Applied Mathematical Modelling 28 (2004) 95107

www.elsevier.com/locate/apm

Macrosegregation development during solidication of a

multicomponent alloy with free-oating solid particles
Matthew John M. Krane
School of Materials Engineering, Purdue University, 1289 Materials, Electrical Eng. Bldg.,
West Lafayette, IN 47907-1289, USA
Received 1 December 2002; received in revised form 11 February 2003; accepted 8 May 2003

Abstract
The macrosegregation patterns and convective behavior of a Pb5wt%Sb35wt%Sn alloy are studied
using numerical treatments of solid particle motion and of transport phenomena occurring during the
solidication of ternary metal systems. At this composition, the solidication in the (Pb)(SbSn) binary
eutectic trough has a signicant eect on these phenomena. The eects of this solidication path on uid
ow and macrosegregation are compared to the more familiar binary alloy patterns and the eect of solid
particle transport is evaluated. The nal predictions of macrosegregation are compared to measured
composition proles.

2003 Published by Elsevier Inc.

1. Introduction
The macroscopic redistribution of alloy constituents during solidication, commonly called
macrosegregation, is a defect which occurs in real metal processing systems. This nonuniformity
of species distribution, especially when it forms a high composition gradient or a poor distribution
of secondary phases, can lead to a nonuniform distribution of mechanical properties and contribute to cracking during extrusion or forging of wrought alloys or when an as-cast piece is
severely loaded in service [1,2]. Macrosegregation studies in binary systems have become quite
common since the introduction of single-domain numerical models which feature one set of
conservation equations and boundary conditions for an entire, xed computational domain
containing solid, liquid and multiphase regions. A complete review up to 1995 has been presented

E-mail address: krane@ecn.purdue.edu (M.J.M. Krane).

0307-904X/$ - see front matter
2003 Published by Elsevier Inc.
doi:10.1016/S0307-904X(03)00121-5

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M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

by Prescott and Incropera [3]. However, most commercial alloys generally have more than two
species in amounts signicant enough to aect the convective ows which lead to macrosegregation and other defects. The formation of secondary solid phases, including eutectic and peritectic reactions, also may occur in commercial metal alloys and should be treated using
appropriate thermodynamic models.
Early studies of macrosegregation during the solidication of multicomponent alloys include
work on aluminum alloys and steel [4,5]. These studies developed models which had severe limitations on the uid ow, but were able to obtain reasonable comparison to experiments in simple
casting congurations. Schneider and Beckermann [6] published a study of macrosegregation in
multicomponent alloys, calculating ow patterns, temperature elds and solute redistribution in
multicomponent steels. They expanded a continuum formulation of the transport equations to
include several alloying elements and studied steels in which those elements combined to provide
up to 1.8 wt% of the composition. These low concentrations of alloying constituents permitted the
use of a thermodynamic model similar to that of Fujii et al. [5], which assumed only primary
ferrite formation. While some small local dierences were present, overall macrosegregation
patterns of the various solutes were found to be similar, as were some composition proles across
the solidied ingots. Because all of the alloying components were rejected into the liquid as the Ferich solid formed, they were redistributed in patterns similar to binary solidication. A simplied
version of this model has been compared favorably to composition measurements in a complex
steel casting [7]. Other continuum models of the heat, mass and momentum transport in solidifying higher-order systems include work on multicomponent Ni-based superalloys by Schneider
et al. [8] and Fellicelli et al. [9].
Krane et al. [10] extended a continuum mixture model for binary alloys to three component
systems and derived supplemental thermodynamic relations needed to close the transport model.
Specically, those relations treat the several primary solid phases, binary eutectic troughs, and
ternary eutectic and peritectic reactions. In a companion work [11], this new model was applied to
the solidication of lead-rich PbSbSn alloys to compare and contrast the behavior of binary
and ternary alloys. Macrosegregation was altered signicantly from the familiar patterns of the
binary systems [3] only when solidication in the doubly saturated binary troughs occurred near
the liquidus surface. If the secondary solidication occurred deep in the mushy zone, the resulting
microsegregation had only small eects on the nal redistribution of solute. Numerical results
using this model with a PbSbSn alloy were compared to experimental results, nding reasonable
agreement in the temperature histories and somewhat less in the composition proles [12]. Limitations of the model illustrated by this comparison were discussed, especially the uncertainty in
the permeability of the mushy zone.
As pointed out in a review of recent literature on modeling solid-phase transport in solidifying
systems [13], the fragmentation and movement of solid particles may aect signicantly an ingots
nal macrosegregation and grain structure. Wang and Beckermann [14] have developed a detailed
multiphase model to account for the presence of free-oating equiaxed dendrites and their eect
on composition and grain structure, linking the model to the macroscopic equations governing
thermosolutal convection and heat and mass transfer. Calculations have been made, some of
which were compared to experiments in saltwater solutions [15,16]. Vreeman et al. [17] accounted
for solid transport with a model based on a continuum mixture approach, using much less sophisticated relations to obtain relative solidliquid velocities. The model was applied to DC cast

M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

97

aluminum alloys [18] and model results have been compared to experiments in industrial scale
billets [19].
The purpose of this paper is to combine the ternary solidication model in [10,11] with the solid
particles transport model of [17] and to investigate the eect of parameters in the solid motion
model on macrosegregation. The results of this parametric study will also be compared to experimental composition data taken from a ternary alloy (Pb5%Sb35%Sn) cast in controlled
conditions [12].

2. Numerical model
The two-dimensional conservation equations used to model mixture mass, momentum, heat
and species transport during the solidication of a ternary alloy are shown below [10]. These
transport equations are discretized using an implicit, control volume formulation and solved using
the SIMPLER algorithm [20] and a line-by-line TDMA. Computational details not discussed here
and thermophysical property data for the PbSbSn system are provided in [1012,21].
oq
r
qV 0
ot

oqu
l u oP
r
qVu r
lL ru  L 
ot
Kx
ox

X
oqv
l v oP
i
gq bi C i  CL;o
gqL bT T  To
r
qVv r
lL rv  L 

ot
Ky
oy iSb;Sn L S L

oqh
k
k
r
qVh r
rh r
rhS  h  r
fS qV  VS hL  hS
ot
cS
cS

oqC i
r
qVC i r
qfL DiL rC i r
qfL DiL rCLi  C i  r
fS qV  VS CLi  CSi
ot
5
These equations constitute a fully coupled, continuum mixture model, which eliminates the need
to explicitly track solidication fronts or to use articial matching conditions at these fronts by
modeling the entire domain with one set of equations. Classical mixture theory was used to derive
these advectiondiusion equations in terms of phase properties and phase mass fractions,
thereby eliminating the need for detailed descriptions of phase interactions [22,23]. The mixture
velocity (V), enthalpy (h), and compositions (C i ) are found from an average of the velocities,
enthalpies, and compositions of the solid and liquid phases, weighted by the phase fractions. The
solid and liquid enthalpies are found assuming that the temperatures of all phases in a given
control volume are the same. Ni and Beckermann [24] showed that this is a good assumption for
the case in which the solid is columnar and rigid, but pointed out that, when the solid is in
the form of free-oating, equiaxed particles, it is expected that some undercooling exists in the
liquid to drive the heat transfer from the solidliquid interface. The assumption here is that the

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M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

undercooling is small compared to the temperature dierence between control volumes. The velocities and compositions of the dierent phases are not treated as the same and are dealt with next.
In Eqs. (1)(5), the solid is assumed to be rigid and stationary (us vs 0) and the solidliquid
interaction is modeled using the BlakeKozeny model with isotropic permeability. Modications
were made to the momentum equations to account for movement of solid particles due to thermosolutal convection and settling [17]. This change in the model resulted in several new terms in
the momentum equations, representing the eect of the solid on the viscous stress and buoyancy,
and the removal of the DArcy drag term for (rigid) solidliquid interaction. The momentum
equation in the vertical direction is
o
qfs
oP
rv  gs qs  qL g 
qv r
qVv r
lL rv  r
lL
ot
oy
qL
i
h
Sb
Sn
Sn
Sb
Sb
gL qL g bSn
f

b
f

f

b
T

T

r
lL us rgs

f
o
T;L
o
o
S;L L
S;L L
i
h
Sb
Sn
Sn
Sb
Sb
gs qs g bSn
S;s fs  fo bS;s fs  fo bT;s T  To r
ls gs rus :
6
The horizontal momentum equation is similar, but lacks the gravity-dependent terms. The solid
velocity of the free-oating dendrites is related to the liquid velocity by
VS  VL

1  gs
qs  qL d 2 g;
18l

where d is a characteristic diameter of the free-oating particles. Lumped into this single, unchanging parameter is the real particle size distribution which varies in time and position during
solidication. Detailed drag models which account for particleliquid interaction in a more sophisticated manner are found in [14,25].
The use of the two sets of momentum equations is accomplished by assuming that the mushy
zone consists of a slurry of free-oating equiaxed dendrites if the solid volume fraction is less than
a designated packing fraction (gs < gs;P ), and of a rigid array of packed solid and interdendritic
liquid if gs > gs;P . This packing fraction is the point at which the dendrite slurry coalesces into a
rigid, stationary structure. Implementation requires that the momentum equations for a slurry of
free-oating dendrites be applied in both the liquid and slurry regions (0 6 gs < gs;P ), while the
momentum equations (2) and (3) are applied to the rigid mushy zone and the solid region
(1 P gs > gs;P ). In general, the packing fraction at which the solid phase forms a rigid structure is
not explicitly known and varies from system to system. Furthermore, the packing fraction is
related to the size distribution of the moving dendrites, the interface morphology, and even the
slope of the rigidslurry interface and thus varies within a particular system depending on local
morphological, thermodynamic, and uid ow conditions.
The transport equations above are not a closed system, as they require knowledge of the local
temperature, phase fractions, and phase compositions. To obtain these quantities, the lead-rich
corner of the linearized PbSbSn equilibrium phase diagram shown in Fig. 1 is employed, using a
method described in [10,11]. In addition to primary solidication, this model accounts for the
possibility of secondary and tertiary crystallization in binary eutectic troughs and at ternary
eutectic and peritectic points. Although diusion in the solid is very slow, for convenience

M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

99

Fig. 1. Linearized phase diagram for PbSbSn system.

compositional equilibrium was assumed on the scale of a dendrite and is not expected to aect
signicantly the macroscopic heat and mass transfer [26,27].
The lead-rich corner of Fig. 1 is bordered by the PbSb and PbSn binary phase diagrams, both
of which are simple eutectic systems. The PbSb system has a eutectic point (ePbSb ) at 251 C and
11.2 wt% Sb. The maximum solid solubility of antimony in the Pb-rich solid is 3.5 wt% Sb. The
Sn
0:619), while the maximum soluPbSn system also contains a eutectic (TEUT 183 C, fEUT
bility of Sn in the solid is 19.2 wt%. The two diagrams intersect at pure Pb, which has a melting
point at 327 C. The ternary PbSbSn diagram is divided into two sections by the psuedobinary
PbSbSn system. The Pb-SbSn system has a eutectic point (ePbSbSn ) at 10 wt%Sb10wt%Sn and
245 C. The partial system PbSbSbSn has a ternary eutectic point (E) at 12 wt%Sb4 wt%Sn
and 240 C. This invariant point is found at the intersections of the binary troughs which represent the ab, ad and bd eutectic separations, where d is the Sb-rich and b the SbSn-rich
primary solid phase. The partial system PbSnSbSn, also has an invariant point, a ternary
peritectic (P ) at 190 C and 2.5 wt%Sb57.5 wt%Sn. Two monovariant curves, the ab and the
bc binary troughs (where c is the primary Sn-rich solid), intersect at P , and the binary valley for
the ac runs down from P to ePbSn at 183 C. All calculations in this study are in the primary Pb
region of the phase diagram.
In order to close the continuum mixture model [10] for the solidication of lead-rich PbSbSn
alloys, certain information must be extracted from the phase diagram and related data presented
by Osamura [28]. Specically, the supplemental thermodynamic relations in [10] require the location of the invariant points (described above), the paths of the binary troughs, the values of the
equilibrium partition coecients and the location of the liquidus surface, all of which are given in
[11]. The values of the partition coecients for the primary solidication are equated to those for
the two binary systems which bound the Pb-rich corner. The liquid compositions at which the b, c
and d solid phases form are all in the binary troughs, which correspond to solid b, c and d
compositions estimated from several isothermal sections of the ternary diagram in [28]. The liquidus surface in the primary a crystallization region is also simplied for ease of calculation. The
surface is divided into four triangular planes (indicated by the dashed lines in Fig. 1), using the
invariant points as vertices. The temperatures on the sides of the triangles are linear interpolations
between the end points. Connecting these points across the faces of these triangles gives the
temperatures on the linearized liquidus surface.
The calculations presented here are designed to be compared to available experimental data
[12], so it is desirable to match the boundary and initial conditions of the calculations to those of

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M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

the experiments as closely as possible. The computational domain for simulating the ingot is 62
mm 57 mm, and has 75 65 control volumes. The domain is truncated at the top of the experimental ingot and at the midplane of the mold, with the latter treated as a plane of symmetry.
The top of the domain is modeled as a free surface, with no shear (ou=oy 0) and no velocity
perpendicular to the surface (v 0). The stainless steel mold found in the experimental work [12]
is included in the calculations (on the bottom and the left of the ingot), and it is assumed that the
mold and the ingot maintain perfect contact. While the bottom of the mold is assumed to be
insulated, the vertical mold wall (on the left in the composition plots below) is chilled by the
water-cooled heat exchangers. To simulate this cooling, the vertical wall temperatures measured
during the experiments were used as the boundary condition for the computations.
The two parameters in the solid transport model which are unknown are the characteristic
diameter of the solid particle, d, and the packing fraction, gs;P . Values for d are chosen to be
smaller than the average primary dendrite arm spacing (130 lm) found in the experimental ingot
[12]. This eective diameter is varied from 5 to 100 lm. A parametric study of the eect of the
packing fraction is also performed. The eect of the value of gs;P on velocity and temperature
elds and solidication fronts was investigated by Ilegbusi and Mat [29]. They studied packing
fractions between 0.2 and 0.625, as suggested by experimental work by Arnberg et al. [30]. Based
on observations made during the freezing of saltwater solutions [31], the model in [17] was developed assuming relatively low packing fraction (gs;P < 0:3). In keeping with those observations,
the present study uses packing fractions between 0 and 0.3, with one additional case using the
commonly used value of 0.6 (although the model is not strictly applicable at high gs;P ). In these
parametric studies, the eect of d and gs;P on the development of the macrosegregation patterns is
of primary interest. The calculated composition elds are compared to each other and proles
across the simulated ingots are compared to available experimental data.

3. Numerical results and comparison to experiments

The solidication of the Pb5wt%Sb35wt%Sn alloy begins with primary a (Pb) crystallization,
but soon its liquid compositions falls into the binary trough [EP ], which is the twofold saturation
curve for and the SbSn-rich b solid phase, and ends its solidication at the peritectic point, P .
Because the solidication path for this initial composition intersects the binary trough at
gs  0:13, one should expect microsegregation due to solidication in the trough to aect ow
development and solute redistribution. It is important to note that for this alloy the tin content of
the liquid along the entire solidication path increases monotonically, while the liquid concentration of antimony only increases during primary freezing. After the liquid composition has
reached the binary trough, the antimony concentration in the liquid falls to half of its initial value.
The slope of this binary trough results in opposite Sn and Sb segregation, similar to the Al and
NiAl3 partition described in Mehrabian and Flemings [4]. The solidication ends with the peritectic reaction, which has no eect on the macrosegregation, as it occurs deep enough in the
mushy zone that liquid velocities are negligible.
A set of calculations was performed uses a packing fraction of 0.2 and varies the characteristic
particle diameter from 5 to 100 lm. The result of these calculations is that no discernible dierence
is seen in the solidication behavior, the uid ow, or the macrosegregation. The slurry of par-

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101

ticles tends to rise and remelt, carried by the relatively powerful buoyancy-induced liquid ow
driven by the large dierences in Sn composition. This result may be surprising, given the d 2
dependence of the relative solidliquid velocity found in Eq. (7). The lack of noticeable change
with variations in d is because, for this range of d and for these solidication conditions, the
dierence in phase velocities (at the maximum particle size) is on the order of 104 m/s, while
the mixture velocities near the packing interface are at least one order of magnitude larger. As the
particle diameter decreases, this discrepancy becomes more pronounced. It should be noted that
this result is not a general one, as it depends on the range of reasonable particle sizes for a
particular system and on the many casting parameters which aect uid ow in the melt (e.g.,
solidication rate, superheat, and ingot size). For the rest of this study, d 100 lm is used.
The other unknown parameter in the slurry model is the packing fraction. Four values of gs;P
are used: 0, 0.1, 0.3, and 0.6. The rst case is gs;P 0, which has no solid motion. At the early time
in the freezing shown in Fig. 2 (t 300 s), before the liquid composition reaches the binary
trough, the macrosegregation patterns are similar to those found in binary systems, which is to be
expected, as only primary solidication has occurred by this time. Both antimony and tin are
rejected into the interdendritic liquid, making that uid lighter and causing it to rise and eventually to be expelled into the melt along the top of the ingot. At this time, channels (A-segregates)
have begun to form in the mushy zone as a result of small instabilities near the liquidus interface
causing local solid dissolution. This dissolved area becomes a preferred ow path, melting more
of the solid and carving out a channel through which interdendritic liquid can leave the
mushy zone. The eect of the decreasing Sb composition in the liquid along the binary trough
begins to be apparent in Fig. 3, which corresponds to t 700 s. While the Sn redistribution
continues as before, with positive segregation along the top of the ingot and a negative cone in the
bottom corner near the cooled wall, the Sb plot reveals some dierences. As the local liquid

Fig. 2. Macrosegregation plots for gs;P 0:0 at t 300 s: (a) Sn and (b) Sb. Dashed lines clockwise streamlines, solid
lines constant volume fraction.

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M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

Fig. 3. Macrosegregation plots for gs;P 0:0 at t 700 s: (a) Sn and (b) Sb. Dashed lines clockwise streamlines, solid
lines constant volume fraction.

concentrations of antimony in regions of secondary solidication begin to decrease. Along the top
of the cavity a region of Sb-depleted liquid has begun to form. Fig. 3 shows a clockwise circulation
pattern which is wholly dominated by solutally driven ow. Although the depletion of heat and
antimony from the liquid causes a downward buoyancy force, the large tin enrichment of the same
liquid is more than enough to create a net force which is strongly positive.
The nal Sn and Sb plots for this case are seen in Fig. 4. Although the Sn macrosegregation in
Fig. 4(a) shows the same pattern seen in binary systems, the redistribution of Sb in Fig. 4(b)
clearly shows the eect of the ternary solidication path. The initial primary solidication occurs
over a long enough time to create in the lower left corner a small cone, negatively segregated in Sb,
and to begin channel (A-segregate) formation. As freezing continues the mush begins to reject Sbpoor liquid, which, buoyed by the large increase in Sn content, remains near the top of the cavity
to form a negative segregate along the top and right walls of the ingot.
The next case introduces the slurry region between the melt and the rigid mushy zone by setting
gs;P 0:1. Examining Figs. 2 and 3, it is clear that the solutally driven ow cell dominating the
uid motion penetrates the rigid mushy zone up to at least gs 0:1. The ow pattern is similar
when the packing fraction is gs;P 0:1 (Fig. 5), although the velocity is lower in the rigid mushy
zone than in the slurry. The similarity in ow elds results in a similar nal macrosegregation
pattern (Fig. 6). The one major dierence between the two cases is that the presence of a slurry for
gs < 0:1 suppresses the appearance of the A-segregates. As noted above, these channels begin by
remelting solid at the interface between the rigid matrix and the freely moving uid. With no
slurry, the rigid mush is very permeable near this interface, whereas it is much more resistant to
uid ow when the packing fraction is greater than zero. Without the relatively open matrix at the
transition between moving and stationary regions, the ow in the rigid mushy zone is too slow to
dissolve the solid and form a channel.

M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

103

Fig. 4. Final macrosegregation plots for gs;P 0:0: (a) Sn and (b) Sb.

Fig. 5. Macrosegregation plots for gs;P 0:1 at t 300 s: (a) Sn and (b) Sb. Dashed lines clockwise streamlines, solid
lines constant volume fraction.

When the packing fraction is increased still further to gs;P 0:3, the ow pattern deviates even
more from the case of an entirely rigid mushy zone. The moving slurry now has velocities several
orders of magnitude higher than the corresponding interdendritic liquid at the same volume
friction in a stationary mushy zone because there is a larger solutal buoyancy force at higher solid

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M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

Fig. 6. Final macrosegregation plots for gs;P 0:1: (a) Sn and (b) Sb.

fractions that is not slowed by drag over stationary solid. With this increased velocity, the slurry
region is much thinner than the analogous region in the rigid case. The microsegregation which
occurs in the binary eutectic trough has more of an opportunity to cause redistribution when the
solid is in motion, as the volume fraction at which it begins is in the slurry region. The result of the
alteration of the ow elds is a much increased macrosegregation (see Fig. 7) and a stronger ow.
The much stronger, counterclockwise, solutally driven cell produces a much more planar rigid

Fig. 7. Final macrosegregation plots for gs;P 0:3: (a) Sn and (b) Sb.

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105

Fig. 8. Predicted and measured horizontal composition proles 49 mm from bottom of mold.

Fig. 9. Predicted and measured vertical composition proles 27 mm from chilled wall.

slurry interface. The level and extent of the segregation at the centerline both increased with this
more vigorous ow of Sb-depleted and Sn-rich uid. As will be seen below, the last case,
gs;P 0:6, has another very large increase in macrosegregation due to the greater penetration of
slurry into the mushy zone.
Figs. 8 and 9 show selected composition proles for four dierent values of gs;P at two locations:
y 49 mm (horizontal, from the cooled mold wall to the centerline) and x 27 mm (vertical,
from the bottom mold wall to the free surface). While the experimental data from [12] do not fall
on the lines for any one particular gs;P , even within the same prole, it is reasonable to conclude
from these data that there is a trend indicating that the packing fraction is in the lower range
(gs;P < 0:3) rather than the higher (gs;P  0:6), as the latter case results in too much macrosegregation. The horizontal proles (Fig. 8) suggests a gs;P in the range of 0.1, while conclusions
drawn from the vertical prole (Fig. 9) are more equivocal due to the small dierences in the
calculated proles for gs;P 0:1 and gs;P 0. Given the uncertainty and simplications made in
the model by using a constant and uniform packing fraction, it is unreasonable to expect perfect
agreement in this system, but this model does predict some general trends in macrosegregation in
spite of the simplications. It would be interesting to see what results the more sophisticated

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M.J.M. Krane / Appl. Math. Modelling 28 (2004) 95107

models (e.g., Wang and Beckermann [14]) would produce for this system and how those predictions would compare to the experimental data.
4. Summary
New models for ternary metal alloy solidication and solid particle transport are combined to
evaluate the eect of the motion of free-oating dendrites on the nal macrosegregation patterns
in a PbSbSn alloy. While the characteristic particle diameter does not have an eect under the
conditions of this study, the packing fraction does change the composition distribution. At low
packing fractions, the solid slurry has only small eects on macrosegregation, specically by
eliminating the growth of channels. Higher values of gs;P increase the redistribution of Sb and Sn
in the ingot. Experimental composition data compares favorably with low packing fractions,
suggesting that use of packing fractions based on that for solid spheres (gs;P  0:6) is inappropriate. The dierence in macrosegregation between a completely rigid mushy zone and one with a
small value of packing fraction gs;P 0:1 is well within the experimental and model uncertainty,
so the agreement between experiment and calculation only indicates a trend in the data and must
be viewed in light of the model limitations.
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