materials
Article
A Comparative Study on Microstructure, Segregation,
and Mechanical Properties of Al-Si-Mg Alloy Parts Processed
by GISS-HPDC and SEED-HPDC
Guo-Chao Gu 1,2,3, * , Li-Xin Xiang 1,2 , Rui-Fen Li 4 , Wen-Hua Xu 1,2 , Hong-Liang Zheng 1,2 , Wen-Hao Wang 5
and Yu-Peng Lu 1,2, *
Citation: Gu, G.-C.; Xiang, L.-X.; Li,
R.-F.; Xu, W.-H.; Zheng, H.-L.; Wang,
W.-H.; Lu, Y.-P. A Comparative Study
on Microstructure, Segregation, and
Mechanical Properties of Al-Si-Mg
Alloy Parts Processed by GISS-HPDC
and SEED-HPDC. Materials 2023, 16,
6652. https://doi.org/10.3390/
ma16206652
Academic Editor: Carlos
Garcia-Mateo
Received: 29 July 2023
Revised: 3 October 2023
Accepted: 3 October 2023
Published: 11 October 2023
Copyright: © 2023 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Materials 2023, 16, 6652. https://doi.org/10.3390/ma16206652
1 Key Laboratory for Liquid-Solid Structural Evolution and Processing of Materials, Ministry of Education,
Shandong University, Jinan 250061, China; 202034221@mail.sdu.edu.cn (L.-X.X.);
xuwh2009@sdu.edu.cn (W.-H.X.); honglz@126.com (H.-L.Z.)
2 School of Materials Science and Engineering, Shandong University, Jinan 250061, China
3 Suzhou Institute, Shandong University, Suzhou 215123, China
4 Shandong Institute for Product Quality Inspection, Jinan 250102, China; liruifen2016@163.com
5 School of Materials Science and Engineering, Shandong Jianzhu University, Jinan 250101, China;
a3068880370@163.com
* Correspondence: guochaogu@sdu.edu.cn (G.-C.G.); biosdu@sdu.edu.cn (Y.-P.L.)
Abstract: There are multiple routes to prepare semi-solid slurries with a globular microstructure
for semi-solid forming. The variations in the microstructure of semi-solid slurries prepared using
different routes may lead to significant differences in the flow behavior and mechanical properties
of rheo-diecasting parts. Therefore, it is crucial to have a comprehensive understanding of the mi-
crostructure evolution associated with different slurry preparation routes and their resulting effects.
In this study, the gas-induced semi-solid process (GISS) and the swirl enthalpy equilibrium device
(SEED) routes were employed to prepare semi-solid Al-Si-Mg slurries for their simplicity and pro-
ductivity in potential industrial applications. The prepared slurries were then injected into the shoot
sleeves of a high-pressure die casting (HPDC) machine to produce tensile test bars. Subsequently, the
bars underwent T6 treatment to enhance their mechanical properties. The microstructure, segregation,
and mechanical properties of the samples were investigated and compared with those of conventional
HPDC. The results indicated that the GISS and SEED can produce semi-solid slurries containing a
spherical α-Al primary phase, as opposed to the dendritic structure commonly found in conventional
castings. The liquid fraction had a significant effect on the flow behavior, resulting in variations in
liquid segregation and mechanical properties. It was observed that a higher solid fraction (>75%) had
a suppressing effect on surface liquid segregation. In addition, the tendency for liquid segregation
gradually increased along the filling direction due to the special flow behavior of the semi-solid
slurry with a low solid fraction. Furthermore, under the same die-casting process parameters, the
conventional HPDC samples exhibit higher yield stress (139 ± 3 MPa) compared to SEED-HPDC
and GISS-HPDC samples, which may be attributed to the small grain size and the distribution of
eutectic phases. After undergoing the T6 treatment, both SEED-HPDC and GISS-HPDC samples
showed a significant improvement in yield and tensile strength. These improvements are a result of
solution and precipitation strengthening effects as well as the spheroidization of the eutectic Si phase.
Moreover, the heat-treated SEED-HPDC samples demonstrate higher ultimate strength (336 ± 5 MPa)
and elongation (13.7 ± 0.3%) in comparison to the GISS-HPDC samples (307 ± 4 MPa, 8.8 ± 0.2%)
after heat treatment, mainly due to their low porosity density. These findings suggest that both
GISS-HPDC and SEED-HPDC processes can be utilized to produce parts with favorable mechanical
properties by implementing appropriate heat treatments. However, further investigation is required
to control the porosities of GISS-HPDC samples during heat treatment.
Keywords: GISS; SEED; semi-solid die-casting; mechanical properties
https://www.mdpi.com/journal/materials
Materials 2023, 16, 6652 2 of 16

1. Introduction
High-pressure die-casting (HPDC) technology is a highly productive near-net-shape
forming process used for aluminum and magnesium alloys. It has found applications in
various industries, such as automotive, aerospace, and 5G communications [1,2]. Blisters
may arise during heat treatment due to air entrapment in the die-casting process, rendering
the die-casting parts unsuitable for heat treatment [3]. Consequently, the application of die
castings with high strength is limited. To overcome this situation, several enhanced casting
processes have been developed, such as high vacuum die-casting, semi-solid die-casting
(rheo-HPDC), etc. [4,5]. In the case of semi-solid die-casting, the higher viscosity promotes
a laminar flow of the slurry in the sleeve and cavity, characterized by a reduced occurrence
of issues like oxidation [2], shrinkage [6], and air entrapment [7]. Moreover, compared to
conventional HPDC, rheo-HPDC involves keeping the alloy at a semi-solid temperature for
a long period of time while ensuring a faster cooling rate during the cooling process. As
a result, the constituents become more uniform, and the size of eutectic and intermetallic
phases located near the α-Al phase is reduced. These factors can greatly reduce the solution
time required for the T6 heat treatment [8].
In the rheo-HPDC process, the solid phase and liquid phase exhibit different flow
behavior, which leads to segregation phenomena. Feng [9] utilized the rheo-HPDC tech-
nique to produce Al-6Si-3Cu-0.4Mg aluminum alloy castings. It was suggested that the
variation in liquid fraction between the edge and center of the samples results in different
mechanical properties. Govender [10] investigated the surface segregation phenomenon
of A356 aluminum alloy in die-casting and observed variations in the thickness of the
segregation layer at different positions of the casting. This variation in thickness was found
to enhance the hardness at specific positions, while not significantly affecting the overall
mechanical properties. Segregation in the die-casting process can result in an uneven
microstructure, which can subsequently affect the mechanical properties of the product.
Hence, it is crucial to investigate the segregation behavior during the die-casting process.
One of the key factors affecting rheo-HPDC is the preparation of semi-solid slurries
with a uniform and spherical microstructure. Since Flemings obtained a semi-solid slurry
with primary spherical grains by stirring Sn-15%Pb alloy in the 1970s, researchers have
invented some new methods to prepare semi-solid slurries [11]. Alcan [12] patented
the SEED method, which involves preparing a semi-solid slurry through heat exchange
and eccentric rotation. Wannasin [13] conducted research on the GISS technology, which
enables a uniform distribution of temperature and solute within the melt through argon
convection and stirring of the graphite rods. This technique effectively limits the growth
of dendrites in primary grains. Lv [14] developed the IUV (Indirect Ultrasonic Vibration)
technology, which utilizes the vibratory effect of a horn to produce semi-solid slurries.
Zhu [15] developed the SCP (Serpentine Pouring Channel) technology, where the stirring
effect of the serpentine channel gradually transforms primary grains into nearly spherical
grains. Jain [16] investigated the RSF (Rapid Slurry Formation) technology, which utilizes
an enthalpy exchange material (EEM) for slurry preparation.
Although many researchers have studied the application of GISS and SEED in differ-
ent alloys and demonstrated their potential for industrialization, there are fewer studies
on the two processes in relation to the forming and mechanical properties of the same
alloy. Therefore, the aim of this study is to comparatively investigate the microstructure,
flow behavior, and mechanical properties of the alloy produced by different rheo-HPDC
processes. In this study, the semi-solid Al-Si-Mg alloy slurries were prepared by the GISS
and SEED routes. The prepared slurries were then injected into the shoot sleeves of a
high-pressure die casting (HPDC) machine to produce tensile test bars. Subsequently, the
bars underwent T6 treatment to enhance their mechanical properties. The differences in
the slurry microstructure of the two were examined. The segregation and mechanical
properties of the samples produced by GISS-HPDC and SEED-HPDC were compared and
analyzed.
 Subsequently, the bars underwent T6 treatment to enhance their mechanical propertie
The differences in the slurry microstructure of the two were examined. The segregatio
and mechanical properties of the samples produced by GISS-HPDC and SEED-HPD
were compared and analyzed.
Materials 2023, 16, 6652 3 of 16

2. Materials and Methods

2.1. Materials
2. Materials and Methods
The Al-Si-Mg aluminum alloy used in this study was prepared using purity aluminu
2.1. Materials
(4 N),The
Si (7 N), and
Al-Si-Mg Al-Mg master
aluminum alloy
alloy used (Al-20
in this wt.%
study wasMg). Theusing
prepared alloypurity
was processed
aluminum accordi
to
(4 the procedure
N), Si (7 N), and depicted in Figure
Al-Mg master 1. Thewt.%
alloy (Al-20 aluminum
Mg). Thealloy
alloywas heated toaccording
was processed 720 °C for melti
◦ for melting
and
to theheld at 690depicted
procedure °C for 30 min. It1. was
in Figure then degassed
The aluminum by heated
alloy was addingtoC720
2Cl6Cand held for 15 m
and held at 690 ◦ C for 30 min. It was then degassed by adding C Cl and held for 15 min.
Al-5Ti-B master alloy (1 wt.%) was added to refine the grains, 2 6and the melt was held for
Al-5Ti-B master alloy (1 wt.%) was added to refine the grains,
min before starting the semi-solid slurry preparation. The chemical and the melt was held forof the GI
compositions
15 min before starting the semi-solid slurry preparation. The chemical compositions of the
and SEED slurries were determined separately, as presented in Table 1.
GISS and SEED slurries were determined separately, as presented in Table 1.

Figure 1. Schematic diagram of the Al-Si-Mg alloy preparation process.

Figure 1. Schematic diagram of the Al-Si-Mg alloy preparation process.
Table 1. Chemical composition of Al-Si-Mg aluminum alloy (wt.%).
Table 1. Chemical composition of Al-Si-Mg aluminum alloy (wt.%).
Si Cu Mg Fe Ti Al
GISS Si
6.840 Cu
0.026 0.492Mg 0.027 Fe 0.037 Ti Bal Al
GISS
SEED 6.840
6.45 0.026
0.098 0.492
0.41 0.13 0.027 0.05 0.037Bal Bal
SEED 6.45 0.098 0.41 0.13 0.05 Bal
2.2. Slurry Preparation and Die-Casting
As illustrated
2.2. Slurry in Figure
Preparation and 2a, the slurry preparation route of GISS involved cooling the
Die-Casting
melt by injecting high-purity argon gas at a flow rate of 0.35 m3 /h through a ceramic rod.
As illustrated in Figure 2a, the slurry preparation route of GISS involved cooling t
The ceramic rod was immersed in the melt at a temperature of 625 ◦ C for 4 min, with a
melt by injecting
revolution speed ofhigh-purity
90 r/min and argon gas atspeed
a rotation a flow rater/min.
of 120 of 0.35After
m3/hthe
through
stirring,a the
ceramic ro
The ceramic
slurry was heldrodforwas
85 s.immersed in the melt
After completing at a temperature
the slurry preparation, itof
was625transferred
°C for 4 min,
to with
revolution speed
a shoot sleeve of theofHPDC
90 r/min andfor
machine a rotation speedofofparts
the production 120 with
r/min. Afterinjection
varying the stirring, t
speeds,was
slurry as depicted
held for in 85
Figure 2b. completing the slurry preparation, it was transferred to
s. After
shootDuring
sleevetheofSEED-HPDC
the HPDC process,
machine thefor
melt was
the poured intoof
production a steel
partscrucible at a tem- injectio
with varying
perature of 625 ◦ C. It was then rotated eccentrically at 150 r/min for 100 s. The resulting
speeds, as depicted in Figure 2b.
semi-solid slurry was transferred to the shot sleeve to obtain castings using the same
die-casting process parameters as the GISS-HPDC process.
The details of the T6 heat treatment were as follows: the test bars were subjected to
a solution treatment at a temperature of 540 ◦ C for 0.5 h in a furnace (CGF1200-25) with
a temperature fluctuation of ±1 ◦ C. After the solution treatment, they were quenched in
60 ◦ C water. Subsequently, the quenched bars were transferred to a furnace (DHG-9076A)
with a temperature fluctuation of ±1 ◦ C for aging at 170 ◦ C for 6 h.
Materials
Materials2023,
2023,16,
16,x6652
FOR PEER REVIEW 4 4of of
16 16

Figure
Figure 2. (a) Slurry
Slurrypreparation
preparationand
anddie-casting
die-casting process;
process; (b)(b) Injection
Injection speed
speed curve;
curve; (c) Dimensions
(c) Dimensions of
of the test bar.
the test bar.

2.3. Microstructure Characterization

During the SEED-HPDC and Mechanical
process, the meltProperties Tests into a steel crucible at a
was poured
Metallographic
temperature of 625 °C.samples
It was of then
slurryrotated
and parts were ground,
eccentrically polished,
at 150 r/min and thens.etched
for 100 The re-
using a semi-solid
sulting 0.5% HF solution.
slurry The
was microstructure
transferred to was the observed
shot sleeve using a Nikoncastings
to obtain metallographic
using the
microscope
same (Nikon
die-casting LV100ND,
process Tokyo, Japan).
parameters Phase identification
as the GISS-HPDC process.and fracture morphology
wereTheanalyzed
details of the T6 heat treatment were as follows: the test barsThe
using a JEOL-7610F scanning electron microscope (SEM). werephase analysis
subjected to a
solution treatment at a temperature of 540 °C for 0.5 h in a furnace (CGF1200-25) with
of the samples was conducted by X-ray diffraction (Rigaku, Ultima IV, Tokyo, Japan) with a
Cu-Kα radiation
temperature at a speed
fluctuation 10◦After
of ±1of°C. per minute between
the solution 10◦ andthey
treatment, 90◦ . were
The solid fraction,
quenched in 60
average grain size (D), and average shape factor (F) were analyzed
°C water. Subsequently, the quenched bars were transferred to a furnace (DHG-9076A) using ImageJ software
(Version 1.53t, https://imagej.nih.gov/ij/index.html). The solid fraction (Fs) was estimated
with a temperature fluctuation of ±1 °C for aging at 170 °C for 6 h.
by measuring the volume fraction of the large light gray α-Al grains, which were preserved
during quenching from a semi-solid state. The detailed procedure for the measurement is
2.3. Microstructure Characterization and Mechanical Properties Tests
given in [17]. During the quantitative image analysis, at least 300 grains for the same sample
wereMetallographic samples ofused
measured. The equations slurry
for and parts were
the analysis are ground,
as followspolished,
(Equationsand(1)then
andetched
(2)):
using a 0.5% HF solution. The microstructure was observed using a Nikon metallo-
√
graphic microscope (Nikon LV100ND, ΣTokyo, N
i =1 4A Japan).
i /π Phase identification and fracture
D= (1)
morphology were analyzed using a JEOL-7610F N scanning electron microscope (SEM).
The phase analysis of the samples was conducted √ by X-ray diffraction (Rigaku, Ultima IV,
ΣiN=1 4Ai
Tokyo, Japan) with Cu-Kα radiationFat=a speed of 10° per minute between 10° and(2) 90°.
The solid fraction, average grain size (𝐷), and Pi2 average shape factor (𝐹) were analyzed
using
where ImageJ
Ai is thesoftware (Version
area grains, Pi is the1.53t, https://imagej.nih.gov/ij/index.html).
perimeter of grains, and N and i are the number The solid
of
fraction
grains. (Fs) was estimated by measuring the volume fraction of the large light gray α-Al
grains, which
Figure 2c were preserved
illustrates during quenching
the dimensions of the testfrombars.a Tensile
semi-solid
testsstate.
were The detailed
conducted
using the Zwick-Z250
procedure tensile machine
for the measurement (ZwickRoell
is given GmbHthe
in [17]. During & Co., Ulm, Germany),
quantitative with a
image analysis,
tensile
at leastspeed of 1 mm/min
300 grains (GB/Tsample
for the same 228.1-2010).
were At least two The
measured. samples in the same
equations used conditions
for the anal-
wereare
ysis tested for repeatability.
as follows (EquationsThe (1) Vickers
and (2)):hardness tests were carried out using an MH-3
micro-hardness tester, and the average of 8 data points was measured. A load of 200 gf was
applied and maintained for 15 s on polished 𝛴 samples
4𝐴 (GB/T𝜋 4340.1-2009).
𝐷 (1)
𝑁

𝛴 4𝐴
𝐹 (2)
𝑃
 MH-3 micro-hardness tester, and the average of 8 data points was measured. A load of
200 gf was applied and maintained for 15 s on polished samples (GB/T 4340.1-2009).

3. Results
Materials 2023, 16, 6652 5 of 16
3.1. Microstructure of Al-Si-Mg Alloy in Various Slurry Preparation Routes
Figure 3 compares the microstructure of the Al-Si-Mg aluminum alloys obtained
through
3. Resultsdifferent slurry preparation methods. In Figure 3a, a conventional liquid solidi-
fied microstructure
3.1. Microstructure is depicted,
of Al-Si-Mg Alloy exhibiting a typical
in Various Slurry α-Al dendrite
Preparation Routes morphology with eu-
tecticFigure
Si distributed around the dendrites. On the other hand, Figure 3b,c show the
3 compares the microstructure of the Al-Si-Mg aluminum alloys obtained
semi-solid microstructure
through different slurry preparation prepared by theInGISS
methods. Figureand3a,SEED methods,
a conventional respectively.
liquid solidified These
microstructures
microstructure are characterized
is depicted, exhibiting aby near-spherical
typical α-Al dendrite grains distributed
morphology in the liquid
with eutectic
phase.
Si Table 2around
distributed presentsthe statistical
dendrites. results
On the for thehand,
other two slurry
Figure microstructures, including the
3b,c show the semi-solid
solid volume fraction, average grain size, and average shape
microstructure prepared by the GISS and SEED methods, respectively. These microstruc- factor of α 1-Al grains. The
tures
resultsareindicate
characterized
that the by semi-solid
near-spherical grains
slurry distributed
prepared in theexhibits
by GISS liquid phase. Table 2 of a
characteristics
presents
55% solid statistical
fraction, results for the two
an average grainslurry
size microstructures,
of 105 μm, and including
an average theshape
solid volume
factor of 0.85.
fraction, average
On the other grainthe
hand, size, and average
SEED methodshape results factor
in aof α1 -Alwith
slurry grains. The results
a 75% indicate an av-
solid fraction,
that the semi-solid slurry prepared by GISS exhibits characteristics of a 55% solid fraction,
erage grain size of 95 μm, and an average shape factor of 0.60. Additionally, the α2-Al
an average grain size of 105 µm, and an average shape factor of 0.85. On the other hand,
grains and eutectic Si phase in the slurries prepared by these two methods are also dis-
the SEED method results in a slurry with a 75% solid fraction, an average grain size of
tributed
95 µm, and around α1-Al.
an average Thefactor
shape α2-Alofgrains are formed the
0.60. Additionally, by the solidification
α2 -Al of the Si
grains and eutectic residual
melt during
phase the die-casting
in the slurries prepared by process.
these twoThe grain size
methods of αdistributed
are also 2-Al grains is much smaller com-
around α1 -Al. The
pared to α -Al grains. The number of α -Al grains
α2 -Al grains are formed by the solidification of the residual melt
1 2 in GISS slurry is much
during higher than that
the die-casting
in SEEDThe
process. slurry,
grainassizeshown in Figure
of α2 -Al grains is3b,c.
much Moreover, Figure 3dtoreveals
smaller compared that the
α1 -Al grains. Theconven-
tional HPDC
number of α2 -Alsample
grains in contains
GISS slurrya larger
is much block-like
higher than eutectic
that inSi phase
SEED in addition
slurry, as shown to the
in Figure 3b,c.
plate-like Moreover,
eutectic FigureFrom
Si phase. 3d reveals
Figure that the it
3e,f, conventional HPDC sample
can be observed that most contains
eutectic Si
aphases
larger block-like
in GISS slurry are in the form of long fibers. In contrast, in SEEDFrom
eutectic Si phase in addition to the plate-like eutectic Si phase. slurry, the
Figure
smaller 3e,f, it canpools
liquid be observed
result in that most eutectic
a smaller spaceSifor phases in GISS slurry
the distribution ofare
theineutectic
the formSiofphases,
long fibers. In contrast, in SEED slurry, the smaller liquid pools result in a smaller space
leading to a denser distribution and a smaller size of eutectic Si phases [18]. Based on the
for the distribution of the eutectic Si phases, leading to a denser distribution and a smaller
XRD results of the GISS and SEED samples shown in Figure 4, it can be inferred that the
size of eutectic Si phases [18]. Based on the XRD results of the GISS and SEED samples
π-Fe phase
shown and4,the
in Figure β-Fe
it can be phase
inferredare present
that the π-Fe inphase
the SEED
and the semi-solid
β-Fe phase slurry. However,
are present in the
β-Fe phase is not clearly indicated in Figure 3f due to the excessive
the SEED semi-solid slurry. However, the β-Fe phase is not clearly indicated in Figure 3f density of the eutectic
Si phase.
due to the excessive density of the eutectic Si phase.

Figure3.3.Microstructure
Figure Microstructure obtained
obtained by by different
different preparation
preparation methods:
methods: (a,d) taking
(a,d) taking at 660 ◦at
samplesample C, 660 °C,
(b,e)GISS
(b,e) GISSmethod,
method, (c,f)
(c,f) SEED
SEED method,
method, andand all three
all three samples
samples were water
were water quenched.
quenched.

Table 2. Comparison of α1-Al grains statistics in GISS and SEED slurry microstructure.

Solid Fraction Average Grain Size/µm Average Shape Factor

GISS 55 ± 4.8% 105 ± 3.0 0.85
SEED 75 ± 4.0% 95 ± 4.2 0.60
 Table 2. Comparison of α1-Al grains statistics in GISS and SEED slurry microstructure.

Solid Fraction Average Grain Size/μm Average Shape Factor

Materials 2023, 16, 6652 6 of 16
GISS 55 ± 4.8% 105 ± 3.0 0.85
SEED 75 ± 4.0% 95 ± 4.2 0.60

Figure 4. XRD patterns of semi-solid Al-Si-Mg alloys prepared

prepared by
by GISS
GISS and
and SEED.
SEED.

The morphology of α -Al grains

α1-Al grains prepared by the GISS method is predominantly
spherical, while in SEED, α -Al grains
spherical, while in SEED, α11-Al grains exhibit exhibit aa more
more complex
complex andand irregular
irregular morphology,
morphology,
appearing
appearing near spherical or rosette-shaped. Although both semi-solid slurry preparation
near spherical or rosette-shaped. Although both semi-solid slurry preparation
methods
methods operate
operate under
underaanucleation-controlled
nucleation-controlledmechanism,
mechanism,there areare
there certain differences
certain differencesin
the slurry
in the produced
slurry produced using thethe
using two preparation
two preparation methods.
methods.The useuse
The of aofgraphite
a graphitecrucible in
crucible
GISS results
in GISS in in
results a lower
a lower cooling
coolingrate,
rate,more
moreuniform
uniformtemperature,
temperature,and andsolute
solute distribution
distribution
in
in the melt, leading to the formation of more spherical α1-Al grains. Additionally, GISS
the melt, leading to the formation of more spherical α1 -Al grains. Additionally, GISS
involves
involves aalonger
longerholding
holdingtime,
time,which
which contributes to larger
contributes α1 -Al
to larger α1grains. TangTang
-Al grains. [19] observed
[19] ob-
aserved
significant decrease
a significant in the average
decrease grain size
in the average grainwith
sizeanwith
increasing coolingcooling
an increasing rate, while
rate,
Gu [17] discovered that the grains grew and even developed dendritic
while Gu [17] discovered that the grains grew and even developed dendritic structures structures through
the Oswald
through the ripening mechanism
Oswald ripening with prolonged
mechanism resting time.
with prolonged resting time.
The
The spheroidization mechanism of the GISS process
spheroidization mechanism of the GISS process involves
involves the
the combined
combined stirring
stirring
effect of a stirring rod and argon. This results in a more uniform temperature and solute
effect of a stirring rod and argon. This results in a more uniform temperature and solute
distribution in the melt, leading to nearly equal growth rates in all directions. This uniform
distribution in the melt, leading to nearly equal growth rates in all directions. This uni-
growth is beneficial for the spherical growth of grains [20]. The formation of primary
form growth is beneficial for the spherical growth of grains [20]. The formation of pri-
spherical α1 -Al grains in SEED is influenced by various parameters such as pouring
mary spherical α1-Al grains in SEED is influenced by various parameters such as pouring
temperature and eccentric rotation speed and time. The combined effects of high grain
temperature and eccentric rotation speed and time. The combined effects of high grain
density, slow cooling, and rotational convection reduce temperature and solute gradients
density, slow cooling, and rotational convection reduce temperature and solute gradients
at the solidification interface, allowing grains to grow in a spherical morphology. Qu [21]
at the solidification interface, allowing grains to grow in a spherical morphology. Qu [21]
developed a Phase-Field-Lattice-Boltzmann model to explain the evolution mechanism of
developed a Phase-Field-Lattice-Boltzmann model to explain the evolution mechanism of
spherical grains in SEED slurry. This model helps to reveal the key control factors for the
spherical grains in SEED slurry. This model helps to reveal the key control factors for the
formation of spherical grains and predict microstructure evolution in other processes.
formation of spherical grains and predict microstructure evolution in other processes.
3.2. Microstructure of the Rheo-HPDC Samples
3.2. Microstructure of the Rheo-HPDC Samples
In order to investigate the flow behavior and segregation during the rheo-HPDC pro-
cess, In
theorder to investigate
microstructure the in
changes flow behavior
parts and segregation
of GISS-HPDC during the
and SEED-HPDC rheo-HPDC
were analyzed.
process, the microstructure changes in parts of GISS-HPDC and SEED-HPDC
Figure 5 displays the microstructures at different positions of the part. The observationwere ana-
lyzed. Figure
positions 5 displays
are marked withthe
redmicrostructures
points labeled asat‘a–e’.
different positions
Figure of the
5a–e shows thepart. The obser-
microstructure
vation
of positions areatmarked
the GISS-HPDC differentwith red points
positions, labeled
including asbiscuit,
the ‘a–e’. Figure
runner,5a–e
andshows
variousthe mi-
areas
of the test bar. From the figures, it can be observed that the proportion of α1 -Al grains
gradually decreases along the filling direction of the slurry, and a large number of small
α2 -Al grains surround the spherical α1 -Al grains. On the other hand, Figure 5(a1 –e1 ) illus-
trates the SEED-HPDC microstructures at corresponding positions. It can be seen that the
 crostructure
crostructure of of the
the GISS-HPDC
GISS-HPDC at at different
different positions,
positions, including
including the
the biscuit,
biscuit, runner,
runner, and and
various
various areas
areas ofof the
the test
test bar.
bar. From
From the
the figures,
figures, itit can
can be
be observed
observed that
that the
the proportion
proportion of of
αα11-Al grains gradually decreases along the filling direction of the
-Al grains gradually decreases along the filling direction of the slurry, and a large slurry, and a large
Materials 2023, 16, 6652 number
number of of small
small αα22-Al
-Al grains
grains surround
surround the the spherical
spherical αα11-Al
-Al grains.
grains. On
On the
the other
other hand,
7hand,
of 16
Figure
Figure 5(a
5(a11–e
–e11)) illustrates
illustrates the
the SEED-HPDC
SEED-HPDC microstructures
microstructures at at corresponding
corresponding positions.
positions. It It
can
can bebe seen
seen that
that thethe microstructure
microstructure is is evenly
evenly distributed
distributed in
in all
all positions,
positions, with
with no
no signifi-
signifi-
cant
cant difference
difference is
microstructure in the
the proportion
inevenlyproportion of
of ααin
distributed 11-Al
allgrains.
-Al grains. The microstructure
Thewith
positions, microstructure of
of the
no significant the part
part is
is similar
difference similar
in the
to that of the
to that of the
proportion slurry.
of slurry.
α1 -Al grains. The microstructure of the part is similar to that of the slurry.

Figure
Figure 5.
Figure 5.
5. Microstructure
Microstructureat
Microstructure atdifferent
at differentpositions
different positionsof
positions ofofthe
thethepart
part
part along
along
along the die-casting
thethe
die-casting
die-casting filling
filling direction,
direction,
filling (a)
(a)
direction,
location
location ‘a’;
‘a’; (b)
(b) location
location ‘b’;
‘b’; (c)
(c) location
location ‘c’;
‘c’; (d)
(d) location
location ‘d’;
‘d’; (e)
(e) location
location ‘e’
‘e’ produced
produced byGISS-HPDC;
byGISS-HPDC;
(a) location ‘a’; (b) location ‘b’; (c) location ‘c’; (d) location ‘d’; (e) location ‘e’ produced byGISS-HPDC;
and
and (a
(a11)) location
location ‘a’;
‘a’; (b
(b11)) location
location ‘b’
‘b’ (c
(c11)) location
location ‘c’;‘c’; (d
(d11)) location
location ‘d’;
‘d’; (e
(e11)) location
location (e)
(e) produced
produced by by
and (a1 ) location ‘a’; (b1 ) location ‘b’ (c1 ) location ‘c’; (d1 ) location ‘d’; (e1 ) location (e) produced by
SEED-HPDC.
SEED-HPDC.
SEED-HPDC.
Figure
Figure666presents
presents
presentsaaacomparison
comparison
comparisonof of the
ofthe statistical
thestatistical results
statistical results for
results for the
for the solid
the solid volume
volume fraction,
solid volume fraction,
Figure fraction,
average
average grain
grain size,
size, and
and average
average shape
shape factor
factor of
of αα11-Al
-Al grains
grains in
in different
different positions
positions (shown
(shown
average grain size, and average shape factor of α1 -Al grains in different positions (shown
in
in Figure
Figure 5)
5) prepared
prepared by
by using
using the
the GISS
GISS and
and SEED
SEED methods.
methods. The
The figure
figure shows
shows that
that in
in the
the
in Figure 5) prepared by using the GISS and SEED methods. The figure shows that in
GISS-HPDC
GISS-HPDC process,
process, the
the solid
solid volume
volume fraction
fraction decreases
decreases
the GISS-HPDC process, the solid volume fraction decreases from 40% to around 20%, from
from 40%
40% to
to around
around 20%,
20%, ex-
ex-
hibiting
hibiting aa asignificant
exhibiting significantvariation
significant variationfrom
variation fromthe
from thebiscuit
the biscuitto
biscuit tothe
to theend
the end of
end of the
of the test
the test bar.
test bar. The
bar. The segregation
The segregation
segregation
of
of α
α 1-Al grains during the filling process is observed to be severe. However, the
1 -Al grains during the filling process is observed to be severe.
of α1 -Al grains during the filling process is observed to be severe. However, the average However, the average
average
grain
grain size
size and
and average
average shape
shape factor
factor remain
remain relatively
relatively stable,
stable,
grain size and average shape factor remain relatively stable, ranging from 95–100 µm ranging
ranging from
from 95–100
95–100 μm and
μmandand
0.75–0.85,
0.75–0.85, respectively.
respectively. On
On the
the other
other hand,
hand, in
in the
the SEED-HPDC
SEED-HPDC
0.75–0.85, respectively. On the other hand, in the SEED-HPDC process, the solid fraction process,
process, the
the solid
solid fraction
fraction
is around
isaround
is 75–80%,
around75–80%,
75–80%, thethe average
theaverage grain
average grain size
grain size ranges
size ranges between
ranges between
between 90 90 and
90 and
and 9595 μm,
95 µm,
μm,and and the
andthe average
theaverage
average
shape factor
shape factor
shape is between
factor isisbetween
between0.55 0.55 and
0.55and 0.60.
and0.60. Compared
0.60. Compared
Compared to to the
to the GISS-HPDC
theGISS-HPDC statistics,
GISS-HPDC statistics, the
statistics, the most
the most
most
noticeable difference
noticeabledifference
noticeable differencein in SEED-HPDC
inSEED-HPDC
SEED-HPDCis is that
isthat
thatthethe solid
thesolid volume
solidvolume fraction
volumefraction remains
fraction remains essentially
remainsessentially
essentially
constant,
constant,and
constant, and
andthethe microstructure
themicrostructure demonstrates
microstructuredemonstrates
demonstratesexcellentexcellent uniformity.
excellentuniformity.
uniformity.

Figure 6. Statistical results of α1 -Al in GISS-HPDC and SEED-HPDC samples: (a) solid fraction; (b)
average grain size and average shape factor.

Figure 7 shows the cross-sectional microstructure of the test bar, specifically at position
‘c’ in Figure 6. The microstructure of the SEED-HPDC sample in the cross-section (Figure 7a)
is found to be similar to its microstructure along the filling direction, exhibiting minimal
 Figure
Figure6.6.Statistical
Statisticalresults
resultsofofαα
1-Al ininGISS-HPDC
1-Al GISS-HPDCand
andSEED-HPDC
SEED-HPDCsamples:
samples:(a)
(a)solid
solidfraction;
fraction;(b)
(b)
average grain size and average shape
average grain size and average shape factor.factor.

Materials 2023, 16, 6652 Figure

Figure7 7shows showsthe thecross-sectional
cross-sectionalmicrostructure
microstructureofofthe thetest
testbar,
bar,specifically
specificallyatat 8 po-
ofpo-
16
sition
sition‘c’‘c’ininFigure
Figure6.6.The Themicrostructure
microstructureofofthe theSEED-HPDC
SEED-HPDCsample sampleininthe thecross-section
cross-section
(Figure
(Figure7a) 7a)isisfound
foundtotobebesimilar similartotoitsitsmicrostructure
microstructurealong alongthe thefilling
fillingdirection,
direction,exhib-
exhib-
iting minimal
iting minimal surface
surface segregation.
segregation. However,
However, the the GISS-HPDC
GISS-HPDC sample exhibits different
surface segregation. However, the GISS-HPDC sample exhibitssampledifferent exhibits different
characteristics.
characteristics.
characteristics. TheThe center
center region
region ofofthethe GISS-HPDC
GISS-HPDC sample
sample consists
consists ofofspherical
spherical αα1-Al
1-Al
The center region of the GISS-HPDC sample consists of spherical α1 -Al grains and a large
grains
grains and
and a alarge
large number
number ofofαα 2-Al
2-Algrains.
grains. Moving
Moving towards
towards the
the middle
middle region,
region, thethe
number of α2 -Al grains. Moving towards the middle region, the number of α1 -Al and
number
number ofofαα 1-Al
1-Alandand αα 2-Al
2-Algrains
grains decreases,
decreases, accompanied
accompanied byby the
the presence
presence ofofeutectic
eutectic
α2 -Al grains decreases, accompanied by the presence of eutectic silicon-rich areas. The
silicon-rich
silicon-rich areas. The edge region, which isisinincontact with the
themold wall, primarily
edge region, areas.
whichThe is inedgecontact region,
with the whichmold contact
wall, primarilywithcontains mold wall,
α2 -Al primarily
grains with
contains
contains α -Al
α2α
2 -Al grains
grains with
with only
only a afewfew α α
1-Al
1-Al grains. In addition, Figure 8 shows thestatis-
grains. In addition, Figure 8 shows the statis-
only a few 1 -Al grains. In addition, Figure 8 shows the statistical results for the α 1 -Al
tical
ticalresults
results for
for the
theα 1-Al
α 1-Al grains
grains ofofthetheGISS-HPDC
GISS-HPDC test
testbar.
bar.
grains of the GISS-HPDC test bar. These results indicate a gradual decrease in the solid These
These results
results indicate
indicate a agradual
gradual
decrease
decreasein
fraction inthe
from the solid
22% at fraction
solid fraction
the center from
from
to 5%22% atatthe
22% atthe
the
edgecenter
center toto5%
region. 5%
Dueatatthe
tothe edge
the edge
rapidregion.
region. Due
cooling Due totothe
rate andthe
rapid
rapid cooling
cooling rate
rate and
and high
high liquid
liquid fraction
fraction ininrheo-HPDC,
rheo-HPDC, the
high liquid fraction in rheo-HPDC, the grains did not undergo plastic deformation, therebythe grains
grains did
did not
not undergo
undergo plastic
plastic
deformation,
deformation,thereby
maintaining athereby maintaining
maintaining
microstructure a amicrostructure
similar microstructure
to that of the similar
similar totothat
semi-solid thatofofthe
slurry. thesemi-solid
semi-solidslurry.
slurry.

Figure
Figure7.
Figure Cross-sectional
7.7.Cross-sectional microstructure
Cross-sectionalmicrostructure
microstructureofoftest
oftest
testbars
barsbarsfrom
from from center
center
center totoedge:
to edge: edge:(a)
(a)GISS-HPDC;
GISS-HPDC;
(a) GISS-HPDC; (b)
(b)
(b) SEED-
SEED-HPDC.
SEED-HPDC.
HPDC.

Figure
Figure8.8.
8.Statistical
Statisticalresults
resultsofof
ofααα
1-Al at the cross-section
cross-sectionofof
ofGISS-HPDC
GISS-HPDCtest
testbar.
Figure Statistical results 11-Al at the cross-section GISS-HPDC test bar.
bar.

3.3.
3.3. Mechanical
3.3.Mechanical Properties
Propertiesofof
MechanicalProperties A356
ofA356 Aluminum
A356Aluminum
Aluminumbyby Different
byDifferent Die-Casting
DifferentDie-Casting Methods
Die-CastingMethods
Methods
Table
Table333and
Table and Figure
Figure999show
andFigure show the
showthe mechanical
themechanical properties
mechanicalproperties
propertiesofof the
ofthe test
thetest bars
testbars produced
barsproduced by
producedby
by
conventional
conventional HPDC,
HPDC, heat-treated
heat-treated conventional
conventional HPDC
HPDC (Conventional-HT),
(Conventional-HT),
conventional HPDC, heat-treated conventional HPDC (Conventional-HT), SEED-HPDC, SEED-HPDC,
SEED-HPDC,
and GISS-HPDC in various heat treatment states. The yield strength, tensile strength, and
elongation of the conventional HPDC samples are 139 MPa, 241 Mpa, and 3.7%, respectively.
GISS-HPDC samples exhibit higher yield and tensile strengths of 136 MPa and 266 MPa,
which are 37.4% and 23.7% higher than those of SEED-HPDC samples. Both heat-treated
GISS-HPDC (GISS-HT) and SEED-HPDC (SEED-HT) samples show increased strengths,
but experience reduced elongation. The SEED-HT samples demonstrate yield and tensile
 Yield Strength/MPa Tensile Strength/MPa Elongation/%
Conventional-DC 139 ± 3 241 ± 3 3.7 ± 0.3
Conventional-HT 210 ± 7 266 ± 8 1.6 ± 0.3
SEED-DC 99 ± 4 215 ± 4 15.1 ± 0.1
Materials 2023, 16, 6652
GISS-DC 136 ± 3 266 ± 4 11.6 ± 0.2 9 of 16
SEED-HT 249 ± 6 336 ± 5 13.7 ± 0.3
GISS-HT 240 ± 3 307 ± 4 8.8 ± 0.2
strengths of 249 MPa and 336 MPa, which are 3.8% and 9.4% higher than those of GISS-
HT. Table
Table 4 also compares
4. Comparison the mechanical
of mechanical properties
properties for of the alloys
several Al-Si-based with similar chemical
alloys.
compositions under different forming processes and different heat treatment processes.
YS−UTS−EL
Alloys Forming Process Solution Aging Ref.
MPa−MPa−and
Table 3. Tensile properties of SEED-HPDC % GISS-HPDC parts.
Al-7Si-0.3Mg-0.1Ti-0.1Fe Low-pressure casting 210−285−14.0 540 °C−4 h 155 °C−3 h [22]
Yield Strength/MPa
Semi-solid squeeze cast- Tensile Strength/MPa Elongation/%
Al-7Si-0.4Mg-0.2Ti-0.13Fe-0.1Cu 201−283−8 540 °C−3 h 160 °C−9 h [23]
ing
Conventional-DC 139 ± 3 241 ± 3 3.7 ± 0.3
Al-7Si-0.6Mg-0.13Fe-0.13Ti Conventional-HT
Sand casting 301±−312
210 7 −0.6 550 °C −2 ±
266 h8 180 °C−22 h 1.6 ± 0.3
[24]
Al-8.2Si-0.53Fe-0.46Mg-0.15Cu-0.0 SEED-DC 99 ± 4 215 ± 4 15.1 ± 0.1
HPDC
GISS-DC 136 ±−208.7
129.5 3 −2.2 -266 ± 4 - [25]
11.6 ± 0.2
1Sr
SEED-HT 249 ± 6 336 ± 5 13.7 ± 0.3
Al-8.2Si-0.53Fe-0.46Mg-0.15Cu-0.0
GISS-HT
Rheo-HPDC 240 ±
279.9 3 −12.5
−358.2 535 °C −1 ±
307 h4 175 °C−2.2 h 8.8 ± 0.2
[26]
1Sr

Figure
Figure 9.9. Tensile
Tensileproperties
propertiesof of
SEED-HPDC
SEED-HPDC and GISS-HPDC
and parts:
GISS-HPDC (a) stress−strain
parts: curve;
(a) stress−strain (b)
curve;
strength and and
(b) strength elongation values
elongation of the
values of parts.
the parts.

TableFigure 10 reveals
4. Comparison the evolution
of mechanical of microhardness
properties in the alloys.
for several Al-Si-based cross-sectional direction,
ranging from the edge (0 mm) to the center (3.2 mm) of the samples. It is observed that as
YS−UTS−EL
Alloys Forming Process Solution Aging Ref.
MPa−MPa−%
Al-7Si-0.3Mg-0.1Ti-0.1Fe Low-pressure casting 210−285−14.0 540 ◦ C−4 h 155 ◦ C−3 h [22]
Semi-solid squeeze ◦ C−3 ◦ C−9
Al-7Si-0.4Mg-0.2Ti-0.13Fe-0.1Cu 201−283−8 540 h 160 h [23]
casting
Al-7Si-0.6Mg-0.13Fe-0.13Ti Sand casting 301−312−0.6 550 ◦ C−2 h 180 ◦ C−22 h [24]
Al-8.2Si-0.53Fe-0.46Mg-0.15Cu-0.01Sr HPDC 129.5−208.7−2.2 - - [25]
Al-8.2Si-0.53Fe-0.46Mg-0.15Cu-0.01Sr Rheo-HPDC 279.9−358.2−12.5 535 ◦ C−1 h 175 ◦ C−2.2 h [26]

Figure 10 reveals the evolution of microhardness in the cross-sectional direction,

ranging from the edge (0 mm) to the center (3.2 mm) of the samples. It is observed that as
the distance from the surface decreases, the microhardness increases. At the center region,
the microhardness values for the GISS-DC, SEED-DC, GISS-HT, and SEED-HT samples
are 59 HV0.2 , 59 HV0.2 , 94 HV0.2 , and 109 HV0.2 , respectively. Similarly, at the edge region,
the values are 75 HV0.2 , 74 HV0.2 , 109 HV0.2 , and 123 HV0.2 for the respective samples.
The GISS-HT and SEED-HT samples both exhibit an increase in microhardness, which
is consistent with their performance in terms of strength. Furthermore, the difference in
microhardness between the SEED-DC and GISS-DC samples is not significant, indicating
that the hardness test is not affected by defects like porosity and oxidation. The higher
 gion, the microhardness values for the GISS-DC, SEED-DC, GISS-HT, and SEED-HT
samples are 59 HV0.2, 59 HV0.2, 94 HV0.2, and 109 HV0.2, respectively. Similarly, at the edge
region, the values are 75 HV0.2, 74 HV0.2, 109 HV0.2, and 123 HV0.2 for the respective sam-
ples. The GISS-HT and SEED-HT samples both exhibit an increase in microhardness,
Materials 2023, 16, 6652 which is consistent with their performance in terms of strength. Furthermore, the dif-
10 of 16
ference in microhardness between the SEED-DC and GISS-DC samples is not significant,
indicating that the hardness test is not affected by defects like porosity and oxidation. The
higher microhardness
microhardness obtainedobtained in the
in the edge edgeofregion
region of all can
all samples samples can be attributed
be attributed to the
to the presence
presence of a relatively higher eutectic phase enriched in alloying
of a relatively higher eutectic phase enriched in alloying elements [27]. elements [27].

Figure 10. Evolution of microhardness

microhardness from edge to center of
of the
the studied
studied parts
parts in
in the
the different
different states.
states.

4.
4. Discussion
Discussion
4.1. Segregation during Die-Casting
4.1. Segregation during Die-Casting
The microstructure distribution in the rheo-HPDC process varies depending on the
The microstructure distribution in the rheo-HPDC process varies depending on the
solid fraction of the semi-solid slurry, as shown in Figures 5 and 7. The flow characteristics
solid fraction of the semi-solid slurry, as shown in Figures 5 and 7. The flow characteris-
of semi-solid slurry can be categorized into liquid-like slurry and solid-like slurry [28].
tics of semi-solid slurry can be categorized into liquid-like slurry and solid-like slurry
The semi-solid slurry prepared by GISS is considered a liquid-like slurry with a low solid
[28]. The semi-solid slurry prepared by GISS is considered a liquid-like slurry with a low
fraction and flow behavior similar to a liquid. In this type of semi-solid slurry, there is
solid fraction and flow behavior similar to a liquid. In this type of semi-solid slurry, there
minimal interaction between α1 -Al grains. Figure 11a illustrates the segregation model
is minimal interaction between α1-Al grains. Figure 11a illustrates the segregation model
of the GISS-HPDC process. As the filling pressure decreases during the filling sequence,
of the GISS-HPDC process. As the filling pressure decreases during the filling sequence,
α1 -Al grains in the flowing slurry forefront lack sufficient driving force to overcome the
α1-Al grains in the flowing slurry forefront lack sufficient driving force to overcome the
viscosity of the residual liquid and fill the designated positions. The liquid phase with better
viscosity ofisthe
flowability residual
squeezed to liquid andforefront
the slurry fill the designated positions.
and edge region, Thetoliquid
leading phaseinwith
a decrease the
better flowability is squeezed to the slurry forefront and edge region,
volume fraction of α1 -Al grains along the filling direction. The edge region, which leading to aisde-
in
crease in
contact thethe
with volume
mold fraction of α1-Al grains
wall, experiences a high along the
cooling filling
rate, direction.
causing The phase
the liquid edge region,
in this
which is
region to in contactrapidly
solidify with the mold
and formwall, experiences
a large number of a high
α2 -Alcooling
grains.rate,
Thecausing the slurry
remaining liquid
phaseα in
with this region to solidify rapidly and form a large number of α2-Al grains. The re-
1 -Al grains rapidly solidifies from the edge to the center, resulting in an increase in
maining slurry
the volume fraction with ofα1-Al grains
α1 -Al grainsrapidly solidifies from
with increasing the edge
distance fromtothe
themold
center,
wallresulting
[29,30].
in an increase in the volume fraction of α 1-Al grains with increasing distance from the
Li [31] prepared a semi-solid slurry with a solid fraction of 25% by the self-inoculation
Materials 2023, 16, x FOR PEER REVIEW 11 of 16
mold wall
method and[29,30]. Li [31]the
die-casted prepared
products, a semi-solid slurry with
and also observed a solid fraction
a decrease of 25%
in the solid by the
fraction
self-inoculation
along method and die-casted the products, and also observed a decrease in the
the filling direction.
solid fraction along the filling direction.
The slurry prepared by SEED belongs to the solid-like slurry. The slurry looks solid
in its static state and becomes thinner when it is sheared. In Figures 5 and 7, the plastic
formation of grains during the SEED-HPDC process was not found. In addition, most
grains were surrounded by a thin liquid layer. This indicates the grains have a slight
connection. The filling of the slurry is driven by the liquid and retains a quasi-uniform
microstructure [32]. The segregation model of the SEED-HPDC is shown in Figure 11b. It
is normal to find slight segregation in the edge region contact with the mold wall.

Figure
Figure11.
11.Segregation
Segregationmodel
modelininthe
therheo-HPDC
rheo-HPDCsamples:
samples:(a)
(a)GISS-HPDC;
GISS-HPDC;(b)
(b)SEED-HPDC.
SEED-HPDC.

Segregation is a common and unavoidable defect in conventional HPDC and

rheo-HPDC processes, which is influenced by elemental contents, structural design,
process parameters, and the solid fraction. Li [30] conducted a study on the segregation
of rheo-HPDC samples of 6061 aluminum alloy with varying Si contents. The study
Materials 2023, 16, 6652 11 of 16

The slurry prepared by SEED belongs to the solid-like slurry. The slurry looks solid
in its static state and becomes thinner when it is sheared. In Figures 5 and 7, the plastic
formation of grains during the SEED-HPDC process was not found. In addition, most
grains were surrounded by a thin liquid layer. This indicates the grains have a slight
connection. The filling of the slurry is driven by the liquid and retains a quasi-uniform
microstructure [32]. The segregation model of the SEED-HPDC is shown in Figure 11b. It
is normal to find slight segregation in the edge region contact with the mold wall.
Segregation is a common and unavoidable defect in conventional HPDC and rheo-
HPDC processes, which is influenced by elemental contents, structural design, process
parameters, and the solid fraction. Li [30] conducted a study on the segregation of rheo-
HPDC samples of 6061 aluminum alloy with varying Si contents. The study found that
liquid-phase segregation improved with increasing Si contents. The pouring temperature
plays a crucial role in the size and morphology of α1 -Al grains, which, in turn, affects their
flow behavior and segregation during the die-casting process. Zhang [33] controlled the
pouring temperature to obtain grains with different morphologies (dendrites and globular
grains) and found that the dendritic structure led to severe segregation in the die-casting
parts. Qi [34] investigated the segregation phenomenon of AC46000 castings at different
wall thickness locations, where different wall thicknesses represented varying cooling rates.
The study revealed that higher cooling rates lead to severe segregation of the primary phase.
Jiao [35] and Gourlay [36] investigated the segregation band on the circular cross-section
of the test bar during the HPDC process and found the position of the segregation band
moved to the mold wall with increasing mold temperature. As the solid fraction increases,
the segregation band varies from poorly defined multiple bands to well-defined single
bands disappearing.

4.2. Difference in Mechanical Properties between GISS-HPDC and SEED-HPDC

Qi [7] produced A356 aluminum alloy parts through the conventional HPDC process.
The yield strength, tensile strength, and elongation of the parts were measured to be
151 MPa, 228 MPa, and 4.3%, respectively. These mechanical property results are consistent
with those obtained in our study. However, due to the limitations of the conventional
HPDC process, subsequent heat treatment was not conducted, which hindered the further
enhancement of the performance of the A356 alloy. In Figure 9, the tensile strengths of
the samples produced by GISS-DC and conventional-DC are higher than those of SEED-
DC. It is evident from Figures 3 and 5 that the microstructure of conventional HPDC
and GISS-DC contains a significant number of fine α2 -Al grains, resulting in an overall
reduction in the grain size of the product. This contributes to the improvement of their
mechanical properties. The strength of the samples is enhanced after T6 heat treatment. This
attributes to solution treatment and artificial aging treatment [37,38]. Solution treatment is
conducted at a high temperature to dissolute Mg-rich phases and promote the homogenized
distribution of elements in the Al matrix. It can also spheroidize eutectic Si. The contribution
of artificial aging to strength depends on the precipitation of the Mg-Si strengthening phase.
Coherent or semi-coherent Mg-Si precipitates a strengthening effect that results from the
Orowan mechanism. The tensile strength of SEED-HT parts is higher than that of GISS-HT
ones. The reasons for the differences in mechanical properties can be discussed in terms of
defects and the microstructure of the test bars.
Figure 12 shows the fracture morphology of GISS-HPDC and SEED-HPDC test sam-
ples in different states. The GISS-DC samples exhibit characteristics of ductile fracture,
including dimples and minor cleavage. On the other hand, the SEED-DC samples display
quasi-cleavage features, with some cleavage and tearing ridges present in their fracture
morphology. In the case of GISS-HT samples, the fracture morphology reveals a large
number of porosities throughout the cross-section. This occurrence of porosities could be
attributed to the low solid fraction during the filling process, which results in air entrap-
ment. Upon reheating the parts to the solution temperature, the high temperature causes
 When the sample is reheated from 𝑇 to a higher temperature 𝑇 during the solu-
tion treatment, the pressure will increase from 𝑃 to a higher pressure 𝑃 . If the pressure
𝑃 exceeds the deformation resistance 𝐹 of the alloy at that temperature, the alloy will
undergo plastic deformation and form blister defects. As the volume of porosity increases,
the pressure 𝑃 will decrease. Additionally, 𝐹 will decrease as the component tempera-
Materials 2023, 16, 6652 12 of 16
ture increases. Once the pressure 𝑃 is smaller than 𝐹 , the growth of porosity will stop.
The porosity level is a critical factor that significantly affects the mechanical properties
of die-casting parts [2]. During tensile tests, the presence of porosity defects can lead to stress
the expansion of entrapped gas, leading to the formation of porosities. The mechanism can
concentration, crack initiation, and propagation, ultimately reducing the mechanical proper-
be explained by Equation (3) [3]:
ties of the part [39]. Notably, the SEED-HTP1 V1 Psamples exhibit minimal porosities on the
2 V2
cross-section of the fracture, indicating that = use
the of a high-solid (3)
fraction semi-solid slurry
T1 T2
results in parts with a denser structure and fewer defects. Consequently, the SEED-HT sam-
where P, V, T represent the pressure, volume, and temperature of the entrapped gas,
ples showcase superior strength and elongation compared to the GISS-HT ones.
respectively.

Figure12.
Figure SEM fractographs
12. SEM fractographsofofGISS-HPDC
GISS-HPDC andand
SEED-HPDC samples
SEED-HPDC in different
samples states: (a,b)
in different GISS-
states: (a,b)
DC; (c,d) (c,d)
GISS-DC; GISS-HT; (e,f)SEED-DC;
GISS-HT; (g,h) SEED-HT.
(e,f)SEED-DC; (g,h) SEED-HT.

When the
Figure sample isthe
13 displays reheated from T1 to of
microstructure a higher temperature
the GISS-HT T2 during the
and SEED-HT solution
samples. Fine
treatment, the pressure will increase from P to a higher pressure P . If the pressure
near-globular eutectic Si particles and α-Al1 were observed in the2 GISS-HT samples.
P2 exceeds the deformation resistance FR of the alloy at that temperature, the alloy will
undergo plastic deformation and form blister defects. As the volume of porosity increases,
the pressure P2 will decrease. Additionally, FR will decrease as the component temperature
increases. Once the pressure P2 is smaller than FR , the growth of porosity will stop.
The porosity level is a critical factor that significantly affects the mechanical properties
of die-casting parts [2]. During tensile tests, the presence of porosity defects can lead to
stress concentration, crack initiation, and propagation, ultimately reducing the mechanical
properties of the part [39]. Notably, the SEED-HT samples exhibit minimal porosities on the
cross-section of the fracture, indicating that the use of a high-solid fraction semi-solid slurry
results in parts with a denser structure and fewer defects. Consequently, the SEED-HT
samples showcase superior strength and elongation compared to the GISS-HT ones.
Figure 13 displays the microstructure of the GISS-HT and SEED-HT samples. Fine near-
globular eutectic Si particles and α-Al were observed in the GISS-HT samples. However,
the SEED-HT samples consist of near-globular eutectic Si particles, needle-shape β-Fe, and
rod-like π-Fe, which were confirmed by EDS analysis as presented in Table 5.

Table 5. EDS quantitative results of β-Al5FeSi and π-Al8FeMg3Si6 (at%).

Fe Phase Al Si Fe Mg
β-Al5 FeSi 72.04 13.43 14.23 0.30
π-Al8 FeMg3 Si6 43.60 32.10 5.30 19.00
 rosities [43]. However, in the Al-Si alloy, the element Fe can have positive effects when
present below the critical content. In this case, the strength, hardness, and
high-temperature properties will increase with increasing Fe contents [44]. Although
Fe-intermetallic compounds were found in the SEED-HPDC samples, the mechanical
properties and elongation of the samples remained high after heat treatment. Future re-
Materials 2023, 16, 6652 13 of 16
search will focus on investigating the Fe content and the morphology of Fe-intermetallic
compounds to further enhance the mechanical properties of the alloys.

Figure13.
Figure 13.Morphology
Morphologyof
ofthe
thesecond
secondphase
phaseafter
afterheat
heattreatment:
treatment:(a)
(a)GISS-HT;
GISS-HT;(b)
(b)SEED-HT.
SEED-HT.

The
Table transformation
5. EDS quantitative of fiber-shaped
results eutectic
of β-Al5FeSi Si into near-globular
and π-Al8FeMg3Si6 (at%). eutectic Si can reduce
the lacerating effect of eutectic Si on the matrix and improve the mechanical properties.
Fe Phase Al Si Fe Mg
Chen [40] investigated the precipitation behavior of Si-containing dispersoids in Al-7Si-
β-Al 5FeSi 72.04 13.43 14.23
Mg aluminum alloys during the solution process and found that part of the Si atoms 0.30
π-Al8FeMg
precipitated 3Si6 form of Si-containing
in the 43.60 32.10
dispersions. 5.30 of these Si-containing
The presence 19.00
dispersions increases the microhardness of the alloys. Chen [24] investigated the effect of
5. Conclusions
different Mg contents on the mechanical properties of the Al-7Si-Mg alloy and suggested
that with
The increasing
tensile testMg contents,
bars of the the densityaluminum
Al-Si-Mg of the Mg-Si strengthening
alloy phases increased.
were successfully manufac-
This
turedenhances the interaction
by GISS-HPDC between the
and SEED-HPDC. Theprecipitated
GISS and SEEDphase and dislocations
methods during
were employed to
deformation, leading to an increase in the yield strength and tensile strength but
prepare semi-solid slurries. After investigating and analyzing the microstructure, segre-a decrease
in the elongation
gation, of the alloy.
and mechanical However,
properties of theexcessive
samples, Mg contents lead
the following to an increase
conclusions in the
were drawn:
number and size of iron-rich intermetallic compounds (π-Al8 FeMg3 Si6 ), which have a
detrimental effect on mechanical properties [41].
The presence of Fe-intermetallic compounds in aluminum alloys can be detrimental as
they can cause damage to the aluminum matrix, create stress concentration, and reduce the
mechanical properties of the aluminum alloy [42]. Furthermore, the β-Fe phase precipitates
before the aluminum grains in the solidification process, resulting in the formation of coarse
and long needle-shaped β-Fe phases. These phases hinder the flow of the melt, leading to
reduced fluidity and the potential for defects like shrinkage and porosities [43]. However,
in the Al-Si alloy, the element Fe can have positive effects when present below the critical
content. In this case, the strength, hardness, and high-temperature properties will increase
with increasing Fe contents [44]. Although Fe-intermetallic compounds were found in the
SEED-HPDC samples, the mechanical properties and elongation of the samples remained
high after heat treatment. Future research will focus on investigating the Fe content and the
morphology of Fe-intermetallic compounds to further enhance the mechanical properties
of the alloys.

5. Conclusions
The tensile test bars of the Al-Si-Mg aluminum alloy were successfully manufactured
by GISS-HPDC and SEED-HPDC. The GISS and SEED methods were employed to prepare
semi-solid slurries. After investigating and analyzing the microstructure, segregation, and
mechanical properties of the samples, the following conclusions were drawn:
1. The dendritic microstructure in conventional HPDC samples can be effectively re-
placed by spherical primary α-Al grains through GISS and SEED methods combined
with rheo-HPDC. The slurry prepared by SEED, which has a lower liquid fraction
(~25 ± 4%), exhibits a smaller grain size (95 ± 4.2 µm) and denser eutectic Si phases
compared to the slurry prepared by GISS. However, the shape factor of the α-Al grains
prepared by SEED (~0.60) is lower as compared to that of GISS (~0.8).
2. The phenomenon of surface liquid segregation is observed in both SEED-HPDC and
GISS-HPDC samples. Furthermore, in the GISS-HPDC samples, there is a gradual
Materials 2023, 16, 6652 14 of 16

increase in the liquid fraction along the filling direction. However, the SEED-HPDC
samples with a low liquid fraction (<25%) in the rheo-HPDC process with proper
process parameters help to minimize the occurrence of segregation. As a result, these
slurries with low liquid fractions enable the production of parts with a more uniform
microstructure.
3. Both heat-treated GISS-HPDC and SEED-HPDC samples exhibit noticeably higher
strength and elongation when compared to conventional HPDC samples. Moreover,
the SEED-HT samples demonstrate superior mechanical properties in comparison to
the GISS-HT samples, owing to their denser structure and reduced porosity. The yield
strength, tensile strength, and elongation of the SEED-HT samples are measured at
249 MPa, 336 Mpa, and 13.7%, respectively.
4. Although good mechanical properties were obtained for the GISS-HPDC samples
after heat treatment, further investigation is needed to minimize porosities during this
process. Additionally, it is important to study the improvement of the shape factor for
primary α-Al grains in SEED slurries and its impact on flow behavior.

Author Contributions: Conceptualization, G.-C.G. and L.-X.X.; methodology, G.-C.G., R.-F.L. and
Y.-P.L.; software, L.-X.X.; validation, G.-C.G., L.-X.X. and R.-F.L.; formal analysis, R.-F.L., W.-H.X. and
H.-L.Z.; investigation, G.-C.G., L.-X.X., W.-H.X. and Y.-P.L.; resources, R.-F.L., W.-H.X., Y.-P.L. and
W.-H.W.; data curation, G.-C.G., L.-X.X. and W.-H.X.; writing—original draft preparation, G.-C.G. and
L.-X.X.; writing—review and editing, G.-C.G. and L.-X.X.; visualization, G.-C.G.; supervision, G.-C.G.;
project administration, G.-C.G. and R.-F.L.; funding acquisition, G.-C.G. and Y.-P.L. All authors have
read and agreed to the published version of the manuscript.
Funding: Project (2021ZLGX01) and (2020CXGC010305) supported by the Key Research and De-
velopment Program of Shandong Province, China; Project (BK20160369) supported by the Natural
Science Foundation of Jiangsu Province, China; Project (No. 51705292) supported by the National
Natural Science Foundation of China (NSFC), China; and Project (ZR201702180340) supported by the
Natural Science Foundation of Shandong Province, China.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The data that support the findings of this study are available from the
corresponding author upon reasonable request.
Acknowledgments: We acknowledge SINOTRUK for the support of die-casting equipment provided
for experiments.
Conflicts of Interest: The authors declare no conflict of interest.

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