J Mater Sci (2019) 54:10600–10608

Ceramics
CERAMICS

Domain growth dynamics in PMN-PT ferroelectric thin

films
Jiayu Pan1,2, Tianlu Men1, Xingyu Xu1, Ze Xu1, Qi Li1, Xiang-Cheng Chu1, Yang Shen1,*,
Bing Han3,*, and Ke Wang1

1
State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University,
Beijing 100084, People’s Republic of China
2
Institute of Flexible Electronics Technology of THU, Zhejiang 314006, Jiaxing, China
3
Department of Orthodontics, Peking University School and Hospital of Stomatology & National Engineering Laboratory for Digital
and Material Technology of Stomatology & Beijing Key Laboratory of Digital Stomatology, Beijing 100081, People’s Republic of
China

Received: 26 December 2018 ABSTRACT

Accepted: 22 March 2019
Published online:
26 April 2019
 Springer Science+Business
Media, LLC, part of Springer
Nature 2019
Pb(Mg1/3Nb2/3)O3–PbTiO3 (PMN-PT) ferroelectric thin films have been widely
used in many areas due to the outstanding piezoelectric and electromechanical
properties. Although many studies have been operated on the properties and
applications of PMN-PT films, few researches focused on the domain growth
dynamics of these materials. In this paper, the domain growth dynamics of
PMN-PT thin films were investigated using piezoelectric force microscopy. The
shape and the size of the artificial domains were imaged and calculated to depict
the relationship between the imposed pulse voltage and the domain behaviors.
A linear relationship between the pulse voltage and the domain size could be
obtained before the saturation of polarization. Meanwhile, the domain size and
the duration show the logarithmic relationship, and such domain growth
dynamics were explained according to previous theories.

Introduction it plays a proper role in plenty of applications such as

Due to the attractive electrical and mechanical
properties, ferroelectric thin films have been applied
in many areas such as information storage, semi-
conductors and optical devices [1]. Among those
ferroelectric materials, Pb(Mg1/3Nb2/3)O3–PbTiO3
(PMN-PT) shows unique properties such as high
piezoelectric coefficients and ultra-high electrome-
chanical coupling factors. Based on these advantages,
ultrasonic transducer for medical imaging, elec-
tromechanical actuator and backscattering micro-
scopy [2–6].
It is widely believed that the advanced properties
such as improved piezoelectric response and poling
efficiency are attributed to the increased allowable
domain states near the morphotropic phase bound-
ary (MPB) [7–9]. The intrinsic contribution for high
piezoelectric activity in relaxor-based crystals near

Address correspondence to E-mail: shyang_mse@tsinghua.edu.cn; kqbinghan@bjmu.edu.cn

https://doi.org/10.1007/s10853-019-03563-z
J Mater Sci (2019) 54:10600–10608
MPB is related to the monoclinic phase, which affects
the ‘‘polarization rotation’’ and the anisotropy of
rhombohedral and tetragonal phases under an
applied electric field [7]. From previous works, the
phases were determined by the composition of the
PMN-PT crystals and the monoclinic phase PMN -
xPT crystals, 0.31 \ x\0.35, exhibited peak values of
piezoelectric response at compositions close to R–M
and M–T phase boundaries [7]. Thus, the composi-
tion of 0.67 Pb(Mg1/3Nb2/3)O3–0.33PbTiO3 (PMN-PT)
near the MPB is used to get investigated in this paper.
In addition, the extrinsic contributions were thought
to be an important factor for the high piezoelectric
response in relaxor-based PMN-PT crystals. A high
level of domain wall mobility was pointed out to be
responsible for the high piezoelectric response of
PMN-PT crystals [7, 10]. Thus, the investigation and
analysis of the dynamics of domain walls are
important for understanding the orientation of
piezoelectric performance and preparing PMN-PT
ferroelectric thin films with improved piezoelectric
properties [10, 11].
Piezoelectric force microscopy (PFM) has been
widely used to investigate the domain structures and
the local piezoelectric properties by applying certain
voltage on the surface of the sample via a probe. As
an efficient method, PFM contains several modes to
study ferroelectric properties. For example, in
lithography mode, it is possible to write domains as
expected by local polarization on the sample surface
[12–17]. The artificial domains could be written in a
range from 10 nm to several micrometers, and the
domains could last for hours or even years for dif-
ferent kinds of materials [18]. Since combining the
functions of imaging, tuning and recording ferro-
electric switching processes, many researches on
domains have been operated using PFM. However,
only a few studies focused on PMN-PT films, and
most of the researches focused on the properties and
its phenomenon logical interpretation. Thus, a more
comprehensive and profound study of domain
motion dynamics is needed [19–25].
In this study, artificial domains were introduced on
the 0.67 Pb(Mg1/3Nb2/3)O3–0.33 PbTiO3 (PMN-PT)
thin films by PFM and the underlying mechanism
was investigated using typical domain growth
dynamic theories. Experiment results on the domain
growth dynamics could also provide some guidance
for preparing high-quality PMN-PT thin films by
controlling and tuning the domain growth.
10601
Experiment
The PMN-PT thin films were deposited by the PLD
method. N-type Si(100) with 10 mm 9 10 mm 9
0.625 mm was used as a substrate. The Si substrate
was ultrasonically cleaned in isopropyl alcohol for
5 min. Then, the Si substrate and targets were put
into the deposition chamber, and the distance
between them was set to 55 mm. The substrate was
heated to a certain temperature under a base pressure
lower than 1.3 9 10-3 Pa. To compensate the mis-
match of crystal size between the PMN-PT and Si
substrate, buffer layers were deposited on the Si
substrate as before. The PLD target materials of an
yttria-stabilized zirconia (YSZ) were prepared by
solid-state sintering process from commercial
8 mol % Y2O3–ZrO2 powder (TZ-8YSB, Tosoh Cor-
poration, Tokyo, Japan) and were pressed into pellets
with a 20 mm diameter. The pellets were sintered in
air at 1500 C for 2 h. CeO2 powder (99.9%, Soekawa
Chemical Co., Ltd, Japan) also pressed and sintered
in air at 1450 C for 2 h. LaSrCoO3 (LSCO) target was
prepared commercial by La2O3 (99.9%, Wako Pure
Chemical Industries, Ltd, Japan), SrCO3 (99.9%, Soe-
kawa Chemical Co., Ltd, Japan) and Co3O4 (99.9%,
Kojundo Chemical Laboratory, Co., Ltd, Japan)
powders. After drying at 105 C overnight, the
powders were weighed according to the composition
ratio and mixed with ethanol. Afterward the mixture
was manually ground for 1 h using mortar and pestle
and calcined at 1300 C for 24 h. The calcined powder
was ground again and pressed into pellet. The pellet
was sintered at 1500 C for 24 h.
Film thickness was measured with a profilometer
(Dektak 3, Sloan Technology Co., Santa Barbara, CA).
The thickness of the thin film was around 200 nm.
Microscale observation was carried out by a com-
mercial PFM (MFP-3D, Asylum Research, USA).
Results and discussion
The surface topography of the deposited PMN-PT
thin film captured using PFM is shown in Fig. 1a.
Contrast was the degree of difference in depth
between the higher and lower parts. The majority
area shows a flat surface within * 4 nm fluctuations
in depth, which is suitable in size and flatness for the
followed electrical analysis using PFM. The several
white dots in the picture are believed to be impurities
10602
introduced during preparation and preservation
process. As the roughness of the surface may affect
the reception of the signals from domains during the
electrical testing process with PFM, the operations
were carried out on the flat areas away from the
white dots which may significantly affect the electric
field and then the dynamic characteristics of domain
growth [23].
In the DART mode of PFM, artificial domain
structures changed with the strength and the dura-
tion of the applied pulse voltage, which was used to
study domain growth dynamics. The method is
based on measuring the contact resonance frequency
using dual AC resonance tracking (DART), where the
amplitude and phase of the cantilever response are
monitored at two frequencies on either side of the
contact resonance. When the resonance frequency
0
changes from f0 to f0 , the difference in the amplitudes
A2 - A1 indicates the direction of the frequency shift.
Therefore, A2 - A1 can be used as the error signal in
a feedback loop where the excitation frequencies f1
and f2 are changed in order to maintain A2 - A1 & 0,
thereby tracking the resonance frequency.
The whole experiment process was divided into
three steps. In the first step, a negative voltage of 10 V
was applied to the probe tip to induce complete
polarization switching in scanned area. This voltage
was large enough for formatting a uniform polar-
ization vector and thus avoiding the effects of
inherent domain structures of the PMN-PT thin films.
Then in the second step, a pulse voltage was induced
to a certain point in the scanned area to write artificial
domains. Figure 1b shows a typical written domain
in scanned area with a fixed tip voltage = 10 V and
Figure 1 Image of surface topography of PMN-PT films using
PFM (a); fixing probe tip at a certain point to write a domain in the
scanned area by inducing a pulsed voltage (b); phase values
J Mater Sci (2019) 54:10600–10608
duration = 1 s. The white area with apparent higher
phase values ([ 100) indicated the change in polar-
ization orientation in the scanned area. The sur-
rounded light brown area with lower phase values
(* 0) proved the uniform polarization vector in first
step. In the last step, upon finishing the domain
writing process, a 1 lm 9 1 lm square area centered
with the probe tip poling location was scanned in the
DART mode of PFM to determine the phase values.
In the area, phase values of 10 9 10 points were
collected and the distribution is shown in Fig. 1c. 0
implies the polarization from the scanned area using
the negative 10 V voltage, while 180 refers to the
polarization induced by the probe tip. The two
obvious peaks of 0 and 180 indicated a complete
polarization of a certain area around the tip. That is,
the phase difference in Fig. 1b was not the ‘‘virtual
domain’’ resulted from static electricity induced from
the probe tip. The results confirm the polarization
switching during domain writing process in step two.
To understand the influence of the voltages and the
duration on the domain growth, two groups of
experiments were taken independently. The first
group featured with fixed duration (1 s) and
increasing voltages, while the other group with fixed
voltage (10 V) and increasing duration. Figure 2
shows the phase images of the first group PMN-PT
thin-film samples. The white areas were the written
domains induced by a pulse voltage in 1 s with dif-
ferent voltages. The domains presented no regular
shapes, which is uncommon according to other
studies. Rodriguez et al. [26] reported hexagonal
written domains by applying negative 10 ms voltage
pulses in LiNbO3 single crystals. Also, isotropic
collected from 100 points in a 1 lm 9 1 lm square area centered
with the probe tip (c).
J Mater Sci (2019) 54:10600–10608
written domains with cylindrical boundaries were
induced in BaTiO3 films [20]. Actually, it is believed
that PFM tip could be modeled by a charged metallic
sphere. The electric filed was determined by the
distance from the point charge to the film surface
[20]. The unique shape of the PMN-PT thin film may
be related to the 180 domain in tetragonal phase [27].
Merz et al. have calculated the 180 domain wall
energy and thickness of BaTiO3 and found that the
180 domain wall was thin and sensitive to mechan-
ical and thermal energy, which may result in the
anisotropy of domain wall energy density during
preparation and operation process [21, 27, 28].
The domain walls were distinct via the significant
color contrast in the amplitude images in Fig. 3. As
the low piezoelectric response of the domain wall, the
dark areas showed the shape of the domains clearly.
One possible reason for the roughness of domain
boundary was believed to be related to the accumu-
lation of the electrostatic charge on the margin of the
domains, which may affect the local electric filed.
Some other researches believed that the roughness
was governed by a thermally activated process. By
calculating the relative displacement of the local
variance of the wall position from an ideal flat con-
figuration, Pertsev et al. [29] reported that the shape
of domain boundaries in (Pb,La)(Zr,Ti)O3 (PLZT)
ceramics was due to minimization of the total domain
wall energy in the presence of defects pinning the
wall locally. In PZT thin films, Guyonnet et al. [30]
found that the AFM-written ferroelectric domain
Figure 2 Phase images of the first group PMN-PT thin-film samples with a fixed pulse duration = 1 s and different tip voltages: 6 V
(a),7 V (b), 8 V (c), 9 V (d), 10 V (e), 12 V (f), 14 V (g), 20 V (h).
10603
walls showed multiaffine scaling, possibly related to
the presence of dislocation defects. Although the
exact origin of the domain wall roughness in PMN-
PT ceramics is yet unknown, the intrinsic disorder
associated with substitution of Mg2? cations with
Nb5? accompanied by the formation of compensating
vacancies seemed to be the most probable reason.
Other defects caused by impurities could also
account for the rough domain wall.
In addition, some diffused phase points were
detected in written domains, which were inferred as
the relaxor ferroelectric domains. In lower voltages,
such microdomains were diffused and then got dis-
missed while the voltage was large enough to form
the distinct domain walls. It is obvious that the
domain size gradually grew with the increase in the
applied pulse voltage, and grew slowly when the
voltage got beyond 14 V. The similar results were
obtained for the second group samples, the domain
size increased when kept the applied voltage as 10 V
and expanded the duration of the voltage (Fig. 4).
To determine the domain size, data processing
software, ORIGIN, was used to simulate the written
domains. Points were inserted along the lineament of
the domain image, and their coordinate values were
extracted into a data sheet. The area of the simulated
domain was calculated using the data of inserted
points. Then the domain size was obtained as the
square root of the area calculated using the software
automatically. Figure 5 shows a typical simulated
domain and the relationship between the number of
10604 J Mater Sci (2019) 54:10600–10608

Figure 3 Amplitude images of the first group PMN-PT thin-film samples with a fixed pulse duration = 1 s and different tip voltages: 6 V
(a),7 V (b), 8 V (c), 9 V (d), 10 V (e), 12 V (f), 14 V (g), 20 V (h).

inserted points and the domain size. The results
showed that the shape of the simulated domain got
close to the original written domain with 50 inserted
points. Furthermore, the domain size became larger
with the increase in inserted points and approached
to a certain value when the number of the inserted
points got big enough ([ 50). We believed the as-re-
ceived value was the most exact approximation of the
original domain size, and we chose the value
obtained from 50 inserted points as the final domain
size for our analysis.
To further investigate the influence of the pulse
voltages and duration on the domains, a quantitative
description of the relationship between the domain
size and the voltage is shown in Fig. 6.
The obtained increasing tendency of the domain
size via the pulse voltage could be divided into two
parts: The linear relationship between the domain
size D and the pulse voltage U (Fig. 6a) before the
saturation of the induced polarization (\ 14 V) has
been reported by many early studies in other crystals
[31–33]. In Pb(Zr0.4Ti0.6)O3 (PZT) films, the domain
size changed from 25 to 50 nm, which was linearly

Figure 4 Phase images of the second group PMN-PT samples with a fixed pulse voltage of 10 V and different durations in a t = 0.01 s;
b t = 0.02 s; c t = 0.05 s; d t = 0.1 s; e t = 0.5 s; f t = 1 s; g t = 2 s; h t = 5 s.
J Mater Sci (2019) 54:10600–10608 10605

Figure 5 Phase images of the second group PMN-PT samples Fig. 4) (a); simulated domain using 50 inserted points (b);
with a fixed pulse voltage of 10 V and 2 s (the contrast of colors relationship between the number of inserted points and the
referred to different phase values which is the same as that in domain size (c).

proportional to the pulse voltage in the range from ec —dielectric constants in directions parallel to the
- 6.5 to - 27 V without no saturation [32]. In con- polar axis, ea —dielectric constants in directions per-
trast to fabrication of domains in thin films showing a pendicular to the polar axis, ew —dielectric constant of
linear relationship between size and the voltage, the external medium and em —dielectric constant of
Agronin et al. found the power law voltage depen- the film substrate.
dence of domain size before subsequent saturation in Umin refers to the minimum value of voltages to
bulk lithium niobate crystals. This behavior sug- provide driving force to start domain formation
gested that the domains represent different stages of possibly [33]. However, the nonlinear increasing
the switching kinetic process in different kinds of mode of domain size is believed to be related to a
ferroelectric crystals [26]. Molotskii analyzed the lin- different growth mechanism. Men et al. [34]
ear relationship between the voltage and the domain explained the similar phenomenon in (K, Na)NbO3
size theoretically as ferroelectric thin films that as the increase in domain
4pPS Cts size fell behind the growth of the pulse voltage, the
D ¼ pffiffiffiffiffiffiffiffi  ðU  Umin Þ ð1Þ relationship between D and U became nonlinear.
ec ea þ ew aS h
Another explanation for the domain radius saturation
where was the free charge carrier injection from the tip to
pffiffiffiffiffiffiffiffi   the sample surface at voltage larger than 14 V. Such
ec ea þ 1 1 1
aS ¼ 2p2 P2S pffiffiffiffiffiffiffiffi pffiffiffiffiffiffiffiffi þ pffiffiffiffiffiffiffiffi ð2Þ charge injection might create a large concentration of
ec ea ec ea þ em ec ea þ ew
charged defects (pinning centers), which interacted
PS —the magnitude of the spontaneous polarization, with the moving domain walls [35]. Significant sup-
Cts —tip–sample capacitance, h—film thickness, pression of polarization switching due to trapping of

Figure 6 Relationship between domain size D and a applied voltage U; b duration t; c domain wall velocity v.
10606
electronic charge carriers was also reported for PZT
thin films [36]. In addition, Sharma et al. reported
that the nonlinear relationship was related to the
pulse width in polymer ferroelectric films. For longer
pulse (1 s), domains show nonlinear voltage behav-
ior, while they show the linear relationship for the
pulse of 1 ms [31].
The power law relationship between the domain
size D and the duration t has also been predicted in
Molotskii’s study [33] and has been proved in many
other studies [31, 37, 38]. Tybell et al. [39] analyzed the
function of the domain size and the pulse width in
Pb(Zr0.2Ti0.8)O3 thin films. Below 20 ms, and down to
100 ns, domain size was found to be constant and
approximately equal to 20 nm. It is believed that this
minimum domain size was related to the typical tip
size used for PFM, whose nominal radius of curvature
is 20–50 nm. The domain size increased logarithmi-
cally with increasing writing time for times longer than
20 ms. In another article, the author explained that the
logarithmic relationship between domain size and
time was possibly linked to domain growth by elec-
trically activated nucleation [38]. Molotskii interpreted
the whole process theoretically [33]. Obstacles during
domain growth may lead to pinning of the domain
walls by oxygen, titanium and zirconium vacancies as
well as by point defect clusters in most of the ferro-
electric thin films. When the domain size was quite
smaller than the obstacles, the lateral sizes of the
domain were small compared with the averaged dis-
tance between the pinning centers, and the obstacles
could not influence the domain growth kinetics sig-
nificantly. As the domain wall grew rapidly without
the effects of obstacles, the relationship between the
domain size and duration can be described as [33]
 
D ¼ D0 1  eaS Mt=pD0 ð3Þ
where D0 —the equilibrium domain size and M—
domain wall mobility.
However, the process lasts only tens of millisec-
onds. After that, when domains continuously grow
equal to the distance between obstacles, the domain
walls are pinned by obstacles and the domain size
and duration show a simple logarithmic relationship
[33]
 
D0 2v1 t
D¼ ln ð4Þ
g gD0
where
J Mater Sci (2019) 54:10600–10608
2pPS dE
g¼ ð5Þ
aS
v1 —the maximum lateral domain wall velocity and
g—the activation field.
The results of this paper corresponded to the latter
mechanism pretty well. The logarithmic relationship
between the domain size and the duration is shown
in Fig. 6b during a long period from 100 ms to 5 s.
The minimum time was bigger than most of the
domain formation times—tens of milliseconds. Thus,
it is believed that as the domains have grown up until
their lateral sizes equals to the distance between the
obstacles, the domain walls were pinned by the
obstacles and the subsequently slower motion can be
defined by the thermal activation from the obstacles
and described as Eq. (4).
In Fig. 6c, the wall velocity m was calculated
according to the lateral size and the growth time of
domains [34]. Paruch et al. [23] analyzed that the
growth mechanism of the domain wall was controlled
by the competition of the applied force and the obsta-
cles. For high driving forces, a linear relationship
between domain wall velocity v and applied force F
was expected, while as for the F being compared to the
pinned obstacles, the relationship became a nonlinear
creep motion [23]. Moreover, under a low driving field,
many early studies have confirmed that the relation-
ship of m on D can be expressed in the following for-
mula [20, 23, 29, 33, 34, 40]
 
U a Ec l
v ¼ v1 exp  ð6Þ
kT E
where Ua —the characteristic activation energy, Ec —
the critical electric field for depinning electric field,
k—Boltzmann’s constant, T—the temperature and
l—the dynamic exponent.
A common approximation indicates that E / 1=D,
which leads to a logarithmic form of Eq. (6) [20, 34]
ln v ¼ ln v0  aDl ð7Þ
The linear relationship in Fig. 6c indicated a
dynamic exponent value l of 1, which was obtained
through data fitting and calculating. The dynamical
exponent l depends on the dimensionality and the
roughness of the domain shape, which are decided in
nature of the defects [20, 23]. In ceramics and thin
films with relatively large thickness, it has been
demonstrated that for random field disorder, l = 1,
while for random bond disorder, l = 0.5 [20]. Thus,
J Mater Sci (2019) 54:10600–10608
the higher value l = 1 here represented the random
field disorders in the PMN-PT films, which indicated
the association with dipolar defects. The results were
in accordance with Miller–Weinreich model corre-
sponding to commensurate pinning of two-dimen-
sional domain walls in the crystal lattice potential
[23]. The similar results were also observed in other
systems such as the polycrystalline Pb(Zr,Ti)O3 thin
films and lead-free ceramics like thinned LiNbO3
single crystals [26, 41, 42].
Conclusion
Piezoresponse force microscopy was used to inves-
tigate the domain growth dynamics in PMN-PT thin
films. The domain size grows with the increase in
value or the duration of pulse voltage. A linear
relationship between the pulse voltage and the
domain size was obtained before the saturation of
polarization (14 V). Meanwhile, the relationship
between the domain size and the logarithmic pulse
time duration could also be depicted in a linear
function. These results are consistent with many
other systems and were explained using some typical
models. In addition, some typical theories were used
to analyze the domain wall movement. The domain
wall movement velocity follows a power law on the
domain size with the value of the exponent l = 1. It
was indicative of the random field defects which may
be caused by local component inhomogeneity in the
samples.
Acknowledgements
This work was supported by the Science Challenge
Project (No. TZ2018003) and the National Nature
Science Foundation of China (Grant Nos. 51822206,
51775304 and 51672009).
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