metals

Article
Microstructure Evolution and Microstructural
Characteristics of Al–Mg–Si Aluminum Alloys
Fabricated by a Modified Strain-Induced Melting
Activation Process
Chia-Wei Lin, Fei-Yi Hung * ID
and Truan-Sheng Lui
Department of Materials Science and Engineering, National Cheng Kung University, Tainan 701, Taiwan;
QQkm0526@gmail.com (C.-W.L.); luits@mail.ncku.edu.tw (T.-S.L.)
* Correspondence: fyhung@mail.ncku.edu.tw; Tel.: +886-6-2757575-31395; Fax: +886-6-2346290

Received: 14 November 2017; Accepted: 19 December 2017; Published: 22 December 2017

Abstract: A modified strain-induced melting activation (SIMA) process is shown to improve

high-temperature formability. The microstructural characteristics of the spheroidized grains of
SIMA-processed alloys affect high-temperature formability. The effects of hot extrusion parameters
and chemical composition on the evolution of spheroidized grains were investigated using several
6xxx series aluminum alloys subjected to a modified SIMA process. The results show that 6066
aluminum alloy is the most suitable alloy for the SIMA process, as it contains sufficient Mg, Si, Cu,
and Mn. Adequate amounts of Mg, Si, and Cu lead to a high liquid fraction, and a sufficient addition
of Mn inhibits grain growth. Proper hot extrusion parameters are essential, because initial fine and
uniform recrystallized grains lead to fine and uniform globules. The phases at the global grain
boundaries of 6066 aluminum alloy are eutectic phases of Al and Si, Al and Mg2 Si, and Al and Al2 Cu,
as analyzed using transmission electron microscopy.

Keywords: Al–Mg–Si alloy; strain-induced melting activation (SIMA) process; spheroidized grains

1. Introduction
The semi-solid metal forming process is a hybrid net-shape process that combines the advantages
of forging and casting [1,2]. Magnetohydrodynamic casting, spray casting, and strain-induced
melting activation (SIMA) are commonly used semi-solid processes for producing fine and globular
grains that can enhance high-temperature formability [3,4]. The SIMA process is low-cost and
utilizes stable procedures and simple equipment compared with other semi-solid processes such
as magnetohydrodynamic casting and spray casting [5,6]. The steps of common and traditional SIMA
process are: (1) casting, which produces a dendritic structure; (2) hot work, which disintegrates the
initial structure; (3) cold work, which introduces strain energy into the alloy; and (4) heat treatment,
which makes the material recrystallize and partially melt at the temperature of solid–liquid coexistence.
It is a three-step process because three steps of casting materials are required in order to obtain
globular grains. A modified SIMA process, which has only two steps after casting, is used in the
present study. Its flow is shown in Figure 1a. The two major differences between the traditional SIMA
process and this modified SIMA process are: (1) this modified SIMA process uses severe hot extrusion
instead of cold work to introduce a large amount of strain energy; and (2) this modified SIMA process
uses a salt bath instead of an air furnace to improve heating uniformity and reduce heating time.
Our previous research showed that this SIMA process can promote high-temperature compressibility
and formability, and that the mechanical properties of SIMA-processed alloys are sufficiently high
for practical applications after artificial aging [7–9]. Casting, hot extrusion, and salt bath (to attain

Metals 2018, 8, 3; doi:10.3390/met8010003 www.mdpi.com/journal/metals

 Metals 2018, 8, 3 2 of 15

Metals 2018, 8, 3 2 of 15
a regime in which solid and liquid phases coexist in equilibrium) [5,6] are the three major steps of
this process. [5,6]
equilibrium) The microstructural
are the three major evolution
steps of this
this SIMA
process.process is shown in Figure
The microstructural 1b. Theofinitial
evolution this
state isprocess
SIMA a typicalis dendritic
shown incasting
Figurestructure. The black
1b. The initial statedots
is aintypical
Figure dendritic
1b represent the secondary
casting structure.phase,
The
whosedots
black melting point1b
in Figure is low. After the
represent the secondary
alloys are subjected
phase, whoseto hotmelting
extrusion, theismicrostructure
point low. After thechanges
alloys
to fine dynamic recrystallized grains. Then, the low melting point phases
are subjected to hot extrusion, the microstructure changes to fine dynamic recrystallized grains.and parts of the eutectic
composition
Then, the lowstart to partially
melting melt and
point phases andpenetrate
parts of the grain
eutecticboundaries
compositionof the recrystallized
start to partiallygrains due
melt and
to their high free energy in the salt bath step. This results in partially melted liquid
penetrate the grain boundaries of the recrystallized grains due to their high free energy in the salt phases surrounding
the fine
bath step.recrystallized
This results in grains. Finally,
partially grain
melted growth
liquid occurs
phases and generates
surrounding the spheroidized grains
fine recrystallized in the
grains.
salt bathgrain
Finally, because
growththe surface
occurs energy of the global
and generates grains is low,
spheroidized and
grains inthe
therestriction between the
salt bath because solid grains
surface
disappears
energy of the[2,3].
global grains is low, and the restriction between solid grains disappears [2,3].

Figure
Figure1.1. (a)
(a)Process
Processflow
flowand
and(b)
(b) mechanism
mechanismof of grain
grain spheroidization
spheroidizationof
ofmodified
modified strain-induced
strain-induced
melting
meltingactivation
activation(SIMA)
(SIMA)process
process(RT:
(RT: room
room temperature).
temperature).

The major components of the 6xxx series aluminum alloys that are used in this study are Mg
The major components of the 6xxx series aluminum alloys that are used in this study are Mg and Si.
and Si. The Mg2Si phase is generated first, since its forming free energy is lower than those of other
The Mg2 Si phase is generated first, since its forming free energy is lower than those of other precipitating
precipitating phases [10–12]. The 6xxx aluminum alloys that have more Si than is required to form
phases [10–12]. The 6xxx aluminum alloys that have more Si than is required to form stoichiometric Mg2 Si
stoichiometric Mg2Si commonly have relatively high strength and low ductility due to the hard and
commonly have relatively high strength and low ductility due to the hard and brittle Si particles in their
brittle Si particles in their matrix. In contrast, 6xxx aluminum alloys with excess Mg have relatively
matrix. In contrast, 6xxx aluminum alloys with excess Mg have relatively low strength and high ductility.
low strength and high ductility. Besides Mg and Si, Cu, Mn, Cr, Zr, Sc, and V are added to these
Besides Mg and Si, Cu, Mn, Cr, Zr, Sc, and V are added to these alloys. Adding Mn inhibits grain growth,
alloys. Adding Mn inhibits grain growth, enhances strength, and increases recrystallization
enhances strength, and increases recrystallization temperature [10,13,14]. Adding Cu improves strength
temperature [10,13,14]. Adding Cu improves strength and hardness due to the refining of the
and hardness due to the refining of the precipitated phase during artificial aging [15,16]. Adding Cr
precipitated phase during artificial aging [15,16]. Adding Cr promotes corrosion resistance [13].
promotes corrosion resistance [13]. Adding Zr enhances strength, since Al Zr is generated and grain
Adding Zr enhances strength, since Al3Zr is generated and grain growth is3 inhibited, and adding Sc
growth is inhibited, and adding Sc or V retards grain growth [17,18].
or V retards grain growth [17,18].
In this research, several extruded 6xxx aluminum alloys were used to investigate the effects of
In this research, several extruded 6xxx aluminum alloys were used to investigate the effects of
components and hot extrusion parameters on spheroidized grains in the modified SIMA process.
components and hot extrusion parameters on spheroidized grains in the modified SIMA process.
The purpose is to understand how to design an alloy that is suitable for this SIMA process. Moreover,
The purpose is to understand how to design an alloy that is suitable for this SIMA process.
the nanoscale microstructural characteristics, phases at globular grain boundaries, and mechanism of
Moreover, the nanoscale microstructural characteristics, phases at globular grain boundaries, and
elemental diffusion are analyzed using transmission electron microscopy (TEM).
mechanism of elemental diffusion are analyzed using transmission electron microscopy (TEM).

2. Materials and Methods

Table 1 shows the codes and compositions of the seven materials used in this research. The
compositions are analyzed by glow discharge spectrometer (GDS) (GDS-750 QDP, LECO
Metals 2018, 8, 3 3 of 15

2.Metals
Materials
2018, 8,and
3 Methods 3 of 15

Table 1 shows the codes and compositions of the seven materials used in this research. The compositions
Corporation, St. Joseph, MI, USA). The salt bath temperature was 620 °C based on previous research
are analyzed by glow discharge spectrometer (GDS) (GDS-750 QDP, LECO Corporation, St. Joseph, MI, USA).
studies [7–9]. All of the materials were extruded sheets except for 6069-rod, which was an extruded
The salt bath temperature was 620 ◦ C based on previous research studies [7–9]. All of the materials
rod. Notably, all of the materials were extruded from a six-inch diameter casting rod, in other words,
were extruded sheets except for 6069-rod, which was an extruded rod. Notably, all of the materials were
the extruded sheets with same thickness have an identical extrusion ratio (the same amount of
extruded from a six-inch diameter casting rod, in other words, the extruded sheets with same thickness
deformation). 6061 and 6061-Mn were used for discussing the effect of Mn addition; their thickness
have an identical extrusion ratio (the same amount of deformation). 6061 and 6061-Mn were used for
is 3 mm and their extrusion ratios were identical. The 6066-3mm and 6066-9mm sheets were used for
discussing the effect of Mn addition; their thickness is 3 mm and their extrusion ratios were identical.
determining the effect of strain introduced by hot extrusion, because their original castings alloy are
The 6066-3mm and 6066-9mm sheets were used for determining the effect of strain introduced by hot
the same. A 6069-sheet with 3 mm thickness and a 6069-rod with 28 mm diameter were used for
extrusion, because their original castings alloy are the same. A 6069-sheet with 3 mm thickness and a
understanding the effect of extrusion shape. The effect of strain also can be analyzed due to the
6069-rod with 28 mm diameter were used for understanding the effect of extrusion shape. The effect
amount of strain at the edge of the rod being larger than that in center of rod. Finally, 6061, 6066,
of strain also can be analyzed due to the amount of strain at the edge of the rod being larger than
6069, and 6082 (with 3 mm thickness, too) aluminum alloys were used for determining the effect of
that in center of rod. Finally, 6061, 6066, 6069, and 6082 (with 3 mm thickness, too) aluminum alloys
composition by observing their microstructural evolution. Optical microscopy (OM) (BX41M-LED,
were used for determining the effect of composition by observing their microstructural evolution.
Olympus, Tokyo, Japan), scanning electron microscopy (SEM) (JSM-7000 & JSM 7001, JEOL,
Optical microscopy (OM) (BX41M-LED, Olympus, Tokyo, Japan), scanning electron microscopy (SEM)
Peabody, MA, USA), and an electron probe X-ray microanalyzer (EPMA) (JEOL, Peabody, MA,
(JSM-7000 & JSM 7001, JEOL, Peabody, MA, USA), and an electron probe X-ray microanalyzer (EPMA)
USA) were used for investigating and analyzing the microstructural evolution, microstructural
(JEOL, Peabody, MA, USA) were used for investigating and analyzing the microstructural evolution,
characteristics, and elemental distribution. The goal was to determine principles for designing alloys
microstructural characteristics, and elemental distribution. The goal was to determine principles for
suitable for the SIMA process.
designing alloys suitable for the SIMA process.
Table 1. Compositions of Al–Mg–Si alloys used in this research (Unit: wt. %).
Table 1. Compositions of Al–Mg–Si alloys used in this research (Unit: wt %).
Code Mg Si Cu Mn Fe Cr V Zr Al
6061 Code 0.88 Mg
0.67 Si
0.16 Cu 0.03 Mn Fe
0.19 Cr0.04 V 0Zr Al0 Bal.
6061-Mn 60610.83 0.75
0.88 0.20 0.16 0.31
0.67 0.03 0.19
0.19 0.040.07 0 00 Bal.0 Bal.
6066-3mm 6061-Mn
1.02 0.83
1.29 0.75
0.95 0.20 1.02
0.31 0.19
0.19 0.070.18 0 00 Bal.0 Bal.
6066-3mm 1.02 1.29 0.95 1.02 0.19 0.18 0 0 Bal.
6066-9mm 1.02 1.29 0.95 1.02 0.19 0.18 0 0 Bal.
6066-9mm 1.02 1.29 0.95 1.02 0.19 0.18 0 0 Bal.
6069-sheet 1.25
6069-sheet 0.75
1.25 0.73 0.73 0.05
0.75 0.05 0.13
0.13 0.160.16 0 00.11 0.11
Bal. Bal.
6069-rod6069-rod
1.30 0.85
1.30 0.72 0.72 0.09
0.85 0.09 0.13
0.13 0.140.14 0.12 0.12 0 Bal.0 Bal.
6082 60820.71 0.71
1.10 1.10
0.06 0.06 0.71
0.71 0.19
0.19 0.230.23 0 0 0 Bal.0 Bal.

Afterthe
After themost
mostsuitable
suitablealloy
alloywas
wasdetermined,
determined,more
moredetailed
detailedmicrostructural
microstructuralanalyses
analyseswere
were
conductedusing
conducted using TEM.
TEM. The
The TEM
TEM samples
samples were
were prepared
prepared using
using a focused
a focused ion
ion beam
beam (FIB).
(FIB).

3.3.Results
Resultsand
andDiscussion
Discussion

3.1.
3.1.Effects
EffectsofofExtrusion
ExtrusionConditions
Conditionsand
andChemical
ChemicalComposition
Compositiononon
Microstructure
Microstructure
The
Theconcept
conceptof an
of equivalent
an equivalentcircle is used
circle in thisinstudy.
is used When the
this study. Whenshapetheofshape
a grain
ofisa not circular
grain is not
incircular
a two-dimensional plane, grain size is represented by the
in a two-dimensional plane, grain size is represented by diameter of the equivalent circle, as shown
diameter of the equivalent
incircle,
Figureas2.shown
The sizein and appearance
Figure 2. The sizeof globular grains are
and appearance of affected
globularby the initial
grains extrusion
are affected bystate and
the initial
alloy composition.
extrusion Thealloy
state and microstructures
composition.ofThe the microstructures
initial extruded alloys
of theused inextruded
initial this research areused
alloys shown in
in this
Figure 3. Their initial grain sizes are shown in Table 2.
research are shown in Figure 3. Their initial grain sizes are shown in Table 2.

Figure
Figure 2.2.Definition
Definitionofof equivalent
equivalent circle
circle diameter.
diameter.

Even though the extrusion ratios of 6061 and 6061-Mn are identical, the initial grain size of 6061 is larger
than that of 6061-Mn. Dynamic recrystallization occurred in both aluminum alloys in the hot
extrusion step, but the grain sizes of the two alloys are not identical due to Mn retarding
Metals 2018, 8, 3 4 of 15

MetalsEven
2018, though
8, 3 the extrusion ratios of 6061 and 6061-Mn are identical, the initial grain size of 6061 4 of is
15
larger than that of 6061-Mn. Dynamic recrystallization occurred in both aluminum alloys in the hot
grain growth
extrusion step, after dynamic
but the recrystallization,
grain sizes since
of the two alloys areitnot
increases
identicalthedue
temperature of recrystallization
to Mn retarding grain growth
[10,13,14].
after dynamic recrystallization, since it increases the temperature of recrystallization [10,13,14].
As the
As the extrusion
extrusion ratio
ratio was
was increased,
increased, the
thelevel
levelof ofdynamic
dynamicrecrystallization
recrystallization increased.
increased. This
This can
can
be shown
be shown by by comparing
comparing the the microstructures
microstructures of of 6066-3mm
6066-3mm and and6066-9mm.
6066-9mm. The higher
higher level
level ofof
recrystallization of
recrystallization of 6066-3mm
6066-3mm led led to
to aa more
moreuniform
uniformand andsmaller
smallerinitial
initialgrain
grainsize.
size. Besides,
Besides, dynamic
dynamic
recrystallization in
recrystallization in 6061
6061 alloys
alloys should
should be be easier
easier than
than that
that in
in 6066-3mm
6066-3mm alloys
alloys due
due toto the
the addition
addition of of
Mn, which
Mn, which increases
increasesrecrystallization
recrystallizationtemperature
temperature[10,13,14].
[10,13,14].

Figure 3. Microstructures of extruded Al–Mg–Si alloys. (a) 6061; (b) 6061-Mn; (c) 6066-3mm; (d)
Figure 3. Microstructures of extruded Al–Mg–Si alloys. (a) 6061; (b) 6061-Mn; (c) 6066-3mm;
6066-9mm; (e) 6069-sheet; (f) 6082 and; (g) 6069-rod.
(d) 6066-9mm; (e) 6069-sheet; (f) 6082 and; (g) 6069-rod.
Metals 2018, 8, 3 5 of 15

Table 2. The average initial grain size, liquid fraction, and growth rate of Al–Si–Mg alloys.

Code Average Initial Grain Size (µm) Liquid Fraction (%) in 10-min Salt Bath K (µm3 ·min−1 )
6061 40 3.2 42,329
6061-Mn 7 7.2 30,054
6066-3mm 3–5 16 16,806
6066-9mm 5–7 15.5 17,024
6069-sheet 7 & 300 10.4 31,579
6069-rod (center) 15 11.2 32,678
6082 8 7.5 24,357

Both coarse and fine grains can be seen in 3-mm thick 6069-sheet alloys. The coarse grains located
near the surface resulted from the high friction heat at the alloy surface. The coarse grains located in the
center zone of the sheets resulted from similar crystal orientations of neighboring grains. According to
the grain coalescence mechanism, if the crystal orientations of neighboring grains are similar, the grains
will easily merge, forming coarse grains. This led to the non-uniform grain distribution in 6069-sheet.
In the 28-mm diameter 6069-rod alloy, fine grains appear in the center, and coarse and fine grains
appear at the edge. This is due to the lower strain in the center of the rod creating a smaller driving
force for grain growth, and the higher strain at the edge of the rod making some crystals with similar
orientations grow and then merge. The initial grains of 6069 alloys are easier to grow than other alloys,
except for 6061 alloy, because Mn is not added. Besides, although the 6069-sheet and 6069-rod did not
contain Mn, the level of grain growth of the 6069 alloys was lower than that of the 6061 alloys due to
the addition of V and Zr.
Equiaxial grains resulted from the dynamic recrystallization in the 3-mm thick 6082 alloy,
which was due to the Mn content. This confirms that Mn inhibits grain growth.

3.2. Microstructural Evolution of SIMA-Processed Alloys

The microstructural evolution in the salt bath step for all of the alloys is shown in Figure 4.
The codes of specimens subjected to a salt bath are marked with the prefix “SB”. The salt bath time
was set as 1 min, 10 min, or 30 min. After the salt bath, grains were spheroidized, and grain boundaries
were broadened due to the low melting point phases melting and penetrating the grain boundaries.
With grain growth, the melting phases aggregated to form liquid pools [3,4]. The alloys fabricated by
the modified SIMA process presented in this research are defined as SIMA alloys. The area ratio of
these melting phases that solidified after cooling is defined as the liquid fraction. With forming at high
temperature, these phases melt again, improving formability [7–9]. Table 2 shows the liquid fraction of
all of the other alloys after a salt bath at 620 ◦ C for 10 min. All of the data were calculated using ImageJ
software and averaged from at least three images. Fine grains, a high degree of spheroidization, and a
high liquid fraction are the major factors for promoting high-temperature formability [7–9].
In general, globular grain growth is based on Lifshitz–Slyozov–Wagner (LSW) theory [3,4,19,20].
The formula is dn − d0 n = Kt, where d is the average grain size, which depends on salt bath duration,
d0 is the initial grain size, t is the salt bath duration, K (units: µm3 ·min−1 ) is the coarsening rate
constant, and exponent n is determined by the diffusive mechanism of grain growth. For n = 3,
the mechanism of grain growth is Ostwald ripening. The theoretical formula can be rewritten as
d3 = Kt + d0 3 . Ostwald ripening is the major mechanism of globular grain growth of SIMA alloys
when the liquid fraction is sufficient [21]. Ostwald ripening is a diffusion-controlled mechanism.
Large grains becomes larger, and small grains become smaller (even disappearing). In this paper, it is
assumed that the grain growth mechanism of all of the materials is Ostwald ripening for comparing
the grain growth rate.
The calculated grain growth rates are shown in Table 2. The grain growth rate of 6061-Mn is
lower than that of 6061, and those of the 6066 and 6082 alloys are lower than those of the other alloys.
This might result from different liquid fraction and adding Mn, since it decreases the rate of globular
grain growth.
Metals 2018, 8, 3 6 of 15
Metals 2018, 8, 3 6 of 15

Figure 4. Microstructural evolution of Al–Mg–Si alloys via salt bath.

Figure 4. Microstructural evolution of Al–Mg–Si alloys via salt bath.

After the salt bath, the grain size of 6066-3mm is smaller than that of 6066-9mm, even though
their After
grain the salt bath,
growth rates the grain
K are size of
almost 6066-3mm
identical, is smaller
as shown than that
in Table of 6066-9mm,
2. This indicates that even thethough
initial
their grain growth rates K are almost identical, as shown in Table 2. This indicates
grain size at the extrusion state affects the spheroidized grain size of SIMA alloys. In other words, that the initial grain
size at the extrusion state affects the spheroidized grain size of SIMA alloys.
finer and more uniform dynamic recrystallized grains are beneficial for obtaining smaller and more In other words, finer and
more uniform
uniform dynamic
spheroidized recrystallized
grains. The samegrains
resultarewas beneficial
found infor theobtaining
center of smaller and more
the 6069-rod. uniform
Its small and
spheroidized grains. The same result was found in the center
uniform initial recrystallized grains led to fine and uniform spheroidized grains. of the 6069-rod. Its small and uniform
initialTable
recrystallized
2 also shows grains
theled to fine
liquid and uniform
fractions of the spheroidized
four kinds of grains.
aluminum alloy during the 10-min
TableThe
salt bath. 2 also shows
liquid the liquid
fractions fractions
are those for, inof order,
the four kinds
6066, of aluminum
6069, 6082, and 6061 alloy(from
during hightheto 10-min
low).
The liquid fractions of a given alloy are similar, except for 6061. In general, the liquid fractionslow).
salt bath. The liquid fractions are those for, in order, 6066, 6069, 6082, and 6061 (from high to of a
The liquid
given alloyfractions
should be of similar.
a given However,
alloy are similar,
the high except
grainfor 6061. and
growth In general,
low liquidthe liquid
fraction fractions
of the 6061of a
given alloy should be similar. However, the high
alloys led to their respective positions affecting the results. grain growth and low liquid fraction of the 6061 alloys
led toThe
theirdegrees
respective positions affecting
of spheroidization oftheallresults.
of the alloys are shown Figure 4. The degrees of
The degrees of spheroidization
spheroidization the 6066 alloysofand all of6069-rod
the alloysarearehigher
shown than
Figurethose
4. Theofdegrees of spheroidization
the other samples. The
of the 6066 alloys and 6069-rod are higher than those of the other samples.
grains of the 6061 and 6069-sheet are non-equiaxial, because the initial coarse grains, The grains of the 6061
and andthe
6069-sheet
globular are non-equiaxial,
grain boundaries of the because
6082 the initial
alloys coarse
cannot be grains,
connectedanddue the globular
to the low grain
liquidboundaries
fraction.
of the 6082their
Therefore, alloys cannotofbe
degrees connected dueare
spheroidization to relatively
the low liquid fraction.
low. The degrees Therefore, their degrees
of spheroidization of
of the
spheroidization are relatively low. The degrees of spheroidization of
6066-3mm sheet, 6066-9mm sheet, and 6069-rod are highest due to their fine and uniform initialthe 6066-3mm sheet, 6066-9mm
recrystallized grains and high liquid fraction.
The elemental distributions obtained using EPMA are shown in Figure 5. Mg, Si, and Cu are the
major elements located at grain boundaries, and Fe, Mn, Cr, and V exist in the particle phases. It
Metals 2018, 8, 3 7 of 15

sheet, and 6069-rod are highest due to their fine and uniform initial recrystallized grains and high
liquid fraction.
Metals The
2018, elemental
8, 3 distributions obtained using EPMA are shown in Figure 5. Mg, Si, and Cu 7 ofare
15
the major elements located at grain boundaries, and Fe, Mn, Cr, and V exist in the particle phases.
indicates that
It indicates thethe
that melting phases
melting in the
phases salt salt
in the bathbath
stepstep
are mostly composed
are mostly composedof Mg,
of Si,
Mg, Cu,
Si,and
Cu,Al.
andThe
Al.
three phase diagrams in Figure 6 show that the eutectic points of Al and Si, Al and
The three phase diagrams in Figure 6 show that the eutectic points of Al and Si, Al and Mg2 Si, and Mg 2Si, and Al and

Al
Al2Cu
andare
Al577 °C, 595 °C,
◦ and 548 ◦ °C, respectively.
◦ Moreover, Table 3 shows the probable maximum
2 Cu are 577 C, 595 C, and 548 C, respectively. Moreover, Table 3 shows the probable
weight
maximum percentages of Mg2Si, Alof2Cu,
weight percentages Mg2excess
Si, Al2Si,
Cu,and the Si,
excess sumandof the
these
sumthree phases
of these for phases
three Al–Mg–Sifor
alloys. They are calculated from the GDS analysis, as shown in Table 1.
Al–Mg–Si alloys. They are calculated from the GDS analysis, as shown in Table 1. The order The order of the sums of
of the
these phases is those for 6066, 6069, 6082, and 6061 (from high to low). This order is
sums of these phases is those for 6066, 6069, 6082, and 6061 (from high to low). This order is consistentconsistent with
the
withorder for the
the order for liquid fractions
the liquid shown
fractions shownin Table 2. 2.
in Table These
Theseresults
resultsshow
showthat
thatthe
themajor
major phases
phases
distributed at globule boundaries are these three
distributed at globule boundaries are these three phases. phases.

Figure 5. Cont.
Metals 2018, 8, 3 8 of 15
Metals 2018, 8, 3 8 of 15

Figure
Figure5.5.Elemental
Elementaldistribution in in
distribution Al–Mg–Si alloys:
Al–Mg–Si (a) 6061;
alloys: (b) 6061-Mn;
(a) 6061; (c) 6066;
(b) 6061-Mn; (d) 6069-rod
(c) 6066; and
(d) 6069-rod
(e)
and6082.
(e) 6082.
 Figure 5. Elemental distribution in Al–Mg–Si alloys: (a) 6061; (b) 6061-Mn; (c) 6066; (d) 6069-rod and
Metals 2018, 8, 3 9 of 15
(e) 6082.

Metals 2017, 7, x FOR PEER REVIEW 10 of 15

(a)

(b) (c)
Figure 6. Phase diagrams of (a) Al–Si; (b) Al–Mg2Si; and (c) Al–Cu.
Figure 6. Phase diagrams of (a) Al–Si; (b) Al–Mg2 Si; and (c) Al–Cu.

Table 3. Weight ratios of Mg2Si and Al2Cu in Al–Mg–Si alloys (wt. %).
Table 3. Weight ratios of Mg2 Si and Al2 Cu in Al–Mg–Si alloys (wt %).

Material Mg2Si Al2Cu Excess Si Sum

Material Mg2 Si Al2 Cu Excess Si Sum
6061
6061 1.11
1.11 0.33
0.33 0.28
0.28 1.72
1.72
6066 1.61 1.76 0.7 3.97
6066 1.61 1.76 0.7 3.97
6069 2.01 1.35 0.07 3.43
6069
6082 2.01
1.12 1.35
0.11 0.07
0.7 3.43
1.93

6082 1.12 0.11 0.7 1.93

Three main factors affect the generation of fine, uniform, and highly spheroidized globular grains
withThree main fractions
high liquid factors affect themodified
in this generation
SIMAof fine, uniform,
process: and highly
(1) a proper spheroidized
composition globular
with sufficient
grains
elements with high
(e.g., Mg,liquid
Si, andfractions in this
Cu) that can formmodified SIMA
low melting process:
point phases(1) a proper in
is necessary composition with
order to enhance
sufficient elements (e.g., Mg, Si, and Cu) that can form low melting point phases is necessary
the liquid fraction for 6xxx series aluminum alloys; (2) the initial extrusion microstructure should
in
order to enhance the liquid fraction for 6xxx series aluminum alloys; (2) the initial
be fine and uniform grains for generating fine and uniform spheroidized grains after the salt bath;
extrusion
microstructure should be fine and uniform grains for generating fine and uniform spheroidized
(3) particular elements (e.g., Mn, V, and Zr) should be added to inhibit grain growth, not only to create
grains after the salt bath; (3) particular elements (e.g., Mn, V, and Zr) should be added to inhibit
fine recrystallized grains in the hot extrusion step, but also to create fine spheroidized grains in the salt
grain growth, not only to create fine recrystallized grains in the hot extrusion step, but also to create
bath step.
fine spheroidized grains in the salt bath step.
In this study, 6066 aluminum alloy was found to be the most suitable material for obtaining finest
In this study, 6066 aluminum alloy was found to be the most suitable material for obtaining
and most spheroidized globules. Therefore, 6066 alloy was used in the subsequent microstructural
finest and most spheroidized globules. Therefore, 6066 alloy was used in the subsequent
analyses with TEM.
microstructural analyses with TEM.

3.3. Microstructural Characteristics of Phases Located at Globule Boundaries in SIMA-Processed 6066 Alloy
The results of energy-dispersive X-ray spectroscopy (EDS) for phases located at globule
boundaries are shown in Figure 7. The image is the backscattered electron image (BEI) of a SEM
Metals 2018, 8, 3 10 of 15

3.3. Microstructural Characteristics of Phases Located at Globule Boundaries in SIMA-Processed 6066 Alloy
The
Metals results
2018, 8, 3 of energy-dispersive X-ray spectroscopy (EDS) for phases located at 10 ofglobule
15
boundaries are shown in Figure 7. The image is the backscattered electron image (BEI) of a SEM
micrograph.
micrograph. Three Three
phases phases canseen.
can be be seen.
The The brighter
brighter globule
globule boundary
boundary phases
phases marked
marked byby b are
b are mainly
mainly composed of Si and Cu. The darker particles marked by c at the grain boundaries and in
composed of Si and Cu. The darker particles marked by c at the grain boundaries and in liquid pools
liquid pools are mostly composed of Si and Mg. Moreover, Si, Mn, Cr, and Fe are the major elements
are mostlyMetals
composed
2018, 8, 3
of Si and Mg. Moreover, Si, Mn, Cr, and Fe are the major elements of the brighter
of the brighter equiaxed particles at the grain boundaries and in the grain interior (marked by10a).ofIn15
equiaxed particles at the grain boundaries and in the grain interior (marked by a). In this
this study, FIB was adopted to cut the TEM samples. A liquid pool was obtained with Mg and Si-rich
study, FIB was
adopted tomicrograph.
cut the TEM Three phases A
samples. can be seen.
liquid poolThe
wasbrighter
obtainedglobule
withboundary
Mg and phases
Si-rich marked
phases by
andb are
Cu-rich
phases and Cu-rich boundaries, two areas that are major positions for nanoscale microstructural
mainly composed of Si and Cu. The darker particles marked by c at the grain boundaries and in
boundaries, two areas that are major positions for nanoscale microstructural observation.
observation.
liquid pools are mostly composed of Si and Mg. Moreover, Si, Mn, Cr, and Fe are the major elements
of the brighter equiaxed particles at the grain boundaries and in the grain interior (marked by a). In
this study, FIB was adopted to cut the TEM samples. A liquid pool was obtained with Mg and Si-rich
phases and Cu-rich boundaries, two areas that are major positions for nanoscale microstructural
observation.

Figure 7. Energy-dispersive X-ray spectroscopy (EDS) analysis of phases at globule boundaries in

Figure 7. Energy-dispersive X-ray spectroscopy (EDS) analysis of phases at globule boundaries in
SIMA-processed 6066 alloy.
SIMA-processed 6066 alloy.
3.3.1. TEM Analysis of Liquid Pool Mostly Composed of Si and Mg
3.3.1. TEM Analysis
Figure 7.ofEnergy-dispersive
Liquid Pool Mostly Composed
X-ray spectroscopy of Si
(EDS) and Mg
analysis of phases at globule boundaries in
The liquid pool is composed
SIMA-processed 6066 alloy. of eutectic phases and is a layer-by-layer structure in the BEI
The liquid
image. Figurepool is composed
8 shows the liquid ofpool
eutectic phases and
morphology is a layer-by-layer
observed by TEM. Two phases structure can in be the
seen. BEI
One image.
Figure phase 3.3.1.
8 shows TEM
is similar Analysis
the liquid
to a river,of Liquid
pool which Pool
morphology is Mostly Composed
observed
distributed theof
in by Si and
TEM.
other TwoMg phases
phase. can be of
The results seen. One phase is
composition
similaranalysis by
to a river,
The EDS
which are is
liquid shown
pool in Figure
distributed
is composed 8B.eutectic
in the
of Four phases
other phases can
phase. Thebe
and observed.
isresults The river-like
of composition
a layer-by-layer structure phase
in the aBEI
analysis byis EDS
composed
are shownimage. of
in Figure Mg
Figure and Si,
8B.8 Four and
showsphases is likely
the liquid Mg
canpool 2Si. Phase b is likely the Al matrix. It can be speculated that
be observed.
morphologyThe river-like
observed by TEM.phaseTwoa is composed
phases of Mg
can be seen. One and Si,
and isphases
likely a and
phase b are the
Mgis2 Si.
similar
Phase to baeutectic
isriver,
likely phase isofdistributed
whichthe Al Al and Mg
matrix. 2Si.
thePhase
Itincan beother c,phase.
the neighboring
speculated The
thatresults
phases phase
of of a, is
composition
a and b are the
composed of Al
analysis by and
EDSCu, areandshown is likely Al2Cu.
in Figure 8B.The composition
Four phases can of bethe large particle
observed. phase d phase
The river-like is similar
a is
eutectic phase of Al and Mg 2 Si. Phase c, the neighboring phase of a, is composed of Al and Cu, and
to thatcomposed
of phaseof c in Figure 7. It is composed of Si, Mn, Cr, Fe, and Al. According
Mg and Si, and is likely Mg2Si. Phase b is likely the Al matrix. It can be speculated that to the diffraction
is likely Al2 Cu.
pattern shown
Theincomposition ofEDSthe results,
large particledphase d is similar to that of phaseCr) c in Figure 7.
phases a andFigure
b are the8C and eutectic phase of phase
Al and Mg is face-centered
2Si. Phase c, the cubic Al15(Fe, Mn,
neighboring phase 3of Si2a,
. Its
is
It is composed
melting of
composed Si,
point isof Mn,
Al and
close Cr,
to 660 Fe,
Cu,°C and
and Al.
is likely
[22]. According
Al2Cu.this
Therefore, to
Thephasethe diffraction
composition pattern
of theuniformly
distributes shown
large particle
in thephasein Figure
d isinstead
alloys 8C
similar and
EDS results, to phase
of melting of d
thatand is face-centered
phase c in Figure
locating at globule 7. cubic
It is Al15 (Fe,ofWhen
composed
boundaries. Mn, Cr)
Si, Mn,the Siduration
3Cr, . Itsand
2 Fe, melting
Al. point
According
of the salt bathistoclose
the to 660 ◦its
diffraction
increases, C [22].
Therefore, pattern
particlethis showndistributes
sizephase
increases. in The
Figure 8Cuniformly
and EDS
coarsening results,
in thephase
mechanism alloys
of thatd is face-centered
instead
phase cubic
of melting
follows the Al
and15(Fe,
Gibbs–Thomson Mn, Cr)
locating Si2.globule
3at
effect Its
to
reduce
boundaries. melting
the
When point
total the isduration
surface close to 660
energy. °C
ofSmall
the [22]. Therefore,
particles
salt this phasetogether
bath aggregated
increases, distributes
its particle uniformly
to form in particle
sizeaincreases.
large the alloys
The instead
phase.
coarsening
of melting and locating at globule boundaries. When the duration of the salt bath increases, its
mechanism of that phase follows the Gibbs–Thomson effect to reduce the total surface energy. Small
particle size increases. The coarsening mechanism of that phase follows the Gibbs–Thomson effect to
particles aggregated together to form a large particle phase.
reduce the total surface energy. Small particles aggregated together to form a large particle phase.

Figure 8. Cont.
 Metals 2018, 8, 3 11 of 15

Metals 2018, 8, 3 11 of 15
Metals 2018, 8, 3 11 of 15

FigureFigure
8. (A)8.Morphology
(A) Morphology of of
resolidified liquidphases;
resolidified liquid phases;(B)(B) composition
composition of phases
of phases analyzed
analyzed by EDS; by EDS;
Figure 8.
and (C) (A) Morphology
diffraction pattern of resolidified
of of
phase liquid phases; (B) composition of phases analyzed by EDS;
and (C) diffraction pattern phased.d.
and (C) diffraction pattern of phase d.
The selective
The selective areaarea diffractionpatterns
diffraction patterns ofofphases
phasesa and
a andb inbFigure 8 are 8shown
in Figure in Figure
are shown in9.Figure
Phase 9. Phase
a is face-centered cubic Mg2Si, and phase b is face-centered cubic aluminum matrix. Notably,
a is The
face-centered
selective area cubic Mg2Si, patterns
diffraction and phase b is face-centered
of phases a and b in Figure cubic
8 arealuminum matrix.9. Notably,
shown in Figure Phase a
according to the overlapping figure, the (220) crystal orientation of Mg2Si and the (200) crystal
isaccording
face-centeredto the overlapping
cubic Mg Si, andfigure, phase bthe (220) crystal cubic
is face-centered orientation
aluminum of Mg 2Si and
matrix.
orientation of Al are2the same. This indicates that the crystal orientations of these two phases are
the (200)
Notably, crystal
according
toorientation of
the overlapping
coherent. Al are the
figure, same.
the (220) This indicates
crystal that
orientation the
of crystal
Mg 2 Si orientations
and the (200) of these
crystal two phases
orientation of Alare
coherent.
are the same. This indicates that the crystal orientations of these two phases are
Phase c in Figure 8 neighbors Mg2Si. The same phenomenon can be seen in Figure 10. The EDS coherent.
Phase ccin
results
Phase inFigure
show Figure 88neighbors
neighbors
that phase c is composed
MgMg Si.Al
2of
2 Si. The
Theandsame phenomenon
Cu. The
same selective areacan
phenomenon can beseen
nanobeam
be seen ininFigure
Figure
diffraction 10.The
pattern
10. TheEDSEDS
results indicates
resultsshow
showthat that this
thatphase phase is tetragonal
phasec cisiscomposed
composedofofAl Al 2Cu. The solidification of Mg2Si occurs before that of Al2Cu
Aland
andCu.
Cu.The
Theselective
selectiveareaareananobeam
nanobeamdiffraction
diffractionpattern
pattern
due to the solidification temperature of Mg2Si being higher than that of Al2Cu. This led to the
indicates
indicates thatthis
that thisphase
phaseisistetragonal
tetragonalAlAl 2Cu.The
2 Cu. Thesolidification
solidificationofofMg Mg 2Sioccurs
2 Si occursbefore
beforethat
thatofofAl
Al 2Cu
2 Cu
obvious interface between Mg2Si and Al2Cu.
duetotothethe
due solidification
solidification temperature
temperature of Mgof2 Si
Mg 2Si being
being higherhigher
than thatthanof that of This
Al2 Cu. Al2Cu.ledThis
to theled to the
obvious
obvious between
interface interfaceMg between
2 Si andMg Al 22Si and
Cu. Al 2 Cu.

Figure 9. Coherence between Mg2Si and the Al matrix. (a) morphology of Mg and Si-rich globule
boundary; (b) diffraction patterns of phases a; (c) diffraction patterns of phases b; (d) merging
diffraction patterns of phases a and b.

Figure9.9.Coherence
Figure Coherencebetween
betweenMgMgSi 2Si and the Al matrix. (a) morphology of Mg and Si-rich globule
and the Al matrix. (a) morphology of Mg and Si-rich globule
2
boundary; (b) diffraction patterns of phases
boundary; (b) diffraction patterns of phases a; (c) diffraction
a; (c) diffraction patternspatterns
of phasesof phases
b; (d) b; (d)
merging merging
diffraction
diffraction
patterns patterns
of phases of phases
a and b. a and b.
 Metals 2018, 8, 3 12 of 15
Metals
Metals 2018,
2018, 8, 38, 3 1215
12 of of 15

Figure
Figure
Figure 10.10.
10. Analysis
Analysis
Analysis ofAl
ofofAl 2Al
Cu 2Cu
2 Cu inliquid
liquid
ininliquid pool.
pool.
pool. (a)
(a)(a) morphology
morphology
morphology ofglobule
globule
ofofglobule boundary;
boundary; (b)
boundary; (b)
(b) composition
composition
compositionofofof
phases
phases
phases analyzed
analyzed
analyzed bybyby
EDS;EDS;
EDS; (c)(c)
(c) diffraction
diffraction
diffraction pattern
pattern
pattern of phase
ofofphase
phaseb.b. b.

3.3.2.
3.3.2.
3.3.2.TEMTEM
TEM Analysis
Analysis
Analysis ofGlobule
Globule
ofofGlobule Boundaries
Boundaries Mostly
Mostly
Boundaries Mostly Composed
Composed
Composed ofSiand
ofofSi Siand
and
CuCu
Cu
Figure
Figure
Figure 1111
11 shows
shows
shows thethe
the microstructure
microstructure
microstructure investigated
investigated
investigated byby by
TEMTEM TEM
of of of Cu-rich
Cu-rich
Cu-rich globule
globule
globule boundaries.
boundaries.
boundaries. Al Al
Al grains
grains
grains areare surrounded
surrounded by by
a a ribbon-like
ribbon-like phase,
phase, which
which is is composed
composed
are surrounded by a ribbon-like phase, which is composed of globule boundaries. At highof of globule
globule boundaries.
boundaries. At At
highhigh
magnification,
magnification,
magnification, itcan
ititcan can
bebebe seen
seen
seen thatthat
thatthe the
the ribbon-like
ribbon-like
ribbon-like phase
phase
phase iscomposed
composed
isiscomposed ofofof alarge
large
a alarge number
number
number ofofof
finefine
fine
piece-like
piece-like phases
phases and and
somesome particle
particle phases.
phases. The The piece-like
piece-like phases
phases areare
thethe tetragonal
piece-like phases and some particle phases. The piece-like phases are the tetragonal Al2 Cu phase, asas
tetragonal Al 2Al
Cu 2Cu phase,
phase, as
determined
determined
determined fromfrom
from the the
the selective
selective
selective areaarea
area diffraction
diffraction
diffraction pattern.
pattern.
pattern.The The
The boundaries
boundaries
boundaries areare
are formed
formed
formed byby
by AlAl2Al
Cu 2Cu
andandAl Al
2 Cu and Al
eutectic
eutectic
eutectic solidification.
solidification.
solidification.

Figure
Figure
Figure11.
11.11. Analysis
Analysis
Analysis ofAl
ofofAl 2Al
Cu 2Cu phase
phase
2 Cu phase atCu-rich
atat Cu-rich
Cu-rich globule
globule
globule boundaries.
boundaries.
boundaries. (a)
(a)(a) morphology
morphology
morphology ofCu-rich
Cu-rich
ofofCu-rich globule
globule
globule
boundary
boundary
boundary and
andand
(b)
(b)(b) diffraction
diffraction
diffraction pattern
pattern
pattern of phase
ofofphase
phase located
located
located at Cu-rich
atatCu-rich
Cu-rich globule
globule
globule boundary
boundary
boundary.

Diffraction patterns
Diffraction taken at three points of the Al2Cu phase
areare shown in Figure 12a. They
areare
Diffractionpatterns
patternstaken
takenatatthree
threepoints
pointsofofthe
theAl
Al2Cu phase shown in Figure 12a. They
2 Cu phase are shown in Figure 12a. They are
the the same phase (Al 2Cu),
andand their orientations
areare rotated
by by a slight angle with respect to each other
thesame
samephase
phase(Al 2Cu),
(Al their orientations rotated a slight angle with respect to each
2 Cu), and their orientations are rotated by a slight angle with respect to each other
other
asasas shown
shown in in Figure
Figure 12b 12b because
because of of
a a high
high cooling
cooling rate
rate (water
(water quenching).
quenching). Figure
Figure 12c12c
shown in Figure 12b because of a high cooling rate (water quenching). Figure 12c confirms the phase
confirms
confirms thethe
phase
phase is 2Al
is Al Cu.2Cu.
TheThe high
high cooling
cooling raterate resulted
resulted in in
thethe immediate
immediate generation
generation of of a large
a large number
number of of
crystals
crystals of 2Al
of Al Cu.2Cu.
Metals 2018, 8, 3 13 of 15

is Al2 Cu. The high cooling rate resulted in the immediate generation of a large number of crystals
Metals
of Al22018,
Cu. 8, 3 13 of 15
Metals 2018, 8, 3 13 of 15

Figure 12. Diffraction

Diffraction patterns of of phases at
at Cu-rich globule
globule boundaries (a)(a) diffraction patterns
patterns taken
Figure 12. Diffraction patterns
Figure 12. patterns of phases
phases at Cu-rich
Cu-rich globule boundaries
boundaries (a) diffraction
diffraction patterns taken
taken
at
at three points (a, b and c); (b) merging of above three diffraction pattern; (c) composition of phases
at three
three points
points (a,
(a, bb and
and c);
c); (b)
(b) merging
merging of
of above
above three
three diffraction
diffraction pattern;
pattern; (c)
(c) composition
composition of
of phases
phases
analyzed by
analyzed by EDS.
EDS.
analyzed by EDS.
The EDS results in Figure 8 show that the Cu-rich globule boundaries are not only composed of
The
The EDS
EDS results
results in
in Figure
Figure 88 show
show that
that the
the Cu-rich
Cu-rich globule
globule boundaries
boundaries areare not
not only
only composed
composed of of
Al and Cu, but also Si. A large number of Si particles exist at the boundaries, as shown in Figure 13.
Al
Al and
and Cu,
Cu, but
but also
also Si. A large
Si. A large number
number of of Si
Si particles
particles exist
exist at
at the
the boundaries,
boundaries, as as shown
shown in in Figure
Figure 13.
13.
The arrows in Figure 13 indicate Si particles identified from EDS. In this figure, spot a is composed of
The
The arrows
arrows in
in Figure
Figure 1313 indicate
indicate Si Si particles
particles identified
identified from
from EDS.
EDS. InIn this
this figure, spot aa is
figure, spot is composed
composed of of
Al grains and Si particles, spot b is composed of Al2Cu and Si particles, and spot c is composed Al
Al
Al grains
grains and
andSiSiparticles, spotb bis is
particles,spot composed
composed of of
Al2Al
Cu and
2Cu andSi particles, andand
Si particles, c is composed
spotspot c is composedAl and
Al
and Al2Cu. These results prove that the eutectic phases of Al and Si, whose melting points are below
Al
and2 Cu. These
Al2Cu. results
These prove
results that that
prove the eutectic phases
the eutectic of Alofand
phases Si, whose
Al and melting
Si, whose points
melting are below
points the
are below
the temperature of the salt bath, existed at the globule boundaries.
temperature of the salt bath, existed at the globule boundaries.
the temperature of the salt bath, existed at the globule boundaries.

Figure 13. EDS analysis of eutectic Si particles.

Figure 13. EDS analysis of eutectic Si particles.
Figure 13. EDS analysis of eutectic Si particles.
TEM data exhibit phases on the globule boundaries of SIMA-processed 6066 aluminum alloy
TEM data exhibit phases on the globule boundaries of SIMA-processed 6066 aluminum alloy
are the
TEM eutectic phases of Al and
data exhibit Mg2Si, Al and Al2Cu, and Al and Si. This is consistent with the
are the eutectic phasesphases on the
of Al and Mgglobule boundaries of SIMA-processed 6066 aluminum alloy
2Si, Al and Al2Cu, and Al and Si. This is consistent with the
EPMA data.
are the eutectic phases of Al and Mg2 Si, Al and Al2 Cu, and Al and Si. This is consistent with the
EPMA data.
EPMA data.
4. Conclusions
4. Conclusions
4. Conclusions
The following conclusions were drawn based on the results and discussion.
The following conclusions were drawn based on the results and discussion.
1. The
Threefollowing conclusions
major factors affect were drawn based
the generation of on theuniform,
fine, results and
anddiscussion.
highly spheroidized globular
1. Three major factors affect the generation of fine, uniform, and highly spheroidized globular
1. grains with high
Three major liquid
factors fractions
affect in this modified
the generation of fine,SIMA process:
uniform, and (a) sufficient
highly elementsglobular
spheroidized to form
grains with high liquid fractions in this modified SIMA process: (a) sufficient elements to form
low melting
grains pointliquid
with high phases; (b) theinaddition
fractions of particular
this modified elements
SIMA process: (a)for inhibiting
sufficient grain growth;
elements to form
low melting point phases; (b) the addition of particular elements for inhibiting grain growth;
and (c) proper extrusion parameters to get a fine and uniform initial extrusion microstructure.
and (c) proper extrusion parameters to get a fine and uniform initial extrusion microstructure.
2. Of the 6xxx series alloys, 6066 aluminum alloy is the most suitable for the modified SIMA
2. Of the 6xxx series alloys, 6066 aluminum alloy is the most suitable for the modified SIMA
process. Mg, Si, and Cu can generate low melting point phases, and Mn can inhibit grain
process. Mg, Si, and Cu can generate low melting point phases, and Mn can inhibit grain
growth.
growth.
Metals 2018, 8, 3 14 of 15

low melting point phases; (b) the addition of particular elements for inhibiting grain growth; and
(c) proper extrusion parameters to get a fine and uniform initial extrusion microstructure.
2. Of the 6xxx series alloys, 6066 aluminum alloy is the most suitable for the modified SIMA process.
Mg, Si, and Cu can generate low melting point phases, and Mn can inhibit grain growth.
3. According to TEM results, the eutectic phases of Al and Mg2 Si, Al and Al2 Cu, and Al and
Si are the major phases at the globule boundaries. EPMA data confirm this result. The high
melting-point phase Al15 (Fe,Mn,Cr)3 Si2 was also identified by TEM.

Acknowledgments: The authors are grateful to the Instrument Center of National Cheng Kung University and the
Ministry of Science and Technology of Taiwan (NSC MOST103-2221-E-006-056-MY2) for their financial support.
Author Contributions: C.-W.L. designed experiments majorly, performed the experiments, analyzed the datas and
wrote the paper, F.-Y.H. and T.-S.L. contributed materials/lab/analysis tools and gave suggestions for improving
this research.
Conflicts of Interest: The authors declare no conflicts of interest.

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