Materials Sciences and Applicatio n, 2011, 2, 758-764
doi:10.4236/msa.2011.27104 Published Online July 2011 (http://www.SciRP.org/journal/msa)
Particle Size Control, Sinterability and
Piezoelectric Properties of BaTiO3 Prepared by a
Novel Composite-Hydroxide-Mediated Approach
Yahong Xie1,3, Takesi Kimura1, Shu Yin1, Takatoshi Hashimoto2, Yuichi Tokano2, Atsushi Sasaki2,
Tsugio Sato2
1Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Japan; 2NEC Tokin Corporation, Koriyama,
Taihaku-ku, Japan; 3Xin Jiang University, Urumqi, China.
Received Feburary 18th, 2011; revised March 9th, 2011; accepted March 21th, 2011.
ABSTRACT
The size of BaTiO3 particles was controlled by adjusting the molar ratio of the starting materials (BaCl2 + TiO2) to
mineralizer (NaOH + KOH) during a composite-hydroxide-mediated approach using a novel hydrothermal reaction
apparatus with a rolling system. The mean particle diameter decreased from 500 to 50 nm with a decrease in the (BaCl2
+ TiO2)/(NaOH + KOH) molar ratio from 0.44 to 0.04. The powders were sintered by normal one-step sintering at
1200˚C for 5 h and two-step sintering in which temperature was raised to 1200˚C at first and then decreased to 1100˚C
and kept at 1100˚C for 5 h. The BaTiO3 particles prepared with the (BaCl2 + TiO2)/(NaOH + KOH) molar ratio of 0.32
and 0.22 showed excellent sinterability and could be sintered to almost full theoretical density by both method. The sin-
tered bodies obtained by both methods showed similarly excellent dielectric and piezoelectric properties.
Keywords: BaTiO3, Synthesis, Low Temperature Sintering, Piezoelectric Properties
1. Introduction
The excellent dielectric and ferroelectric properties of
barium titanate make it attractive material in the field of
electrceramic and microelectronics. However, the con-
ventional synthetic methods for BaTiO3 involves calcina-
tion of a BaCO3 and TiO2 powder mixture above 1200˚C,
and thus often results in polydispersity and the introduc-
tion of impurities and the powders prepared by this
method consist of non-uniform and coarse particles [1-3].
To overcome these deficiencies, a number of innovative
synthesis methods and chemical prcedures have been
developed [4-7]. Among them, the composite-hydroxide-
mediated (CHM) approach has been considered as an
effective method to synthesize high purity BaTiO3
[8-10].
In the present research a novel ball-milling assisted
hydrothermal reaction was used to promote the diffusion
of chemical species for a higher reaction rate as well as
the uniformity of the product [11-12]. By combining with
the addition of a Li2CO3 and V2O5 mixed sintering addi-
tive [13-16], BaTiO3 could be sintered to almost full
theoretical density at a low sintering temperature of
1200˚C for 5 h.
The tendency of the electronic industry towards mini-
aturization leads to high interest in fabricating some ma-
terials with nanometer-scale structure. The conventional
sintering prcesses are generally accompanied by rapid
grain growth, which has greatly hampered efforts to
produce dense materials with nanometer-scale structure.
Two-step sintering is a promising approach to obtain
dense nanograin ceramics because it suppresses grain
growth in the final stage of sintering. The two-step sin-
tering prcedure consists of the following two steps: (1) at
first step, sintering at a constant rapid heating rate until a
normal sintering temperature; (2) lowering the tempera-
ture by ca.100˚C afterwards followed by sintering at a
lowered temperature until it is fully dense. In this paper,
two-step sintering approach is used to densify the pre-
pared BaTiO3 ceramics at low temperature [17-19].
2. Experimental
2.1. Synthesis Techniques
A mixture of 460 mmol of anhydrous hydroxides (NaOH/
KOH molar ratio = 51.5:48.5) was put into a Teflon®-

Particle Size Control, Sinterability and Piezoelectric Properties of BaTiO Prepared by a Novel 759
3
Composite-Hydroxide-Mediated Approach
lined stainless steel autclave with 100 cm3 of internal
volume and a 5.5 cm outer diameter, followed by the
addition of 100, 75, 50, 30, 10 mmol of BaCl2 and TiO2
(anatase) with ten Teflon® balls, 1.1 cm in diameter.
Then, the autclave was sealed and placed in an electric
oven and heated at 200˚C for 24 h with a rotation speed
of 100 rpm during the reaction. After the reaction, the
autclave was taken out to allow to cool down to room
temperature. The product was dispersed in deionized
water to remove the hydroxide on the surface of the par-
ticles, then centrifuged and rinsed with ethanol, deion-
ized water and acetone, three times, respectively. Finally,
the obtained powders were dried overnight at 60˚C in a
vacuum oven.
The prepared BaTiO3 powders and commercial Ba-
TiO3 powders (Sakai Chemical Industry Co., BT-05,
which is considered the best commercial pure BaTiO3
having excellent properties) were precalcined at 800˚C
for 1 h followed by mixing well with 0.3 wt% Li2CO 3
and 0.04 wt% V2O5 powder by a wet-ball milling with
acetone and ZrO2 balls of 10 mm in diameter in a Tef-
lon® container at a rolling rate of 90 rpm for 12 h, re-
spectively. Then, the powders were collected, dried and
uniaxially pressed at 20 MPa in a steel die to form pellets,
20 mm in diameter and 3 mm thick, and then isostatically
pressed at 200 MPa. The pellets were then sintered by
normal one-step sintering at 1200˚C for 5 h which was
designated as (1200/5) with a heating rate of 10˚C/min.
The two-step sintering designated as (1200/1100/5) was
also conducted, in which the sample was heated at first
from room temperature to the first sintering temperature
T1 (1200˚C) with a heating rate of 10˚C/min, then the
temperature was held at 1200˚C for 1 min, after that rap-
idly decreased to T2 (1100˚C), and held at T2 for 5 h, as
illustrated in Figure 5 (insert). The densities of the sin-
tered pellets were measured by the Archimedes’ methods.
The rectangular bars of 2 mm × 4 mm × 12 mm were
prepared for piezoelectric measurements. Gold paste was
fired on both sides of the disks at 800˚C as electrode. The
specimens were poled in a stirred silicon oil at 80˚C by
applying DC electrical fields of 2 - 3 kV/mm for 30 min.
About 24 h later of the poling, the dielectric and piezo-
electric properties were measured using an Agilent 4294
A precision impedance analyzer at a frequency of 100
kHz.
2.2. Characterizations
The X-ray diffraction (XRD) analysis of the obtained
powder samples was carried out using CuK radiation
with a pyrolytic graphite monchromator mounted on a
powder diffractometer (Shimadzu XD-D1). Thermogra-
vimetric analysis (TG-DTA, Rigaku, TG8101D) was
performed for the powders from room temperature to
1200˚C with a heating rate of 10˚C/min in air. The parti-
cle morphology and the microstructures of the sintered
bodies were observed by a scanning electron microscope
(SEM; Hitachi S-4100).
3. Results and Discussion
3.1. Crystalline Phase
Figure 1 shows the XRD patterns of the BaTiO3 powders
synthesized by the composite-hydroxide-mediated ap-
proach at 200˚C for 24 h with the molar ratio of starting
materials (BaCl2 + TiO2) to mineralizer (NaOH + KOH)
of (A) 0.44, (B) 0.32, (C) 0.22, (D) 0.12, (E) 0.04. The
peaks of (002) and (200) around 2θ = 45.5˚ were en-
larged in the insert to compare the powder tetragonality.
All peaks of the synthesized powders were consistent
with the single perovskite phase. The slight peak splitting
around 2θ = 45.5˚ to (002) and (200) suggested the for-
mation of the tetragonal BaTiO3. The tetragonality (c/a)
decreased from 1.0055 to 1.0038, 1.0032, 1.0025 and
1.0013 with a decrease of the (BaCl2 + TiO2)/(NaOH+
KOH) molar ratio from 0.44 to 0.32, 0.22, 0.12 and 0.04,
respectively, which probably due to the difference in the
particle size, since the tetragonality (c/a) of barium titan-
ate is strongly dependent on particle size.
3.2. Thermal Analysis
The TG-DTA curves of the samples are shown in Figure
2. All samples showed three steps of weight losses. The
weight loss up to 200˚C, 200˚C - 800˚C and above 800˚C
may be due to the elimination of water adsorbed on the
surface, dehydration from the OH incorporated in the
lattice and elimination of CO2 from the contaminated
BaCO3, respectively. The weight losses of the present
samples were much smaller than those prepared by con-
ventional hydrothermal reactions [24], especially the
samples with the (BaCl2 + TiO2)/(NaOH + KOH) molar
ratio of 0.32 and 0.22 showed quite little weight losses of
ca.1.05 and 1.30%, respectively, indicating formation of
high purity stoichiometric BaTiO3 powder. According to
the TG-DTA curves, the powders were calcined at 800˚C
for 1 h prior to the sintering.
3.3. Morphology of the Powders
Figure 3 shows the morphologies of the prepared Ba-
TiO3 powders together with those of commercial BaTiO3
powders. All samples showed high quality crystal char-
acteristics of cubes or tetrahedrons. The average particle
size of BaTiO3 prepared in the present study decreased as
400, 200, 100, 60 and 50 nm with a decrease in the
(BaCl2 + TiO2)/(NaOH + KOH) molar ratio as 0.44, 0.32,

Particle Size Control, Sinterability and Piezoelectric Properties of BaTiO Prepared by a Novel 760 3
Composite-Hydroxide-Mediated Approach
Figure 1. XRD patterns of the samples prepared with the (BaCl2 + TiO2)/(NaOH + KOH) molar ratio of (A) 0.44, (B) 0.32, (C)
0.22, (D) 0.12 and (E) 0.04.
Figure 2. TG-DTA curves of the samples prepared with the
(BaCl2 + TiO2)/(NaOH + KOH) molar ratio of (A) 0.44, (B)
0.32, (C) 0.22, (D) 0.12 and (E) 0.04.
0.22, 0.12 and 0.04 (Figure 3 A, B, C, D and E), respec-
tively. The samples A and B showed broad size distribu-
tion from 50 to 500 nm. In contrast, the samples C, D and
E showed relatively narrower size distribution of 30 to
100 nm. Generally, in the solution prcess the formation
of nuclei and growth of crystals cur. When the (BaCl2 +
TiO2)/(NaOH + KOH) molar ratio is low, the
Figure 3. SEM images of the samples prepared with the
(BaCl2 + TiO2)/(NaOH + KOH) molar ratio of (A) 0.44, (B)
0.32, (C) 0.22, (D) 0.12, (E) 0.04 and (F) commercial Ba-
TiO3.
formation rate of BaTiO3 is slow, therefore, the BaTiO3
crystals grow from the initially produced nuclei without

Particle Size Control, Sinterability and Piezoelectric Properties of BaTiO Prepared by a Novel 761
3
Composite-Hydroxide-Mediated Approach
agglomeration because of the high viscosity of the
NaOH/KOH melt, resulting in final nanostructure with
narrow size distribution (sample C, D and E). On the
other hand, at higher molar ratio (sample A and B) since
the formation rate of BaTiO3 is fast, the nuclei are
formed not only in the initial stage but also in the middle
stage of the reaction, and the agglomeration of particles
and grain growth tends to prceed due to the decrease of
the viscosity because of the formation of water as shown
by Eq. (1).
BaCl2 + TiO2 + 2NaOH = BaTiO3 + 2NaCl + H2O (1)
Therefore, the product consisted of larger crystals with
a large particle distribution. These results indicate that
the lower (BaCl2 + TiO2)/(NaOH + KOH) molar ratio
seems to be beneficial to obtain a narrower size distribu-
tion as well as a smaller particle size. Comparing with
the commercial BaTiO3 particles showing irregular phase
with average particle size of ca. 400 - 500 nm (Figure 3.
F), BaTiO3 powders prepared in the present study exhib-
ited a smaller average particle size (Sample C, D and E)
and a regular cubical shape.
3.4. Sinterablity
The sample powder was sintered at 1200˚C for 5 h with a
heating rate of 10˚C.min–1 with a 0.3 wt% Li2CO3 and
0.04 wt% V2O5 complex sintering additive. The relative
densities and grain sizes of the sintered bodies are shown
in Figure 4 as a function of the (BaCl2 + TiO2)/
(NaOH + KOH) molar ratio. The average grain size
changed as 10 μm, 25 μm, 20 μm, 8 μm and 5μm for the
samples with the (BaCl2 + TiO2)/(NaOH + KOH) molar
ratio of 0.44, 0.32, 0.22, 0.12 and 0.04. The samples with
the (BaCl2 + TiO2)/(NaOH + KOH) molar ratio of 0.32
and 0.22 could be sintered to almost full theoretical den-
sity (> 98%), but the density of other samples were less
than 94%. From Figure 4, it is seen that the powder pre-
pared with the (BaCl2 + TiO2)/(NaOH + KOH) molar
ratio of 0.22 possessed the highest sinterability in the
present samples. These results agreed with the results
that the sample showed the high purity, small particle
size and uniform particle size distribution (Figures 2 and
3).
Morphology of Ceramics Bodies
Figure 5 showed the scanning electron micrographs of the
fracture surfaces of the sintered bodies by normal one-step
sintering (1200/5) and two-step sintering (1200/1100/5)
using the powders with the (BaCl2+ TiO2)
/(NaOH + KOH) molar ratio of 0.22 without and with a
0.3 wt% Li2CO3 and 0.04 wt% V2O5 complex sintering
additive. For comparison the morphology of sintered bod-
ies using the commercial BaTiO3 powder are also shown.
Figure 4. Relative densities and grain sizes of the BaTiO3
ceramics sintered at 1200˚C for 5 h using a 0.3 w t% Li2CO3-
0.04 wt% V2O5 mixed sintering additive as a function of the
(BaCl2 + TiO2)/(NaOH + KOH) molar ratio.
Figure 5. SEM images of the polished surfaces of the sintered
bodies.A, B, C, D: BaTiO3 with the (BaCl2 + TiO2)/(NaOH +
KOH) molar ratio of 0.22., E, F, G, H: commercial BaTiO 3, A,
E: two-step sintering (1200/1100/5) without additive, B, F:
two-step sintering (1200/1100/5) with a 0.3 wt% Li2CO3-0.04
wt% V2O5 mixed sintering additive, F, G: one-step sintering
(1200/5) without additive, D, H: one-step sintering (1200/5)
with a 0.3 wt % Li2CO3-0.04 wt% V2O5 mixed sintering addi -
tive.

Particle Size Control, Sinterability and Piezoelectric Properties of BaTiO Prepared by a Novel 762 3
Composite-Hydroxide-Mediated Approach
Table 1. Density, grain size and dielectric and piezoelectric properties of the BaTiO3 samples prepared with the (BaCl2 +
TiO2)/(NaOH + KOH) molar ratio of 0.22 and commercial BaTiO3 sintered by the normal one-step sintering (1200/5) and
two-step sintering (1200/1100/5).
Prepared BaTiO3 Commercial BaTiO3
Two-step sintering
(1200/1100/5)
One-step sintering
(1200/5)
Two-step sintering
(1200/1100/5)
One-step sintering
(1200/5)
Without additive With additive Without
additive With additiveWithout additive
With addi-
tive
Without
additive
With
additive
Density/% 98.1 96.3 99.1 98.3 89.6 97.4 90.2 96.8
Grain size /μm 1 15 5 20 0.5 30 1 80
T
33 0
/


(100KHz) 1785 1256 1668 1274 2478 1452 3081 1074
Qm (-) 476 245 584 749 106 811 123 221
kp (-) 0.27 0.29 0.29 0.38 0.16 0.32 0.18 0.34
E
11
S (pm2/N) 8.03 4.8 8.0 7.9 15.0 6.3 17.2 7.3
k31 (-) 0.16 0.26 0.19 0.21 0.05 0.15 0.13 0.20
d31 (pC/N) 56.8 63.5 68.9 67.2 31.4 48.7 46.9 59.0
d33 (pC/N) 173 152 226 181 154 183 168 180
tan δ (%) 0.31 0.96 0.38 0.68 1.13 2.21 0.24 0.40
Although it was difficult to densify the comercial powder
without sintering aid by both sintering prcess (Figure 5
E and G), where the mean grain sizes of the sintered
bodies by two-step sintering and one-step sintering were
0.5 and 1 μm, respectively, the prepared BaTiO3 could be
densified without sintering aid (Figure 5 A and C),
where the mean grain sizes of the sintered bodies by
two-step sintering and one-step sintering were 1 and 8
1μm, respectively. It can be observed that the average
grain sizes of the samples prepared by the two-step sin-
tering were smaller than those by normal one-step sin-
tering. Additionally, the addition of a 0.3 wt% Li2CO3
and 0.04 wt% V2O5 complex sintering additive greatly
increased the average grain size and decreased the poros-
ity, especially in the case of the commercial powder.
3.5. Dielectric Properties of Ceramics Bodies
The relative density, grain size, dielectric constant (ε),
dielectric loss (tan
δ ), piezoelectric constant (d31, d33, k31,
S11), mechanical quality factor (Qm) and electr˚Chemical
coupling factor (kp) of the BaTiO3 samples prepared with
the (BaCl2 + TiO2)/(NaOH + KOH) molar ratio of 0.22
and commercial BaTiO3 sintered by the normal sintering
(1200/5) and two-step sintering (1200/1100/5), respec-
tively, are listed in Table 1. All samples could be sin-
tered to almost full theoretical density using a 0.3 wt%
Li2CO3 and 0.04 wt% V2O5 complex sintering additive,
and the dielectric properties of the sample prepared by
the one-step sintering and two-step sintering did not
change so much, indicating that the two-step sintering is
useful to decrease the sintering temperature without loss
of the dielectric properties. It is notable that the samples
using prepared BaTiO3 powders showed lower dielectric
constant and larger piezoelectric constant than those
prepared using the commercial powder, this result can be
illustrated by the grain size effect and the dielectric con-
stant at room temperature decreased with increasing
mean grain size from grain size of 1μm (GS > 1 μm), but
below 1 μm, dielectric constant at room temperature de-
creased with decreasing the mean grain size for the same
sample. Comparing with the samples sintered without
sintering additive, it can be seen that the addition of sin-
tering additive decreased the dielectric constant at the
room temperature, increased dielectric loss and changed
the piezoelectric properties for the specimens sintered by
both one-step sintering and two-step sintering.
4. Conclusions
The size of BaTiO3 particles was controlled by adjusting
the (BaCl2 + TiO2)/(NaOH + KOH) molar ratio during a
composite-hydroxide- mediated approach using a novel
hydrothermal reaction apparatus with a rolling system.
The mean particle diameter decreased from 500 nm to 50
nm with the decrease of the (BaCl2 + TiO2)/(NaOH+KO
H)molar ratio from 0.44 to 0.04, where the sample with
the molar ratio of 0.22 exhibited the excellent sinterabilty
and dielectric properties due to the small particle size,
uniform morphology and narrow size distribution. The
two-step sintering was useful to decrease the sintering
temperature and to obtain the mean grain size without
loss of the dielectric properties.
5. Acknowledgements
This research was partially supported by the Ministry of
Education, Culture, Sports, Science and Technology,
“Special Education and Research Expenses, Post-Silicon
Materials and Devices Research Alliance” and G-COE
program “International Center of Research & Education

Particle Size Control, Sinterability and Piezoelectric Properties of BaTiO Prepared by a Novel 763
3
Composite-Hydroxide-Mediated Approach
for Molecular Complex Chemistry (IREMC)”.
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