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Coherent -Precipitates at Singular and Rough Grain

Boundaries in a Model Ni-Base Superalloy
SUNG BO LEE, DUK YONG YOON, and MICHAEL F. HENRY

In a model Ni-base superalloy of Ni-24Co-4A1–4Ti-5Cr-5Mo (by wt pct), the singular and rough
grain boundaries that exist at a temperature range between 1050 °C and 1200 °C can be identified by
observing the shapes of coherent -precipitates by transmission electron microscopy (TEM). Some
grain boundaries become locally curved with the impinging spherical -precipitates. These grain
boundaries must be rough. Some grain boundaries maintain their flat shapes even at the contact
areas with the -precipitates and triple junctions. Such flat grain boundary shapes indicate that these
grain boundaries are singular. Some grain boundaries have hill-and-valley shapes and some of their
segments also show flat shapes with impinging precipitates. These boundary segments must also be
singular. The results show that the singular and rough grain boundaries in this alloy can be clearly
identified by the shape distortions produced by the impinging -precipitates.

I. INTRODUCTION oriented planes of small neighboring grains were observed

ALL crystals are predicted to have polyhedral equilib-
rium shapes at 0 K with flat faces and sharp edges.[1–5] The
observed equilibrium shapes of crystals at low tempera-
tures appear to agree with this prediction.[6–9] The flat faces
are also called singular, because their orientations
correspond to the singular points (cusps) in the polar plots
(the Wulff plots) of the surface energy against surface
normal. At high temperatures, crystals develop curved edges
and corners, and may become nearly spherical.[6–12] The
curved surfaces are atomically rough.[13] A flat surface of
a crystal of finite size thus becomes curved at its rough-
ening transition temperature.[13,14,15] Therefore, the
equilibrium shape is a manifestation of the surface struc-
ture (either singular or rough).
The roughening transition of the crystal surface was first
predicted by Burton et al.[16] on the basis of Onsager’s
solution[17] of the two-dimensional Ising model. Kosterlitz
and Thouless[18,19] and van Beijeren[20] obtained complete
solutions of the statistical models, which were equivalent to
the solid-on-solid model for crystal surface.[15,21] These
theoretical analyses predicted an infinite order surface rough-
ening transition.
The roughening transition of symmetric low-angle grain
boundaries was predicted by Rottman[22] by making an anal-
ogy to the surface roughening. Westmacott and Dahmen[23]
made an in-situ transmission electron microscopy (TEM)
observation of the reversible roughening of grain boundary
segments of an Al island grain at high temperatures. In
alumina doped with SiO2 and CaO, the singular grain bound-
aries between the (0001) plane of a large grain and randomly
SUNG BO LEE, Researcher, is with the Max-Planck-Institut für Met-
allforschung, D-70569 Stuttgart, Germany. Contact e-mail: bolee@hrem.mpi-
stuttgart.mpg.de DUK YONG YOON, Professor, is with the Department
of Materials Science and Engineering, Korea Advanced Institute of Sci-
ence and Technology, Taejon 305-701, South Korea. MICHAEL F. HENRY,
Metallurgist, is with the General Electric Corporate Research and Devel-
opment Center, Niskayuna, NY 12309.
Manuscript submitted August 20, 2002.
to become curved and hence rough when MgO was added.[24]
A similar roughening transition of singular grain boundaries
in TiO2-excess BaTiO3 was observed upon changing the
heat-treatment atmosphere from air to hydrogen.[25,26] The
defaceting transitions of hill-and-valley (h&v) grain
boundaries with both special and general misorientation
angles were observed in Al,[27] Au,[27] Ni,[28] 316L stainless
steel,[29,30] and a model Ni-base superalloy[31] with temper-
ature increase. Because some segments of the h&v grain
boundaries are expected to be singular, the defaceting
transitions indicate roughening transitions of the singular
boundaries. The observed temperature dependence of grain
growth,[32,33] grain boundary migration,[34,35] and grain bound-
ary sliding[36,37] also indicated the roughening transitions.
The formation of -precipitates, grain growth, and grain
boundary defaceting were previously observed in a model
Ni-base superalloy.[31,38] This alloy of Ni-24Co-4Al-4Ti-5Cr-
5Mo (by wt pct) was designed to reduce the lattice mismatch
between the -matrix and the coherent -precipitates to the
minimum. The -precipitates were found to have either
spherical or curved dendritic shapes,[38] indicating that the
interface between the -precipitate and the -matrix was
rough. The solvus temperature of the -phase was deter-
mined to be slightly (probably a few degrees) above 1150 °C.
When this alloy was heat-treated at 1300 °C and quenched,
all grain boundaries were smoothly curved with local
distortions by fine -precipitates produced during the
quenching.[31] The grain boundaries were therefore rough
at 1300 °C. When heat-treated at a lower temperature of
1200 °C, most of the grain boundaries showed h&v shapes,
indicating that at least some of their flat segments were
singular.[31] These results thus showed that most of the grain
boundaries in this alloy underwent roughening transitions at
temperatures between 1200 °C and 1300 °C.
Because the grain boundaries in a polycrystal become
rough at different temperatures, it is possible that both rough
and singular grain boundaries coexist at temperatures below
1200 °C and even at temperatures below the solvus
temperature (1150 °C) of the -phase. But there is normally
some ambiguity in identifying the singular or rough grain

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boundary segments by their shapes. If a grain boundary has

a flat shape at all scales of observation (including high
resolution TEM) and lies on the well-defined crystallographic
plane of either grain or both grains, it is likely to be singular.
However, some suggested that such grain boundaries could
appear because of their low migration velocity and hence
did not represent their equilibrium shapes.[39] Rough grain
boundaries will usually have curved shapes, but if the
neighboring grains have an equal size, a rough grain
boundary between them may have a flat shape. Furthermore,
a grain boundary with an h&v shape can have rough
segments with flat shapes.[1,2,40] Therefore, it is often difficult
to clearly identify the singular or rough grain boundaries by
their shapes.
The purpose of this work is to show that these two grain
boundary types can be clearly identified by observing the
distortions produced by the -precipitates. There were some
indications from the previous work[31] that the rough grain
boundaries were distorted by the impinging precipitates while
the singular grain boundaries maintained their flat shapes
like the twin boundaries.[41] The equilibrium shapes of crys-
tals on planar surfaces or grain boundaries were analyzed
by Winterbottom[42] and Cahn and Hoffman.[43] It will be
Fig. 1—A TEM micrograph of a singular grain boundary and coherent
shown that a singular grain boundary behaves like a planar -precipitates in a specimen heat-treated at 1050 °C for 24 h with a triple
surface when there is an impinging precipitate and a rough junction marked by an arrow.
grain boundary behaves like a deformable surface. The results
of this work can also have practical implications, because
it was earlier observed that the grain boundaries could
become serrated by the growing -precipitates.[38]

II. EXPERIMENTAL PROCEDURE

The experimental procedure was identical to that described
earlier.[31] The alloy of Ni-24Co-4Al-4Ti-5Cr-5Mo (by wt
pct) was made by spray forming and hot isostatically pressed
at 1050 °C. The alloy specimens of about 7 mm in diame-
ter and 12 mm in height were heat-treated at 1200 °C for 10
minutes in a tube furnace with a flowing Ar atmosphere.
They were quenched in water after the heat-treatment. The
specimens were heat-treated again at 1050 °C (below the
solvus temperature of 1150 °C for the -phase) for 24 or
100 hours, and water quenched. The -precipitates and grain
boundaries were examined by TEM.

III. RESULTS AND DISCUSSION

The -precipitates of about 0.07 m in average diam-
eter formed during quenching after the heat-treatment at
1200 °C, as shown earlier.[31] During the reheat-treatment
at 1050 °C for 24 hours, the -precipitates in the grains
grew to an average diameter of about 0.5 m, as shown
in Figures 1, 2, and 4. The precipitates were slightly larger
after heat-treating for 100 hours at this temperature. These
precipitates are coherent with the  -grains. [38,41] Their
nearly spherical shape indicates that the lattice mismatch
between the  -precipitates and the  -matrix is very
small[38,41] and the interface between the two phases is
rough. The dendritic growth of the -precipitates after
directly cooling to temperatures close to the solvus tem-
perature or during slow cooling also confirms the rough
interphase boundary.[38,41]
Fig. 2—A TEM micrograph of a hill-and-valley grain boundary and coherent
-precipitates (A and B) in the same specimen as Fig. 1.
After the heat-treatment at 1050 °C for 24 hours, the
precipitates at grain boundaries showed two distinct
morphologies. In the first type shown in Figure 1, it appeared
as if the precipitate was truncated by a flat grain boundary.
The boundary between the -precipitate and the grain of
different orientation at the bottom of Figure 1, which is an
incoherent - boundary, was co-planar with the - grain
boundary without any puckers or ripples at the triple junctions.
Another examples of such a precipitate morphology are shown

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Fig. 3—A schematic diagram for the equilibrium at a triple junction with
parallel singular segments of Gg and Gi and equilibrium precipitate shape.
in Figure 2 by the precipitates marked A and B on a grain
boundary with h&v shape. It was determined by electron dif-
fraction that there was no special orientation relationship
between the grain pairs in both Figures 1 and 2. Previously,
similar -precipitates that appeared to have been truncated by
flat twin boundaries were reported for the same alloy.[38,41]
Such a precipitate morphology at a grain boundary is pos-
sible if, and only if, both - grain boundary (designated as
Bg) and incoherent - boundary (designated as Bi) are sin-
gular. The force equilibrium at the triple junction of Bg, Bi,
and the coherent -’ boundary (designated as Bc) is schemat-
ically shown in Figure 3 using the capillarity vector () of
Hoffman and Cahn[43,44] projected on the plane perpendicular
to the triple junction. Because the -plots have the same shapes
as the equilibrium grain and precipitate shapes, the flat and
the curved segments represent the singular and rough bound-
aries, respectively. In Figure 3, Gi, Gc, and Gg are the -plots,
respectively, of the precipitate embedded in the other grain
with an incoherent boundary, the precipitate in the same grain
with a coherent boundary, and the first grain embedded in the
second grain with a grain boundary (the grain boundary Wulff
plot). The shape of Gc is circular at the projection plane
because of the spherical precipitate shape, and the singular
boundaries of Gi and Gg are drawn parallel to each other. Both
centers of Gi and Gg are located at the common point C. The
possible triple junction equilibria are obtained by moving
the center of Gc along the boundary of Gi and forming the
triangles of the three vectors, i, c, and g, of the corresponding
-plots. It is readily seen that the equilibrium triple junctions
with co-planar Gi and Gg are possible. Using similar -plots,
it can be easily shown that if one of Bg and Bi is rough and
the other singular, the triple junction equilibrium with coplanar
Bg and Bi is not possible. (It is actually possible for a partic-
ular dihedral angle, but the rough boundary cannot remain
flat over its length because of the grain size effect.) If all
boundaries are rough, Bg cannot be coplanar with Bi, as will
be shown later.
If the grain boundary Wulff shapes have flat singular
segments connected to other singular or rough (curved)
segments with slope discontinuities, the grain boundaries in
polycrystals are likely to have h&v shapes. Some of the h&v
boundary segments are likely to be singular, although they
cannot normally be distinguished from the rough segments
METALLURGICAL AND MATERIALS TRANSACTIONS A
by their shapes because both types of grain boundary segments
will be flat. However, in Figure 2, the grain boundary
segments on which the precipitates A and B impinge must
be singular because of the co-planar Bg and Bi.
The grain boundary precipitates shown in Figures 1 and
2 actually exhibit the general wetting behavior on singular
interfaces, and the shaded region of the truncated circle in
Figure 3 displays the equilibrium precipitate shape if it is
determined by capillarity. At the triple junction, the surface
tension component of Bc perpendicular to Bg and Bi is
balanced by the torque components of Bg and Bi. Winter-
bottom[42] and Cahn and Hoffman predicted the equilibrium
precipitate shapes assuming planar interfaces at the triple
junctions. Such a junction with co-planar boundaries is
possible if, and only if, both are singular. Therefore, the
model of Winterbottom[42] and Cahn and Hoffmann[43] for
wetting will apply when the singular interface still remains
singular even in contact with the wetting phase.
The wetting angle  defined in Figure 3 is related to the
interfacial energies i, c, and g of the boundaries Bi, Bc,
and Bg as
i  g  c cos  [1]
With   150 deg from Figures 1 and 2,
i  g  0.9c [2]
Because g and c represent the energies associated with
orientation and composition changes across the boundaries,
respectively, i is expected to be approximately equal to the
sum of g and c. Therefore, the observed value of  roughly
agrees with the expected relation between the three interfa-
cial energies. If i is exactly equal to the sum of g and c,
the precipitate will not wet the grain boundary and have a
spherical shape, as can be seen by drawing a smaller circle
for Gc with its radius equal to the distance between the sin-
gular planes of Gi and Gg, which is equal to the difference
between i and g.
Although there was almost a tenfold coarsening of the
precipitates and hence general microstructural evolution dri-
ven by capillarity during the heat-treatment at 1050 °C for
24 hours, the shapes of the grain boundary precipitates shown
in Figures 1 and 2 are likely to deviate from the equilibrium
shapes. Probably most of these precipitates were not in con-
tact with the grain boundaries in the initial stages of the
heat-treatment. If some of them impinged on the grain bound-
aries after they had grown to relatively large sizes, their
shape equilibration would have taken a long time. The pre-
cipitate shapes could also deviate from truncated spheres
because even small localized lattice mismatch between the
two phases will tend to make the precipitates cubic and the
precipitates are still undergoing slow diffusion-controlled
coarsening. In spite of these possible kinetic and strain effects
on the precipitate shape, the planar Bi and Bg at the triple
junctions are possible only if they are singular.
The morphologies of the precipitates at other grain bound-
aries were characteristically different from those shown in
Figures 1 and 2. As shown in Figure 4, the precipitates
impinging on some grain boundaries were nearly spherical
with curved Bi and Bg at the contact areas to accommodate
the nearly spherical precipitate shape. These curved Bi and
Bg must be rough. If the boundary energies are isotropic, the
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Fig. 4—A TEM micrograph of a rough grain boundary and coherent
-precipitates in the same specimen as Fig. 1.
magnitudes of the -vectors are identical to the corresponding
boundary energies. The condition for the triple junction equi-
librium is schematically shown in Figure 5(a) with the same
meanings for the symbols as in Figure 3. As pointed out by
Winterbottom[42] and Cahn and Hoffman,[43] the equilibrium
configuration cannot be simply described in this case, but
generally, Bi and Bg will be curved and not co-planar at the
junction, as illustrated in Figure 5(b). It will therefore appear
as if the precipitate is protruding into the other grain at the
contact area. The morphology described in Figure 5 is actu-
ally that of wetting on a surface that has previously been
assumed to be reactive or deformable.[43] A surface will be
deformable under capillary forces if it is rough.
If i is nearly equal to the sum of g and c, the contact
angle between Bi and Bg will be close to 180 deg and the
precipitate will be nearly dewetting the boundary, as can be
seen in Figure 5. For the two precipitates indicated by arrows
in Figure 4, it appears that is indeed close to 180 deg, but
Bi and Bg are curved along the spherical boundaries of the
precipitates. Although the curved boundary shapes resemble
those depicted for rough boundaries in Figure 5, the Bi and
Bg boundaries also can deviate from their equilibrium shapes.
When some precipitates that are initially not in contact with
the grain boundaries impinge on them during their coarsen-
ing, the rough Bi and Bg segments can be easily bent and
moved, thereby forming more sharply serrated boundaries
than that determined by the equilibrium condition. Thus,
although the shapes of the Bi and Bg segments may be deter-
mined by both equilibrium and kinetic conditions, their curved
shapes still indicate their rough structure. The singular Bg, in
contrast, could remain co-planar with singular Bi because of
their resistance to bending during the impingement and growth
of the precipitate on the grain boundary.
For some grain boundaries with a general high-angle
mis-orientation relationship between the grains in other
1436—VOLUME 34A, JULY 2003
Fig. 5—A schematic diagram (a) for the equilibrium at a triple junction
with rough boundaries and (b) the equilibrium precipitate and boundary
configuration.
polycrystalline materials, flat boundary planes were observed
to lie on the low index planes of one of the grain pairs and
high index planes of the other.[45,46,47] Ichinose and Ishida[47]
observed that about 30 pct of the grain boundaries observed
in polycrystalline Au were such a type, which was referred
to as low index crystal plane grain boundaries. In alumina
doped with SiO2 and CaO, large grains, either artificially
produced with a sapphire crystal or naturally produced by
abnormal grain growth, formed flat grain boundaries on their
(0001) planes with many randomly orientated small grains.[24]
Similarly, abnormally large grains in TiO2-excess BaTiO3
formed flat grain boundaries on their (111) planes with many
randomly orientated small grains.[25,26] Such grain boundary
shapes are possible if, and only if, these low index grain
boundaries are singular.[26,45] It thus appears that at least
some of the singular grain boundaries observed in this alloy
could have low index lattice planes on one side.
As reported earlier,[31] many grain boundaries in this alloy
after heat-treating at 1200 °C showed h&v shapes. Figure 2
shows such an h&v grain boundary in the specimen heat-treated
at 1050 °C. It was previously suggested in pure and single-
phase systems[24–26,28–31,4–47] that, when many grain boundaries
have h&v shapes, at least some of the boundary segments were
likely to be singular. Figure 2 shows an example that confirms
such a possibility. It was also observed earlier[31] that when
this alloy was heat-treated at 1200 °C and quenched, the h&v
METALLURGICAL AND MATERIALS TRANSACTIONS A
02-417A.qxd 20/6/03 9:40 PM Page 1437
grain boundaries showed flat segments in spite of the imping-
ing precipitates. Because, in this work, the specimens were
heat-treated at 1200 °C and again at 1050 °C after quenching
from 1200 °C, some grain boundaries, which were rough at
1200 °C, could have become singular at 1050 °C. The grain
boundary shown in Figure 4, however, did not develop any
fine-scale h&v structures, indicating that it remained rough at
1050 °C when the precipitates were growing.
Crystals at equilibrium have flat or curved surfaces, and
therefore, according to the current theories, all surface seg-
ments are either singular or rough. The results of this work
and others[23–31,45–47] indicate that all grain boundaries may
also exist in either singular or rough state.
IV. CONCLUSIONS
The singular or rough grain boundaries can be identified
from the grain boundary Wulff shape (the equilibrium shape
of an island grain), but such an observation is difficult
because an island grain tends to shrink and disappear. In
polycrystals, if a grain boundary is flat at all scales of obser-
vation, it is likely to be singular. If it is curved at all scales
of observation, it is rough. Often, however, there can be
some ambiguity in distinguishing these boundary types by
their shapes, because even a rough grain boundary can have
a flat shape if the neighboring grains have approximately
the same size. An h&v grain boundary will usually have flat
segments, which can be either singular or rough. In this
work, it has been demonstrated that the two grain boundary
types can be clearly distinguished by the shape distortions
produced by impinging precipitates that are coherent with
one of the grain pairs. The strong torque effect of the singular
grain boundaries has been confirmed. The results also show
that, at 1050 °C, there are both singular and rough grain
boundaries in this alloy. It is expected that with temperature
the fraction of the rough boundaries will increase, as shown
earlier in this alloy[31] and other metals.[28,29,30] An intriguing
question is if a singular grain boundary with a shallow cusp
in its Wulff plot can have enough resistance to bending by
the growing precipitates to keep its flat shape. In equilibrium,
a singular boundary will not become curved.
ACKNOWLEDGMENTS
This work is supported by the Korea Ministry of Science
and Technology through the National Research Laboratory
(NRL) Program, and by the General Electric Corporate
Research and Development Center. The authors are grateful
to Mr. Hyun Min Jang for his assistance in the preparation
of this manuscript.
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