castings, AM and recycled AM samples. It can be seen
tion of the aluminum alloy. that the dendritic structure was finer in ingot castings with SDAS value
The energy required for the production and sintering of AlSi10Mg of 24.1 ± 4 μm compared to SDAS of 33.1 ± 5 μm of recycled AM
powder is provided by fiber laser. Energy input value in the AM tech­ castings. The Si morphology was almost the same for both parameters
nologies is calculated by Equation (1). In this formula, LP and Lss with fine and modified fibrous structure. However, beta-Fe intermetallic
represent laser power and laser scan speed, Hd and Lt, respectively, the phases were found in ingot castings whereas alfa-Fe intermetallic was
scanning range and layer thickness [56]. seen in recycled AM castings. OES analysis was carried out on the
( ) samples after the recycling tests and the chemical composition of the
E
J
=
LP (W)
( ) (1) alloys are given in Table 3. The major difference between the alloys
mm3 Hd (mm)∗Lt (mm)∗Lss mms appears to be in Ni and Ti content. In the recycled AM, Ti is quite low as
0.009 wt% whereas it is 0.025 in recycled ingot. Ni content is 0.028 in

Fig. 5. X-ray images of machined parts (a) recycled AM, (b) ingots (sample dimension: Ø8 x 160 mm).

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M. Coşkun et al. Materials Chemistry and Physics 289 (2022) 126411

Fig. 6. Microstructures of (a) ingot castings, (b) AM, and (c) recycled AM.

Table 3
OES analysis of recycled alloys.
Si Fe Cu Mn Mg Cr Ni Ti Al

Ingot 9.65 0.55 0.079 0.052 0.239 0.015 0.007 0.025 Rem.
AM 9.44 0.35 0.006 0.011 0.256 0.018 0.028 0.009 Rem.

recycled AM, it is 0.007 wt% in the ingot. In the vertical section of the Weibull analysis were made on the tensile test results. From the
AM samples, approximately 200 × 50 μm melt pool were found which is characteristic value and Weibull modulus, survivability plots were made
similar to the findings in literature [59,60]. for YS, UTS and elongation at fracture. These graphs can be seen in

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M. Coşkun et al. Materials Chemistry and Physics 289 (2022) 126411

Table 4
Characteristic tensile properties from Weibull analysis.
Yield stress Tensile stress Elongation at fracture
(MPa) (MPa) (%)

AM 221.7 415.8 5.15


AM recycled 179.1 247.4 3.16
Ingot 212.3 250.8 1.51
recycled

recycled AM had the lowest YS value of 179.1 MPa. As it can be seen


from Fig. 7, ingot castings have the lowest value of 165 MPa which is
higher than recycled AM. However, the reproducibility was low with
high scatter of YS changing between 165 and 225 MPa.
For the UTS values, ingot and recycled AM have almost the same
value with same scatter and reliability with an average of 250 MPa. On
the other hand, AM has significantly higher UTS value of 415.8 MPa.
Silvestri [61] had used three different commercially available equip­
ment and looked into the effect of building angle on the tensile prop­
Fig. 7. Survivability plot of yield stress. erties. UTS values were found be ranging between 350 and 380 MPa for
AlSi10Mg alloy regardless of the device and no effect of the building
angle was reported.
Elongation at fracture is the highest in AM: 5.1%. Ingot castings has
the same reproducibility showing the same slope as AM but an average
of 1.51% which is almost 5 times lower. The recycled AM results exhibit
the highest scatter where elongation value varies between 0.5 and 6%
which reveals that the reliability is significantly low in the recycled AM
for elongation at fracture.
From the Weibull analysis, the characteristic values of test parame­
ters were measured, and the summary is given in Table 4. It can be seen
that after recycling, yield stress of AM was decreased 20.6% whereas the
difference between AM and ingot was only 6.7%. Comparing the yield
stress of ingot and recycled AM, it can be seen that there is a 14.8%
decrease for recycled AM. For the ultimate tensile strength, AM has the
highest value of 415.8 MPa which is approximately 42.5% higher than
recycled AM and the ingot castings. For the elongation at fracture
values, AM again reveals the highest value of 5.15%. Ingot castings had
the lowest value of 1.51% which is 73.1% lower than AM. On the other
hand, recycled AM test results show that the characteristic elongation at
fracture was 3.16% which is 45.4% lower than AM but 50.7% higher
Fig. 8. Survivability plot of ultimate tensile stress.
than ingot casting.
Piette [62] had found that yield stress, ultimate tensile, hardness and
elongation was significantly improved compared to cast alloy. They
reported about 64% increase in YS, 60% increase in UTS and 45% in­
crease in elongation but only in horizontal build direction. In vertical
build direction, elongation at fracture values of AM and cast were the
same. Shakil [63] has used three different cooling regimes after solution
heat treatment in AM manufactured AlSi10Mg alloy. It was found that
furnace cooled samples had the highest plasticity with the lowest
indentation strength followed by air cooled samples. Water quenching
and as fabricated samples had similar micromechanical properties.
These results were also compared with castings. Water- and air-cooled
cast samples had exhibited better micromechanical properties than
AM manufactured samples. On the hand, as fabricated AM plasticity was
lower than cast samples.
SEM images were taken from the cross-section of the fracture sur­
faces of tensile test samples. In Fig. 10 a and b, dendritic structure can be
clearly seen which is an indication of porosity in the samples produced
by casting of ingots [64–67]. Additionally, beta-Fe intermetallic phases
were observed which were associated with porosity (indicated by ar­
rows). Fe phases in the microstructural analysis (Fig. 6) were also
Fig. 9. Survivability plot of elongation at fracture.
observed in SEM. Several works [3,4] had reported the detrimental ef­
fect of Fe phases that decreased the ductility of Al–Si alloys.
Figs. 7–9. Similar kind of porosity and dendrites were also observed in recycled
Based on the survivability plot of YS, it can be seen that AM has the AM samples as well (Fig. 10 c and d). Occasionally, clusters of spherical
highest reproducible results with an average of 221.7 MPa. Ingot cast­ particles sizes ranging between 6 and 50 μm were also observed on the
ings revealed 212.3 MPa which was very close to AM. On the other hand,

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M. Coşkun et al. Materials Chemistry and Physics 289 (2022) 126411

Fig. 10. SEM images of the fractured surfaces of (a and b) ingot, (c and d) recycled AM.

fracture surface (Fig. 10 d). This reveals that some of the particles had Due to the high surface area compare to the weight of spherical
possibly remained unmelted due to the surface tension of the spherical particles of AM structure, after recycling, the material loss to dross was
particles having been oxidized and thus remained in the structure. This around 17% for recycled AM which was around 3% for the recycled
is most likely the reason for the scattered elongation at fracture values ingot.
for recycled AM (Fig. 9). After recycling of AM, some unmelted spherical particles in the size
The weight of material charged, and the amount of dross collected of 6–56 μm were observed in the fracture surface of tensile samples that
was measured. Both charges were selected to start with approximately 3 lead to scattered ductility.
kg. It was found that the amount of dross in the ingot was 84 gr, whereas AM produced AlSi10Mg exhibits the highest tensile test values
the dross collected from AM recycling was 494 g. Thus, it was recorded compare to cast and recycled AM. The difference is approximately
that AM material loss was 17.1% and it was 2.9% for the ingot. There is doubled for all values. The reliability and reproducibility of the me­
almost 6 folds of difference in the material loss. The main reason could chanical properties of AM was significantly high with almost no scatter
possibly be the high surface are of the AM recycling materials as seen in at all.
Fig. 3. Kvithyld [13] had reported similar results with the coated Ultimate tensile value of recycled AM is similar to cast alloy. How­
aluminum sheets. When the coatings were not removed prior to ever, YS was decreased by 15% with 50% increase in elongation
remelting, the material loss was up to 40%. Also, it was reported that compare to cast alloy. On the other hand, recycled AM had 50% lower
during recycling of sheets, due to the heat generated during melting, the UTS and elongation at fracture compare to AM.
oxide layer on the surface of the sheets were thickening and thereby
leaving less metal to be melted to be collected in the crucible. CRediT authorship contribution statement

4. Conclusion Mert Coşkun: Investigation, Formal analysis. Kerem Can Dizdar:


Investigation, Formal analysis. Gürkan Tarakçi: Investigation, Formal
Recycling of aluminum alloys have gained a lot of attention due to analysis. Gökhan Özer: Conceptualization, Methodology, Resources,
environmental factors and sustainability issues. The use of secondary Validation. Derya Dispinar: Conceptualization, Methodology, Super­
aluminum is increasing. Additive manufacturing has great advantages vision, Validation.
such as the ability to produce complex geometry with minimal material
loss compared to the use of runner and feeder in cast parts. Therefore, in Declaration of competing interest
this work, the recycling of AM manufactured AlSi10Mg alloy was
investigated. The material loss as well as the microstructural and me­ The authors declare that they have no known competing financial
chanical property change was evaluated. interests or personal relationships that could have appeared to influence

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