ARTICLES

Sintered compacts of nano and micron-sized BaTiO3:

Dramatic influence on the microstructure and
dielectric properties
Vishnu Shanker and Tokeer Ahmad
Department of Chemistry, Indian Institute of Technology, Hauz Khas, New Delhi 110016, India
Henry Ip
Department of Chemistry and Biochemistry, Center for Materials Research and Education,
Rowan University, Glassboro, New Jersey 08028
Ashok K. Gangulia)
Department of Chemistry, Indian Institute of Technology, Hauz Khas, New Delhi 110016, India

(Received 16 April 2005; accepted 3 October 2005)

Sintered compacts of nano-sized and micron-sized BaTiO3 show sharp ferroelectric

transition and high dielectric constant at specific compositions. The sintered compacts
with 1 wt% nano-BaTiO3 show a maximum dielectric constant of 1680. At the
transition temperature (Tc) there are two maxima at 0.5 and 2 wt%. The variation in
the dielectric constant at Tc is also reflected in the behavior of the ferroelectric
transition as studied by differential scanning calorimetry. This interesting oscillatory
variation of the dielectric constant and dielectric loss with increase in the amount of
nanoparticles in the sintered compacts is observed for the first time. The variation of
the dielectric properties and the ferroelectric transition of the sintered compacts could
be related to subtle changes in the microstructure.

I. INTRODUCTION disperse nanoparticles of BaTiO3 could be obtained

BaTiO3 has been the cornerstone of research in elec-
tronic materials due to its stability (chemical and me-
chanical) and wide ranging applications as a ferroelectric
material.1–4 Added to the unique properties is its simple
structure (perovskite), which allows new theoretical
models to be developed and the results to be compared
with experimental data.
The dielectric properties of BaTiO3 depends on several
factors, like the structure, grain size, temperature, etc.5–7
At room temperature, BaTiO3 has a tetragonal structure
that changes to cubic at the ferroelectric transition tem-
perature. However the structure also changes with grain
size and smaller grains lead to a cubic structure. The
properties of BaTiO3 (micron-sized grains) have been
discussed in detail in many reports.1,2,8–10 More recently
the synthesis and properties of nanocrystalline barium
titanate has been of interest. Fine particles of barium
titanate have been synthesized by the sol-gel11,12 and
polymeric precursor routes.13–16 Uniform and mono-
a)
Address all correspondence to this author.
e-mail: ashok@chemistry.iitd.ernet.in
DOI: 10.1557/JMR.2006.0102
using microemulsions at low temperature of 800 °C.17
Evidence for tetragonal distortion has been found in
these nano-sized (20–25 nm) particles of barium titanate
from careful x-ray diffraction studies as well as from
Raman spectroscopy. The grain size shows an increase
on sintering being 35 nm at 900 °C to 120 nm at 1100 °C,
which is much lower than the grain size (0.5–1 ␮m)
obtained at this temperature by the normal solid-state
route. The dielectric constant depends on sintering tem-
perature and is found to increase from 210 (900 °C sin-
tering) to 520 (1100 °C sintering) at 100 kHz. It is known
that well-sintered barium titanate is normally prepared
at temperatures of ∼1350 °C. The grain size is around
2–4 ␮m in these solids. The dielectric properties of
barium titanate improve with larger grain sizes and less
grain boundaries. In an attempt to see the effect of the
nanoparticles on the dielectric properties of barium titan-
ate, we embarked on a study of the dielectric properties
of sintered mixtures of nano- and micron-sized particles
of barium titanate (in varying weight percent). Although
chemically both the components (the nanoparticles and
the micron-sized particles) are same (BaTiO3) and hence
the term “composite” may not be exactly correct, and the
phrase “sintered compacts” may be more accurate; how-
ever, for simplicity we will use this term in this paper.

816 J. Mater. Res., Vol. 21, No. 4, Apr 2006 © 2006 Materials Research Society
V. Shanker et al.: Sintered compacts of nano and micron-sized BaTiO3: Dramatic influence on the microstructure and dielectric properties

We believe this is the first report of such a study of

sintered compacts containing nano-BaTiO3. Here, we
discuss the microstructure, thermal studies, and dielectric
properties of the sintered composites of nano- and micron-
sized BaTiO3.

II. EXPERIMENTAL
Composites of barium titanate were prepared by mix-
ing nano- (∼30 nm) and micron-sized (2 ␮m) barium
titanate and heating them to obtain sintered compacts by
the solid-state route. The starting materials, nano and
bulk (micron-size) barium titanate were synthesized by FIG. 1. Powder x-ray diffraction pattern of (a) nano barium titanate
the reverse micellar route17 and the solid-state route,3,4 and (b) bulk barium titanate prepared by reverse micellar route and
respectively. Bulk barium titanate was prepared by using solid-state route, respectively.
Ba(NO3)2 and TiO2. The stoichiometric amount of reac-
tants was homogenized and then loaded in recrystallized
alumina crucible and heated at 900 °C for 15 h in a III. RESULTS AND DISCUSSION
programmable furnace. The powder was further heated Bulk barium titanate (micron-sized) was synthesized
after intermittent grinding at 1000 °C for 14 h. The de- by the solid-state method at 1000 °C for 14 h with in-
tails of the synthesis of nano-BaTiO3 is given else- termittent grinding to obtain a pure phase of BaTiO3
where.17 Different weight percents of nano and bulk (Fig. 1). The nano-BaTiO3 (30 nm) was obtained by the
barium titanate were taken to synthesize the composites reverse micellar route as reported earlier.17 The nano-
of BaTiO3. The well-ground powder of nano and bulk BaTiO3 shows very weak tetragonal distortion as the 002
barium titanate, homogenized in agate mortar pestle was and 200 reflections merge in the PXRD [Fig. 1(a)]. How-
loaded in recrystallized alumina crucibles and sintered at ever careful analysis of these reflections using slow scan
1100 °C for 12 h. The composites were characterized by shows the weak tetragonal distortion.17 The bulk BaTiO3
powder x-ray diffraction (PXRD), differential scanning shows clear tetragonal distortion [Fig. 1(b)]. Composites
calorimetry (DSC), and scanning electron microscopy of BaTiO3 were synthesized by solid-state method by
(SEM). PXRD studies of the composites containing taking different weight ratios of nano-BaTiO3 and bulk
nano-BaTiO3 were carried out after every heating stage BaTiO3. The above mixture was sintered at 1100 °C for
on a Bruker D8 Advance x-ray diffractometer (Karls- 12 h. Powder x-ray patterns were taken of all composites
ruhe, Germany) with a step size of 0.03° and a scan speed to check for any impurity phase. It was found that all the
of 1 s per step in the 2␪ range of 10° to 70°. Powdered composites (0.25% to 30% by weight of nano-BaTiO3)
samples of bulk barium titanate and composites were could be indexed on the basis of a tetragonal cell, as
treated with 5% aqueous solution of polyvinyl alcohol known for barium titanate, a ⳱ b ∼ 3.99 Å and c ∼ 4.03 Å
(PVA) and then compacted into disks at the pressure of (Fig. 2).
8–9 tons. These disks were sintered at 1100 °C for 12 h.
Scanning electron micrographs (SEM) was obtained on
the sintered disks using a Cambridge Stereoscan 360
electron microscope (Cambridge, UK) to study the grain
size and morphology of the sample. The refined lattice
parameters were obtained by a least-squares fit to the
observed d-values. The DSC measurement was carried
out of all samples using TA Instruments Q600 SDT
(New Castle, DE) at the ramp rate 10 °C per minute in N2
atmosphere (flow rate 100 ml/min). The dielectric prop-
erties were studied on sintered pellets (with coated silver
as electrodes) using an HP 4284L LCR meter (Santa
Rosa, CA) in the frequency range of 50–500 kHz in the
temperature range of 25–300 °C. The density of sintered
pellets of pure barium titanate and composites of barium
FIG. 2. Powder x-ray diffraction pattern of composites of barium
titanate was measured using the Archimedes method. titanate containing different wt% of nano-BaTiO 3 as follows:
The measured density varied between 94% and 96% of (a) 1 wt%, (b) 1.5 wt%, (c) 2 wt%, (d) 2.5 wt%, (e) 3 wt%, (f) 5 wt%,
the theoretical density. (g) 10 wt%, (h) 20 wt%, and (i) 30 wt%.

J. Mater. Res., Vol. 21, No. 4, Apr 2006 817

V. Shanker et al.: Sintered compacts of nano and micron-sized BaTiO3: Dramatic influence on the microstructure and dielectric properties

1620 to 1100 °C in the nanoparticles of BaTiO3 is prob-

ably a bit unreasonable to expect as discussed later in our
DSC studies. On the other hand, it is possible that due to
excessive surface area and highly curved surfaces, the
surface diffusion mechanism becomes more prominent in
nano particles.23 Another possibility may be the presence
of a weak surface melting transition or grain boundary
stress induced amorphization.24,25 High densification in
nanoparticles may also be due to accelerated sintering
by solid state processes. The particles are much larger
(5–10 ␮m) and are densely packed in the composites of
barium titanate [Fig. 4(a)] compared to that of pure
micron-sized BaTiO3 [Fig. 4(b)]. The composites of
higher weight percent (2.5–3.0) of nanoparticles have
more spherical edges, and we can also clearly see neck
formation in these composite nanopowders [Fig. 5(a)].
The grains appear to diffuse together with further in-
crease in the weight percent of nanoparticles. The sign of

FIG. 3. Scanning electron micrograph of (a) bulk barium titanate and

(b) composite with 1 wt% of nano-BaTiO3.

SEM images were recorded on fracture surfaces of the

sintered disks. SEM studies show dramatic changes in
the morphology and grain size in the BaTiO3 composites
as compared to the bulk BaTiO3. Figure 3(a) shows the
micrograph of bulk barium titanate. A very uniform
surface with no sign of melting is clearly discernible.
Pure BaTiO3 (bulk) is known to have a melting tempera-
ture of 1620 °C. Thus the sintering in these micron-sized
particles (carried out at 1100 °C) leads to grain coarsen-
ing by surface diffusion (instead of densification) as is
known for bulk powder.18 Note that the composite with
1 wt% of nano-BaTiO3 shows densely compacted grains
with some sign of melting at the surface [Fig. 3(b)]. This
change in the microstructure may occur due to an ease of
fusion since nanoparticles have excessively large surface
area per unit volume than bulk powder and hence high
surface energy, which lowers the melting point.19–22 FIG. 4. Closer look at the SEM of (a) composite with 1 wt% of
However such drastic lowering of the melting point from nano-BaTiO3 and (b) bulk barium titanate.

818 J. Mater. Res., Vol. 21, No. 4, Apr 2006

V. Shanker et al.: Sintered compacts of nano and micron-sized BaTiO3: Dramatic influence on the microstructure and dielectric properties

spherical edges of the grains (instead of facets) and the

larger grains observed in the composites indicate that the
increased concentration of nanoparticles in the composite
lead to ease of particle growth and sinterability. Note that
smaller grains, especially in nanometer regime show
more faceted grains due to specific faces having lower
surface energy which is important for nanoparticles
where surface effects dominate. In the absence of a melt-
ing process (as will be clear from DSC studies discussed
later) the unusual variation in the microstructure of the
composites may be explained through a solid-state sin-
tering process, which leads to an enhanced densification
at optimum amount of nanoparticles (1 wt%). There are
many mechanisms involved during a solid-state sintering
process. Among them, surface and grain-boundary diffu-
sion may be the most important processes towards den-
sification in the absence of melting. Significant grain
growth occurs mainly by grain-boundary diffusion
mechanism.26 We find that addition of minor amounts
(even 1 wt%) of nanoparticles causes considerable mi-
crostructural changes. Both experimental and simulation
studies have indicated extremely fast sintering behavior
of nanoparticles.27–31 As the amount of nano-sized
BaTiO3 increases (>3 wt%), we find a distribution of
grain sizes [Fig. 5(b)]. Note that these grains do not have
sharp faces and are also morphologically different to the
grains shown in Fig. 5(a). It appears that at high concen-
tration of nano-BaTiO3 the grain growth is not uniform
(discontinuous grain growth) and distribution of grain
size widens [Figs. 5(b) and 5(c)].
We have carried out DSC studies for all the sintered
composites. We find that apart from the ferroelectric
transition (∼120 °C, to be discussed later) there does not
appear to be any transition to suggest any melting of the
grains till 1250 °C. Hence the dramatic changes in the
morphology and grain size at particular compositions
must be related to accelerated sintering of nanoparticles
due to solid-state processes as has been earlier dis-
cussed.32 It is reported that a 1000-fold decrease in grain
size leads to a 12-fold increase in sintering rates. It may
be recalled that the microstructure for the composite with
1 wt% additive was uniquely compacted [Fig. 4(a)]. The
uniqueness of a particular ratio of nano- to micron-sized
particles reflects that packing of grains, and their con-
solidation may be a major controlling factor of the sin-
tering and morphological characteristics of such compos-
ites.
The dielectric properties of the composites also show
an interesting behavior. The dielectric constant measured FIG. 5. SEM of composite with (a) 2.5 wt%, (b) 5 wt%, and (c) 30 wt%
at room temperature shows an oscillatory behavior nano-BaTiO3.
(Fig. 6) with the maximum dielectric constant at 1 wt%.
Note that the dielectric loss is a minimum at this concen- for that composition. The oscillatory behavior is clearly
tration. It appears that this ratio of nano-sized to micron- observed with another weak maximum at ∼5 wt%.
sized grain leads to optimum densification of grains. This The measurements at the ferroelectric transition tem-
may explain the high dielectric constant and a low loss perature (∼122 °C) show a slightly modified behavior

J. Mater. Res., Vol. 21, No. 4, Apr 2006 819

V. Shanker et al.: Sintered compacts of nano and micron-sized BaTiO3: Dramatic influence on the microstructure and dielectric properties

FIG. 6. Variation of the dielectric constant (␧) and the dielectric loss
(D) in the composites with proportion of nanoparticles at 25 °C. Inset
shows a small region to emphasize the oscillatory variation of the FIG. 8. The ferroelectric transition of various composites of BaTiO3
dielectric properties. studied by DSC with the proportion of nano-BaTiO3.

(Fig. 7). The dielectric constant shows two sharp

maxima, one at 0.5 wt% and another at 2 wt% and weak
maxima at 5 wt% and 30 wt% (the weak maxima are also
observed in the room temperature dielectric plot). This
behavior of the variation of dielectric constant at the
ferroelectric transition temperature is closely mimicked
by the plots obtained by DSC measurements at low tem-
perature below 140 °C (Fig. 8). This is understandable
since the DSC measurements reflect the phase transition
and hence should be close to the property near the tran-
sition temperature. However, we find a difference in the
dielectric and the DSC studies regarding the shift in the
transition temperature. The ferroelectric transition tem-
perature as obtained from the peak position (of the di-
electric constant versus temperature plots, Fig. 9) does
not show any significant variation (122 ± 2 °C) for the
entire series of composites. The transition temperature
obtained from the DSC measurements, on the other hand, FIG. 9. Variation of the dielectric constant (␧) with temperature for
shows a shift as the concentration of nano-BaTiO3 is (a) bulk barium titanate and composites with (b) 1 wt%, (c) 1.5 wt%,
(d) 2 wt%, (e) 3 wt%, and (f) 5 wt% nano-BaTiO3.
increased. We obtain a Tc of 124 ± 3 °C and 128 ± 3 °C

for the 0.5 and 2 wt% composite, respectively (Fig. 8).

FIG. 7. Variation of the dielectric constant (␧) and the dielectric loss
(D) in the composites with proportion of nanoparticles at Tc (∼122 °C).
Inset shows a small region to emphasize the oscillatory variation of the
dielectric properties.
Interestingly, the ferroelectric transition observed by the
DSC measurement at 0.5 and 2 wt% are quite sharp with
the latter being more intense and sharper than the former.
If we look at the plot of dielectric constant versus weight
percent of nano-BaTiO3 measured at the transition tem-
perature (Fig. 7), we find the two major peaks are again
at 0.5 and 2 wt% with the latter being more intense than
the former. Thus, it appears that there is a very close
relationship in the oscillatory behavior of the dielectric
constant (at Tc) and the phase transition (ferroelectric)
studies by DSC. It is also clear from these plots (Figs. 7
and 8) that the transition is very weak for the composites
having 1.5 and 3 wt% of nano-BaTiO3. Note that all the
values of dielectric constant plotted are those obtained at
Tc. The sharpness of the ferroelectric transition is also

820 J. Mater. Res., Vol. 21, No. 4, Apr 2006

V. Shanker et al.: Sintered compacts of nano and micron-sized BaTiO3: Dramatic influence on the microstructure and dielectric properties
observed at exactly the same compositions from dielec-
tric constant studies as a function of temperature (Fig. 9).
Note that the dielectric loss starts increasing just after Tc
and shows a maxima around 250 to 275 °C for all the
composites (Fig. 10).
The oscillatory behavior of the dielectric constant, due
to the increase in weight percent of nano-BaTiO3 may be
explained by the changes in the microstructure as evident
from SEM [Fig. 4(a)]. We have earlier discussed the
SEM pictures in Figs. 4 and 5. If we look carefully, we
find that the 1 wt% composite has larger grains with very
little pores [Fig. 4(a)]. As we increase the amount of
nano-BaTiO3 (2.5–3.0 wt%) as seen in Fig. 5(a), we find
that the grains show sign of grain growth with some
spherical edges. The decrease in the dielectric constant
for these samples (2.5–3.0 wt%) may be attributed to the
formation of small amounts of amorphous regions
around the surface of bigger crystalline grains. It may be
noted that the presence of partially amorphous surfaces
will not be observed by x-ray diffraction because the
scattering from the crystalline bulk will dominate the
intensities. On further increase in concentration of nano-
particles (>5.0 wt%) the dielectric properties do not show
a significant variation.
Thus there appears to be an oscillatory variation of the
dielectric constant as a function of the nano-additive,
though it is not exactly clear as to why this variation is
oscillatory in nature. Note that the dielectric loss also
shows a similar oscillatory behavior (Figs. 6 and 7). We
believe that this behavior is linked to the porosity and
grain size of the micron-size (bulk) BaTiO3. The opti-
mum concentration of the nano-additive (for achiev-
ing high dielectric constant) would probably change if
the particle size and porosity of the bulk BaTiO3
FIG. 10. Variation of the dielectric loss (D) with temperature for
(a) bulk barium titanate and composites with (b) 1 wt%, (c) 1.5 wt%,
(d) 2 wt%, (e) 3 wt%, and (f) 5 wt% nano-BaTiO3.
J. Mater. Res., Vol. 21, No. 4, Apr 2006
changes. It may be possible that the high dielectric con-
stant at certain compositions is due to the stabilization of
oriented domain structures at those compositions. How-
ever, a study of only micron-sized BaTiO3 sample with
varying particle size and porosity (without nano-
additive) would be able to show the same effect if there
were no role for the nano-additive and needs further veri-
fication.
We observe an interesting difference between the
variation of dielectric loss with composition at room tem-
perature (Fig. 6) and at Tc (Fig. 7). In the former, the
dielectric loss is minimum for compositions having high
␧ whereas in the latter the loss varies in a manner akin to
the variation of the dielectric constant. This difference
suggests two different mechanisms of dissipation at room
temperature and at Tc.
It is interesting to note that in some studies of cluster
melting and melting of nanostructures in thin films, it has
been observed that there are certain magic numbers at
which the melting points are high, implying added sta-
bility of those nanoclusters. Oscillations of the melting
points or the heat of melting is known,33 especially in
clusters 2–4 nm in size (1,000–10,000 atoms). Our ex-
perimental studies, however involve nanoscale materials
(the BaTiO3 nanoparticles are 20–40 nm in size) and
sintered composites containing nano-BaTiO3 (which
have larger grains) and thus may have different origins
for such behavior of ordered domains. We believe our
observations are interesting to share with the scientific
community and may stimulate further experimental and
theoretical investigations on this oscillatory variation of
the dielectric constant as a function of the nanoparticle
concentration. It may be noted that there is one report34
describing a peak in the dielectric constant with respect
to the grain size and this value of the dielectric constant
was higher than the dielectric constant of a single crystal
of BaTiO3. This high dielectric constant was explained as
possibly due to domain size and stress effects in small
particles.
IV. CONCLUSION
Our studies show that addition of nano-BaTiO3 to bulk
BaTiO3 leads to microstructural changes that result in an
oscillatory variation of the dielectric properties. The op-
timal composition containing 1 wt% nanoparticles in the
composite of barium titanate leads to the highest dielec-
tric constant at room temperature. Composites of high or
low dielectric constant with variation of the additive con-
centration may be linked to the enhanced densification
by accelerated sintering due to nano-sized grains. It is
also possible that at certain optimum concentration
of nano-additive oriented domains are formed leading
to high dielectric constant. The sharpness of the ferro-
electric transition also has an oscillatory behavior as
821
V. Shanker et al.: Sintered compacts of nano and micron-sized BaTiO3: Dramatic influence on the microstructure and dielectric properties
observed by both dielectric properties (at Tc) and dif-
ferential scanning calorimetric investigations. There
appears to be a shift in the Tc shown by DSC mea-
surements, but it is not observed from the dielectric stud-
ies. Overall, we believe that packing characteristics of
micron- and nano-sized particles and enhanced sinter-
ability (through solid-state processes) of optimum con-
centration of nanoparticles lead to the observed oscilla-
tory behavior.
ACKNOWLEDGMENTS
A.K.G. thanks the Department of Science and Tech-
nology (DST), Government of India for financial
assistance. T.A. thanks the Council of Scientific and
Industrial Research (CSIR), Government of India for a
fellowship. The authors also thank the referees for con-
structive comments.
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