Color Metallography and Electron Microscopy

Techniques Applied to the Characterization

of 413.0 Aluminum Alloys
George Vander Voort,
1
Juan Asensio-Lozano,
2,
* and Beatriz Surez-Pea
3
1
Consultant, Struers Inc., 2887 N. Southern Hills Drive, Wadsworth, IL 60083-9293, USA
2
Materials Science and Metallurgical Engineering Department, The School of Mines, The University of Oviedo,
Oviedo, Asturias 33004, Spain
3
Materials Science and Metallurgical Engineering Department, The University of Oviedo, Gijn Polytechnic School
of Engineering, Viesques Campus, Gijn, Asturias 33203, Spain
Abstract: The influence on alloy 413.0 of the refinement and modification of its microstructure was analyzed
by means of several microscopy techniques, as well as the effect of the application of high pressure during
solidification. For each treatment and solidification pressure condition employed, the most suitable microscopy
techniques for identifying and characterizing the phases present were investigated. Color metallography and
electron microscopy techniques were applied to the qualitative microstructural analysis. Volume fraction and
grain size of the primary a-Al were characterized by quantitative metallographic techniques. The results show
that the effect caused by applying high pressure during solidification of the alloy is more pronounced than that
caused by modification and refinement of the microstructure when it solidifies at atmospheric pressure.
Furthermore, it has been shown that, for AlSi alloy characterization, when aiming to characterize the primary
a-Al phase, optical color metallography observed under crossed polarized light plus a sensitive tint filter is the
most suitable technique. When the goal is to characterize the eutectic Si, the use of optical color metallography
or electron microscopy is equally valid. The characterization of iron-rich intermetallic compounds should
preferably be performed by means of backscattered electron imaging.
Key words: optical color microscopy, scanning electron microscopy, quantitative metallographic characteriza-
tion, cast aluminum alloys, grain refining, eutectic modification, high pressure die casting
INTRODUCTI ON
The 413.0 ~Al12Si! eutectic alloy exhibits excellent fluidity
and a low tendency to develop microshrinkage, resulting in
sound components of high compactness ~Liao & Sun, 2003!.
As constituents of the eutectic alloy differ notably in terms
of their melting temperatures and their weight ratios, it is
referred to as an abnormal eutectic. These two aspects,
together with physical and chemical heterogeneities occur-
ring during solidification, determine the resulting micro-
structure ~Abbaschian et al., 2009!. Therefore, owing to the
relationships between microstructure parameters and prop-
erties, mechanical properties of the alloy can also be esti-
mated ~Vander Voort & Asensio-Lozano, 2009!.
In this particular eutectic system, the first constituent
to solidify is the one with the higher melting point ~Si!,
which will then be followed by the other constituent ~a-Al!
in the amount necessary for the residual liquid to maintain
the appropriate composition ~12.6 wt% Si!. The growth rate
of the Si particles in the eutectic is faster than that of a-Al
because of the greater driving force for solidification of this
phase ~this will be proportional to the temperature differ-
ence between the solidification temperature of the constitu-
ent phases in the eutectic and the eutectic temperature:
14145778378C for silicon, whereas it will be proportional
to 660577838C for eutectic aluminum! ~Massalsky, 1986;
Gruzleski, 2000a!. Consequently, the timetemperature
transformation curve for Si will be much closer to the time
origin than that of Al. This results in rapid nucleation of the
Si, which will develop quickly before being enveloped by an
a-Al amount such that the solid reaches the eutectic com-
position. As a result of nonequilibrium cooling and slight
variations in composition, the presence of polyhedral parti-
cles of Si is often observed ~Nogita & Dahle, 2001!.
The commercial importance of near-eutectic AlSi al-
loys has been a topic of many research projects. The eutectic
silicon in unmodified AlSi alloys is present as a flake-like
morphology and it has a deleterious effect on the ductility.
Small additions of strontium lead a morphological transi-
tion from coarse flakes to fine fibers ~Nogita et al., 2006!.
The benefits of modification with strontium are more im-
portant in sand castings, although certain benefits are also
observed when the cooling rates increase ~Lim, 2009!. More-
over, most of commercial eutectic AlSi alloys solidify with
a large fraction of primary a-Al in their microstructures.
Additions of titanium and boron have been used to try to
refine the a-Al grains. The weight ratio needed to form the
nucleating TiB
2
particles is Ti:B 2.2:1, although most of
the grain refiners present higher ratios of Ti:B, such as
3Ti1B, 5Ti1B, and 5Ti0.2B. The Al5TiB is an efficient
grain refiner in pure aluminum and in alloys with a low Si
content. However, when the content in silicon is higher than
Received August 2, 2012; accepted March 8, 2013
*Corresponding author. E-mail: jasensio@uniovi.es
Microsc. Microanal. 19, 10191026, 2013
doi:10.1017/S1431927613000585
MicroscopyAND
Microanalysis
MICROSCOPY SOCIETY OF AMERICA 2013
or equal to 7 wt%, the refining power of this master alloy is
less than that of master alloys with a lower Ti:B ratio
~Sritharan & Li, 1997; Murty et al., 2002!. On the other
hand, it is clear that improving the quality of the aluminum
alloys requires a more in-depth understanding of the micro-
structure development. Conventional etching techniques tra-
ditionally used in microscopy observation does not allow an
analysis of the microstructural evolution of the phases
present or the mechanisms of segregation and nucleation
governing solidification of Al12Si alloys.
The present work analyzes the influence of the modifi-
cation and refinement of the alloy 413.0 microstructure, as
well as the effect of the application of high pressure during
solidification. For each treatment and solidification pressure
condition employed, the most suitable microscopy tech-
niques for identifying and characterizing the phases present
were investigated. Color metallography techniques ~Vander
Voort, 2004a! employing light optical microscopy ~LOM!
~Vander Voort, 2004b! and scanning electron microscopy
~SEM! were used as analytical tools.
MATERI ALS AND EXPERI MENTAL
PROCEDURES
Figure 1 describes the experimental procedure followed for
the different samples at different stages of the manufactur-
ing process. Ingots of the 413.0 alloy composition from
Alcoa ~Avils, Spain! were melted in an induction furnace.
The melting temperature was in the range of 7407708C.
Then, the liquid metal was degassed first with nitrogen and
thereafter with argon; the degassing rate was ;22 L/min for
7 min. At this stage, a small amount of liquid was poured at
;7208C into a mold ~gray iron, preheated to 3508C!.
The composition of the commercial alloy in the first
stage of this study, coded Alloy 1, is shown in Table 1. A
second cast was additionally obtained, coded Alloy 2
~Table 2!, by adding 0.05 wt% Sr ~Al10Sr! and 0.05 wt%
Ti ~Al3TiB! to the melt in a treatment ladle, as modifier
and refiner of the microstructure, respectively. In this
second stage, hot metal was also extracted to solidify under
the aforementioned atmospheric conditions.
Both heats, base alloy and grain-refined alloy, were first
transferred to a holding furnace. Then, predetermined
weights of hot metal of both heats were transferred to the
cold chamber metal injection molding machine, where solid-
ification took place at 34 MPa. Components manufactured
from both alloys were subsequently set aside. Metallographic
samples were then obtained of the two alloys solidified un-
der the aforementioned conditions.
Etching of the samples was performed at room tem-
perature, using in some cases an aqueous solution of HF
at 0.5 vol% ~Warmuzek, 2004!, and in others the re-
agent developed by Weck and Leistner ~1986! for aluminum
alloys. This consists of a solution of potassium permanga-
Figure 1. Experimental procedure followed for the different sam-
ples at different stages of the manufacturing process.
Table 1. Chemical Composition* of the 413.0 Commercial Alloy ~Alloy 1!.
Si Fe Cu Mn Mg Ni Zn Pb Ti Cr
12.90 0.82 0.04 0.20 0.01 0.006 0.03 0.02 0.008 0.013
All values expressed in wt%.
*Other products may pertain to the composition but are not listed, for example, Ag, Zr, Sb, Co, V, Be, B, Ca, etc.
Table 2. Alloy Identification Based on the Basic Chemistry in Ti and Sr Content. Quantitative Results for the Volume Fraction ~V
V
! and
Mean Grain Size ~ N A
a
! of a-Al in the Two Different Solidification Conditions Studied with Indication of the 95% Confident Limits of the
Determinations.
Solidification Pressure
0.1 MPa 34 MPa
Alloy Identification
Ti
~wt%!
Sr
~wt%!
V
V
~a-Al! 6CL
95%
~vol%!
N A
a
6CL
95%
~ mm
2
!
V
V
~a-Al! 6CL
95%
~vol%!
N A
a
6CL
95%
~ mm
2
!
Alloy 1 ~commercial alloy! 21.87 62.16 11,296 6823 46.23 64.14 553 635
Alloy 2 ~refined and modified! 0.05 0.05 31.71 63.14 1,302 6141 53.48 65.19 307 6 23
1020 George Vander Voort et al.
nate, sodium hydroxide, and water in the following
proportions:
Distilled water ~100 mL!
KMnO
4
~4 g!
NaOH ~1 g!
In some cases, several cycles of final polishing and etching
were needed to obtain a suitable contrast of the microcon-
stituents ~Vander Voort, 1981!. The equipment used for
observations was a Nikon Epiphot ~Nikon Instruments Inc.,
Tokyo, Japan! inverted metallographic microscope con-
nected to a Kappa ImageBase image analyzer ~Kappa optron-
ics GmbH, Gleichen, Germany! for LOM, and a JEOL JSM
6100 ~JEOL Ltd., Tokyo, Japan! for SEM.
The volume fraction and grain size of the primary a-Al
were characterized by quantitative metallographic techniques
~Vander Voort, 1999; Muirhead et al., 2000; Roebuck, 2000;
Higginson & Sellars, 2003!. A manual point counting tech-
nique was used to obtain the volume fraction, whereas the
grain size was characterized by means of the semiautomatic
areal analysis technique ~ASTM E138297, 2010!. In order
to minimize statistical errors in the determinations, 250
grains were counted for the volume fractions or, failing that,
25 micrographs were assessed ~Vander Voort, 1994, 1996!.
To determine the grain size of the a-Al, 400 grains were
evaluated or, failing that, 25 micrographs were assessed. In
both cases, a relative error of less than 0.05 was sought.
RESULTS
Figures 2 and 3 show the microstructure of Alloy 1 solidi-
fied at atmospheric pressure in a preheated chill cast mold.
Observation under LOM was performed after etching with
the HF reagent in Figures 2a and 3a for black and white
~B&W! imaging and using Wecks reagent in Figures 2b and
3b for color imaging. Bright field ~BF! illumination was
employed in Figures 2 and 3a, and polarized light plus the
sensitive tint filter ~XPST! in Figure 3b ~Chapon & Szkli-
niarz, 2001!. All the aforementioned micrographs confirm
the presence of primary aluminum embedded in an AlSi
Figure 2. Light optical microscopy microstructure of Alloy 1 so-
lidified at atmospheric pressure in a preheated chill cast mold.
Observation performed after etching with: ~a! HF reagent and
~b! Wecks reagent. Bright field illumination was employed.
Figure 3. Microstructure of Alloy 1 solidified at atmospheric pres-
sure in a preheated chill cast mold. Observation was performed:
~a! after etching with HF and bright field illumination and ~b! af-
ter etching with Wecks reagent and polarized light plus sensitive
tint to filter.
Color LOM and SEM Applied to Al12Si Alloys 1021
eutectic matrix. Furthermore, lamellae of the intermetallic
compound b-AlFeSi can be observed in Figure 3b, appear-
ing as needles on the polished plane of the micrograph over
a yellow background. In Figure 2b, the color etching tech-
nique reveals the presence of microsegregation in the pri-
mary a-Al, as evidenced by a darker orange coloring in the
center and yellow coloring at the edges. This is observed in
both the primary and secondary dendrite arms. However,
this technique does not allow us to identify a net boundary
between the primary and the eutectic a-Al, and therefore
impedes the quantitative characterization of the volume frac-
tions and grain size of this primary phase. Moreover, a less
pronounced staining found between the center and borders
of a-Al lamella in the eutectic suggests a less pronounced
segregation compared with that found in primary a-Al. The
technique is appropriate for the unambiguous identification
of cuboidal and acicular Si via their gray coloring.
Study of the sample under LOM employing XPST
~Fig. 3b! allows us to distinguish the interface between the
AlSi eutectic phase and the a-Al dendrites. This technique
is ideal for defining the outline of the a-Al dendrites,
allowing precise quantitative characterization of this phase.
The technique also allows characterization of the intermetal-
lic b-AlFeSi, which, as already mentioned, is seen on the
micrograph as dark needles over a pale yellow background.
This technique likewise enables us to appreciate the segrega-
tion of the primary a-Al and its absence in the a-Al of the
AlSi eutectic phase.
Figure 4 is a SEM-backscattered electron image ~BEI!
micrograph of Alloy 1 and shows the appearance and out-
line, both of the eutectic Si and the b-AlFeSi needles. This
technique allows us to differentiate both types of needles, as
those rich in Fe show a brighter contrast.
In industrial practice, modification and refinement of
the microstructure is used to improve the mechanical prop-
erties of alloys of this type ~Asensio-Lozano et al., 2007!. Sr
brings about changes in the morphology of the eutectic Si,
which becomes globular ~Asensio-Lozano et al., 2005!. It
also leads to a decrease in the size of the Si cuboids and an
increase in the volume fraction of the a-Al phase ~Sritharan
& Li, 1997; Hengcheng et al., 2002!. Ti causes an increase in
the volume fraction and refinement of the a-Al phase ~Liu
et al., 2004!. The results ~Table 2! show that there is a
significant decrease in the grain size of the primary a-Al
phase in Alloy 2, solidified at atmospheric pressure in a
preheated chill cast mold, when its microstructure is modi-
fied with 0.05% Sr and refined with 0.05% Ti ~Asensio-
Lozano et al., 2006!. The micrographs in Figure 5 correspond
to the BF micrograph of Alloy 2 ~refined and modified!
solidified at atmospheric pressure after the color etching
technique under LOM and reveal the segregation of the
primary a-Al. They also reveal two different sized popula-
tions of b-AlFeSi needles, which are made evident because
the coarse fraction serves as the heterogeneous nucleation
sites for primary a-Al dendrites, whereas a smaller sized
Figure 4. Backscattered electron image micrograph of Alloy 1
solidified at atmospheric pressure after etching with HF reagent
showing the appearance of the eutectic Si and the b-AlFeSi nee-
dles. Those rich in Fe show brighter. Scale bar 10 mm.
Figure 5. Bright field color etching technique under light optical
microscopy reveals the segregation in primary a-Al: ~a! two differ-
ent sized populations of b-AlFeSi needles are observed and ~b! het-
erogeneity occurs with modification of the eutectic Si.
1022 George Vander Voort et al.
fraction appears well dispersed within the eutectic phase.
The different degrees of modification of the eutectic phase
can be appreciated by the existence of regions of different
fineness of eutectic silicon ~Fig. 5b!. Figure 6 is an SEM
micrograph of Alloy 2, solidified at atmospheric pressure,
after etching with HF. This figure shows the fragility of the
smaller b-AlFeSi needles, which appear fragmented at sev-
eral points, and the power of heterogeneous nucleation that
the larger needles exhibit over other phases of the system.
The high pressures required for pressure molding of
these alloys can modify the information that emerges from
the equilibrium diagrams. The results ~Fig. 7a and Table 2!
show the variation in the microstructure of the alloy after
being subjected to forming via the injection molding tech-
nique. The very high cooling conditions and high pressure
exerted during solidification facilitate the development of a
more refined uniformly dispersed a-Al phase compared
with atmospheric solidification ~Fig. 2!. In contrast, Fig-
ure 7b and the results in Table 2 show that the combined
effect of Sr and Ti, when the alloy is solidified at high
pressure, provides finer grains and a higher degree of homo-
geneity in the distribution of the phases present.
The SEM micrograph in Figure 8 corresponds to Al-
loy 2 solidified at high pressure. It shows in detail the
irregular outline of the eutectic Si as a result of a zig-zag
growth mechanism leading to frequent changes of direction
within individual particles during growth. Fe-based com-
pounds are identified, once more, using BEI ~Gruzleski,
2000b; Gndza et al., 2004!.
DI SCUSSI ON
The eutectic alloy has a Si content of approximately 12 wt%
and its microstructure is formed by the eutectic of a-Al
with silicon. However, certain factors, such as the contents
of Fe, Mn, and Mg, and the solidification rate, may signifi-
cantly alter the microstructure expected from the equilib-
rium phase diagram, with the possible appearance of primary
a-Al dendrites and silicon cuboids. Iron is one of the most
important impurities in aluminum alloys and is always
present in die cast commercial alloys. Eutectic AlSi alloys
for pressure die casting include a certain percentage of iron
added to avoid the risk of welding to the dies.
In addition, the eutectic AlFeSi composition occurs
for Fe contents of 0.8 wt%. It is not unusual to find
recommendations for the Fe content to range from 0.8 to
1.1 wt% for these alloys. However, Fe can promote the
formation of brittle plates of b-AlFeSi or the other complex
intermetallics in the presence of Mn. The Mg level is usually
specified as below 0.10 wt% to avoid the formation of
Mg
2
Si, which results in deterioration of the tensile strength.
~Gruzleski & Closset, 1999; Shankar & Apelian, 2002!.
In those structures adequately modified by the precise
addition of Sr, the eutectic silicon is found in the form of
Figure 6. Backscattered electron image micrograph of Alloy 2
solidified at atmospheric pressure after etching with HF reagent
showing the fragility of the b-AlFeSi needles and the power of
heterogeneous nucleation that large needles exhibit. Scale bar
10 mm.
Figure 7. Color etched microstructure ~bright field! observed un-
der light optical microscopy reveals that the very high cooling
conditions and high pressure exerted during solidification facili-
tates the development of a refined uniformly dispersed a-Al phase
in: ~a! Alloy 1 and ~b! Alloy 2.
Color LOM and SEM Applied to Al12Si Alloys 1023
fine fibers. Refining of the a-Al phase grains by means of
the addition of elements such as Ti and B is a common
industrial practice. In the present work, the influence on
alloy 413.0 of the modification and refinement of its micro-
structure was analyzed by means of several microscopy
techniques, as well as the effect of the application of high
pressure during solidification. For each treatment and solid-
ification pressure condition employed, the most suitable
microscopy techniques for identifying and characterizing
the phases present were investigated. The most novel method
used was color etching, based on a reagent developed by
Weck and Leistner ~1986! for LOM observation of alumi-
num alloys.
Microstructure of Alloy 413.0 Solidified at
Atmospheric Pressure
Color metallography applied to structures of Alloy 1 solidi-
fied at atmospheric pressure in chill cast molds ~Figs. 2b, 3b!
shows that the solidification of this quasi-eutectic alloy does
not begin with the sequential nucleation of the eutectic Si
and a-Al. Gruzleski ~2000a! suggests the possibility that the
primary a-Al crystals are the first to nucleate ~Fig. 9!, doing
so below the eutectic temperature with a certain degree of
undercooling ~see point 2!. As these nuclei grow, the Si
content in the fluid surrounding them increases, approach-
ing the coupled zone ~shaded area in Fig. 9!. If thermo-
dynamic and kinetic conditions are appropriate, the eutectic
phase will eventually nucleate from the Si-enriched liquid
~see point 3! in the area known as the coupled zone.
Thus, when solidification is completed, the alloy has a pri-
mary a-Al alloy and a eutectic phase made up of Si polyhe-
dral particles and needles surrounded by a-Al ~Figs. 2, 3!.
During the solidification process, segregation phenomena
occur in the a-Al dendrites, generating differences between
the electrochemical potential between periphery and core
~Osorio et al., 2007!. The use of color metallography tech-
niques has allowed us to highlight this phenomenon of
segregation ~Figs. 2b, 3b! through differences in coloring
evidencing the rejection of solute from the growing solid to
the liquid interface, resulting in dendrite microsegregation.
It is also possible to appreciate that the eutectic phase does
not exhibit microsegregation, as its solidification takes place
at constant temperature in a succession of liquid homogeni-
zation microequilibrium stages. Needles of the intermetallic
b-AlFeSi compoundcanbe observedaccompanying the afore-
mentioned phases, the presence of which can be appreciated
in the micrographs obtained by the color metallographic tech-
nique ~Figs. 2b, 3b!. These can also be distinguished using
the BEI technique ~Fig. 4!, the B&W technique ~Figs. 2a, 3a!
being suitable only for their qualitative evaluation. The BEI
micrographs allow us to differentiate the needles of the Fe-
rich compound from those of the eutectic Si and reveal their
sequence of formation during solidification ~Fig. 4!. In fact,
eutectic Si needles can be seen nucleated on lamellae or rods
of intermetallic b-AlFeSi, indicating that these Fe compounds
were formed before the eutectic phase.
The results in Table 2 show that the size of the primary
a-Al in Alloy 2 has been reduced by about 88% compared
with the commercial alloy with no modification or refine-
ment ~Alloy 1!. Furthermore, the volume fraction of a-Al
has increased by 10%, underlining the a-forming nature of
the Ti. The colorings adopted by the microconstituents after
etching also highlight the segregation of dendrites in Alloy 2
~Fig. 5!. These colorings show that optical color metallogra-
phy facilitates the identification of poorly modified regions
in the eutectic phase, which present a darker tone ~Fig. 5b!.
Detailed analysis of the Fe-rich intermetallic com-
pound in Alloy 2 reveals the existence of two populations
for the needle size of this phase, which constitutes a distin-
guishing feature with respect to Alloy 1. On the one hand,
thick needles grew in the liquid phase, which can act as
nucleating agents of the primary a-Al and the eutectic Si
Figure 8. Backscattered electron image micrograph of Alloy 2
solidified at high pressure after etching with HF reagent showing
the irregular outline of the eutectic Si originated in its zig-zag
growth mechanism. Scale bar 10 mm.
Figure 9. Solidification route for Al12Si alloy after Gruzleski
~2000a!.
1024 George Vander Voort et al.
phases ~Figs. 5a, 6!. Some are seen trapped between den-
drites of the latter phase, denoting their proeutectic nature.
On the other, there are small amounts of thin needles of
this intermetallic compound, of similar coloring, intermin-
gled with the eutectic phase ~Figs. 5, 6!. Precipitation of
primary b-phase needles in the liquid is a result of oversat-
uration of Fe in the presence of the Sr added to the mixture.
Sr causes generalized undercooling of the eutectic phase
and a shift in its composition towards higher Si contents
~Tenekedjiev et al., 1995!. This makes the alloy slightly
hypoeutectic and favors the formation of primary a-Al on
the pre-existing Fe needles ~Narayan et al., 1994!. Owing to
the low solubility of Fe in Al, the a-Al dendrites continue to
grow, ejecting Fe into the residual liquid. On reaching the
eutectic temperature, the Fe needles precipitate once again.
As this occurs at lower temperatures, these needles are
smaller and more abundant than those formed previously.
Effect of Solidification at High Pressure on the
Microstructure of Alloy 413.0
Previous research ~Suarez-Pea et al., 2007! concluded that
an increase in pressure during solidification leads to an
increase in the temperature of solidification and the shifting
of the eutectic point toward higher Si contents ~Fig. 10!. As
occurred in the samples solidified at atmospheric pressure
in the presence of Sr ~Alloy 2!, this results in hypoeutectic
solidification. It can be seen ~Table 2! that a more than
twofold increase in the volume fraction of primary a-Al is
produced in Alloy 1, allowing us to estimate the eutectic
composition at 18 wt% Si under the action of pressure.
Comparing the volume fraction of the a-Al phase in
Alloy 1 solidified at high pressure with that of Alloy 2
solidified at atmospheric pressure ~Table 2!, we find that the
former is 15% higher. Furthermore, after solidification at a
pressure of 34 MPa, the grains of the a-Al phase exhibit an
almost equiaxial morphology ~Fig. 7a!, with sizes 57% smaller
than those obtained when the alloy is cooled at atmospheric
pressure after modification and refinement ~Fig. 5!. In con-
clusion, the effect of pressure on the a-Al phase is more
pronounced than that of modification and refinement in
samples solidified at atmospheric pressure.
When these alloys solidify at a high pressure, modifica-
tion and refinement do not bring about significant changes
in the morphology of the a-Al phase, which remains equi-
axial. However, an increase of around 7% in the volume
fraction of this phase can be appreciated together with a
decrease in grain size of 45% ~Fig. 7, Table 2!. This shows
the complementary effect of pressure jointly with modifica-
tion and refining on the microstructural changes of the
a-Al primary phase. Changes in the morphology and size of
the eutectic Si can also be observed with a globular morphol-
ogy ~point-like eutectic!, although these globules are not as
fine as those found in the modified and refined alloy ~Al-
loy 2! cooled at atmospheric pressure ~Figs. 5, 7b!.
Electron microscopy ~Fig. 8! confirms the tendency of
the Fe-rich intermetallic compound to develop in acicular
form; in particular, its preferential development in the eu-
tectic region of Alloy 2 solidified at high pressure.
CONCLUSI ONS
The present investigation analyzes the influence on 413.0
alloy of the refinement and modification of its microstruc-
ture, as well as the effect of the application of high pressure
during solidification. In addition, it reports a novel tech-
nique for the qualitative and quantitative characterization
of the phases present. The methodology employed, which
combines the use of color metallography and electron micros-
copy, provides a valuable tool for researching and develop-
ing AlSi-based alloys.
In summary, the conclusions of the study are summa-
rized as follows:
1. Within the limit of the experimental parameters being
used in the present study, it can be stated that the effect
caused by applying high pressure during solidification of
eutectic AlSi alloys is more pronounced than that caused
by modification and refinement of the microstructure
when it solidifies at atmospheric pressure.
2. When aiming to characterize the primary a-Al phase,
optical color metallography observed under crossed XPST
is the most suitable technique.
3. When the goal is to characterize the eutectic Si, the use of
optical color metallography or electron microscopy is
equally valid.
4. The characterization of iron-rich intermetallic com-
pounds should preferably be performed by means of
backscattered electron imaging.
REFERENCES
Abbaschian, R., Abbaschian, L. & Reed-Hill, R.E. ~2009!. Solid-
ification of metals. In Physical Metallurgy Principles, Gowans,
H. ~Ed.!, pp. 408461. Stamford, CT: Cengage Learning.
Asensio-Lozano, J., Del Campo, J.J. & Suarez-Pea, B. ~2005!.
Correlation between microstructure and mechanical properties
Figure 10. Modification of equilibrium AlSi phase diagram ~ p
1 atm! by the effect of high pressure applied during solidification;
and simplified microstructure evolution for Al12Si from the
liquid to the solid state.
Color LOM and SEM Applied to Al12Si Alloys 1025
of escalator steps made by high pressure die casting. Microsc
Microanal 11~Suppl 2!, 17161717.
Asensio-Lozano, J., Suarez-Pea, B. & Vander Voort, G.F.
~2006!. Microstructural optimization of chill cast Al-Si eutectic
alloys. Microsc Microanal 12~Suppl 2!, 16081609.
Asensio-Lozano, J., Suarez-Pea, B. & Vander Voort, G.F.
~2007!. Interpretation of the mechanical quality index through
the microstructure in hypoeutectic and eutectic treated Al-Si
alloys. Microsc Microanal 13~Suppl 2!, 110111.
ASTM E138297 ~2010!. Standard Test Methods for Determining
Average Grain Size Using Semiautomatic and Automatic Image
Analysis. West Conshohocken, PA: ASTM International.
Chapon, J. & Szkliniarz, W. ~2001!. Quantitative metallography
of two-phase titanium alloys. Mater Charact 46, 149154.
Gruzleski, J.E. ~2000a!. Polyphase solidification. In Microstruc-
ture Development During Metalcasting, American Foundry-
mens Society Inc. ~Eds.!, pp. 196210. Des Plaines, IL: American
Foundrymens Society.
Gruzleski, J.E. ~2000b!. Morphological modification in industrial
alloys. In Microstructure Development During Metalcasting. Amer-
ican Foundrymens Society Inc. ~Eds.!, pp. 232233. Des Plaines,
IL: American Foundrymens Society.
Gruzleski, J.E. &Closset, B.M. ~1999!. Aluminum-silicon foundry
alloys. In The Treatment of Liquid Aluminum-Silicon Alloys.
American Foundrymens Society Inc. ~Eds.!, pp. 1324. Des
Plaines, IL: American Foundrymens Society.
Gndza, M., Kayab, H., adirli, E. & zmenc, A. ~2004!.
Interflake spacing and undercoolings in AlSi irregular eutectic
alloy. Mater Sci Eng A 369, 215229.
Hengcheng, L., Yu, S. & Guoxiong, S. ~2002!. Correlation be-
tween mechanical properties and amount of dendritic a-phase
in as-cast near eutectic Al-11.6% Si alloys modified with stron-
tium. Mater Sci Eng A 335, 6266.
Higginson, R.L. & Sellars, C.M. ~2003!. Worked Examples in
Quantitative Metallography. London: Maney Publishing.
Liao, H.C. & Sun, G.X. ~2003!. Mutual poisoning effect between
Sr and B in Al-Si casting alloys. Scr Mater 48, 10351039.
Lim, Y.P. ~2009!. Evaluation of Al-5Ti-1B and Al-10Sr in LM6 sand
castings. J Achievements Mater Manufact Eng 34, 7178.
Liu, L., Samuel, A.M., Samuel, F.H., Doty, H.W. & Valtierra, S.
~2004!. Characteristics of a-dendritic and eutectic structures in
Sr-treated Al-Si casting alloys. J Mater Sci 39, 215224.
Massalsky, T.B. ~1986!. Binary Alloy Phase Diagrams. Metals Park,
OH: American Society for Metals.
Muirhead, J., Cawley, J. & Strang, A. ~2000!. Quantitative
aspects of grain size measurement. Mater Sci Tech-Lond 16,
11601166.
Murty, B.S., Kori, S.A. & Chakraborty, M. ~2002!. Grain refine-
ment of aluminum and its alloys by heterogeneous nucleation
and alloying. Int Mater Rev 47, 329.
Narayan, L.A., Samuel, F.H. & Gruzleski, J.E. ~1994!. Crystalli-
zation behavior of iron-containing intermetallic compounds in
319 aluminum alloy. Metall Mater Trans A 25, 17611773.
Nogita, K. & Dahle, A.K. ~2001!. Eutectic solidification in hypoeu-
tectic AlSi alloys: Electron backscatter diffraction analysis.
Mater Charact 46, 305310.
Nogita, K., Yasuda, H., Yoshida, K., Uesugi, K., Takeuchi, A.,
Suzuki, Y. & Dahle, A.K. ~2006!. Determination of strontium
segregation in modified hypoeutectic AlSi alloy by micro
X-ray fluorescence analysis. Scripta Mater 55, 787790.
Osorio, W.R., Spinelli, J.E., Ferreira, I.L. & Garcia, A. ~2007!.
The roles of macrosegregation and dendritic array spacings on
the electrochemical behavior of an Al4.5 wt.% Cu alloy.
Electrochim Acta 52, 32653273.
Roebuck, B. ~2000!. Measurements of grain size distribution in
engineering materials. Mater Sci Tech-Lond 16, 11671174.
Shankar, S. & Apelian, D. ~2002!. Mechanism and preventive
measures for die soldering during Al casting in a ferrous mold.
J Oper Manage 54, 4754.
Sritharan, T. & Li, H. ~1997!. Influence of titanium to boron
ratio on the ability to grain refines aluminum-silicon alloys. J
Mater Process Technol 63, 585589.
Suarez-Pea, B., Asensio-Lozano, J. & Vander Voort, G.F.
~2007!. Metallographic research of the pressure effect on the
final microstructure of eutectic Al-Si alloys. Microsc Microanal
13~Suppl 2!, 10301031.
Tenekedjiev, N., Mulazimoglu, H., Closset, B. & Gruzleski,
J.E. ~1995!. Microstructures and Thermal Analysis of Strontium-
Treated Aluminum-Silicon Alloys. Des Plaines, IL: American
Foundrymens Society.
Vander Voort, G.F. ~1981!. Etching techniques for image analysis.
In Microstructural Science, Petzow, G.R., Paris, R., Albrecht,
E.D. & McCall, J.L. ~Eds.!, vol. 9, pp. 137154. New York:
Elsevier North-Holland.
Vander Voort, G.F. ~1994!. Precision and reproducibility of quan-
titative measurements. In Quantitative Microscopy and Image
Analysis, Diaz, D.J. ~Ed.!, pp. 2134. Materials Park, OH: ASM
International.
Vander Voort, G.F. ~1996!. Image analysis. In Materials Charac-
terization, Mills, K. ~Ed.!, vol. 10, pp. 309322. Materials Park,
OH: ASM International.
Vander Voort, G.F. ~1999!. Metallography: Principles and Practice.
Materials Park, OH: ASM International.
Vander Voort, G.F. ~2004a!. Color metallography. In Metallogra-
phy and Microstructures, ASM Handbook, Vander Voort, G.F.
~Ed.!, vol. 9, pp. 493512. Materials Park, OH: ASMInternational.
Vander Voort, G.F. ~2004b!. Light microscopy. In Metallography
and Microstructures, ASM Handbook, Vander Voort, G.F. ~Ed.!,
vol. 9, pp. 332354. Materials Park, OH: ASM International.
Vander Voort, G.F. & Asensio-Lozano, J. ~2009!. The Al-Si
phase diagram. Micros Microanal 15~Suppl 2!, 6061.
Warmuzek, M. ~2004!. Metallographic techniques for aluminum
and its alloys. In Metallography and Microstructures, ASM Hand-
book, Vander Voort, G.F. ~Ed.!, vol. 9, pp. 711751. Materials
Park, OH: ASM International.
Weck, E. & Leistner, E. ~1986!. Metallographic Instructions for
Color Etching by Immersion, Part III: Non-Ferrous Metals, Ce-
mented Carbides and Ferrous Metals, Nickel-Base and Cobalt-
Base Alloys. Dusseldorf, Germany: Deutscher Verlag fr
Schweitechnik.
1026 George Vander Voort et al.