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Journal of Alloys and Compounds 895 (2022) 162665

Contents lists available at ScienceDirect

Journal of Alloys and Compounds


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

Effect of building orientation and heat treatment on the anisotropic


tensile properties of AlSi10Mg fabricated by selective laser melting ]]
]]]]]]
]]

⁎ ⁎
C.G. Wang a, J.X. Zhu a,b, G.W. Wang a, , Y. Qin a, M.Y. Sun a, J.L. Yang a, X.F. Shen a, , S.K. Huang a
a
Institute of Machinery Manufacturing Technology, China Academy of Engineering Physics, Mianyang 621900, China
b
School of Mechanical and Electrical Engineering, Nanchang University, Nanchang 330031, China

a r t i cl e i nfo a bstr ac t

Article history: In this paper, we investigated the effects of building orientation and heat treatment temperature on the
Received 22 August 2021 anisotropy of SLM-formed AlSi10Mg specimens. Three different deposition orientations of 0°, 45° and 90°
Received in revised form 17 October 2021 and heat treatment temperatures of 270 °C, 300 °C and 330 °C were used to hold the specimens for 2 h,
Accepted 4 November 2021
followed by furnace cooling. The metallographic organization, fracture morphology, grain size and mor­
Available online 14 November 2021
phology, grain orientation and distribution were characterized by optical microscopy (OM), scanning
electron microscopy (SEM) and electron backscatter diffraction (EBSD). SEM metallographic shows that the
Keywords:
Additive manufacturing white cell structure is eutectic Si where Si grid-like structure distributes around α-Al dendrites. EBSD results
Selective laser melting show that all specimens consist of a large number of grains growing along < 001 > direction, which is the
AlSi10Mg preferred orientation. The organizational changes in grain size, distribution and low-angle grain boundaries
Anisotropy (LAGBS) caused by orientation and heat treatment were analyzed to confirm the anisotropy of the SLMed
Heat treatment AlSi10Mg alloy and to analyze and explain the reasons for the poor plasticity of the 90° orientation. The
Tensile properties present results provide new insights into the effects of deposition direction and heat treatment parameters
on the microstructure and properties of AlSi10Mg alloy prepared by SLM.
© 2021 Elsevier B.V. All rights reserved.

1. Introduction Many researches have been done in additive manufactured


AlSi10Mg, involving the feasibility of manufacturing part [9], pro­
Additive manufacturing has gradually become a vital processing cessing parameters optimization [10], fatigue performance and its
method for customized parts with complex geometries. It is also influences on fatigue mechanism [11], the feasibility of forming
widely used in small batch production due to its low-cost advantage. special structural parts etc. [12]. Through tensile tests, compression
Additive manufacturing applications include aerospace, military creeps tests and forming part cutting, multi-dimensional tests etc.,
equipment, biomedical, mold design, development and testing of the mechanical properties are optimized. In addition, at the present
new products and materials [1–3]. Aluminum alloy, especially the stage, scholars have investigated the mechanical properties and
AlSi10Mg, is commonly used in additive manufacturing [4]. The microstructure characteristics in two different orientations [13]. A
morphology and size of the eutectic silicon phase formed during few scholars have investigated the microstructure characteristics in
solidification of cast AlSi10Mg have a significant influence on the three different orientations [14], and investigated the effect of Si
properties [5,6]. However, problems such as insufficient mechanical morphology on plastic deformation under heat-treated conditions.
properties due to excessive roughness are common in aluminum The adjustment of toughness and plasticity during heat treatment
castings. With the development of laser melting, the effects of rapid explains the anisotropy of the alloy to some extent.
heating and rapid cooling rates during SLM on its properties has Z.H. Xiong et al. [15] think that the anisotropy is caused by melt
attracted much attention [7]. To improve mechanical properties, the pool boundary (MPB), and systematic research has been carried out. It
SLM process addresses the lack of mechanical properties of con­ is concluded that the pores, residual stress and HAZ positioning of
ventionally cast AlSi10Mg [8]. MPB contribute to the weakness of the alloy, and it is believed that the
specimen is placed horizontally. It has a good combination of strength
and plasticity when stretched. Ch et al. [16] studied SLMed AlSi10Mg
and carried out tensile and compression tests to test the correlation

Corresponding authors. between mechanical properties and process parameters. It has been
E-mail addresses: gwwang13s@alum.imr.ac.cn (G.W. Wang),
reported that SLMed AlSi10Mg tensile test pieces with different
xianfeng_shen@163.com (X.F. Shen).

https://doi.org/10.1016/j.jallcom.2021.162665
0925-8388/© 2021 Elsevier B.V. All rights reserved.
C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

forming orientations and analyzes their anisotropy. Their tensile me­ process parameters are determined. Section 2.2 describes the pre­
chanical properties are mainly obtained in the horizontal and vertical paration method and experimental conditions for tensile specimens.
directions, without heat treatment. From the existing research, we can Section 2.3 describes the micro-hardness, SEM (Scanning Electron
be concluded that the AlSi10Mg produced by SLM exhibits anisotropy. Microscope), EBSD (Electron Backscattered Diffraction) and other
In macroscopic view, it shows the difference in mechanical properties. specimen preparation and characterization methods. In this article,
On microscopic level, the SLM-formed AlSi10Mg alloy has a refined letter abbreviations and corresponding numbers will be used to
microstructure. Moreover, the distribution and morphology of the describe specimens, such as HT-270°C-2 h, where HT, 270°C and 2 h
various directions are apparent. stand for heat treatment, heat treatment temperature of 270°C, and
Many additive manufacturing studies show that the columnar heat treatment time of 2 h, respectively. When the 0 °-HT-270°C-2 h
crystals grow epitaxially on micro-level [17]. Epitaxial growth of grains related signs appear, it means that the specimen was built at 0°, and
leads to the anisotropy of mechanical properties as it is related to the was heat-treated at 270°C for 2 h; 90°-As-built represents that it was
orientation of the grains relative to the load: when the load is per­ built at 90° without heat treatment.
pendicular to the forming direction, dislocations accumulate along the
columnar grain boundaries, leading to the formation of microcracks 2.1. Specimen preparation and parameter
along these boundaries, resulting in poor ductility [18,19]. When the
load is parallel to the construction direction, this phenomenon is hin­ The experimental specimens were made by EOS M290 equip­
dered. According to the above-mentioned scholars' research results, ment from Germany, and the raw materials used were Al-10.13Si-
crystal texture also leads to the anisotropic mechanical properties of 0.28Mg-0.04Fe (wt%) powder from AVIC Matte. The powder has the
additive manufacturing specimens. The crystal structure orientation advantages of good fluidity and uniform particle size and is suitable
affects the stress state of grains, leading to anisotropic mechanical for additive manufacturing. To explore the effects on anisotropy of
properties [5,20]. The above findings differ from the current paper. different building orientations and annealing states, with the hor­
According to the distribution of Schmidt factor and texture measured izontal direction as the starting position, the angle of clockwise ro­
by EBSD, the results of this paper show that although there is texture at tation is the deposition direction, and the samples are taken from 0°,
the micro-level, the Schmidt factor distribution shows tiny differences, 45° and 90° directions respectively. Four kinds of heat treatments
which will not significantly affect the mechanical properties. (270°C, 300°C, 330°C, as-built) were set. Under this processing
The research on the anisotropy of AlSi10Mg is mainly focused in condition, the heat-treated specimens are heated in the furnace to
two orientations, horizontal and vertical. Some scholars have paid the corresponding temperature, kept for 2h, and cooled in the fur­
more and more attention to the contrast between inclined forming nace. (Table 1).
and horizontal and vertical forming [5]. In addition, the related re­ Four groups of rectangular AlSi10Mg specimens of x mm × y mm
search cases did not compare the heat treatment state with the as- × z mm were built with EOS M290. The rectangular parts were
fabricated state. They did not show that the heat treatment can horizontally placed according to the coordinate system shown in
eliminate the weld pool boundary or the fuzzy molten pool. The Fig. 1(a). The size of the rectangular parallelepiped specimen is
boundary is a well-known indicator that affects properties, so we 80 mm × 15 mm × 15 mm. The building orientation is parallel, ver­
cannot rule out that the anisotropy can be caused by the grain shape, tical, and inclined at 45° to the long side, and the building orienta­
distribution, and orientation [21,22]. This requires heat treatment of tion is along the Z-axis, as is shown in Fig. 1(b). Before additive
the tensile specimen, combining its macroscopic mechanical prop­ manufacturing, we preheated the substrate temperature up to 35°C,
erty data with microscopic characterization, and further discussion closed the cabin, and filled the interior with high purity argon and
for the reason that may cause anisotropy. exhausted oxygen to ensure the processing environment's stability.
Gao et al. [23] have studied the effect of heat treatment at 460°C Other machining parameters are shown in Table 2.
~540°C of SLMed AlSi10Mg specimens but without different built or­
ientations. In this paper, we systematically studied effect of building
2.2. Tensile test specimen preparation
orientation and heat treatment on the anisotropic tensile properties of
AlSi10Mg fabricated by selective laser melting in different orientations
The rectangular parallelepiped specimens manufactured by SLM
and different low-temperature heat treatment states. Scholars have
were processed into standard tensile test pieces according to the
tested the microstructure and room temperature mechanical properties
dimensional standards shown in Fig. 2. The processed tensile test
of cast and heat-treated AlSi10Mg specimens, and the results have
pieces were shown in Fig. 3. The tensile test was carried out on a
contributed to the study of anisotropy. Various specimens’ tensile
tensile tester at room temperature, and the stretching speed was
fracture morphology and microstructure were observed and analyzed
2.1 mm/min without using an extensometer.
by SEM and EBSD microscopic characterization methods. The speci­
mens' mechanical properties, fracture morphology, and microstructure-
morphology in the above-mentioned three orientations were analyzed. 2.3. Characterization methods and specimen preparation
This research focuses on comparing macroscopic data to confirm the
anisotropy, and the anisotropy shows a trend change at different or­ In the section perpendicular to the tensile direction, 2.5–3 mm
ientations. The reason for the anisotropy is analyzed in combination thick samples were taken for microscopic characterization, as shown
with the microstructure. The attempt to clarify the differences in me­ in Fig. 4. Every specimen was cut at the end of each formed specimen
chanical properties comes from the bath boundary, crystal type, dis­ for SEM (also used to observe metallography), micro-hardness
tribution, and orientation. Furthermore, through a set of heat treatment testing and EBSD. The characterization surface was perpendicular to
parameters optimization, it has been found that for the alloy by SLM the axis of the tensile specimens.
manufacturing, the toughness and plasticity is more in line with the
match's requirements by determining its regularity, plasticity, and Table 1
Orthogonal experiment design and variant sets.
toughness, which can be more accurately adjusted as needed.
Orientation heat treatment 0° 45° 90°
2. Experiments HT-270 °C-2 h √ √ √
HT-300 °C-2 h √ √ √
This chapter will introduce the experiment content. In Section HT-330 °C-2 h √ √ √
As-built √ √ √
2.1, the specimen processing scheme is designed, and the equipment

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 4. Cutting strategy of characterizing specimens.

and distribution of the grains, as well as the fracture surface to


analyze the fracture mechanism.
After the sample was polished to the mirror surface with 3 µm
polishing solution, the surface was cleaned with deionized water
and ethanol. The micro-hardness was tested with 5 N force for 15s.
Three different positions were randomly selected for testing and an
average value was calculated.
The specimens used for EBSD characterization are specimens
Fig. 1. Building orientations of specimens. (a)Specimen building state. (b) Molten pool without the inlay. The process is the same with that for SEM. After
direction in the specimen.
mechanical polishing to mirror level, it needs to be vibration po­
lished for 6–8 h without corrosion. In order to observe the micro­
Table 2
structure of SLMed AlSi10Mg alloy in an all-around way, besides the
SLM parameters for specimen fabrication.
EBSD test pieces shown in Fig. 4, we also cut out a cube from the
Parameter Hatch In fill Recoating Stripe width
specimens with three build angles of As-built and characterized its
Speed 1300 mm/s 1300 mm/s 70 mm/s – three surfaces. So we can see the distribution of crystal grains in
Power 370 W 370 W – – three-dimensional space.
Volume 0.19 mm – – 7 mm
Layer thickness 0.03 mm 0.03 mm – –
3. Results and analysis

This chapter will analyze the macroscopic test and microscopic


characterization results of specimens in three building orientations
and four heat treatment states (heat treatment temperature 270°C,
300°C, 330°C and As-built). In Section 3.1, the tensile test data was
analyzed and compared, including ultimate tensile strength (UTS),
yield strength (YS), elongation value (EV). In Section 3.2, the micro-
hardness data was studied. In Sections 3.3–3.5, we analyzed the
microstructure using optical microscopy, SEM and other equip­
ments. The distribution of Si in the Al matrix and the influence of
Fig. 2. Engineering drawing of specimens used for tensile test. heat treatment temperature on it were primarily analyzed. In addi­
tion, the connection between microstructure and mechanical prop­
erties is established by combining fracture morphology, grain shape
and size, orientation deviation, weave and Schmidt factor distribu­
tion to analyze the strengthening mechanism.

3.1. Mechanical properties

Fig. 5 shows the tensile curves of the specimens. From the end of
the tensile curve in the figure, it is easy to find that the as-built
specimen has no apparent section reduction, but after heat treat­
ment, the section shrinkage is significant. The sequence of the sec­
tion reduction of the specimens was 0° > 45° > 90°.
For the as-built specimens, elongation at fracture of the 0° spe­
Fig. 3. Horizontal and vertically and aslant built tensile specimen orientations. cimen is close to 10.1%, the 45° specimen 8.6% and the 90° specimen
7.0%. Similar to the prefabricated specimens, the elongation at break
Following this the specimens used for SEM were inlaid, the sur­ of the heat treated specimens, 0° > 45° > 90°, is the same with that
face layers were sanded with 320#, 600#, 800#, 1200# and 2000# reported by U. Tradowsky [24]. The elongation at fracture increases
sandpaper, then polished with 9 µm, 3 µm diamond polishing liquid, significantly with increasing heat treatment temperature, but the
and finally polished with 20 nm SiO2 emulsion. The specimens were difference among the three-building orientations becomes less ob­
polished to mirror level, placed in alcohol, vibrated for 10 min in vious. For example, after 330°C heat treatment, the elongation at
ultrasonic, and then etched for 35 s with Keller reagent (95.0% fracture becomes 21.7%, 21.1%, 19.8%, respectively.
deionized water + 2.5% HNO3 + 1.5% HCl + 1.0% HF, volume fraction). As shown in Table 3, the values of yield strength decrease with
We used an optical microscope (OM, ZEISS inverted microscope) to increasing heat treatment temperature, indicating a nonlinear re­
observe the metallurgy, then used SEM to observe the micro­ lationship between heat treatment temperature and mechanical
structure and morphology of the melt pool, the morphology, size properties. Based on this, the mechanical properties of temperature

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 5. Stress-Strain curves of specimens with different build-up directions and post treatment conditions. (a)As-built(b) 270 °C-2 h (c)300 °C-2 h (d)330 °C-2 h.

Table 3 the ductility of 0° specimens is significantly better. This is the same


Tensile properties of samples.
with the conclusion reached by Tobias Maconachie et al., in their
  Direction YS (MPa) UTS (MPa) Elongation (%) study on the effect of build orientation on the quasi-static and dy­
As-built 0° 237.67 464.33 10.1 namic response of SLMed AlSi10Mg [5]. By combining Fig. 5, Fig. 6
45° 250.33 471.67 8.6 and Fig. 7 and analyzing the test data of as-built and heat-treated
90° 228 478.33 7 specimens, the following rules can be found:
270 °C-2 h 0° 198.33 303 13.8
45° 205.33 315 13.2
90° 209.33 320.33 12.5
1. For as-built state, the tensile strength of 90° specimens is about
300 °C-2 h 0° 162 250.67 19.2 5–10 MPa higher than that of 45° specimens, and the tensile
45° 164 253.33 19.0 strength of 45° specimens is about 5–10 MPa higher than that of
90° 167.67 262 16.3 0° specimens. It can be seen that there is a slight difference in the
330 °C-2 h 0° 142.33 221 21.7
tensile strength of the specimens formed at different angles.
45° 143.67 226 21.1
90° 147.33 231.33 19.8 2. For heat-treated state, the tensile strength difference between
different buildings orientations did not change significantly
compared with the as-built. However, the ultimate tensile
between 270°C~ 330°C were fitted using logarithm. The properties of strength of three orientations decreases simultaneously, and the
the alloy can be predicted and designed using this function, as relationship between tensile strength and orientation maintains
shown in Fig. 6(b). 90° > 45° > 0°.
In Fig. 7(a) we analyzed the results of the elongation test. The 3. The yield strength of the specimens built in the three construc­
relationship between the elongation rate and the build angle is tion angles is quite different. With the increase of heat treatment
0° > 45° > 90°. Both the as-built state and the heat-treated state temperature, the yield strength difference in different construc­
follow this trend, and the elongation rate of the 45° specimen is tion angles gradually decreases, positively correlated with the
better than that of the 90° specimen. Similarly, this trend is con­ heat treatment temperature. When heat-treated at 330°C, it
sistent with the maximum strain trend because the expression of tends to be consistent.
elongation is [(L2-L1)/L1]* 100%, and the expression of strain is 4. Heat treatment reduces the yield strength of the 90° specimen to
(L2-L1)/35. Both of them belong to the same trend of properties lesser extent and reduces the yield strength of the 0° specimen to
indicators. The functional relationship between elongation value and greater extent, resulting in the change in material properties. The
heat treatment temperature was obtained by using the same fitting final performance between yield strength and building angle is
method, as shown in Fig. 7(b). 0° > 45° > 90° after heat treatment.
As shown in Fig. 5 and Fig. 6, there are regular differences in 5. Heat treatment improves the elongation of the parts, indicating
tensile strength of specimens at different building orientations, and that the plasticity is improved. The higher the heat treatment

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 6. (a) Ultimate tensile strength and yield strength tests, (b) Function curve.

temperature, the more significant the elongation. However they manifested in tensile strength, yield strength, elongation, maximum
show nonlinear changes. With the increase of temperature, the strain, etc. There is a monotonous relationship among 0°, 45°, 90°,
elongation increases slowly. which accords this alloy's common law: the more vital plasticity, the
6. The process method of 2 h heat treatment adopted in this paper better ductility and the lower strength. However, heat treatment
can regulate the properties of SLMed alloy by adjusting the heat cannot eliminate this anisotropy (nor can it be eliminated under
treatment temperature. Thus, in the range of 270°C ~ 330°C, the low-temperature conditions and short holding times).
properties of the alloys are functionally related to temperature. A It is worth noted that the heat treatment changes the yield
logarithmic nonlinear fitting method fits the following functional strength characteristics of the 0°, 45°, 90° specimens. The relationship
model with an orthogonal distance regression method for itera­ between the yield strength and the building angle is 0° > 45° > 90° in
tive calculations. By this method, the function of UTS/YS/EV and the as-built state. After the heat treatment, it becomes 90° > 45° > 0°,
heat treatment temperature is obtained as shown in Fig. 6(b) and and tends to be consistent along with the temperature increases. The
Fig. 7(b). If we want to produce parts with a UTS of 270 MPa and anisotropy of these properties is eliminated.
better plasticity, we can pass the curve and fitting equation in By controlling the orientation of the building and the heat
Fig. 6. The 0° sample has a better ductility ratio of 45° and 90°, so treatment process, we can obtain multiple parts with the same YS
you can use the heat treatment at 280°C for two hours to get the but different UTS.
0° direction of the sample is what we need. In the formula, a, b
and c are the fitting coefficients, whose values have been in­ 3.2. Micro-hardness
troduced in the corresponding figure. y is the dependent variable,
representing the measured physical quantity, which can be The micro-hardness tests were performed on twelve specimens.
strength or hardness, etc, x is the universal independent variable, The influence of different building angles and heat treatment tem­
the heat treatment temperature. perature on micro-hardness was explored.
The experimental results are shown in Fig. 8(a). There is little
y=a b*ln (x + c) (1)
difference in micro-hardness among 0°, 45°, and 90° specimens.
According to the room temperature tensile test data and analysis Each error bar has an overlapping range, so the average micro-
results, it can be proved that the forming angle of SLMed AlSi10Mg hardness has no apparent law. The surface micro-hardness was ob­
will produce anisotropy to a certain extent. The anisotropy is tained independent of building orientation and was not anisotropic.

Fig. 7. (a)Elongation value tests, (b) Function curve.

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 8. (a) Hardness distribution of different specimens, (b) Function curve.

For different heat treatment temperatures, the hardness of AlSi10Mg pool is approximately 100 µm. The irregular-sized macro pore can be
alloy in As-built is about 125 ± 5 HV, heat-treated at 270°C is about seen in each graph.
95 ± 5 HV, 77 ± 5 HV at 300°C and 70 ± 5 HV at 330°C. It can be At the same time, the density of three orientations was measured
found that the heat treatment results in a significant decrease in the using metallographic method as 99.86% (0°), 99.84% (45°), and
hardness of the SLMed AlSi10Mg alloy. With the increase of the heat 99.89% (90°), respectively, as is shown in Fig. 9. It can be seen that
treatment temperature, the hardness of the AlSi10Mg alloy gradually the difference in building orientation does not affect the density.
became lower, but the decline was reduced. Fig. 10 shows four high magnification optical images (a) - (d)
Similarly, to facilitate the on-demand production of the alloy, based corresponding to the 90° heat treatment state and 90° as-built state.
on the SLM process and heat treatment process used in this paper, we Scanning traces and microspores can be observed on the surface. The
also fitted the function relationship between Vickers hardness and heat morphology of the scanning trace is as broad as about 40–100 µm,
treatment temperature, as shown in Fig. 8(b). It is easy to conclude that and its border shows white and black interphase regions. With the
they are also nonlinear variations of the Logarithmic function. increase of heat treatment temperature, 270°C, 300°C, and 330°C,
there is a tendency of gradually narrowing the track boundary width,
the white and black interphase regions fade away.
3.3. Microstructure The reason for this is that heat treatment changes the distribu­
tion of α-Al and Si phases. The boundary of the melt channel is the
The metallographic, fracture morphology and microstructure fast cooling zone, and the cooling rate inside the melt pool is rela­
characteristics of the alloy were observed by using OM, SEM, EBSD tively small. The different precipitation rates and amounts of Si at
etc. to analyze the relationship between microstructure and me­ the center and the boundary lead to the phenomenon in Fig. 10(d).
chanical properties and explore the anisotropy of tensile properties. After heat treatment, Si precipitates and enriches in the Al matrix,
Fig. 9 shows a local magnification morphology of the cross-section and its distribution is more uniform, as shown in Fig. 10(a), and the
of the tensile specimen under optical microscope. In 0°-built spe­ width of the melt pool boundary becomes small. The higher the
cimen, as shown in Fig. 9(a), a curved section of the molten pool was temperature, the more pronounced the phenomenon as shown in
observed. The cross-sectional size of the melt pool varies, which is Fig. 10(b) and (c).
caused by the different angles between the scan path direction and Specimens with three building orientations were characterized by
the layer cross-section. In the metallographic diagram of the 45° SEM, as shown in Fig. 11. In Fig. 11(a), (c) and (e), the boundary of the
specimen, Fig. 9(b), both the approximately parabolic pool and the molten pool can be seen. In (a) and (c), the melt pool appears as a fish
long strip pool can be observed, which is caused by the observation scale shape, and in (e), the scanning rotation angle is 67°. The boundary
angle. Fig. 9(c) shows melt profiles with different deflection direc­ regions marked in (a), (c) and (e) were observed at high magnification
tions. Significant width differences can be observed in 90°-built spe­ as shown in (b), (d) and (f), and the white Si grid-like was visible. In (b),
cimens. The interlayer rotation angle is 67°, which is determined by the grains are columnar, with a width of about 0.5 ~ 2 µm and a length
the interlayer rotation scanning strategy. The size of a single molten

Fig. 9. OM images of cross-section microstructure of tensile specimen. (a) 0°-as-built,(b) 45°-as-built, (c) 90°-as-built.

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 10. OM images of Cross section microstructure of tensile specimen. (a) 90°-HT-270 °C-2 h,(b) 90°-HT-300 °C-2 h, (c) 90°-HT-330 °C-2 h,(d) 90°-as-built.

of about 1 ~ 5 µm. In (d) and (f), the grid-like structure has equiaxed different lines can be seen on the fracture surface, fish scale traces
shapes with diameters of about 0.5 ~ 2 µm. In addition, it is easy to find exist at 0°, and obvious 67° scan tracks exist at 45° and 90°, as shown
that the white Si grid-like is smaller near the pool boundary and more in Fig. 13(a) (b) (c). The means that the building orientation sig­
prominent near the pool center. The grid-like Si phase is white in the Al nificantly affects the fracture behavior of the specimen.
matrix, which was reported in the study of selective laser melting of As shown in Fig. 14, three heat-treated samples are analyzed in
AlSi10Mg alloy by K. Kempen [25]. the 90° direction. Observation at low magnification showed un-
Fig. 12 shows the high magnification SEM images of morphology melted AlSi10Mg powder particles and micropores defects. Under
at 90° and heat-treated at 300°C. Compared to those without heat high magnification observation, a cluster structure similar to co­
treatment, we can found that the Si is flake-like distributed. At lumnar crystals can be seen at the fractures under low-temperature
300°C, the white Si grid becomes uniform Si particles with sizes heat treatment, which is cell segregation rather than crystal grains.
ranging from several hundred of nanometers to several microns, There are apparent dimples at the fracture shown in Fig. 14 (d)-(f)
indicating that the heat treatment process affects the distribution of and unfused powder in Fig. 14 (b) and micropores in Fig. 14(c); they are
the Si phase in the Al matrix. That explains the phenomenon ob­ commonly found in specimens of various building orientations and
served in Fig. 10 and verifies the conjecture. temperatures. At HT-270°C-2 h, the number of dimples in the fracture
is small and less than 1 µm. At HT-300°C-2 h, more dimples were ob­
served at the fracture surface of the sample, and their sizes were
3.4. Fractography
1–2 µm. Under the hT-330°C-2 h condition, the dimples were bigger,
and their sizes mainly ranged from 1 µm to 4 µm. By analyzing of the
In order to better understand the influence of building orienta­
number and size distribution of dimples, we can conclude that heat
tion and heat treatment on the properties, we studied the fracture
treatment increases the number and size of dimples. With the increase
morphology of the SLMed AlSi10Mg specimen, and the results are
of heat treatment temperature, the size of dimples increases, which is
shown in Fig. 13.
manifested as plasticity enhancement. In this regard, combined with
Fracture surface images of the ruptured specimens taken at higher
the mechanical properties, it can be seen that heat treatment can in­
magnifications are presented in Fig. 13(d)-(f). The red arrows in the
crease the number and size of dimples, which is manifested as plastic
figure show a certain number of surfaces. The formation of destructive
enhancement, tensile strength and yield strength reduction.
surfaces and destructive steps indicate that the fracture of the specimen
may have occurred with the crystal. However, the fracture morphology
shows more relatively deep dimples, so the fracture is ductile. 3.5. EBSD
In addition, the pore and unfused powder were considered to be
caused by the parameter of the SLMed AlSi10Mg process, which may Fig. 15 shows the EBSD inverse pole diagrams (IPF) of SLMed 0°
lead to fracture. There are a few pores on the fracture surface, as as-built AlSi10Mg collected in an extensive range. It shows the three-
shown in Fig. 13(c). With the change of building orientation, dimensional IPF for different building orientations, where (a) (b) (c)

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 11. SEM image of the SLMed specimens. (a)-(b) 0° as-built, (c)-(d) 45° as-built, (e)-(f) 90° as-built.

Fig. 12. SEM image of the 90° SLMed specimens. (a)90° as-built, (b)90° HT-300 °C-2 h.

indicates the deposition directions of 0°, 45°, and 90°, respec­ grain zone. The fine grain size of the melt pool boundary is about
tively. < 001 > directional textures can be easily seen in each graph. It 2–10 µm. At the same time, the grains in the melt channel have a
can be seen from the grain distribution on the upper surface of significant tendency to preferential orientation < 001 > .
Fig. 15(c) that the melt channel fringes are mainly composed of in­ The upper surface of the 0°-as-built shown in Fig. 15(a) and the
ternal coarse grain zone, heat-affected zone, and boundary fine- upper surface of the 45°-as-built shown in Fig. 15(b) have different

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 13. SEM images of the fracture surface of the as-built specimens.

Fig. 14. SEM images of the fracture surface of the heat treatment specimens.

crystal grain shapes and distributions. This is because the detection Combining the EBSD data of the specimen's front surface with 0°
surface of the former is the longitudinal direction of the molten pool. morphology shown in Fig. 15(a), it can be determined that the white
The cross-section is a plane parallel to the growth direction, and the grid-like structure is not the grain boundary but the eutectic Si and
detection surface of the latter is the oblique section of the molten α-Al matrix. The distribution is the cell segregation produced during
pool, that is, a plane that is 45° to the construction direction. crystal growth. The black area is the α-Al matrix, and the white is the

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 15. EBSD inverse pole figure (IPF) maps in three-dimensional views of as-built SLMed AlSi10Mg. (a) 0° built, (b) 45° built, (c) 90° built.

Fig. 16. Comparison and analysis for properties of SLMed FCC structure alloy [16,29–33].

Si phase. Si is distributed in a grid structure in the matrix. The grid been found that 90° has lower elongation and higher UTS than 0°
shape is similar to the overall shape of the crystal grains, but the size when studying the effects of different construction orientations on
is small. It can be concluded from the grain distribution on the upper properties (Fig. 16), contrary to the findings in this paper. In this
surface of Fig. 15(b) that the size of the alloy grains is mostly regard, we analyzed the reasons for such differences.
2–70 µm, while the white grid-like size shown by SEM is about The properties studies of SLMed AlSi10Mg and 316 L with dif­
0.5–2 µm, which also shows that the white grid structure is not ferent orientations show that 316L has better plasticity when built
crystal. along 90°, while AlSi10Mg has better plasticity when constructed
The grain orientation we observed is consistent with the gen­ along 0° [16,29–33]. Both of them were FCC structures and should
erally accepted direction of grain growth [26]. The phenomenon have the same properties characteristics. However, because the α-
occurs in both face-centered cube (FCC) and body-centered cubic Al dendrites are covered by Si lattices when external forces stretch
(BCC) crystals [27,28]. Although the degree and distribution of the them, and then the slip starts, dislocation accumulation of dif­
preferred orientation may be different due to different process ferent degrees is easily formed on the slip surface due to the
parameters, it indicates apparent texture in the fabrication of SLMed presence of Si particles, which hinders slip. Since the 90° con­
AlSi10Mg. structed specimen is stretched along < 001 > and the slip direction
The above phenomenon indicates anisotropy inside the SLM- is < 011 > , the dislocation packing will increase with the develop­
formed parts of AlSi10Mg, and the difference is related to the ment of the slip. However, the 0° constructed specimen is stret­
forming angle. It is proved that for the tensile properties of 0°, 45° ched vertical to < 001 > , and the slip direction is < 110 > , so the
and 90°, the highest tensile strength of 90° may relate to this factor, dislocation pile-up will not increase with slip. More grains in this
because this direction is the growth direction of the columnar direction will have stronger ability to coordinate deformation. That
crystal, and the columnar crystal in this direction has the preferred results in poorer ductility and higher strength when AlSi10Mg is
orientation. However, for many materials with FCC structure, it has constructed along 90°.

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 17. EBSD inverse pole figure (IPF) maps in three-dimensional views of SLMed AlSi10Mg. (a) 0 °-As-built, (b) 0 °-HT-270 °C-2 h, (c) 0 °-HT-300 °C-2 h, (d) 0 °-HT-330 °C-2 h.

In the following we compare the microstructure of the tensile 0° direction account for about 98.05% of the grains with a diameter of
cross-section of the 0° specimens at 270°C, 300°C, and 330°C an­ fewer than 26 µm. The heat treatment reduces the grains with a
nealing heat treatment for 2 h and As-built. The plane of observation diameter of less than 26 µm. The percentage decreases to 97.03%,
is parallel to the building orientation. The distribution of morpho­ 96.96%, and 96.04% at annealing temperatures of 270°C, 300°C, and
logical grains is relatively regular; the inside of the molten pool is all 330°C, respectively, and the proportion of grains larger than 26 µm
narrow and long columnar crystals, the boundary of the molten pool increases simultaneously. Therefore, it can be seen that after heat
is fine equiaxed crystals, and the columnar crystals have no evidence treatment of the 0° sample, the grain diameter greater than 26 µm
of epitaxial growth. From Fig. 17, it can be seen that the size of the increases significantly, and the grain diameter smaller than 26 µm
molten pool is about 100–200 µm, and it is mainly composed of decreases slightly with increasing heat treatment temperature, the
equiaxed crystals and columnar crystals. The columnar crystals in­ percentage of grains larger than 26 µm in diameter increases.
side the molten pool are about 10–20 µm wide. It is 30–60 µm long Comparing the microstructure of the tensile cross-section of the
and exhibits epitaxial growth. The equiaxed crystal size at the 90°-as-built with the 90° heat-treated specimens, the as-built shows
boundary of the molten pool is mainly 2–10 µm in diameter. obvious grain distribution with the preferred orientation of the
The grain distribution of the heat treatment specimen is dif­ scanning trace. This phenomenon can also be seen in the heat-treated
ferent. The boundary of the melt pool is no longer obvious, and a specimen. However, with the increase of heat treatment temperature,
large number of small grains disappear at the boundary. In contrast, the traces of the melt channel gradually fade, and the number of
the narrow columnar crystals in the melt pool become coarse co­ grains with the same orientation inside the melt channel is sig­
lumnar crystals an undeniable feature of epitaxial growth. Among nificantly reduced. Similarly, the size of the columnar crystal increases
them, the grains of the heat-treated at 270°C have obvious grain in the 0° direction, and the grain size and morphology changed after
growth compared with the morphology, Fig. 17(a), Fig. 17(b), but heat treatment (as shown in Fig. (19)), inferring that the heat treat­
there is no obvious change compared with that heat-treated at ment may have caused remelting and recrystallization of the grains.
300°C, Fig. 17(c). That is in line with the research of many other For the specimens built at 90°, as shown in Fig. 20, the grain size
scholars. The following gradient temperature heat treatment of Al­ is 3–72 µm, and the proportion of crystal grains with a diameter of
Si10Mg will not significantly differ in grain size [26,42]. Fig. 17(d) 26 µm or less is about 99.69%, and the balances after heat treatment
shows the grain distribution of the heat-treated specimen at 330°C. at 270°C, 300°C and 330°C are reduced to 99.32%, 99.06%, 98.97%. It
Compared with the morphology, the grains become longer and shows the same law with that of the 0° specimens.
coarser, the grain boundary area decreases, and the intergranular The grain size detected for 0° specimens is the longitudinal section of
bonding force decreases. In macroscopic mechanics, the tensile the columnar crystal, and the crystal grain size detected for 90° speci­
strength decreases and the plasticity increases. mens is the cross-section. The variation range of the small crystal grains
From the grain size distribution diagram shown in Fig. 18(a, b), we of 0° specimens is 96.04%− 98.05% (Fig. 18), and that of 90° specimens is
know that the grain size is in the range of 3–72 µm. From Fig. 18(c), it 98.97%− 99.69% (Fig. 20). It can be judged that the temperature of heat
can be seen that the morphological specimens constructed along the treatment influenced the morphology of columnar crystals.

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 18. Grain size distribution map of the specimens built along the 0° direction.

Fig. 19. EBSD inverse pole figure (IPF) maps in three-dimensional views of SLMed AlSi10Mg. (a) 90°-As-built, (b) 90°-HT-270 °C-2 h, (c) 90°-HT-300 °C-2 h, (d) 90°-HT-330 °C-2 h.

According to Fig. 21, it can be observed that the proportion of of "correlated" grain boundaries (LAGBS) with an orientation angle of
grains with a diameter of fewer than 26 µm is related to the building about 5° was found in each specimen, showing anisotropy. Furthermore,
angle, which is mainly manifested as less 0°, more 45° specimens, this fraction increased dramatically as the heat treatment temperature
and most 90° specimens. This trend is primarily because the de­ increase in As-built. The fraction of the grain boundaries with mis­
tection surface of the 0° specimen is the longitudinal section of the orientation angle around 45° was noticed a little high in 0° building
columnar crystal, 90° is the cross-section of the columnar crystal, orientation specimen. However, lower in 45° building orientation spe­
and 45° is the oblique section. cimen and finally was very flat between misorientation angles around
Combining with the mechanical properties of the alloy and its 25°~45°. AlSi10Mg is FCC material, while a peak at 60° indicates the
microstructure, we obtained the variation pattern of mechanical presence of twinning [34,35]. As can be seen from Fig. 22, there is no
properties with heat treatment. We can also find the variation pattern twinning in SLMed AlSi10Mg alloy. Heat treatment results in an increase
of grain size with different heat treatment. These experimental results in 0°− 15° misorientation, Fig. 22(a)-(d), Fig. 22(e)-(h), Fig. 22(i)-(l).
confirm the existence of fine grain strengthening in the micro­ In Fig. 23, we analyzed the 0°, 45°, 90° building orientation
structure before heat treatment. Under the heat treatment conditions specimens’ LAGBS. The more LAGBS, the higher dislocation density,
described in this paper, the grain will grow, and the growth of the Si the more storage of distortion energy, the higher the grain hardness
phase can also prove that the coexisting solution strengthening in the strength, and the lower toughness. According to this theory, the
microstructure before heat treatment disappears. plastic properties of 90° specimens should be worse, which is con­
The grain boundary evolution was also found to be associated with sistent with the increasing plastic properties of 90°, 45° and 0°
the motion of the slip system. As shown in Fig. 22, the largest proportion specimens shown in the tensile data.

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 20. Grain size distribution map of the specimens built along the 90° direction.

strengthening mechanism and the solid solution strengthening


mechanism will weaken or even disappear after heat treatment.
The Al-Si alloy particles are melted in the selective laser melting
process to reach equilibrium. The Si element is uniformly distributed
in the Al liquid, and the content can reach 7.6%, which is greater than
its maximum saturation of 1.65%. The molten pool is cooled at a rate
of about 106–108 K/s [39], which inhibits diffusion, segregation and
grain growth of alloying elements. The Si phase is supersaturated
and dissolved in the α-Al matrix and enriched in a small area to form
solid solution strengthening and improves the mechanical proper­
ties of the alloy. This coarsening of the Si particles upon providing
time and temperature is attributed to the coalescence of the parti­
cles and Ostwald ripening [40,41]. Ostwald ripening occurs by
atomic diffusion or coalescence,where two or more particles con­
solidate to make a more extensive particle mainly because the atoms
on the particle's surface are energetically more unstable than those
inside the particle [37].
For the Si phase, its enriched shape is related to the growth di­
Fig. 21. Grain size distribution of as-built specimens built along different directions. rection and shape of the crystal grains. The cross-section of the
narrow columnar crystal axis is a grid with a length of 2–5 µm. The
For as-built each orientation, with the increase of heat treatment cross-section of the equiaxed crystal and the narrow columnar
temperature, the LAGBS (0°~15°) gradually increases, and the more crystal is a grid with a diameter of 0.5–2 µm. After heat treatment,
LAGBS, the better plasticity. This is because even though the heat the Si phase dissolves and solid solution strengthening fails,con­
treatment caused the increase in the percentage of LAGBS, disloca­ sistent with Le Zhou et al.[6].
tion density increased. The heat treatment causes the fusion The mechanical properties of Al-Si alloys mainly depend on the
strengthening of the eutectic Si phase initially distributed at the morphology and distribution of Si. The more uniform Si is dis­
grain boundaries of the α-Al matrix, which reduces its influence on tributed in the α-Al matrix, the more effectively the mechanical
the grain dislocation motion, resulting in the softening of the α-Al properties of Al-Si alloys can be improved. The SEM image of the
matrix and the reduction of both UTS and YS of the material. morphology shows supersaturated precipitation. The distribution of
Si in the α-Al matrix is uniformly distributed in a grid shape, and the
properties are suitable. The SEM image of the heat treatment state
4. Analysis and discussion shows that Si is unevenly enriched. The grid-like Si distribution
disappears, indicating that larger Si particles exist in the α-Al matrix,
Based on the above phenomena and data, in the following we the maximum size can reach about 1 µm. The uneven distribution of
analyze the cause of the difference in tensile properties and micro- Si after segregation causes the mechanical properties of the alloy to
hardness of the SLMed AlSi10Mg specimens. decrease because the strengthened phase eutectic Si dissolved. From
This paper's final results differ from those of other literature on the first aspect that the ultimate tensile strength and yield strength
the anisotropic properties of the constitutive orientation and heat gradually decrease with increasing heat treatment temperature.
treatment on additively manufactured parts. However, our results on In addition, according to the theory of fine grain strengthening,
the tensile properties of SLM-formed AlSi10Mg are consistent. the Hall-Petch formula is used to describe the relationship between
Furthermore, the difference in the results may be due to the differ­ grain size and material strength:
ence in process parameters. According to previous studies, the ten­ 1/ 2
= 0 + kd (2)
sile strength of SLMed AlSi10Mg without heat treatment is about
450 MPa, and the yield strength is about 280 MPa [36,37], which is In the formula, d is the crystal grain diameter of polycrystal,
consistent with the results of our work (~460 MPa, ~260 MPa). which represents the friction force preventing dislocation slip, and k
Many studies have shown two strengthening mechanisms for is the influence coefficient of the orientation difference of adjacent
selective laser melting formed AlSi10Mg alloy [38]. On the one hand, crystal grains on the movement of the dislocation. This formula
The Si exists in the form of solid solution in the α-Al matrix, showing explains the correlation between the strength of the material and
a reliable solution strengthening mechanism, and on the other, the the sum of the ideal single crystal yield strength and grain size
formed structure has refined grains and thus offering a fine-grain terms. The larger the grain size, the lower the strength, and the finer
strengthening mechanism. Nevertheless, both the fine-grain the grains, the higher the strength. Because the refined grains will

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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

Fig. 22. The statistical distribution of misorientation angle of each specimen.

increases. The heat treatment process will cause the Si phase to


segregate. Si precipitates from the eutectic structure. The eutectic
structure is reduced and the network Al-Si interface is greatly re­
duced and disappeared. The mechanism to prevent the movement of
dislocations no longer exists, resulting in strengthening failure, so
the resistance to the tensile strength limit is reduced and the plas­
ticity is enhanced. This explains from the third aspect why the ul­
timate tensile strength, micro-hardness and yield strength gradually
decrease with the increase of heat treatment temperature.

5. Conclusions

We studied the effects of heat treatment and construction or­


ientation on the SLMed AlSi10Mg alloy. The tensile properties, mi­
crostructure characteristics and texture of the AlSi10Mg alloy
fabricated by SLM were systematically studied. The following con­
clusions can be drawn:

1. The microstructure of the specimens was similar in three


building orientations. Scan traces, melt pools, columnar crystals,
equiaxed crystals, cellular dendrites, reticulated eutectic Si, and
Fig. 23. The statistical distribution of LAGBS of each specimen. enriched and grown Si particles after heat treatment can be ob­
served in the microstructure.
increase the number of grain boundaries and at the same time 2. EBSD shows grain size has not significantly increased with heat
produce a large number of Al-Si interfaces inside the grains, effec­ treatment, and an < 001 > orientation texture parallel to building
tively reducing movement between dislocations under external orientation can be found in specimen of different orientations.
force. This explains from a second aspect why the ultimate tensile However, the grains are not entirely parallel to the building or­
strength and yield strength gradually decrease with the increase of ientation but slightly deviate from it.
heat treatment temperature. 3. Tensile results of specimens with different orientations and heat
There is also a particular eutectic strengthening mechanism in treatments show that the SLMed alloy is slightly anisotropic, and
AlSi10Mg. In the eutectic reaction, a network of Al-Si eutectic its orientation angle size is inversely related to plasticity. Such
structures will be precipitated to form many Al-Si interfaces, which inverse relationship may be caused by different degrees of dis­
hinder the generation of dislocation movement, so the strength location pile-up in the horizontal and vertical directions because

14
C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665

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[24] U. Tradowsky, J. White, R.M. Ward, N. Read, W. Reimers, M.M. Attallah, Selective
nancial interests or personal relationships that could have appeared
laser melting of AlSi10Mg: influence of post-processing on the microstructural
to influence the work reported in this paper. and tensile properties development, Mater. Des. 105 (2016) 212–222.
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This work was supported by NSAF (grant number U1930207) and structure of selectively laser melted AlSi10Mg alloy with heat treatments, Mater.
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