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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.
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. 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.
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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.
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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665
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.
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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665
5. Conclusions
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C.G. Wang, J.X. Zhu, G.W. Wang et al. Journal of Alloys and Compounds 895 (2022) 162665
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Declaration of Competing Interest [23] C. Gao, Z. Liu, Z. Xiao, W. Zhang, K. Wong, A.H. Akbarzadeh, Effect of heat
treatment on SLM-fabricated TiN/AlSi10Mg composites: microstructural evolu
The authors declare that they have no known competing fi tion and mechanical properties, J. Alloy. Compd. 853 (2021) 156722.
[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.
[25] K. Kempen, L. Thijs, J. Van Humbeeck, J.P. Kruth, Mechanical properties of
Acknowledgments AlSi10Mg produced by selective laser melting, Phys. Procedia 39 (2012)
439–446.
[26] N. Takata, H. Kodaira, K. Sekizawa, A. Suzuki, M. Kobashi, Change in micro
This work was supported by NSAF (grant number U1930207) and structure of selectively laser melted AlSi10Mg alloy with heat treatments, Mater.
CAEP Foundation (grant number CX20210005). Sci. Eng. A 704 (2017) 218–228.
[27] L. Thijs, K. Kempen, J.P. Kruth, J. Van Humbeeck, Fine-structured aluminium
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