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Abstract
In the present study, three aluminum–silicon alloys containing 7, 10 and 19 wt % silicon were synthesized using a novel technique
commonly known as disintegrated melt deposition technique. The results following processing revealed that a yield of at least 80% can be
achieved after defacing the shrinkage cavity from the as-processed ingots. Microstructural characterization studies conducted on the
as-processed samples revealed an increase in the volume fraction of porosity with an increase in silicon content. Porosity levels of 1.07,
1.51 and 2.65% attained in the case of Al–7Si, Al–10Si, and Al–19Si alloys indicates the near-net shape forming capability of the
disintegrated melt deposition technique. The results of aging studies conducted on the aluminum–silicon alloys revealed similar aging
kinetics irrespective of different silicon content. Results of ambient temperature mechanical tests demonstrate an increase in matrix
microhardness and 0.2% yield stress and decrease in ductility with an increase in silicon content in aluminum. Furthermore, the results of
an attempt to investigate the effect of extrusion on Al–19Si alloy revealed that the extrusion process significantly assists in reducing
porosity and improving microstructural uniformity, 0.2% yield strength, ultimate tensile strength and ductility when compared to the
as-processed Al–19Si alloy. The results of microstructural characterization and mechanical properties of aluminum–silicon alloys were
finally correlated with the amount of silicon in aluminum and secondary processing technique. 1999 Elsevier Science S.A. All rights
reserved.
0925-8388 / 99 / $ – see front matter 1999 Elsevier Science S.A. All rights reserved.
PII: S0925-8388( 99 )00062-6
M. Gupta, S. Ling / Journal of Alloys and Compounds 287 (1999) 284 – 294 285
in the present study to synthesize Al–Si alloys in both as the lubricant. Extrusion was conducted in order to study
hypo- and hypereutectic composition range. This tech- the effect of secondary processing on the microstructural
nique, in the past, has been successfully utilized to and mechanical properties variation of as-processed Al–Si
synthesize monolithic and reinforced materials [11,12] and alloy.
involves, in principal, the disintegration of superheated
molten metal slurry using inert gas jets followed by its
subsequent deposition on the metallic substrate. The 2.4. Quantitative assessment of silicon
dynamic disintegration and deposition steps enables this
technique to synthesize bulk materials with improved Quantitative assessment of Si in the as-processed and
microstructural homogeneity when compared to conven- extruded Al–Si samples was carried out using standardized
tional casting techniques [11,12]. energy dispersive spectroscopy (EDS) method.
Accordingly, the objective of the present study was to
investigate the microstructure and mechanical properties of
2.5. Density measurement
the disintegrated melt deposited Al–Si alloys (both in
hypo- and hypereutectic composition range) in order to
The densities of the as-processed and extruded Al–Si
assess the feasibility of the disintegrated melt deposition
samples were measured by Archimedes’ principle to
technique to synthesize the Al–Si family of alloys. Par-
quantify the volume fraction of porosity [6,11,12]. The
ticular emphasis was placed, in addition, to study the effect
density measurements involved weighing polished cubes of
of secondary processing on the microstructure and me-
the extruded samples in air and when immersed in distilled
chanical properties of the hypereutectic (Al–19Si) alloy
water. The densities, derived from the recorded weights,
synthesized in the present study.
were then compared to the theoretical densities from which
the volume fractions of porosity were calculated. The
samples were weighed using an A&D ER-182A electronic
2. Experimental procedure
balance to an accuracy of 60.0001 g.
2.1. Materials
2.6. Aging studies
In this study, an aluminum alloy AA1050 ($99.5 wt %
Al) was used as the base alloy and silicon ($98.5 wt % Si) Aging studies were carried out in order to obtain the
was used as an addition element to synthesize hypo- and peak hardness time for the as-processed and extruded
hypereutectic Al–Si alloys. Al–Si samples. Specimens (10 mm diameter37 mm
height) were solutionized for 1 h at 5298C, quenched in
2.2. Processing cold water and aged at 1608C for various intervals of time.
Rockwell superficial hardness measurements were made
In the present study, synthesis of hypo- and hypereutec- using a 1.58 mm diameter steel ball indenter with a 15 kg
tic Al–Si alloys with starting weight percentages of 7, 10 load using a GNEHM HORGEN digital hardness tester
and 20 wt % of Si was carried out using the DMD following ASTM standard E18-92. A minimum of three
technique. The synthesizing procedure involved: super- hardness readings were taken for each specimen.
heating of properly cleaned elemental materials to a
temperature of 9506108C in graphite crucible, impeller
assisted stirring to ensure complete mixing of elemental 2.7. Microstructural characterization
materials followed by argon gas-assisted melt disinte-
gration at 0.18 m from the melt pouring point and Microstructural characterization studies were conducted
subsequent deposition in a metallic mould (55 mm on the as-processed and extruded Al–Si samples in the
diameter375 mm long) located at 0.25 m from the gas peak aged condition to investigate the grain morphology,
disintegration point. The experiment was carried out under presence of porosity, morphological characteristics and
controlled atmospheric conditions. The Al–Si alloy ingots distribution of the secondary phases, and Si–Al interfacial
obtained following processing were weighed in order to characteristics.
determine the deposited yield of the starting raw materials. Microstructural characterization studies were primarily
accomplished using an optical microscope and a JEOL
2.3. Secondary processing scanning electron microscope equipped with EDS. The
samples were metallographically polished prior to exami-
Al–Si alloy ingot with starting weight percentage of nation. Microstructural characterization of the samples was
20% silicon was machined to a diameter of 35 mm and conducted in both etched and unetched conditions. Etching
then hot extruded at 3508C employing a reduction ratio of was accomplished using Keller’s reagent [0.5 HF–1.5
13:1 on a 150 ton hydraulic press using colloidal graphite HCl–2.5 HNO 3 –95.5 H 2 0].
286 M. Gupta, S. Ling / Journal of Alloys and Compounds 287 (1999) 284 – 294
Vickers microhardness of the matrix of as-processed and Alloy Processing Wt % Si Density Porosity
extruded Al–Si samples was determined on a Matsuzawa designation condition (g cm 23 ) (vol %)
MXT50 Automatic Digital microhardness tester using an Al–7Si As-processed 7 2.6460.01 1.07
indentation load of 100 g. Vickers microhardness measure- Al–10Si As-processed 10 2.6260.02 1.51
Al–19Si As-processed 19 2.5560.01 2.65
ments were made in order to provide insight into the
Al–19Si(Ext) Extruded 19 2.6060.06 0.65
ability of secondary phases to strengthen the metallic
matrix.
Smooth bar tensile properties were determined on the 3.3. Quantitative assessment of silicon
as-processed and extruded samples in the peak aged
condition following ASTM standard E8M-91. Tensile tests The results of standardized EDS chemical analysis
were conducted using an automated servohydraulic Instron conducted for Si element determination in the as-processed
8501 testing machine on 4 mm diameter specimens using a Al–Si alloys with starting silicon weight percentages of 7,
crosshead speed of 0.254 mm per minute. 10 and 20 and extruded Al–Si alloy (with starting silicon
weight percentages of 20) revealed that approximately 7,
2.9. Fracture behavior 10, 19 and 19 wt % Si was retained, respectively, follow-
ing DMD processing (see Table 1). Accordingly, these
Fracture surface characterization studies were carried materials will now be referred as Al–7Si, Al–10Si, Al–
out on the tensile fractured samples in order to provide 19Si, and Al–19Si(Ext) in the forthcoming sections.
insight into the various fracture mechanisms operative
during tensile loading of the peak aged samples. Fracture 3.4. Density measurement
surface characterization studies were primarily accom-
plished using a JEOL scanning electron microscope The results of density measurements conducted on the
equipped with EDS. Al–7Si, Al–10Si, Al–19Si, and Al–19Si(Ext) samples and
the volume percent of the porosity computed using the
experimentally determined density values are shown in
Table 1.
3. Results
3.5. Aging studies
3.1. Processing
The results of aging studies conducted on the as-pro-
The deposited yield of the Al–Si alloys with starting cessed and extruded samples are shown in Fig. 1. The
weight percentages of 7, 10, and 20 wt % of silicon was results exhibit the presence of a hardness peak at 9 h for all
found out to be 89, 88 and 86%, respectively. The the samples. Both the as-solutionized and peak hardness
preforms in all the three cases were associated with a small values were found to increase with an increase in the
shrinkage cavity on the top. After defacing the ingots so as silicon content in aluminum and from the as-processed to
to remove the shrinkage cavity, the final yield was extruded condition in the case of hypereutectic Al–19Si
determined to be 85, 84 and 80%, respectively. The overall alloy. The results also reveal an increase in the magnitude
dimensions of the disintegrated melt deposited preforms of age hardening with an increase in the weight percentage
following defacing were approximately 35 mm in height of silicon in the case of as-processed samples. The
and 55 mm in diameter. The preform of the Al–Si alloy
with starting weight percentage of 20 wt % Si was
subsequently machined to a diameter of 35 mm so as to fit
in the extrusion container. The specimens for heat treat-
ment, microstructural analysis and mechanical properties
characterization were removed randomly from the as-pro-
cessed and extruded rods.
3.2. Macrostructure
Table 2
Results of the aging studies
Alloy As-solutionized Peak hardness Peak aging Magnitude of age
hardness (HR15T) (HR15T) time (h) hardening (HR15T)
Al–7Si 41.261.2 44.860.9 9 3.6
Al–10Si 43.761.5 52.461.4 9 8.7
Al–19Si 44.861.3 58.261.8 9 13.4
Al–19Si(Ext) 56.660.3 59.860.8 9 3.2
288 M. Gupta, S. Ling / Journal of Alloys and Compounds 287 (1999) 284 – 294
Fig. 4. Optical micrograph showing the presence of primary silicon and Fig. 5. Optical micrograph showing the salient microstructural features
eutectic silicon in the case of DMD processed Al–19Si samples. exhibited by DMD processed Al–19Si(Ext) samples.
Table 3
Results of microstructural characterization
Material Microstructural feature Vf a Parameter Roundness
Eq. size (mm) l (mm)b
Al–7Si Eutectic silicon 0.065 2.6 10.2 N.D
Al–10Si Eutectic silicon 0.162 2.7 6.7 N.D
Al–19Si Primary silicon 0.093 77.5 254.0 7.34
Eutectic silicon 0.074 7.5 27.5 3.21
Al–19Si(Ext) Primary silicon 0.131 65.5 181.0 5.13
Eutectic silicon 0.125 3.7 10.5 2.64
a
Computed using image analysis.
b
Computed using the formula suggested by Nardone and Prewo [22]: l 5(lt /Vf )1 / 2 where l is the interparticle spacing and t, l and Vf are the thickness,
length and volume fraction of the secondary phases, respectively.
M. Gupta, S. Ling / Journal of Alloys and Compounds 287 (1999) 284 – 294 289
Fig. 7. SEM fractograph showing the fracture surface features in the case
of Al–7Si samples.
4. Discussion
4.1. Processing
of finer distribution of these phases at the extrusion elsewhere [27]. It may further be noted that the increased
temperature leading to their increased presence at magnifi- precipitation of the secondary phases and hence the
cations up to 20003. It may be noted that the coalescence increase in magnitude of age hardening may be attributed
of finer phases assists in reducing the particle / matrix to the ability of the defect structure to serve as a heteroge-
interfacial area and the relaxation of misfit strains in the neous nucleation site during aging treatment. In related
matrix [23]. Further work is continuing to establish the studies, for example, investigators have shown using
variation in distribution pattern of these phases (especially transmission electron microscopy the precipitation of
in the finer size range) as a function of extrusion step using strengthening phases on the lattice defects such as disloca-
high magnification metallography techniques. tions [28]. The progressive increase in the peak hardness
Another interesting feature observed in the case of when compared to as-solutionized hardness with an in-
hypereutectic Al–19Si samples was the presence of silicon crease in weight percentage of silicon also indicates that
segregation in the immediate vicinity of primary Si much superior mechanical properties can be realized
particles (see Fig. 6). This can be attributed to the localized following aging heat treatment. This is also consistent with
presence of point defects and line defects in the interfacial the work reported elsewhere [16] which suggest a clear
region of primary Si particles during solid state quenching correlation between hardness and strength. The results are
as a result of a difference in the coefficient of thermal also consistent with the similar findings made on an
expansion between the aluminum matrix and Si particles Al–7Si based alloy supplied by Duralcan, USA [6].
(CTE (Al) / CTE (Si) : 3.1 [24]). The presence of an Regarding the influence of silicon content on the aging
increased number of defects assists in promoting the kinetic, the results of the aging studies suggest that the
diffusion of alloying elements from the adjacent region variation in silicon content in the range of 7–19 wt % was
leading to the segregation in the interfacial region. These not sufficient to bring the microstructural changes capable
results are also consistent with the similar studies con- of altering the aging kinetics of the aluminum matrix. This
ducted on the conventionally cast A390 alloy [4]. is consistent with the work of other investigators who
suggested that the aging kinetics of the metallic matrix
4.3. Aging studies containing the secondary phases with different CTE can
only be influenced if the variation in microstructure as a
The results of aging studies conducted on as-processed result of their presence is significant [29].
Al–Si alloys revealed three salient features: Regarding the effect of extrusion, the results show that
the hot extrusion step used in the present study increases
• an increase in as-solutionized and peak hardness with the as-solutionized hardness significantly while maintain-
an increase in the weight percent of silicon, ing the peak hardness similar to that observed in the case
• an increase in the magnitude of age hardening with an of as-processed Al–19Si samples (see Fig. 1). The increase
increase in the weight percent of silicon, and in as-solutionized hardness of the extruded samples may be
• an aging kinetics independent of weight percent of attributed to the reduction in the volume fraction of
silicon porosity as a result of the extrusion (see Table 1) and a
minimal amount of age hardening suggests that the hot
The increase in the as-solutionized and peak hardness of extrusion step assists in establishing a uniform distribution
Al–Si alloys with an increase in the weight percent of pattern of silicon based phases as a result of high tempera-
silicon can be attributed to an increase in the volume ture exposure (3508C) during extrusion and subsequent
fraction of harder silicon based phases in the aluminum cooling to room temperature resulting into partial dissolu-
matrix (see Table 3). The silicon based phases refer to tion and reprecipitation of silicon based phases in the
eutectic silicon in the case of hypoeutectic Al–Si alloys matrix. As a result of this, the effect of age hardening are
and primary and eutectic silicon in the case of hypereutec- minimized as reflected in only a 5.65% increase in
tic Al–Si alloys. It may be noted that the hardness of hardness of the Al–19Si(Ext) samples when compared to
silicon (10 9 kg m 22 ) [25] is significantly higher when 29.9% in the case of the as-processed Al–19Si samples in
compared to that of aluminum (19310 6 kg m 22 for 99.6% the peak aged condition.
Al) [26].
The increase in the magnitude of age hardening with 4.4. Mechanical behavior
silicon content may be attributed to the capability of
increasing volume fraction of silicon based phases to The results of the mechanical properties characterization
generate increasing volume fraction of the defect structure revealed an increase in the matrix microhardness with an
in the matrix (see Table 3). The formation of defect increase in the weight percentage of silicon in the as-
structure can be attributed to a significant difference in processed Al–Si alloys (see Table 4). This is consistent
coefficients of thermal expansion of aluminum and silicon with the increase in the cumulative volume fraction of the
phases (CTE (Al) / CTE (Si) : 3.1 [24]). Such a correlation harder silicon based phases (see Table 3). It may be noted
has been convincingly established by the researchers that an increase in the volume fraction of the harder silicon
292 M. Gupta, S. Ling / Journal of Alloys and Compounds 287 (1999) 284 – 294
based phases and the associated defect structure will lead [16,34]. Bocchini [16] and Payne et al. [34], for example,
to higher constraint in the localized deformation of softer asserted that the presence of pores lead to weakening of a
matrix under the application of indentational load. In the material by reducing the amount of stress bearing area and
case of Al–19Si(Ext) samples, however, a significant therefore lowers the amount of stress the material is able to
increase in microhardness when compared to the Al–19Si withstand. Similarly, the presence of plastically incompat-
samples can be attributed to the significant microstructural ible phases lead to the stress accumulation at the interface
refinement and enhanced microstructural uniformity com- with the ductile matrix and under conventional tensile
monly achieved following extrusion process [30]. loading microcracks / microvoids may appear either at the
The results of tensile properties characterization re- pole or equator locations depending on the mechanical
vealed an increase in 0.2% YS and a decrease in ductility properties of the strengthening phase [35], thus preventing
with an increase in silicon content. An increase in 0.2% the optimum realization of UTS by the material.
YS with an increase in the amount of silicon can be The results of the tensile properties characterization
attributed to the relatively higher constraint exerted by an conducted on Al–19Si(Ext) samples revealing an increase
increasing volume fraction of the silicon based phases in in ultimate tensile strength and ductility when compared to
the aluminum matrix for the onset of the slip process. It the as-processed Al–19Si samples are consistent with the
may be noted that an increase in the dislocation pinning dependence of these properties on the morphology of
sites (such as silicon based phases and the associated plastically incompatible phases and the volume fraction of
defect structure) delays the onset of plastic deformation porosity. Since the constitution of Al–19Si and Al–
which is reflected in the values of the 0.2% YS obtained in 19Si(Ext) samples is the same, the volume fraction of
this study for Al–Si alloys [31]. In a related work [26], for silicon based phases will also be the same since the
example, it has been shown that general yield stress (so ) identical near-equilibrium primary processing technique is
can be expressed as: used to synthesize them [17]. The only difference may be
in the shift in the distribution pattern of the silicon based
so 5 ss 1 si (1)
phases towards the coarser side due to the hot extrusion
where ss is the stress to operate the dislocation sources and step used in the case of Al–19Si(Ext) samples. This is
si is the friction stress representing the combined effect of consistent with the results of the microstructural characteri-
all the obstacles to the motion of dislocations arising from zation studies (Table 3) which show an increase in the
the sources. In the present study, based on microstructural volume fraction of micron-size silicon based phases and
characterization results (see Table 3), it is evident that an more interestingly show the lower roundness (indicating
increase in the amount of silicon leads to an increase in the increasing equiaxed nature) values. The decrease in the
si as a result of an increase in the volume fraction of roundness value of the silicon based phases will be
silicon based phases. This is also consistent with the instrumental in increasing the resistance of the aluminum
similar 0.2% YS values obtained in the case of Al–19Si matrix to microcracking as a result of the decrease in the
and Al–19Si(Ext) samples (see Table 4). The same stress concentration at the sharp edges, thus leading to
amount of silicon in these two different category of superior values of UTS and ductility. Similarly, a reduction
samples is indicative of the similar volume fraction of in porosity from 2.65 to 0.65% (see Table 1) may also be
silicon based phases [17] and hence the similar values of attributed to an increase in UTS and ductility values of
0.2% YS (within each other’s standard deviation) arising Al–19Si(Ext) samples when compared to Al–19Si sam-
from similar si . ples. This is consistent with the work of other investigators
The decrease in ductility with the increasing amount of [25] who reported an increase in the value of UTS by
silicon may be attributed to the increasing volume fraction about 51 MPa as a result of reduction in porosity by about
of plastically incompatible silicon based phases in the soft 2% in the case of Al–5Si samples heat treated to T6
and ductile aluminum matrix. It has been, for example, condition. It may be noted that in the present study an
established that the increasing volume fraction of plastical- increase in UTS by about 51 MPa was realized as a result
ly incompatible phases decreases the cavitation resistance of a reduction in porosity by about 2% in the case of T6
of the matrix leading to early microcracking and hence the heat treated Al–19Si samples. The tensile testing results
reduced ductility under the application of tensile loads thus obtained are consistent with the microstructural
[31–33]. characterization results obtained in the present study and
The inferior ultimate tensile strength exhibited by Al– the work of other investigators [25].
19Si samples when compared to Al–7Si and Al–10Si
samples may be primarily attributed to the coupled effects 4.5. Fracture behavior
of the presence of primary Si and an increase in the
porosity and volume fraction of plastically incompatible The results of fractographic studies conducted on the
silicon based phases. The porosity associated reduction in hypoeutectic Al–7Si and Al–10Si samples revealed similar
strength has been previously established by other inves- fracture surface features exhibiting ample evidence of
tigators for steels, copper and aluminum based alloys matrix plastic deformation (see Figs. 7 and 8). The fracture
M. Gupta, S. Ling / Journal of Alloys and Compounds 287 (1999) 284 – 294 293
surfaces, in common, also showed the presence of rela- cant increase in the degree of brittleness in the hy-
tively flat and featureless zones which may be indicative of pereutectic samples when compared to the hypoeutectic
crack propagation along the embrittled boundaries of a-Al samples. The results also revealed that the fracture
dendrites / grains. This may be attributed to the presence of mode can be changed from predominantly brittle to
the hard and brittle eutectic silicon phase as shown in Figs. predominantly ductile following extrusion.
2 and 3. The fracture surface of Al–19Si samples was
significantly different when compared to Al–7Si and Al–
10Si samples and exhibited a high degree of brittleness and
Acknowledgements
cracked primary silicon particles (see Fig. 9). This may be
attributed to the reduced ability of metallic matrix to
The authors would like to thank Mr. Tham Leung Mun
deform due to the increased number of crack nucleation
and Mr. Tung Siew Kong (National University of Singa-
sites such as increased volume fraction of hard and brittle
pore, Singapore) for their valuable experimental assistance
silicon based phases and porosity. On the contrary, the
and for many useful discussions and to Ms Neerja Gupta
fracture surface of Al–19Si(Ext) samples revealed evi-
for improving the readability of this manuscript.
dence of significant matrix plastic deformation (see Fig.
10) and the presence of cracked and / or partially debonded
primary silicon particles. The plastic deformation ability
exhibited by Al–19Si(Ext) samples may be attributed to References
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