J. Am. Ceram. Soc.

, 85 [6] 158593 (2002)

journal

Abnormal Grain Growth in Alumina with Anorthite Liquid and the

Effect of MgO Addition
Chan Woo Park and Duk Yong Yoon*
Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology,
Daejeon 305-701, Korea
Abnormal grain growth (AGG) in alumina with anorthite
liquid has been observed with varying anorthite and MgO
contents, at 1620C. When only anorthite is added to form a
liquid matrix, the grainliquid interfaces have either flat or
hill-and-valley shapes indicating atomically flat (singular)
structures. The large grains grow at accelerated rates to
produce AGG structures with large grains elongated along
their basal planes. This is consistent with the slow growth at
low driving forces and accelerated growth above a critical
driving force predicted by the two-dimensional nucleation
theory of surface steps. With increasing temperature, the AGG
rate increases. The number density of the abnormally large
grains increases with increasing anorthite content. The addition of MgO causes some grainliquid interfaces to become
curved and hence atomically rough. The grains also become
nearly equiaxed. With increasing MgO content the number
density of the abnormally large grains increases until the grain
growth resembles normal growth. This result is qualitatively
consistent with the decreasing surface step free energy associated with partial interface roughening transition.
I.

normalized grain size distribution is usually narrow. AGG is thus

characterized by changing (normalized) grain size distribution (or
equivalently, the lack of self-similarity in the grain microstructure)
during the heat treatment. It has been suggested by Yoon et al.13
that because the AGG behavior can gradually change to normal
growth with temperature or composition, the two grain growth
modes are indistinguishable, and hence any deviation from normal
growth can be described as AGG. Because the mechanism of AGG
is closely related to the anisotropic surface energy, the grains
growing abnormally often develop elongated shapes, especially in
the hexagonal crystal systems.
It was recently proposed that the polyhedral grains dispersed in
a liquid matrix coarsen abnormally because the grains grow by
two-dimensional nucleation of steps if they are free of defects.12,13
If they have defects such as dislocations, twins, and contact edges,
the grains can still coarsen abnormally, because the variation of the
growth velocity with the driving force arising from the capillarity
can still be nonlinear. If the amount of the liquid matrix phase is
quite small, as in most of the alumina systems, the grain surfaces
at the intergranular liquid films and grain triple junctions can have
singular planes and hence they may grow by two-dimensional
nucleation of steps. The first goal of this work is to observe the
dependence of AGG in alumina containing anorthite liquid on
temperature and anorthite content, and analyze the results in terms
of the two-dimensional nucleation theory.
The second goal of this work is to examine the well-known
effect of MgO on grain growth in alumina.14 18 Earlier, we have
shown that MgO addition to alumina with small amounts of CaO
and SiO2 causes grain boundary roughening and hence the transformation from AGG to normal growth behavior.19 In this work,
we observed the effect of MgO addition on grain growth in
alumina containing anorthite liquid and analyzed the results in
terms of the grain surface roughening transition. Because the
surface roughening implies the decrease of the surface step free
energy, the effect of MgO addition is closely related to the step
nucleation mechanism, which is used to explain AGG with
anorthite liquid without MgO. As noted earlier, the polyhedral
grains in liquid matrix with singular surfaces coarsen abnormally,
but if the grain surface becomes rough and hence the shape
becomes spherical at high temperatures or with an additive, the
grains grow normally controlled by diffusion in the liquid matrix.12,13 Such an effect of the interface roughening transition on
grain coarsening has been observed in NbCFe with both temperature increase and B addition.20,21 Since the initial proposal by
Burton, Cabrera, and Frank,22 the surface roughening transition
has been extensively studied both theoretically2327 and experimentally.28 30 The effect of the crystal surface structure, which
can be either atomically flat or rough, on crystal growth from
supersaturated melt or vapor has also been studied both theoretically31,32 and experimentally.30,33,34 In this work we will attempt
to apply these theories to the grain growth in the aluminaanorthite
liquidMgO system by observing the growth behavior and the
shape of the grain surfaces at the junctions between two and three
grains.

Introduction

N MOST alumina products, there are small amounts of liquid

phase with compositions close to anorthite.1 4 The grains often
grow abnormally during the sintering treatment.1 4 Some contact
areas between the neighboring grains are separated by liquid films
with grain surfaces of hill-and-valley structures2,57 while other
contact regions between the grains are separated by grain boundaries.8 Such hill-and-valley grain surfaces and grain boundaries
indicate that there are deep cusps in the radial plot of the surface
or grain boundary energy relative to the boundary normal direction.7 In this paper the interfaces between grains and the liquid
matrix are called grain surfaces.
In normal growth of grains with a liquid matrix phase, the grain
size distribution (normalized to the average size) is relatively
narrow and remains invariant during heat treatment for various
periods.9 11 The grains are usually spherical or equiaxed with
rounded shapes because of their rough surface structure.12 In
abnormal grain growth (AGG), some grains grow to large sizes
relative to the matrix grains, which grow very little. As the large
grains grow into the regions of the fine matrix grains, they impinge
on each other. When only the impinged large grains remain, the

L. C. Kleincontributing editor

Manuscript No. 188441. Received June 26, 2000; approved March 8, 2002.
Supported by the Korea Ministry of Science and Technology through the National
Research Laboratory (NRL) Program and by the Korea Ministry of Education through
the Brain Korea 21 (BK21) Program.
*Member, American Ceramic Society.

Present address: Wireless Communication Devices Department, Basic Research

Laboratory, Electronics and Telecommunications Research Institute, Daejeon 305350, Korea.

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II.

Experimental Procedure

In this paper all additive contents will be specified by weight

percent. The amount of CaO2SiO2 added will be designated by
the equivalent weight percent, which is equal to the weight
percent of anorthite formed with Al2O3. Thus 1 equiv wt% of
anorthite is equal to 0.633 wt% of CaO2SiO2. The anorthite
content was varied between 0.05% and 1%, and the MgO
content was also varied. For the sources of SiO2, CaO, and
MgO, Si(OC2H5)4 (99.999%), Ca(NO3)2xH2O (99.99%),
and Mg(NO3)26H2O (99.9%) were used. The alumina powder was mixed with the dopants in ethyl alcohol and dried at
70C. The doped powder was pressed into cylindrical compacts
and then isostatically at 100 MPa. The compacts were heated to
950C for 1 h to convert the dopant chemicals to oxides and to
remove ethyl alcohol. The compacts were then sintered and
heat-treated mostly at 1620C in air in a high-purity alumina
tube furnace. The heating and cooling rates for the sintering
treatment were 150C/min and 300C/min, respectively. The
polished surfaces of the sintered specimens were thermally
etched at temperatures about 30C lower than the sintering
temperatures for 30 min for examinations under optical and
scanning electron microscopes (SEM; Model 515, Philips,
Holland). The specimens for transmission electron microscopy
(TEM; JEM-3010, JEOL, Tokyo, Japan) were thinned by
mechanical grinding and ion-beam milling. The equivalent
sphere radii of the grains were measured by tracing on optical
micrographs using a digitizer connected to a personal computer.

III.

Vol. 85, No. 6

Results and Discussion

Because the major experimental variables in this work were the

anorthite content, the heat-treatment temperature, and time, each
specimen (without MgO) will be designated by these variables;
thus, for example, 0.15%/1620C/12 h for the specimen with
0.15% anorthite heat-treated at 1620C for 12 h. The specimen
series with the same anorthite content heat-treated at the same
temperature for different periods will be designated by its anorthite
content and heat-treatment temperature; thus 0.15%/1620C for
the series with 0.15% anorthite heat-treated at 1620C for various
periods.
When alumina was sintered at 1620C without adding any
anorthite, normal growth was observed as shown in Fig. 1. This
result agreed with previous observations.16,17,19 As exhibited in
Fig. 2 for the 0.15%/1620C series, all specimens with anorthite
showed AGG. After sintering for 5 min the specimen was quite
dense with only a few pores remaining and some large abnormal
grains appeared as shown in Fig. 2(a). The measured distributions
of the equivalent sphere sizes of the grains are shown in Fig. 3.
After 10 min (Fig. 2(b)), more large grains appeared with typical
elongated shapes as also observed previously3,18 when the impurity content (usually containing some SiO2) was relatively high.
After 20 min (Fig. 2(c)), most of the large grains impinged on each
other, but some fine grains still remained. After sintering for 1 h
(Fig. 2(d)), most of the large grains impinged on each other and
they grew slowly on further sintering for 6 h (Fig. 2(e)) and 12 h
(Fig. 2(f)). These microstructures and grain distributions showed a
typical AGG pattern.
The TEM observations showed liquid pockets at all of about 30
randomly selected grain triple junctions as exhibited in Fig. 4(a).
All grain surfaces at all triple junctions examined were either flat
or faceted with sharp edges. Although the intergranular regions
were not extensively examined, some intergranular liquid films
showed flat grain surfaces and hill-and-valley structures as exhibited in Fig. 4(b). The flat grain surface on the upper side of Fig.
4(b) might be a basal plane of that grain. These flat and faceted
grain surface shapes at the triple junctions and hill-and-valley
intergranular liquid films are consistent with a polyhedral equilibrium shape of alumina in anorthite liquid. When the anorthite
contents are relatively low, as in our specimens, portions of the
equilibrium surfaces are expected to be exposed at the triple

Fig. 1. SEM microstructure of pure alumina sintered at 1620C for 12 h.

junctions, and the grain surfaces at the intergranular regions will

have either flat or hill-and-valley shapes as shown by Kim et al.5
and Blendell et al.7
When grain surfaces and grain boundaries are singular with
orientations corresponding to the cusps in the polar plots of the
interface energy against the normal directions, they can move either
by two-dimensional nucleation of steps or on existing steps produced
by dislocations.22 For our qualitative analysis we assume the twodimensional nucleation mechanism. Because the movement of the
liquid pockets at the triple junctions can control the overall grain
coarsening kinetics, the two-dimensional nucleation process can
control the grain coarsening in defect-free materials with a liquid
phase. The predominant dependence of the two-dimensional nucleation rate R on experimental variables is given by
R D exp(G*/kT)

(1)

where D is approximately the diffusivity in the liquid and G* is

the activation energy for step nucleation given by
G*

V ms2T
hg

(2)

where Vm is the molar volume of the solid phase, s(T) the surface
step free energy per unit length, h the height of the step, and g the
driving force. The driving force for the growth g(r1) of a grain of
size r1 may be expressed as
gr 1 2V m

1
1

r
r1

(3)

where is the interfacial energy and r is the size of the grain which
neither grows nor shrinks. According to Eq. (1), R is small for
small values of g and increases rapidly as g exceeds a certain
value. If the grain size distribution is relatively narrow and r is
large, g(r1) will be small even for the largest grains. Then the
grains will undergo slow coarsening limited by the low rate of step
nucleation. We proposed13 to call such a process stagnant
growth to distinguish it from normal grain growth.
The observed AGG behavior shown in Fig. 2 appears to be
qualitatively consistent with this two-dimensional nucleation of
steps as proposed earlier.12,13 The small matrix grains undergo
slow stagnant growth, and apparently some large grains, probably
with dislocations, grow rapidly to form the abnormally large
grains.
The observed dependence of AGG on heat-treatment temperature is shown in Fig. 5. The compacts with 0.05% anorthite were
first sintered at 1500C for 12 h to obtain almost fully dense
structures with nearly uniform grain sizes. They were heat-treated

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Fig. 2. Optical microstructures of the specimens with 0.15% anorthite heat-treated at 1620C for (a) 5 min, (b) 10 min, (c) 20 min, (d) 1 h, (e) 6 h, and
(f) 12 h.

again for 12 h at higher temperatures to observe the grain growth

behavior. At 1520C, which is below the eutectic temperature
(1553C)35 of anorthite, there was some grain growth with a few
grains apparently beginning to grow abnormally as shown in Fig.
5(a). At 1560C some large grains appeared as shown in Fig. 5(b),
and at 1580C the large grains became elongated probably along
their basal planes as shown in Fig. 5(c). At 1600C all of the large
grains impinged on each other as shown in Fig. 5(d). The series of
microstructures at increasing temperatures in Fig. 5 shows that the
rates of formation of abnormal grains and their growth increase
with temperature as expected from the temperature dependences of
D and the exponential term in Eq. (1). The step free energy s(T)
is not expected to decrease substantially in this relatively small
temperature range.
Figure 6 shows a striking dependence of AGG behavior on
anorthite content at 1620C. These microstructures obtained

after heat-treating for 12 h showed the abnormal grains which

impinged on each other. The number of the abnormal grains
increased and hence their average size after the impingement
decreased with increasing liquid content as shown in Fig. 6.
This observation appears to be consistent with kinetic roughening of the abnormal grains during their growth. When a
crystal with a singular surface grows by nucleation of steps
under high driving forces, the step nucleation rate can be so
high that the singular surface can be kinetically rough as
proposed earlier.36 Such a surface is predicted to grow continuously with its rate (in a multicomponent system) determined
by diffusion flux. The growth rates of the abnormal grains can
hence be determined by diffusion in the liquid matrix and
therefore depend on the liquid volume fraction. If the grain
growth is limited by the movement of the triple junctions, its
rate will increase with decreasing size of the liquid pocket at the

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Fig. 3.

Vol. 85, No. 6

Measured equivalent sphere grain sizes of the specimens shown in Fig. 2.

Fig. 4. TEM microstructures of (a) a liquid pocket at a triple grain junction and (b) an intergranular liquid film in a specimen with 1% anorthite heat-treated
at 1620C for 10 min.

triple junctions as in other systems which undergo diffusioncontrolled Ostwald ripening.9 11 The growth of the fine matrix
grains, however, will still be limited by the rate of twodimensional nucleation and hence independent of liquid content. Because with lower liquid content, the growth rates of the
large grains relative to the smaller ones will be higher, fewer
grains will grow to larger sizes as observed in Fig. 5. The
growth behavior of the system of grains of various sizes is fairly
complex and needs to be further examined by numerical
analysis and other methods. The previous observations of AGG
in alumina during infiltration with anorthite liquid by Lee et
al.37 showed a similar dependence on liquid volume fraction
and can also be explained by diffusion-controlled growth of the
abnormal grains.
In the second part of this study, the effect of MgO addition (to
the powder mixtures) was investigated in the specimens with
varying anorthite contents. In Fig. 2 was shown a typical AGG

behavior in the 0.15%/1620C series exhibiting large grains

elongated along the basal planes. When 0.3% MgO was added to
this specimen, the grains were nearly equiaxed as shown in Fig. 7.
As shown in Fig. 8, the grain size distribution became wider with
increasing sintering time, indicating still an AGG behavior, but not
as pronounced as those for the specimens without any MgO shown
in Figs. 2 and 5. But with MgO the number density of the abnormal
grains was much larger and therefore their sizes after their
impingement were smaller than those of the specimen without any
MgO, as can be seen by comparing Figs. 2(d,e,f) and 3 to Figs. 7
and 8. When the MgO addition was increased to 1%, the abnormal
grains were more numerous and their sizes even smaller as shown
in Fig. 9. But again AGG appeared to occur as indicated by the
widening grain size distribution as shown in Fig. 10. When 0.5%
MgO was added, the grain structures were intermediate between
those with 0.3% (Fig. 7) and 1% MgO (Fig. 9). When a maximum
amount of 2% MgO was added, the grain evolution appeared to be

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Fig. 5. Optical microstructures of the specimen with 0.05% anorthite heat-treated at 1500C for 12 h and further at (a) 1520, (b) 1560, (c) 1580, and
(d) 1600C for 12 h.

Fig. 6.

Optical microstructures of the specimens with (a) 0.05%, (b) 0.15%, (c) 0.25%, and (d) 1% anorthite heat-treated at 1620C for 12 h.

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Vol. 85, No. 6

Fig. 7. Optical microstructures of the specimens with 0.15% anorthite and 0.3% MgO heat-treated at 1620C for (a) 1, (b) 6, and (c) 12 h.

Fig. 8.

Measured equivalent sphere grain sizes of the specimens shown in Fig. 7.

identical to those with 1% MgO (Fig. 9). We observed similar

effects of MgO addition when 0.1% MgO was added with 0.1%
anorthite, 0.03% MgO with 0.05% anorthite, and 2% MgO with
1% anorthite.
The TEM observations of the liquid pockets at grain triple
junctions of the 1%/1620C/10 min specimen with 2% MgO
revealed some curved grain surfaces as shown in Fig. 11(a). But
some grain surfaces still appeared to be flat at the triple junctions.
A triple junction in a specimen with 0.1% anorthite and 0.1% MgO
also showed a curved grain surface meeting with a flat segment
with apparently a discontinuous change of the slope. Out of about
40 triple junctions examined in the specimens with MgO, 4 of
them showed curved grain surfaces as shown in Fig. 11(a), while
the rest still showed only faceted or flat grain surfaces. A liquid
film in the specimen with 1% anorthite and 2% MgO showed a
curved grain surface on one side and a hill-and-valley grain surface
on the other as shown in Fig. 11(b). In contrast, the specimens
without any MgO always showed either flat or hill-and-valley
grain surfaces at the liquid pockets and films as shown in Fig. 4.
These results show that when MgO is added, the corners, edges,
and possibly some flat (singular) surfaces (in the equilibrium shape
of the alumina grains) become rounded with atomically rough
structures, while some low index surfaces, probably those with

very low surface energies like the basal planes, still remain
singular. The surface normal appeared to change discontinuously
from a curved surface segment to a flat region when observed at a
triple junction as described earlier, and such a discontinuous
surface slope change is consistent with the hill-and-valley structure
of a grain surface shown in Fig. 11(b) between two grains. If some
grain surface segments are singular, they will move by twodimensional nucleation of steps. Because the movement of the
singular surface segments is likely to control grain coarsening,
AGG can still occur even with partial roughening of some surface
segments. But with the roughening at the corners and edges, the
areas of the surfaces that still remain singular will decrease. This
means that the step free energies of those singular surfaces also
decreased approximately in proportion to their decreasing radii.27,38 In phenomenological theories,39,40 the surface roughening
induced by additives was attributed to the decrease of step free
energy caused by segregation at the edges of the steps. The MgO
segregation at the nonbasal planes apparently decreased their
surface energies sufficiently to make the grains nearly equiaxed. It
is possible that the effect of MgO is that of nullifying the effects
of CaO and SiO2, which appear to increase the anisotropy of the
interfacial energy and produce singular interfaces.

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1591

Fig. 9. Optical microstructures of the specimens with 0.15% anorthite and 1% MgO heat-treated at 1620C for (a) 1, (b) 6, and (c) 12 h.

Fig. 10.

Measured equivalent sphere grain sizes of the specimens shown in Fig. 9.

If the step free energies of these remaining singular surfaces are

reduced by MgO addition, the activation energy for step nucleation
is reduced in accordance with Eq. (2). Therefore, for a certain grain
size distribution, the number of grains which can grow rapidly is
expected to increase when MgO is added. The increased number
density of the abnormal grains with MgO addition shown in Figs.
7 and 9 is thus consistent with the decrease of step free energy,
which is indicated by the curved grain surfaces. As noted earlier,
further increase of the MgO content did not cause any change of
the grain growth behavior, indicating that there is a limit to the
decrease of the step free energy with increasing MgO content. It
thus appears to be impossible to roughen all alumina surfaces in
contact with anorthite liquid by adding more MgO. If all alumina
surfaces become rough, all grains can grow continuously and
hence normal growth will occur. When 1% MgO was added with
0.15% anorthite, the step free energy apparently became so small
that most of the large grains could grow continuously, closely
resembling the normal growth as shown in Fig. 9. As proposed
earlier by Yoon et al.,13 AGG behavior can approach normal
growth, if the number density of the abnormal grains is increased
by the reduction of step free energy, which can be induced either
by temperature increase or by an additive like MgO in alumina.

As shown in Fig. 6, the number density of the abnormal grains

substantially increased with increasing anorthite liquid content.
This can arise from the diffusion-controlled growth of the abnormal grains as proposed earlier in this paper. If there is an increase
of the liquid volume fraction with MgO, it can likewise increase
the number density of the abnormal grains. But it was indicated
previously4,41 that the MgO addition can actually decrease the
amount of SiO2-rich liquid because of increased solubility in
alumina. Changes of liquid diffusivity and grainliquid interface
energy with MgO addition can also alter the AGG behavior, but
such a drastic change of the AGG behavior from Figs. 2(d), (e),
and (f) to Figs. 9(a), (b), and (c) appears to occur predominantly
from the partial grain surface roughening.
The surface roughening and the suppression of AGG induced by
MgO addition in alumina is analogous to similar changes in
NbCFe induced by temperature increase or B addition.21 But in
NbCFe the grain shape changes from cubic to spherical by the
roughening transitions could be readily observed because of much
larger liquid volume fraction (on the order of 20%) and the
interface roughening was so complete that the grains became
spherical and the grain coarsening completely normal.21 It should
also be noted that the MgO addition caused both grain surfaces in

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Vol. 85, No. 6

Fig. 11. TEM microstructures of (a) a liquid pocket at a triple grain junction and (b) an intergranular liquid film in a specimen with 1% anorthite and 2%
MgO heat-treated at 1620C for 10 min.

contact with vapor and grain boundaries (which were made

singular by CaO and SiO2) to become completely rough.19,42 The
roughening effect of MgO thus appears to be quite general for all
types of alumina interfaces.

IV.

Conclusions

By observing the shapes of the grain surfaces at grain triple

junctions and intergranular liquid films, it was possible to relate
the interface atomic structure to grain growth behavior in
alumina with anorthite liquid. If the singular interfaces move by
step nucleation, AGG can occur because only a few large grains
can grow rapidly by kinetic roughening of their interfaces. The
striking dependence of AGG behavior on the anorthite content
is consistent with the possibility that the rapid growth of abnormally large grains is controlled by diffusion in liquid matrix. The
grainliquid interfaces became partially rough by MgO addition
and observed increase of the number density of the abnormal
grains with MgO content is consistent with decrease of the step
free energy. All observations can thus be qualitatively explained
by the step nucleation theory. We are currently carrying out a
detailed numerical analysis of the model to compare with these
observations.
It is possible that dislocations and other surface defects can
influence the growth behavior and particularly the stagnant growth
at relatively low driving forces. But the relationship between the
growth rate and the driving force will still be nonlinear and hence
AGG can occur if the interfaces are singular.
In this work it was shown that AGG in alumina with anorthite
liquid can be nearly suppressed by adding MgO. Earlier, we have
shown that AGG in alumina doped with CaO and SiO2 at relatively
low concentrations to avoid liquid formation could be completely
suppressed by adding MgO.19 With or without a liquid phase the
suppression of AGG was ironically achieved by enhancing the rate
of forming large grains. This work is another example which
showed that there is a gradual change from AGG to normal
growth, which may be regarded as the limit of AGG where all
grains can continuously grow with no energy barrier to step
nucleation. Another general strategy for suppressing AGG in
practice can be to prolong the stagnant growth period by decreasing the heat-treatment temperature or using additives to increase
the step free energy. Indefinite stagnant growth might also be
achieved by increasing the initial average grain size above a
critical value.

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