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Effect of grain refinement and dissolved

hydrogen on the fluidity of A356 alloy


M. Di Sabatino* and L. Arnberg
Norwegian University of Science and Technology, Department of Materials Technology, A. Getz v. 2B,
N-7491 Trondheim, Norway

The influence of grain refinement and dissolved 0.15 wt-%Ti was added to an Al–4.5 wt-%Cu alloy
hydrogen on the fluidity of A356 alloy has been tested with a vacuum fluidity apparatus. Tiryakioglu
investigated. A spiral casting test method, recently et al.11 found no effect on grain refinement in A356
developed, has been used to measure fluidity in a and 319 alloys, adding 0.04 wt-%Ti as AlTi5B1
reproducible way. The grain refinement reduces the master alloy tested in a sand moulded spiral.
grain size of the spirals, particularly at the tip, but no Lang12 found a significant increase in fluidity with
significant influence on the fluidity has been revealed. boron additions in the range 0.04–0.07 wt-%B to Al–
The hydrogen additions in the melt have not affected Si alloys tested with a bar die casting. Dahle et al.13
the fluidity but have, of course, significantly increased observed a more complex variation in fluidity with
the porosity. IJC/556 successive additions of AlTi5B1 in Al–7 wt-%Si–Mg
and Al–11 wt-%Si–Mg alloys tested with a sand
# 2005 W. S. Maney & Son Ltd. Manuscript received
moulded spiral. The reproducibility of the test
1 December 2004; accepted 1 February 2005.
apparatus was about 10% and the fluidity was
Keywords: Fluidity; Grain refinement; Hydrogen effect; reduced with grain refinement below 0.12 wt-%Ti,
Porosity; Grain size; Inclusions while it increased with additions above 0.12 wt-%Ti.
The fluidity length decreased 5% with 0.01 wt-%Ti
Introduction and increased up to 9% with a further addition of
0.12 wt-%Ti.13 Moreover, Dahle et al.14 studied five
Fluidity is an important feature of aluminium alloys levels (0, 0.01, 0.03, 0.05 and 0.12 wt-%) of AlTi5B1
because it restricts their applicability for casting grain refiner additions to Al–1 wt-%Mg, Al–5 wt-%Mg,
purposes. The knowledge of the parameters influenc- Al–2 wt-%Cu and Al–4 wt-%Cu alloys. The fluidity
ing fluidity is important in order to achieve good measurements were assessed using a vacuum fluidity
quality and thin walled castings. Fluidity has been test apparatus of about 7% reproducibility. For all
investigated by many researchers and is affected by alloys the fluidity was lower at the highest grain
many factors. Portevin and Bastien1 have shown that refiner content than in the unrefined alloy. Kwon
fluidity varies inversely with solidification range et al.15 studied the effect of grain refinement on A356
(liquidus minus solidus temperatures) in most alloy alloy. The fluidity test apparatus consisted of a steel
systems. The larger the solidification range, the lower mould with eight thin channels and had 10%
is the fluidity of the alloy system.1 The maximum reproducibility. Whereas 0.03 wt-%Ti as AlTi5B1
fluidity of a binary system is obtained at the pure grain refiner appreciably improved the fluidity at
component and eutectic compositions.2 The Al–Si the lowest pouring temperature (700uC), the addition
system, however, shows maximum fluidity at a of 0.2 wt-%Ti did not have appreciable effect on the
hypereutectic composition3 owing to the high heat fluidity of the base alloy. Kwon et al.15 also reported
of fusion of silicon and a skewed coupled zone in the that oxide inclusions in the melt decreased the fluidity,
Al–Si system.4,5 Melt superheat (the difference especially at a low pouring temperature.
between the melt temperature and the liquidus The effect of dissolved hydrogen on fluidity in Al–
temperature) is also a key factor influencing fluidity. Si and Al–Si–Cu alloys has not yet been published.
Many authors6–8 have reported that, for a given alloy A new version of the spiral test method has recently
composition, the fluidity increases linearly with been developed and shown to give results with
increasing melt temperature. Kolsgaard8 has reported improved reproducibility.9 The purpose of the present
that an increase of 1 K in the melt temperature study is to use this improved test method to
gives an increase of 1% in the fluidity length of Al– investigate the influence of grain refinement and
7 wt-%Si–0.6 wt-%Mg alloy reinforced with 10–30% hydrogen additions on the fluidity of one of the most
SiC particles. This finding has been confirmed by commercially important Al–Si alloys, A356 alloy.
recent work9 on A356 alloy.
Controversial results on the effect of grain refine-
ment on fluidity have been reported in the literature. Experimental
Mollard et al.10 showed a reduction in fluidity when
Fluidity test apparatus and alloy
The main parts of the fluidity test apparatus are
*Corresponding author, email marisa.di.sabatino@nt. shown in Fig. 1. It consisted of a pouring cup, a short
ntnu.no circular tapered sprue, a stopper rod connected to a

DOI 10.1179/136404605225022982 International Journal of Cast Metals Research 2005 Vol. 18 No. 3 181
182 Di Sabatino and Arnberg Effect of grain refinement and dissolved hydrogen on fluidity of A356 alloy

(a) (b)

2 a as-cast spiral in sand mould and two loca-


tions where samples were taken for each inves-
tigated spiral (B – base of spiral, close to
pouring basin; T – tip of spiral) and b cross-
section of spiral

Ti became 0.07, 0.08 and 0.1 wt-% respectively. Ten


spirals each were cast at 715uC with 0.01, 0.02 and
0.04 wt-%Ti additions. Four spirals for the unrefined
alloy and four spirals for each addition of grain
refiner were studied. For each investigated spiral, two
samples were subjected to metallographic study: one
from the base (close to the pouring cup) and one from
the tip of the spiral. Figure 2 shows an as-cast spiral
in a sand mould, the two locations where the samples
1 Fluidity test apparatus. Main parts are: A – were taken and the cross-section (4610 mm2) of each
stopper rod; B – pouring cup; C – sand mould; investigated spiral. The samples were polished down
D – metallic clamps; E – pneumatic cylinder to 1 mm and anodized in a solution of HBF4. A series
of images were taken using optical microscopy
pneumatic cylinder and a silica sand mould made with without (Fig. 3) and with (Fig. 4) polarized light.
a core shooter using the cold box process (phenolic The grain sizes were measured using the linear
urethane resin cured with amine vapour). The intercept method.16
movable stopper rod initially closed the bottom of
the pouring cup and automatically opened the gate Hydrogen addition
when the molten metal temperature reached a preset In order to study the effect of hydrogen on fluidity,
value, measured by a thermocouple in a fixed position three levels of hydrogen were chosen. The first level
in the pouring cup. The pneumatic valve, controlled was chosen as the initial hydrogen level in the melted
by a PC, regulated the movement of the stopper rod. alloy, and the second was measured after purging
When the gate opened, the metal filled the spiral sand pure argon (99.99 wt-%Ar) with a rotating impeller
mould. In this way the equipment provided an for 45 min. During purging the melt temperature was
accurate melt superheat. A more detailed description kept between 700 and 720uC, which is known to give a
of the test apparatus and its reproducibility was high efficiency during degassing.17 The third hydro-
previously presented.9 The alloy used in the experi- gen level was measured after plunging pieces of wood
ments was A356 with the chemical composition beneath the surface of the molten metal. The three
shown in Table 1. A batch of 50 kg of the alloy hydrogen levels obtained were 0.13, 0.15 and 0.43 ml
was melted at 760uC in a resistance furnace. The per 100 g for the argon purged (P), as-received (A)
spiral length was taken as the fluidity value. and hydrogen up-gassed (H) melts respectively.
Spirals were cast under the same atmospheric
Addition of grain refiner condition (same relative air humidity and room
In order to study the effect of grain refinement on temperature). The hydrogen concentration in the
fluidity, three different amounts of an AlTi5B1 rod
Table 2 Chemical composition (wt-%) of grain refi-
type grain refiner were added to the molten A356 ner AlTi5B1
alloy. The chemical composition of the grain refiner is
given in Table 2. Grain refiner was added to increase Alloy Si Fe Ti B V
the Ti content by 0.01, 0.02 and 0.04 wt-%. Because
AlTi5B1 0.07 0.11 4.8 1.0 0.06
the alloy contained Ti as received, the total amount of

Table 1 Chemical composition of A356 alloy (wt-%)


Al Si Mg Fe Sr Ti Ga Cu Mn Zn Ca

Bal. 6.6 0.378 0.198 0.021 0.059 0.01 0.004 0.004 0.005 0.003

International Journal of Cast Metals Research 2005 Vol. 18 No. 3


Di Sabatino and Arnberg Effect of grain refinement and dissolved hydrogen on fluidity of A356 alloy 183

(b)

3 Optical micrographs of refined sample 1R2 (0.01 wt-%Ti) from a base and b tip of spiral

(b)

4 Polarised light images of refined sample 1R2 (0.01 wt-%Ti) from a base and b tip of spiral

melt was measured with an AlscanTM apparatus. For PoDFA tests20 were performed to correlate the level
each hydrogen level, ten spirals were cast at 700uC. of inclusions to fluidity measurements. For the PoDFA
Optical microscopy and porosity studies were made tests, two samples were taken after argon purging and
on the selected samples. The tendency to porosity hydrogen addition respectively. Backscattered electron
formation was evaluated qualitatively with a reduced micrographs were taken as well as microprobe analyses
pressure test (RPT).18,19 during the cast trials, and of the selected area of the samples, taken from the filter
quantitatively from the density measurements. The cake just above the filter.
selected samples were weighed in air and water, and
the density was calculated according to Archimedes’ Results
principle. The percentage porosity was defined by the
relationship Table 3 shows the average length of the fluidity
r {r measurements and the standard error in the mean
%Porosity~ max |100 : : : : : : (1)
rmax Table 3 Average length of fluidity measurements
where rmax is the density of the fully dense material and standard error in mean values for 10
(alloy density) and r is the experimentally observed spirals cast without and with grain refiner
density given by additions

Wa Grain refiner additions, wt-%Ti Average length ¡ sm, mm


r~ r : : : : : : : : : : : (2)
j Ww j 0 0 540¡10
0.01 550¡10
where Wa is the weight in air, Ww is the weight in
0.02 560¡10
water and r0 is the density of water at room 0.04 550¡20
temperature.

International Journal of Cast Metals Research 2005 Vol. 18 No. 3


184 Di Sabatino and Arnberg Effect of grain refinement and dissolved hydrogen on fluidity of A356 alloy

(b)

5 Samples from reduced pressure test: a after purging (hydrogen level 0.13 ml per 100 g); b after hydro-
gen addition (hydrogen level 0.43 ml per 100 g)

values for 10 spirals cast without and with grain calculated from the density measurements for selected
refiner additions. Table 4 shows the grain size spirals and the standard error in the mean values, sm
measurements from the base and tip of each (%), for the three hydrogen levels.
investigated spiral. The average of the grain size The volume concentration of inclusions for low and
measurements for each investigated spiral and the high levels of hydrogen was calculated from the
standard error in the mean values were also PoDFA samples in Table 7. Microprobe analyses
calculated. Figures 3 and 4 are optical and anodized were performed to identify the types of inclusion in
micrographs of the same spiral sample taken from the the samples. Figure 6 shows backscattered electron
base (Figs. 3a and 4a) and tip (Figs. 3b and 4b) of the micrographs of the microstructure of the purged and
spiral. up-gassed samples. The type of inclusions present in
Table 5 shows the average length of the fluidity both samples is also indicated.
measurements for the three hydrogen levels and the
standard error in the mean values. Figure 5 shows Discussion
two samples from the reduced pressure test (RPT)
that were taken after purging, giving a hydrogen level The fluidity measurements for three additions of
of 0.13 ml per 100 g, and after hydrogen addition, AlTi5B1 reveal that fluidity does not significantly
giving 0.43 ml per 100 g. Table 6 shows the porosity change with these additions. Table 3 shows that the
difference between the average fluidity lengths for
the three additions is within the standard error in the
Table 4 Grain size measurement averages from
mean values. Therefore, no statistically significant
base and from tip of each spiral, and
their average¡sm (standard error in mean effect of grain refinement on the fluidity of A356 can
values) be concluded. The result is in accord with Tiryakioglu
et al.11 who for the same alloy and a similar test
Grain refiner Base grain Tip grain method made the same conclusion. Also, Kwon and
additions, size average, size average, Average ¡ sm, Lee,15,21 using a different test method, found no
wt-%Ti mm mm mm
appreciable variation in fluidity of A356 when
0 358 247 300¡30 measured above 700uC for a 0.2 wt-%Ti addition.
0.01 302 238 270¡30 The reason why the grain refinement does not affect
0.02 244 192 215¡30 fluidity is not yet well understood. For instance, some
0.04 204 160 180¡25 influence on fluidity by the grain refinement process
might be expected, since it has been shown6 that fine
Table 5 Average length of fluidity measurements particles are more effective in stopping a flowing
for three hydrogen levels and standard stream than an equivalent percentage by weight of
error in mean values for 10 spirals with
three hydrogen levels (P – after purging Table 6 Porosity (%) calculated from density mea-
with Ar, A – as received, H – after wood surements for selected spirals and stand-
addition to melt) ard error in mean values, sm(%), for three
hydrogen levels
Average
Hydrogen content, ml per 100 g length ¡ sm, mm Hydrogen, ml per 100 g Porosity, % sm, %

P 0.13 420¡20 P 0.13 1.9 0.1


A 0.15 420¡30 A 0.15 1.4 0.4
H 0.43 430¡40 H 0.43 3.7 0.2

International Journal of Cast Metals Research 2005 Vol. 18 No. 3


Di Sabatino and Arnberg Effect of grain refinement and dissolved hydrogen on fluidity of A356 alloy 185

(b)

6 Backscattered electron micrographs of a purged sample with low hydrogen content (0.13 ml per 100 g)
and b up-gassed sample with high hydrogen content (0.43 ml per 100 g)

coarse particles. In this case, fluidity might be grain size measurements (Table 4) show that the
expected to decrease with grain refinement. grain refinement affects the grain size of the spirals.
Conversely, however, it has also been shown13 that However, the decrease in grain size achieved after the
grain refinement postpones the dendrite coherency additions is not dramatic because the A356 alloy
point, which can be supposed to be related to already contains 0.059 wt-%Ti. In confirmation of
fluidity.9,22 The flow of the liquid stream can be this behaviour it has been reported24 that small
assumed to be impaired when the dendrites at the tip amounts of grain refiner at high superheat, compar-
become coherent, which means that a late coherency able with that used in the present work, produced
would be expected to give a better fluidity. Therefore, significant grain size reductions, but with further
in this case, fluidity might be expected to increase with additions only producing minimal additional benefit.
grain refinement. However, for the levels of Ti Table 4 shows that the tip of the spirals has a finer
investigated, the coherency point varies between 24 structure than the base, as might be expected because
and 25%,13 which is likely to give no significant effect of the increase in the cooling rate from the base
on fluidity. towards the tip and possibly as a result of dendrite
As suggested by Easton and St John,23 because fragmentation.
aluminium casting alloys such as A356 already Table 5 shows the average length measurements of
contain high solute levels and have a high growth the spirals for three hydrogen levels. Clearly, there is
restriction factor (GRF) [the GRF of 7 wt-%Si is no statistically significant effect of hydrogen on
equivalent to that of 0.17 wt-%Ti (Ref. 24)], the fluidity of the A356 alloy. In contrast, and, of
optimum grain refiner only needs to contain nucleant course, as is to be expected, the reduced pressure
particles, such as TiB2 in the case of AlTi5B1 grain test (Fig. 5 and Table 6) shows greatly increased
refiner (but no additional alloy to confer additional porosity after the addition of hydrogen. The PoDFA
growth restriction). The microstructure investigations samples (Table 7) have shown a similar concentration
of A356 alloy (Figs. 3 and 4) show no morphological of inclusions, 2.2 and 1.5 ppm (by volume), for the
changes associated with increased Ti additions and purged (P) samples and the increased hydrogen (H)
the alloy has remained as fine equiaxed dendrites. samples respectively. It has been shown25 that
Easton and St John23 observed the same morphology degassing with a rotating impeller can, in some
in the unrefined and refined A356 alloy. The circumstances, increase the oxide content in the melt.
microstructure analyses (Figs. 3 and 4) and the Therefore, whereas purging the molten A356 alloy

Table 7 Volume concentration of inclusions for low and high level of hydrogen, P and H, respectively
Fine dark Larger dark Larger grey
Oxide film, inclusions, ppm inclusions, ppm inclusions, ppm Total, ppm
Sample ppm (by vol.) (by vol.) (by vol.) (by vol.) (by vol.)

P 0.07 2.1 0.03 n.d* 2.2


H 0.03 1.4 0.10 0.03 1.5

*n.d ~ not detected.

International Journal of Cast Metals Research 2005 Vol. 18 No. 3


186 Di Sabatino and Arnberg Effect of grain refinement and dissolved hydrogen on fluidity of A356 alloy

with pure Ar for 45 min decreased the hydrogen Norwegian University of Science and Technology;
content, in this case it appeared to increase the and SINTEF. The authors thank the industrial
concentration of oxides. Microprobe analyses have partners and the Norwegian Research Council for
shown that the inclusions present in both samples are financial support.
dispersed oxides in various forms: c-Al2O3 as
elongated films and a-Al2O3 as thicker films. MgO
is also present as dispersed clusters in addition to the References
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International Journal of Cast Metals Research 2005 Vol. 18 No. 3

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