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Studies of the influence of alloying elements on the growth of ferrite from

austenite under decarburization conditions: Fe-C-Nl alloys

Article  in  Metallurgical and Materials Transactions A · April 2004

DOI: 10.1007/s11661-004-0297-z

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Studies of the Influence of Alloying Elements on the Growth
of Ferrite from Austenite under Decarburization Conditions:
Fe-C-NI Alloys
A. PHILLION, H.S. ZUROB, C.R. HUTCHINSON, H. GUO, D.V. MALAKHOV, J. NAKANO,
and G.R. PURDY

We have evaluated controlled decarburization as a method for probing the effect of alloying elements
on ferrite growth from austenite. The technique permits the exploration of longer-time ferrite layer
growth; it minimizes the effects of interface structure on ferrite growth; and it permits the isolation of
the effects of temperature and alloying element concentration on ferrite/austenite interface motion. The
study of the decarburization of initially homogeneous Fe-C-Ni alloys was complemented by experi-
ments using specimens with a controlled nickel concentration gradient. Although the decarburization
method yields consistent results at longer times, it is found to be less appropriate for the study of ini-
tial ferrite growth. Nucleation in the gas/solid interface region, coupled with uncertainties about the
precise time of decarburization, leads to large relative errors at the earliest times. For these reasons,
the method is considered a valuable complement to studies based on precipitation boundary conditions.

I. INTRODUCTION
THE problem of the quantitative description of the growth
of proeutectoid ferrite from alloyed austenite has long been
an area of interest from both the practical and the purely
scientific points of view. The simple addition of a percent
or less of substitutional alloying elements often yields kinetic
results of great practical significance; however, the funda-
mental quantitative prediction of these effects remains elu-
sive. The third workshop on alloying element effects in steels
(of which this presentation is a part) is evidence for a timely
and encouraging renewal of interest in this area.
Much has been learned from the study of the growth of
grain boundary allotriomorphic precipitates, under isothermal
conditions and in simple, well-characterized and homogenized
alloys. However, that technique, as usually practiced, suffers
from uncertainties associated with metallographic sectioning,
as well as difficulties in deconvoluting nucleation from
growth. Growth interfaces are quite generally inhibited by
structural factors associated with orientation relationships
(which are thought to be set upon nucleation). In addition,
the impingement of diffusion fields from opposite sides of a
given grain often occurs early in the transformation sequence,
and this introduces a further limitation on the range of inter-
face velocities accessible through this “classical” method.
A. PHILLION, Graduate Student, is with the Department of Metals and
Materials Engineering, University of British Columbia, Vancouver, BC,
Canada V6T 1Z4. H.W. ZUROB and C.R. HUTCHINSON, Postdoctoral
Fellows, are with the Laboratoire de Thermodynamique et Physico-Chimie
Métallurgiques, INPG/ENSEEG, Domaine Universitaire, 38402, St. Martin
d’Hères, France. H. GUO, Postdoctoral Fellow, D.V. MALAKHOV, Asso-
ciate Professor, J. NAKANO, Graduate Student, and G.R. PURDY, Pro-
fessor, are with the Department of Materials Science and Engineering,
Hamilton, ON, Canada L85 4L7. Contact e-mail: purdyg@mcmaster.ca
This article is based on a presentation given in the symposium “The Effects
of Alloying Elements on the Gamma to Alpha Transformation in Steels,”
October 6, 2002, at the TMS Fall Meeting in Columbus, Ohio, under the
auspices of the McMaster Centre for Steel Research and the TMS-ASM
Phase Transformations Committee.
Rather less attention has been paid to the process of decar-
burization. This process, also of some considerable industrial
interest, offers the potential for the study of a “single inter-
face” transformation in which a ferrite layer nucleates and
grows into an austenitic polycrystal. For a binary iron-carbon
alloy, the process can be described on the basis of a local
equilibrium model, as suggested by Figure 1. Here, the ferrite
is supposed to nucleate quickly, and rapidly to develop a
planar interface with the parent austenite. The rate of growth
of the ferrite layer is then determined by diffusion of carbon
in both the ferrite and austenite phases; the difference of the
two diffusive fluxes is taken up by interface motion. The
rate of growth is never simply controlled by diffusion through
the ferrite layer as long as concentration gradients remain
in the austenite phase (as long as the austenite remains semi-
infinite). Referring again to the binary model, it is clear that
the composition of the original austenite will play a role in
the rate of motion of the interface: for a given temperature,
higher carbon alloys will decarburize more slowly.
The role of temperature is also of interest. Since the solubi-
lity of carbon in ferrite approaches zero as the reaction tem-
perature approaches the transformation temperature of pure
iron, the rate of decarburization by the growth of a planar
ferrite layer will also approach zero as the temperature is
raised toward this temperature. A maximum rate of ferrite
growth is therefore expected at some lower temperature.[1]
The method has several advantages from an experimental
point of view. Rates of ferrite growth can be measured with
great accuracy over long times without the need to consider
the effects of impingement of diffusion fields from other fer-
rite fronts. Specimen geometry is simple and controllable;
sectioning errors are negligible. As will be shown, interfacial
structure effects on interface mobility, often so prominent
in the isothermal precipitation case, are minimized, particularly
for longer ferrite growth times. The method also has some
disadvantages; these will be noted in Section IV.
The objective of this work was to explore the utility of
the decarburization boundary condition as a research tool,
and then to use the technique to investigate the migration

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 35A, APRIL 2004—1237


Fig. 1—Schematic concentration profile for a binary decarburization
experiment.
characteristics of ferrite/austenite interfaces in simple alloys.
It was our expectation that much of value could be learned
about the dynamic interaction of the alloying element with
the transformation interfaces. The system Fe-C-Ni was
chosen for initial study. Nickel is thought to be rather weakly
segregated to the interphase interface in equilibrium; the
carbon-nickel interaction (indexed in approximation by
the Wagner interaction parameter) is small and mutually
repulsive.[2]
The existing experimental evidence on ferrite precipitation
in pure Fe-C-Ni alloys suggests that, provided that there is
no long-range redistribution (partitioning) of the alloying
element, the observed growth rates will fall between two
theoretical limits. The first is calculated on the basis of para-
equilibrium (PE)[3–6] and the second using local equilibrium-
nonpartitioned (LE-NP). [7–13] Each of these limits is purely
thermodynamic, the first based on the assumption that the
transformation interface encounters no dynamic segregation
of the alloying element beyond that in the bulk alloy, and
the second on the assumption that a full local equilibrium
for the alloying element (with an associated diffusion “spike”)
exists in the austenite at the interface. Each method assumes
that the highly mobile solute, carbon, is in local equilibrium.
Solute drag theory has been employed in several attempts
to bridge these two kinetic limits. For the quantitative imple-
mentation of this approach, one requires a knowledge of the
equilibrium segregation of the alloying element to the trans-
formation interfaces, and the diffusion coefficient of the
alloying element within the interface. The latter quantity is
a priori unknown.
As will be shown, the decarburization method permits the
exploration of the kinetics of ferrite/austenite interface motion
and its comparison with the limiting cases referred to pre-
viously; it also has the potential to yield, indirectly, values
of the trans-boundary transport coefficient for the alloying
element.
II. EXPERIMENTAL METHOD
The simplicity of the experimental setup is one of the
main advantages of the present approach. In general, the
samples were spot welded to a thermocouple and inserted
1238—VOLUME 35A, APRIL 2004
Table I. Compositions of the Alloys Used
in This Investigation
Alloy Ni (Wt Pct) C (Wt Pct) Temperature (°C)
A 0 0.51 775
B 0.97 0.50 775
C 1.66 0.50 775
D 1.03 0.38 800
E diffusion couple 1-5 pct Ni, 775
0.47-0.42 pct C
through an O-ring seal into the tube furnace, under argon
flow. A heating time of 5 minutes allowed the samples to
austenitize and to reach the desired decarburization tem-
perature. Water-saturated hydrogen (25 °C) was then used
to decarburize the samples for the desired period of time.
Finally, the system was purged with Ar for 1 minute before
quenching the samples in water. Blank samples (no hydrogen
flow) were used to verify that the Ar purging steps resulted
in no ferrite formation. Overall, the temperature was con-
trolled to within less than 62 °C and quenching times were
generally less than 5 seconds.
Four alloys and one diffusion couple were studied using
the preceding technique. The compositions and temperatures
were chosen to highlight the difference between the PE
and LE-NP models. The experimental conditions are sum-
marized in Table I. In addition, the Fe-Ni-C isothermal sec-
tions at 775 °C and 800 °C are shown in Figure 2.
The alloys were prepared by arc melting high-purity stocks
Fe, Ni, and graphite under an argon atmosphere. The samples
were then homogenized for 3 days at 1100 °C. Preparation
of the diffusion couple (sample E) involved the diffusion
bonding, at 900 °C, of two binary alloys, containing 1 and
5 pct Ni. The diffusion couple was then homogenized for
4 days at 1400 °C, leading to a diffusion profile of about
600 mm. Finally, the diffusion couple was carburized to a
constant carbon activity using a CO/CO2 ratio of 200:1 and
a temperature of 1200 °C. The resulting carbon concentration
varied from 0.47 pct at the 1 pct Ni end to 0.42 pct C at
the 5 pct end.
III. RESULTS
The experimental results are conveniently presented in
two sections. In Section A, the ferrite growth kinetics for
homogenous alloys A through D are presented. In Section B,
we present data on the decarburization of the diffusion couple
(sample E).
A. Kinetic Measurements
The ferrite-layer thickness was measured as a function
of the decarburization time for samples A through D. In all
cases, the shortest time was 2 minutes and the longest 256 min-
utes. The results are presented in Figures 3 through 6. Two
models were used to analyze the experimental data; the dot-
ted curves were calculated using the steady-state analytical
model of Malakhov and Purdy[14] and assuming that the
carbon diffusion coefficient is independent of concentration.
The solid curves were calculated using an implicit finite
METALLURGICAL AND MATERIALS TRANSACTIONS A
 (a) Fig. 4—Ferrite layer growth during decarburization of alloy B at 775 °C.
The upper limit of PE and the lower limit of LE-NP are both shown. The
text provides details.

(b)
Fig. 2—Isothermal cross section of the Fe-Ni-C ternary phase diagram at
(a) 775 °C and (b) 800 °C. The para-equilibrium boundaries and the envelope
Fig. 5—Ferrite layer growth during decarburization of alloy C at 775 °C. The
of no partition are also shown. The insert lists the interfacial concentrations
upper limit of PE and the lower limit of LE-NP are both shown. The text pro-
of carbon for samples B through D. These values were calculated iteratively,
vides details.
starting from the bulk concentration of the alloy. The text provides details.

Fig. 6—Ferrite layer growth during decarburization of alloy D at 800 °C.

Fig. 3—Evolution of ferrite layer thickness during the decarburization of The upper limit of PE and the lower limit of LE-NP are both shown. The
a binary Fe-0.51 mass pct C alloy at 775 °C. text provides details.

difference routine that considers transient effects as well as were evaluated by applying a second-order Taylor series
the concentration dependence of the carbon diffusion coef- expansion of the concentration profiles in the ferrite and
ficient. In this numerical model, the fluxes at the interface the austenite at the interface.[15,16] In both models, diffusion

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 35A, APRIL 2004—1239

control is assumed and the kinetics is determined by the car-
bon concentrations as given by PE (upper limit) and LE-NP
(lower limit).
A number of key observations can be made, starting with
alloy (A). In this binary alloy, the evolution of the ferrite-
layer thickness can be modeled reliably. The relevant carbon
concentrations are given by the equilibrium phase diagram.
The excellent agreement between the experimental data and
the models indicates that diffusion control (as opposed to
surface control) is the dominant condition during our decar-
burization experiments. In addition, the agreement confirms
the accuracy of the carbon diffusion coefficients that are
used in the model.[17] Turning our attention to Figures 4
through 6, it is clear that the experimental data lie between
the upper limit of PE and the lower limit LE-NP, and gener-
ally approach the LE-NP limit rather closely. This is particu-
larly clear when the results of the finite-difference model
are considered. We believe that the finite-difference approach
provides a better description of the present problem because
it takes into account the concentration dependence of the
carbon diffusion coefficient. This is critical, because the inter-
face motion is driven by small differences between the
incoming and outgoing fluxes. As such, these quantities must (a)
be calculated very accurately.
At this stage, it is important to comment on the uncertainty
associated with the experimental points. In general, the uncer-
tainties decreased as the duration of the treatment and the
thickness of the layers increased. For times greater than
16 minutes and layers thicker than ,30 mm, the ferrite layers
were very uniform and variations in layer thickness were
minimal (,5 mm). The greatest uncertainties arise at the
shortest times. At these times, the ferrite layers are not very
uniform and, in some extreme cases, discontinuous. Further
difficulties arise from the issue of time control. Using a sim-
ple model of plug flow, we are led to believe that it takes
30 to 90 seconds to displace the Ar from the furnace.
Because of the large uncertainties at short times, it is
difficult to investigate the possibility of a change in kinetics
at early times. We considered that the previously dif-
ficulties could be overcome to some extent by using a
wedge-shaped sample. The preferential decarburization
associated with the wedge geometry makes it possible to
sample a range of interface velocities in a single sample.
As a result, the time uncertainty is no longer a concern.
In addition, the uncertainty resulting from ferrite layer
thickness variations is less significant. We examined a
number of wedge samples with different wedge angles; (b)
two examples are shown in Figure 7. We found that the
ferrite-austenite interface moved in a manner consistent Fig. 7—(a) and (b) Ferrite layer profiles in wedge samples. In each case,
with constant interfacial carbon concentrations throughout alloy D was decarburized for 50 minutes at 800 °C. In each case, the solid
curve represents the predicted profile under LE-NP conditions. The dotted
the wedge. In other words, no evidence was found for a curve is for the PE limit.
kinetic transition, which would be manifested in a greater-
than-calculated total distance moved by the faster moving
B. Diffusion Couple
interface (at the apex). Figure 7(a) especially shows excellent
agreement between the LE-NP model and the experimental Our isothermal results indicate that the LE-NP limit
data, even in the corner, where overlapping diffusion fields provides a very good description of the decarburization
have caused the interfaces to move through a greater distance kinetics. To investigate the robustness of this conclusion,
in a given time. we decarburized a number of diffusion couples at 775 °C
At the shortest times (,2 minutes), the ferrite layer was (sample E). Two examples are shown in Figures 8(a) and (b).
no longer continuous and the results were difficult to inter- The micrographs correspond to samples that have been decar-
pret. As such, the possibility of a kinetic transition at the burized for 4 and 16 minutes, respectively. X-ray micro-
shortest times could not be confirmed or eliminated. analysis indicates that the Ni content is 1.9 6 0.2 pct Ni at

1240—VOLUME 35A, APRIL 2004 METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 8—Decarburization profiles for the Fe-Ni-C diffusion couple (E). The
decarburization temperature was 775 °C, and the time was (a) 4 min and
(b) 16 min. In both cases, the ferrite layer terminates at a Ni concentration
of 1.9 6 0.2 pct in agreement with the LE-NP limit.
the point where the ferrite layer terminates. This concentra-
tion is to be compared with the values of 1.95 and 2.85 pct
Ni, predicted by the LE-NP and PE conditions, respectively.
The present observation is consistent with the observations
of Section A and confirms that the system closely approaches
the LE-NP limit. The implications of the diffusion couple
experiments are discussed in detail in the following section.
There is some suggestion of ferrite precipitation in front of
the planar interface in figures 8(a) and (b); we believe that
this is due to ferrite formation during quenching in the
carbon-depleted region of the austenite.
IV. DISCUSSION
With this contribution, we evaluate controlled decarbur-
ization as a method for the isolation of the effects of alloying
elements on ferrite growth from austenite. By carefully con-
trolling the bulk alloy composition, the temperature, and the
decarburization conditions, one can optimize the distinction
between different theoretical limiting interfacial boundary
conditions while simultaneously minimizing the uncertainties
associated with crystallographic (structural) constraints on
interfacial mobility.
We have chosen PE and LE-NP as the two relevant limit-
ing cases; each involves the local equilibrium of the mobile
solute (carbon). These two cases differ in the local behav-
ior of the substitutional solute, which is considered com-
pletely unaffected by the passage of the interface (PE) or
to be in full local equilibrium (LE-NP). Intermediate kinetic
conditions bridging these limits would correspond, concep-
tually, to a local enrichment of the substitutional solute at
the transformation interface; these intermediate states have
been characterized by reference to solute drag theory.[18–21]
The current experimental results (and comparable series of
METALLURGICAL AND MATERIALS TRANSACTIONS A
experiments exploring other alloying elements) offer the pos-
sibility of an indirect kinetic probe of the solute fields within
and near the moving interfaces, an adjunct to the more direct
microchemical analytical methods reported elsewhere.
We have also explored the possibility of using the decar-
burization condition to search for kinetic transitions within
the window defined by the limiting cases. As will be noted
later, the earliest stages of the transformation are not easily
accessible; it seems that traditional metallographic studies
of the isothermal growth of ferrite from supersaturated
austenite are the more promising methods for the study of
this aspect of the problem.
However, the longer time kinetics reported here are infor-
mative in the following ways.
1. The growth of ferrite is closely parabolic in all cases.
The binary iron-carbon experiments are consistent with
interface motion controlled by carbon diffusion. Given
the rather small experimental uncertainty, there is no evi-
dence of a structural barrier to growth in any of the results
reported here.
2. All of the ternary Fe-C-Ni experimental kinetics fall
within the window defined by the PE and LE-NP limits,
and closely approach the computed LE-NP condition.
This is a clear indication that the interface motion is
determined by carbon diffusion, and that the interfacial
carbon concentrations in ferrite and austenite are approxi-
mately constant and determined by the presence of the
alloying element (nickel in this case).
3. The LE-NP condition describes the experimental obser-
vations rather well, in spite of the minimal estimated sub-
stitutional diffusion penetration of the parent phase (atomic
dimensions or less). It may be that the LE-NP condition
is closely approached when the transformation interface
is effectively “loaded” with substitutional solute and when
there is a minimal solute drag contribution to the inter-
face resistance; the matter requires further investigation.
4. The kinetics of decarburization is very sensitive to the
Ni content and annealing temperature. For example,
increasing the temperature by as little as 5 °C in Fig-
ure (6) would bring the modeling results into exact agree-
ment with the experimental data. As such, very accurate
temperature and composition control is needed.
The observation that the kinetic interface states (and, by
inference, the local substitutional solute distributions) appear
to remain similar over large variations in interface velocity
deserves further comment. One expects that the thermody-
namic driving force for interface motion will decrease with
decreasing velocity. In the present case, the major component
of this force will be derived from a departure from equilib-
rium of the interstitial solute, carbon. The inferred constancy
of interfacial carbon concentrations implies that the resistance
to interface motion is relatively small. The effects of inter-
facial crystallography have been effectively eliminated. It is
to be noted that the interface velocities sampled with the
present experiments are low, but that they span two orders
of magnitude (2 3 1029 to 2 3 1027 m/s).
Wedge samples were used to probe for transitions from
a higher velocity branch. Uncertainties related to the initial
nucleation and growth of ferrite frustrated this search, how-
ever, as systematic planar motion of the interfaces was seen
VOLUME 35A, APRIL 2004—1241
 only at times exceeding about 8 minutes. However, the mor-
phologies of the ferrite layers formed on corners were again
broadly consistent with constant interfacial carbon compos-
itions, suggesting that any fast ferrite growth state did not
survive much past the nucleation stage.
The nickel-gradient samples were especially informative.
It is clear that the growth of the ferrite layer terminates at
the solubility limit for nickel in pure iron (which also cor-
responds to the LE-NP envelope at zero carbon content).
The paraequilibrium solubility limit (2.85 pct Ni) is much
higher; however, no evidence was found for ferrite layer
growth above the equilibrium solubility.
V. CONCLUSIONS
We have evaluated decarburization as a method for prob-
ing alloying element effects on ferrite growth from austenite.
The technique involves the rather precise control of the decar-
burization process: it permits the exploration of longer-time
ferrite layer growth; it minimizes the effects of interface
structure on ferrite growth; and it permits the isolation of
the effects of temperature and alloy composition on ferrite/
austenite interface motion.
Although the decarburization method yields consistent (and
closely parabolic) results at longer times, it is inappropriate
for the study of initial ferrite growth. Nucleation in the
gas/solid interface region, coupled with uncertainties about
the precise time of decarburization, leads to large relative
errors at the earliest times. For these reasons, attempts to
sample the possible transitions from paraequilibrium through
a solute-drag regime to a near LE-NP condition were not
successful. (There is some evidence for the existence of near-
paraequilibrium kinetic states at early stages of ferrite growth
under conditions of precipitation from austenite;[22] it is also
well established that ferrite forms rapidly at temperatures and
compositions somewhat above the LE-NP limit in precipita-
tion studies of simple Fe-C-Ni alloys[20]).
The present results were obtained for a very simple ternary
system, Fe-C-Ni, one for which no attractive interaction with
carbon exists. The method is therefore considered appropriate
for the experimental test of current theories of substitutional
solute drag as it affects the growth of proeutectoid ferrite
from austenite.
We consider that the use of controlled decarburization
experiments can play the role of a valuable adjunct to the
1242—VOLUME 35A, APRIL 2004
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more usual precipitation studies; neither is optimal for the
study of the full range of dynamic states. However, taken
together, the two methods offer promise for the advancement
of our understanding of this important area.
ACKNOWLEDGMENTS
This research was supported by the Natural Sciences and
Engineering Research Council of Canada. One of the authors
(CRH) acknowledges the financial support of IRSID Labo-
ratories and CNRS (France). We are grateful to Professor
Yves Bréchet, Institut National Polytechnique de Grenoble,
for stimulating discussions; and to Mr. Jim Garrett, the
Brockhouse Institute for Materials Research, for assistance
with the design and execution of the experiments.
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METALLURGICAL AND MATERIALS TRANSACTIONS A