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Materials Characterization 57 (2006) 371 385

Combined grain refining and modification of conventional and


rheo-cast A356 AlSi alloy
Shahrooz Nafisi 1 , Reza Ghomashchi ,2
Advanced Materials and Processing Research Group, University of Quebec at Chicoutimi, Chicoutimi, Quebec, Canada G7H 2B1
Received 6 June 2005; accepted 8 March 2006

Abstract
This paper describes a comprehensive study on the combined addition of TiB grain refiner and Sr modifier elements to A356
AlSi alloy. Using different qualitative and quantitative techniques in conventional and semi-solid metal castings, it is shown that,
while the refiner and modifier elements affect respectively the nucleation and eutectic reactions, the combined addition not only
replicates both individual element effects but also gives the added bonus of better globularity in the semi-solid metal process. A
new innovative concept is introduced for fluidity measurement by using the magnitude of remaining liquid in the form of drainage,
which is increased by combined treatment.
2006 Elsevier Inc. All rights reserved.
Keywords: Semi-Solid Metal; Rheocasting; SEED Process; Grain refiner; Modifier; Thermal analysis

1. Introduction
Grain refining and modification of AlSi alloys offer
substantial benefits in casting processes. Finer grains
ensure better mechanical properties, improved machinability, better feeding, while with modification the
silicon morphology changes from flake to fibrous,
resulting in improved properties, especially ductility [1
4]. Thus it is reasonable, and has become the norm for
the last two decades, to use treatments that combine
grain refining and modification, in order to take
advantages of both methods [5]. However, as reported
Corresponding author.
E-mail address: reza.ghomashchi@ampr-institute.com
(R. Ghomashchi).
URL: http://www.ampr-institute.com/.
1
Research fellow, Facility for Electron Microscopy Research,
McGill University, Montreal, Canada.
2
Former NSERC-ALCAN-UQAC Professor and Chair holder;
Director, Advanced Materials and Processing Research Institute.
1044-5803/$ - see front matter 2006 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2006.03.016

by the authors [6,7], each treatment has its own


characteristics and, with combination, considerable
changes may occur in the percentages, shapes and
sizes of both primary -Al and eutectic Si.
During the last two decades, there has been intensive
research into finding new and improved casting routes
to compensate for some of the drawbacks of conventional casting routes. Such efforts eventually led to the
introduction of semi-solid metal (SSM) processing.
SSM processing was realized as a side issue in a PhD
study [8] and has since attracted more attention, in both
the scientific and the technological domains, due to the
many potential technical, technological and economic
advantages.
In conventional diecasting, melt treatment, i.e.,
refining and modification, is not very common. This
can be explained by the nature of the process, which
involves high cooling rates to deliver finer microstructures. For SSM die casting, however, the process is
divided into a two-stage solidification, wherein a slowly

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S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

Fig. 1. Schematic of the SEED process.

cooled mush (liquid and solid mixture) with a mainly


globular structure is injected into a die assembly capable
of imposing rapid cooling of the mush, i.e., rheocasting.
An alternative is also recognized in which the slowly
cooled and solidified mush is reheated to temperatures
above the solidus and then injected into a die cavity to
shape, i.e., thixocasting.
One of the main aims of SSM processing, with
specific emphasis on Al alloys, is to obtain a primary
phase of globular structure, in order to improve the
thixotropic behavior and the mechanical properties of
the alloy. As a result, most of the studies have focused
on globule refinement [912] and there has been little
published on the combined effects [13]. The purpose of
the present paper is to report on the findings of the
combined effects of TiB and Sr-based additions to an
Al7Si0.35Mg alloy using a recently patented SSM
processing route involving the swirled enthalpy
equilibration device (SEED) [14].
2. Experimental procedure
The purpose of this research was to examine the
effects of the combined addition of grain refiner and
modifier in conventional casting and in SSM processing
of AlSi alloys. The semi-solid slurry for the SSM
processing was prepared using the SEED technology
(Fig. 1).

Grain refining and modification were carried out


on Al7Si0.35 Mg alloy by adding titanium, boron
and strontium in the forms of Al5Ti1B and
Al10Sr master alloys respectively. The additions
were made between 680 and 700 C, after which
the degassed melts rested for 2030 minutes before
sampling, then stirred for two minutes immediately
prior to sampling. The chemical compositions
before and after the combined treatment are given
in Table 1.
Graphite cups of 25 mm inner diameter and 5 mm
wall thickness were used for conventional casting.
These were immersed into the melt for approximately
1 min before sampling to ensure uniform temperature
distribution across the sample at the beginning of
solidification. Each cup with 50 g of alloy was
transferred to the cooling station and two K-type
thermocouples were quickly immersed into the melt,
near the center and the mold wall, with thermocouples tips located 10 mm from the bottom of the
cups. Temperature readings were collected using a
high-speed high resolution National Instrument data
logger system with a sampling rate of 10 readings
per second. For these series of experiments, the
cooling rate was between 1.5 and 2 C s 1 above
the liquidus temperature. The analysis of thermal
data was carried out based on analysis of the AlSi
solidification temperature [15,16] and the following

Table 1
Chemical analysis of A356 melts (wt.%)

Base alloy
Treated alloy

Si

Mg

Fe

Mn

Cu

Ti

Sr

Al

6.68
6.68

0.4
0.39

0.07
0.08

0.003
0.003

0.001
0.001

0.0058
0.058

0.0001
0.0098

0.0003 max.
0.0003 max.

0.000
0.014

bal.
bal.

S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

critical points (temperature, T, and time, t) were


identified:
TnucAl: start of primary -Al dendrites nucleation
TminAl: newly nucleated crystals have grown to such
an extent that the latent heat liberated balances out
the heat extracted from the sample
TgAl: recalescence of steady state growth temperature due to release of latent heat of primary -Al
dendrites
TRec: temperature difference between unsteady
(TminAl) and steady (TgAl) states growth temperatures of primary -Al particles
tRec: time difference between TminAl and TgAl, the
times associated with TminAl and TgAl (in the
literature, it was called the liquidus undercooling
time, [16,18])
Tnuceut: start of eutectic nucleation
Tmineut and Tmaxeut: minimum and maximum of
eutectic temperatures.
For SSM processing, 2 kg of the alloy were poured at
645 C into a SEED cylindrical refractory-coated steel
mold of diameter 75 mm and length 200 mm (Fig. 1).
The mold was initially swirled at 2.5 Hz for a certain
duration to form approximately 0.20.3 fraction solid.
After a short resting period, the bottom enclosure of the
mold was opened to drain the remaining liquid for a
specific period of time. The overall casting procedure
did not exceed 90 s. After draining, the billet was
quenched into cold water. The quenching temperature
was 596 2 C. In all experiments, a 0.8 mm diameter
K-type thermocouple was inserted in the mold center at
a distance 80 mm from the bottom of the mold to collect
thermal data. The cooling rate during solidification was
about 5 C s 1 for the SEED billets.
Transverse samples were prepared by sectioning the
cylindrical billets near the thermocouple tips (that is,
10 mm and 80 mm from the bottom of the conventional
and the SEED billets respectively). For a complete
description of the microstructure, it was necessary to
characterize and quantify such microstructural parameters as the primary -Al particle size, grain size,
number density, sphericity3, and area to perimeter ratio,
A/P, which is proportional to the inverse of the surface
area per unit volume4, Sv. For this purpose, a Clemex

4pA

3
Sphercity 2 , where A is total area of primary particles and P
P
is perimeter of liquidsolid interface. The closer the sphericity to 1,
the higher is the globularity of the particle.
4P
4
Sv , where Sv is specific volume surface of the particles (an
pA
estimation of 3D).

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image analysis system was used and a routine written to


differentiate effectively the contrast variations between
the eutectic and the primary -Al particles, and a macroetching technique was employed for better distinction. In
order to obtain a representative structure, all the data
were obtained from image processing of the resultant
microstructure between the center and the wall surface of
the billet. A total of 85 randomly selected fields with the
total area of 255 mm2 were scanned (at a magnification
of 50) for the -Al particle measurements, while 50
fields with a total area of 1.5 mm2 (magnification 500)
were examined in order to evaluate the silicon
morphology (conventional cast specimens only).
Because the silicon morphology changes due to the
addition of Sr in the SEED process were beyond the
resolution limit of the light optical microscope of the
image analysis system, a Hitachi S4700 scanning
electron microscope (SEM) was used to characterize
the structure using deep-etched (10% HF) specimens.
3. Results and discussion
3.1. Conventional casting
3.1.1. Thermal analysis
Fig. 2 shows the nucleation and growth segments of
typical cooling curves for primary -Al formation and
the eutectic reaction of both untreated and treated alloys.
As is evident, the nucleation and growth temperatures
have shifted up for the primary -Al, while the eutectic
reaction has been suppressed to lower temperatures as a
result of the grain refiner and modifier co-addition.
From the solidification point of view, Fig. 2(A), as
the temperature falls at a given cooling rate below the
nucleation temperature, TnucAl, the nucleation rate rises
exponentially to such an extent that it compensates heat
extraction and eventually overrides it after the minimum
temperature, TminAl. In other words, the evolution of
latent heat retards the cooling rate up to the minimum
and thereafter the melt is reheated to TgAl due mainly to
the growth of primary nuclei. It is quite important to
note that by the time recalescence is complete, all the
nucleation opportunities have ceased and the final grain
density is predictable.
The effects of separate individual additions of refiner
and modifier to the A356 AlSi alloy have been
reported previously by the authors [6,7]. Individual
additions of the grain refiner raised the primary -Al
nucleation temperature by as much as 45 C, while
sole additions of the Sr-based modifier depressed
eutectic temperature by almost 78 C. In other
words, if both additives performed in the same manner

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Fig. 2. Cooling curves before and after additions. (A) Beginning of solidification; (B) Eutectic reaction zone.

in the combined case, the solidification range (TnucAl


Tnuceut) should increase by 1113 C. This, in fact, is
what was observed in the present case for the combined
addition (see Fig. 3). Widening the solidification range
may not be regarded important for conventional casting
or even be a drawback due to increasing the incident of
porosity, but it is quite crucial for SSM processes.
Furthermore, development of a wider freezing range
slows down directional solidification, which is again a
point in favor for SSM processing.
As was mentioned previously, the small addition of
Ti and B shifted the curves up and recalescence
decreased. In other words, the addition of grain refiners
has catalyzed the nucleation of primary -Al sooner and
with more nuclei in the melt. Furthermore, both
nucleation and growth temperatures of the -Al

particles increased but the temperature rise was greater


for TnucAl, as can be seen clearly in Fig. 3(A). This
means that there are more nuclei with a lower chance of
growth at any one time during nucleation and early
growth of the primary phase.
Fig. 3(C) and (D) show the changes in Tnuceut,
Tmaxeut, eutectic undercooling (=TmaxeutTmineut),
and the solidification range (T) due to the combined
treatment. As has been shown in previous publications
[6,7], the changes in eutectic temperature parameters are
the same for the individual and the combined treatments,
which may confirm the independent functions of the
grain refiner and the modifier during solidification. In
other words, the strong affinity of B for Ti to form TiB2
nucleants impedes any reaction between Sr and B to form
SrB6 compounds and thus deactivate Sr as a modifier.

S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385


Fig. 3. (A, B) Variation of nucleation and growth temperatures of -Al particles due to the grain refiner effect. (C, D) Variation of nucleation, maximum, and recalescence of eutectic and T due to the
modifier effect.
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It is evident from Fig. 3(C) and (D) that the eutectic


nucleation temperature and eutectic maximum temperature decreased with the addition of Sr, while at the same
time, the eutectic undercooling, , increased by
2 C. In addition, the depression of the eutectic
temperature gave rise to a larger -Al solidification
range and consequently more -Al formation. The
interesting point here is that the increase in T is a little
more here when comparison is made with the Sr
addition alone since the addition of the refiner brought
about an increase in the -Al particle nucleation
temperature and in the solidification range.
3.1.2. Microstructure
The light optical micrographs in Fig. 4 illustrate the
resulting microstructural changes due to combined
treatment. The primary -Al phase has a fully columnar
(dendritic) and transforms to an equiaxed morphology

with the combined addition. Such an effect is believed to


be solely due to the grain refiner segment of the
combined treatment. The eutectic mixture is also
affected by this treatment, with the flake silicon present
in the untreated specimen (Fig. 4(A) and (B)) transforming fully to a fibrous structure (Fig. 4(C) and (D)), the
effect being due to the Sr content.
The correlation between the average grain size
measurement, the -Al nucleation temperature and the
liquidus under-cooling time is demonstrated in Fig. 5.
With the simultaneous addition of Ti, B and Sr, the grain
size was reduced more efficiently than when the grain
refiner was added separately, the final grain size being
520 m (a 56% reduction as against 33% by the
refiner by itself). It seems that combined effect gives
better refinement than the addition of individual master
alloys. Such a conclusion may be reached if the
recalescence values for the combined ( 0.5 to 0.1)

Fig. 4. Light optical micrographs showing the effect of the combined treatment. (A, B) Untreated base alloy; (C, D) alloy after the addition of 580 ppm
Ti, 98 ppm B, 140 ppm Sr.

S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

377

Fig. 5. Relationship between grain size and the parameters TnucAl and (TgALTminAl).

Fig. 6. Polarized light micrographs showing the effect of Ti, B


addition: (A) base alloy without any additions; (B) alloy with the
addition of 580 ppm Ti, 98 ppm B and140 ppm Sr.

Fig. 7. SEM micrographs of selected samples, deep-etched in 10% HF.


(A) Base alloy without any additions; (B) alloy with the addition of
580 ppm Ti, 98 ppm B, 140 ppm Sr.

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Fig. 8. Microstructural parameters of eutectic Si. (A) Si %; (B) number density of Si particles; (C) circular diameter and area/perimeter ratio; (D) percentage of particles having aspect ratio greater than 2.

S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

and the sole treatment ( 1.0 to 0.5) are compared. It is


well established that the smaller the magnitude of
recalescence, the more effective is the grain refiner.
Interestingly, by calculation of the liquidus undercooling time, tRec, it was observed that this time
decreased by refiner addition. A small value of tRec
signifies that the grains do not have a long growth
period. In other words, longer values of tRec are related
to more growth opportunity and consequently more
dendrite formation. This is in line with the micrographs shown in Fig. 6 and with previous findings on
the effects of refiner additions to the AlSi alloys
[17,18].
The refiner addition gave rise to an increase in the Al nucleation temperature due to the presence of more
potent and effective nucleants in the bulk liquid. When
there is a high density of nucleants in the system, i.e.,
multiplication or copious nucleation, the mean free path

379

between the nuclei becomes small and thus grain growth


is restricted. Furthermore the heat flow becomes
multidirectional due to the high density of nucleants.
Such solidification conditions should eventually lead to
the formation of somewhat spherical primary phase
particles, Fig. 6.
As mentioned in the previous section, the Sr content
of the combined treatment modifies the morphology of
eutectic Si. This can be seen in the two SEM
micrographs in Fig. 7, where the change of the flaky
structure of the Si to a fibrous one and a seaweed-like
structure is visible.
3.1.3. Image analysis
Fig. 8 shows the data obtained from image processing of the microstructure. The percentage of Si in the
microstructure increases with the addition of the
modifier Sr, as expected based on the thermal analysis

Fig. 9. Light optical micrographs showing the effect of simultaneous melt treatment in the SEED process. (A, B) Untreated base alloy; (C, D) alloy
with the addition of 580 ppm Ti, 98 ppm B, 140 ppm Sr.

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istic of highly branched structures, e.g., fibrous


morphology.
3.2. SEED process
3.2.1. Microstructure
The light optical micrographs in Fig. 9 show the
effect of the combined treatment. Grain refining
efficiency is obvious through the size reduction of the
globules and the presence of more primary particles.
The Sr modifier effect, the morphological change of the
Si particles from lamellar to fibrous, can be seen in the
higher magnification images of Fig. 10.
It may be argued that there is not much difference
between the morphology of the -Al particles of the
untreated alloy and that of the treated alloy. For the
untreated alloy it has to be mentioned that, in most
cases, the -Al particles have a complex morphology
and therefore two-dimensional characterizations are not
good enough to comprehend the complete characteristics of the particles. In other words, what is supposed
to be one globule may have stretched or interconnected

Fig. 10. Variation of silicon morphology due to Sr addition: (A)


without Sr, (B) 140ppm Sr.

described in the previous section. The addition of Sr


depresses the eutectic point and shifts it to the right. A
simple lever rule calculation on the AlSi phase
diagram confirms this conclusion.
The transformation of Si flakes to a fibrous
morphology is also visible through the number density,
the area-to-perimeter ratio, and the aspect ratio, as
shown in Fig. 8. With the addition of the modifier, the
number density increased while the average circular
diameter, the area/perimeter ratio, and the aspect ratio
decreased.
It should be noted that a correlation always exists
among the above-mentioned parameters to confirm the
morphological changes of flake to fibrous growth of the
eutectic Si. The rapid rise of the number density of the Si
particles together with the reduction in the eutectic Si
size in the form of the circular diameter and the lower
aspect ratio verify a greater number of Si branches
intersecting the 2D polished surface. This is character-

Fig. 11. (A) Polarized light micrograph and (B) schematic representation of dendrites transformation to cramped dendrites due to stirring.

S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

381

optimum or, indeed, the desired structure is that one


grain in the macrostructure has the same size of one
globule.
The effect of the combined treatment in rendering
better globularity of the primary -Al particles could
also be explained in terms of the modifier and its
effect on the morphological changes in the Si. This is
due to the growth nature of the fibrous structure of Si
in the eutectic mixture, which encompasses the
primary -Al phase without being a continuation of
it. Therefore, the globules are indeed true globules
when Sr is added. As was shown by Dahle et al. [19],
in unmodified alloy the eutectic grows from the
primary phase, while for Sr-modified alloy eutectic
grains nucleate and grow separately from the primary
dendrites.
The Si morphological changes due to the combined
treatment are illustrated by the SEM micrographs in

Fig. 12. Polarized light micrographs of SEED quenched billets. (A)


Untreated base alloy, (B) alloy after treatment with 580 ppm Ti,
98 ppm B and 140 ppm Sr.

to other globules. This concept is illustrated in Fig. 11,


a magnified polarized light micrograph of an actual
polished sample together with a model proposed for
this evolution. By stirring and forced flow, i.e.,
convection, pre-formed dendrites are compelled either
to break up by fragmentation [20] or by a root remelting mechanism [21], or, in another case, may be
plastically bent, the final shape being a cramped
dendrite. Fig. 11 confirms that the individual globules
could indeed be part of one single cramped dendrite
and only appeared as globules due to metallographic
sectioning. In order to determine whether the globules
are independent grains or segments of larger cramped
-Al phase, polarized light microscopy must be used.
The polarized light micrographs in Fig. 12 confirm the
effectiveness of the combined treatment in generating
better globularization of the primary -Al. As is
evident, the number of globules in the -Al particles
colony is higher in the untreated specimen. The

Fig. 13. SEM micrographs of selected SEED samples, deep etched in


10% HF. (A) Untreated base alloy; (B) alloy after treatment with
580 ppm Ti, 98 ppm B, 140 ppm Sr.

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S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385
Fig. 14. Microstructural parameters of the SEED samples. (A) Primary -Al percentage; (B) circular diameter and number density of the -Al particles; (C) area/perimeter ratio and aspect ratio; (D)
sphericity.

S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

Fig. 13. The flaky structure of the Si has changed to a


fibrous morphology having seaweed-like attribute.
Furthermore, in contrast to the conventional cast
specimens (see Fig. 7), extra refinement of the
structure is attributed partly to the quenching of the
SSM slurries from the mushy zone and partly to the
fluid flow and thermal uniformity within the SSM
mold. This means that branching of the Si fibers is not
hindered and it can branch off in any direction since
there is no directional heat flow in the mold (for more
details, see [7]).
3.2.2. Image analysis
As discussed in the previous sections, the
microstructure is quite fine in the SSM billets and
optical quantitative metallography was not viable for
the eutectic Si. Therefore, the results as presented in
Fig. 14 are concentrated solely on the primary -Al
phase.
The primary -Al percentage appears to have
increased which is due to the higher number of effective
nuclei from the refining side plus the increase in the Al solidification range arising from the Sr, Ti, and B
additions (the combined treatment increased the -Al
solidification range by 1113 C).
It was shown previously that with modification
alone the number density of the primary -Al particles
remained unchanged while the quantity increased and
hence the average circular diameter rose. This is not the
case for the combined treatment in this situation, as can
be seen in Fig. 14(B), where the average circular
diameter decreased slightly but the change in number
density is more pronounced. This is attributed to the

383

grain refining effect in shifting the nucleation temperature to higher values and causing the formation of
more nuclei per unit volume. The greater number of
nuclei compensates for the enlargement of the solidification range due to the combined treatment. Furthermore, the average area/perimeter ratio is approximately
constant while the percentage of -Al particles with
aspect ratio > 2% decreases. Such a finding, coupled
with the increasing sphericity values as shown in Fig.
14(D), is an indication of improving globularity of the
structure.
As was mentioned in the experimental procedure
section, drainage is part of the SEED process to provide
a self-standing billet, but it is the belief of the authors
that it can also be an indication of the fluidity of the
alloy. Here it has to be noted that this may be
contradictory to the classical meaning of fluidity,
which is normally defined as the distance to which a
metal will run before solidification. The drainage
percentage increased with the combined treatment, as
can be seen in Fig. 15. Such a finding may look
contradictory to the fact that, by increasing the primary
-Al percentages, the drainage should decrease due to
the agglomeration and blockage of the mold bottom
orifice.
Drainage augmentation could be explained from
different aspects. According to the literature on
conventional casting [22], the dendrite coherency
point, DCP, has a direct relationship with the fluidity
concept, where in a postponed DCP improves fluidity,
i.e., smooth channels without interlocking pathways for
liquid flow. On the other hand, from the modification
point of view, Sr postpones the DCP, meaning that, in

Fig. 15. Drainage of liquid during the SEED process.

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S. Nafisi, R. Ghomashchi / Materials Characterization 57 (2006) 371385

spite of the increasing -Al percentage, more flow exists


in the slug. This is supported by the better sphericity
numbers where more globular particles are formed with
the combined treatment. That is to say, there are
smoother inter-particle channels in which liquid can
flow. These are in line with the increased fluidity of the
modified and refined alloys [2325].
4. Conclusions
A comprehensive study has been reported on the
combined addition of grain refiner and modifier
elements to A356 AlSi alloy. Using different qualitative and quantitative techniques in conventional and
semisolid castings, it has been shown that, while the
refiner and modifier elements affect, respectively, the
nucleation and eutectic reactions, combined addition not
only replicates both effects but also gives the added
bonus of better globularity in the SSM process. A new
innovative concept is introduced for fluidity measurement by using the magnitude of remaining liquid in the
form of drainage, which is increased by combined
treatment.
Acknowledgments
The work reported here is part of an NSERCALCAN-UQAC industrial research chair, grant No.
IRCPJ268528-01, on the Solidification and Metallurgy of Al alloys. The financial support provided by
NSERC and ALCAN International Limited is gratefully acknowledged. Special thanks are due to
Professor H. Vali, Director of Electron Microscopy,
and Mrs. L. Mongeon of the Facility for Electron
Microscopy Research at McGill University for the
SEM analysis.
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