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The Influence of the Electrode Type on the Electric-Ferroelectric Properties

of Sandwich PbZr0.2Ti0.8O3-BiFeO3-PbZr0.2Ti0.8O3 Structure
L. Pintilie a; C. Drgoi a; V. Stancu a; I. Pintilie a
a
National Institute of Material Physics Magurele — Bucharest, Romania

To cite this Article Pintilie, L., Drgoi, C., Stancu, V. and Pintilie, I.'The Influence of the Electrode Type on the Electric-
Ferroelectric Properties of Sandwich PbZr0.2Ti0.8O3-BiFeO3-PbZr0.2Ti0.8O3 Structure', Ferroelectrics, 391: 1, 58 — 66
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 Ferroelectrics, 391:58–66, 2009
Copyright © Taylor & Francis Group, LLC
ISSN: 0015-0193 print / 1563-5112 online
DOI: 10.1080/00150190903001235

The Influence of the Electrode Type on the

Electric–Ferroelectric Properties of Sandwich
PbZr0.2 Ti0.8 O3 -BiFeO3 –PbZr0.2 Ti0.8 O3 Structure

L. PINTILIE, C. DRǍGOI, V. STANCU,∗ AND I. PINTILIE

National Institute of Material Physics Magurele — Bucharest, P.O. Box MG-7,
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077125, Romania

PbZr0.2 Ti0.8 O3 -BiFeO3 -PbZr0.2 Ti0.8 O3 (PZT-BFO-PZT) structure was prepared by sol-
gel method on Pt/Si wafers. Three metals were tested as top electrod: Au, Cu, and Pt.
A double hysteresis loop was observed in all cases, suggesting an antiferroelectric-like
behavior. The values for remnant polarization and coercive field are about 3 µC/cm2 and
115 kV/cm, respectively. The saturation polarization is about 22 µC/cm2 . Capacitance
and leakage current show significant dependence on the top metal electrode. The results
were explained considering the presence of a Schottky-type contact at the PZT-metal
interface.

Keywords Multilayers; multiferroics; antiferroelectric behavior

Introduction
Ferroelectric thin films enjoy a considerable interest in the last decades due to their attractive
properties, which can be exploited in a variety of applications such as non-volatile memories,
tunable capacitors, microwave devices, actuators, pyroelectric detectors, electro-optical
components, etc [1]. The continuous reduction in size is posing also some fundamental
problems, related to the stability of the ferroelectric phase in small volumes. Interfacial
phenomena start to play a much more significant role in thin film multilayers compared to
bulk ceramics, affecting quantities like capacitance and leakage current [2–5].
A unique class of ferroelectric materials are the multiferroics, which are materials pos-
sessing ferroelectric and magnetic properties in the same time [6]. The prototype material
for multiferroics is the bismuth ferrite BiFeO3 (BFO). It is known that BFO in bulk is ferro-
electric and antiferromagnetic at room temperature, and that the ferroelectric polarization
can be as high as 100 µC/cm2 [7, 8]. This value is comparable with that recently reported
for high quality epitaxial Pb(Zr,Ti)O3 (PZT) layers [9], making the material very attractive
to substitute lead-based ferroelectrics in applications. However, the progress towards appli-
cations is hindered by the large value of the leakage current, which is the major drawback
of BFO capacitors [10]. Among the possible causes for this situation can be: the smaller
band gap compared to tetragonal PZT (2.6–2.8 eV [11] compared to 3.6–4 eV [12]); pos-
sible segregation of Fe3 O4 (magnetite, with good electric conductivity) [13]; uncontrolled
impurities incorporated in the film during the deposition process.

Received August 5, 2008; in final form September 9, 2008.

∗
Coresponding author. E-mail: stancu@infim.ro
[438]/58
 Influence of the Electrode Type on PZT–BFO–PZT [439]/59

A lot of effort is made in order to reduce the leakage current in BFO capacitors.
One method is to dope the film with homo or heterovalent atoms such as Cr, La, Nb,
Sc, Mn, etc [14, 15]. Solid solutions, especially BiFeO3 -BiCrO3 , proved to be effective
in reducing leakage current while preserving good ferroelectric properties [16]. Another
method to reduce the magnitude of the leakage current is to use buffer layers from more
insulating materials. For example, it was recently shown that a buffer layer of (Bi,La)Ti3 O12
is significantly reducing the leakage current in epitaxial BFO layers [17]. However, the
ferroelectric properties are also affected.
The idea of the present communication is to use as buffer layer a material which posses
a polarization value comparable to BFO, and a lower leakage current. This material is PZT.
A tri-layer structure was realized in order to maintain the symmetry of the interfaces. The
PZT-BFO-PZT structure was deposited by sol-gel on platinized Si (Pt/TiO2 /SiO2 /Si) wafers.
Three metals were used as top electrodes, Cu, Au, Pt, in order to check the prevalence of the
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interface or bulk controlled conduction mechanisms in the multilayer. The interesting result
is the presence of a double hysteresis loop for all metals, suggesting antiferroelectric-like
behavior for the tri-layer. The change of the top electrode is affecting the magnitude of the
capacitance, the shape of the capacitance-voltage (C-V) characteristics, and the behavior
of the leakage current. All these suggest that, although there are internal interfaces between
BFO and PZT layers, the effect of the electrode interfaces on the electric properties is still
visible.

Experimental Methods
The tri-layer structure was obtained by successive deposition of PZT, BFO and PZT layers
on Pt/Si substrate. The deposition was performed by spin-coating. The precursor solutions
were prepared using the following materials: lead acetate Pb(CH3 COO)2 *3H2 O (Reac-
tivul Bucuresti), titanium isopropoxide Ti[OCH(CH)2 ]4 (Alfa) and zirconium n-propoxide
Zr[OCH2 CH2 CH3 ]4 (Alpha) for PZT; hydrated bismuth nitrate (Bi(NO3 )5 *5H2 O), iron (III)
nitrate (Fe(NO3 )3*9H2 O), acetic anhydride and thriethanolamine for BFO. 2-metoxiethanol
was used as solvent in both cases. The Bi and Pb losses during the thermal annealing were
compensated by adding 10% molar Bi and 5% molar Pb excess respectively, in precursor
solutions. Crystallization annealing was performed after each layer deposition. The PZT
films were crystallized by rapid thermal annealing (RTA) at 650◦ C/15 min, while the BFO
layer was crystallized by RTA at 600◦ C/10 min.
The analysis of the structure was performed by using X-ray diffraction (XRD) and
scanning electron microscopy (SEM). The XRD spectra had revealed the presence of the
characteristic diffraction peaks for both PZT and BFO materials. We mention here that the
Zr/Ti ratio was 20/80, thus the PZT films are in the tetragonal phase. The SEM analysis
had revealed that the total thickness of the tri-layer is about 260 nm, with about 150 nm
for the central BFO layer and about 55 nm for the buffer PZT films. Although the SEM
photographs do not reveal very clear interfaces between PZT and BFO layers, due to the
weak contrast difference, the energy dispersive spectroscopy (EDAX) study had shown that
Bi and Fe are concentrated in the middle of the tri-layer structure, while Pb, Zr, and Ti are
in higher concentrations on the sides. Therefore, even some diffusion may be present, the
studied structure is not a PZT-BFO solid solution [18, 19].
Top electrodes were deposited by radio-frequency (RF) sputtering using a shadow
mask. The Cu, Au, and Pt electrodes were deposited successively on the same tri-layer
structure, ensuring in this way that all the capacitors were obtained in the same conditions,
 60/[440] L. Pintilie et al.
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Figure 1. Hysteresis loops for PZT-BFO-PZT tri-layers with different metals as top electrode.

the only difference being the metal for the top contact. Therefore, the bottom electrode was
always Pt, while the top contact was changed. The area of the top contact was 0.2 mm2 in
all cases.
Electrical measurements at different temperatures were performed by inserting the
samples in a Janis cryostat. The hysteresis loops were obtained either with Radiant Tech-
nology RT66, or with AixACCT TF 2000 analyzer. The capacitance measurements were
performed with Agilent 4263B LCR meter, and the current measurements with Keithley
6517 electrometer.

Results and Discussions

The results of the hysteresis measurements are shown in Figure 1. It is very surprising
that, although both component of the tri-layer are ferroelectric, a double hysteresis loop
is obtained for all the metals used as top contacts. We will not detail this aspect as is the
subject of a separate paper submitted for publication elsewhere. However, we may shortly
mention that there are two explanations for the “double” loop: the model of the “pinched”
hysteresis, in which it is said that a hysteresis loop constricted near origin can be obtained
if there are pinned ferroelectric domains [20]; the presence of an antiferroelectric coupling
at the PZT-BFO interface, inducing an antiferroelectric (AFE)-like behavior of the tri-layer
[21]. The difference between the two situations is that the “pinched” hysteresis disappear
after a few cycles, while the AFE-like behavior should be present even after few thousands
cycles. In our case, fatigue measurements had revealed that the characteristics of the AFE-
like behavior are still visible after 105 cycles. This fact suggests that the second explanation
is more probable.
Another aspect that has to be underlined is that the AFE-like behavior is present no
matter the metal used for top electrode. We can conclude that the probable presence of an
AFE coupling is related to the presence of the PZT-BFO interfaces, being only little affected
by the change of the metal for top contact. This is not the case for the capacitance-voltage
 Influence of the Electrode Type on PZT–BFO–PZT [441]/61
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Figure 2. Capacitance-Voltage characteristics of PZT-BFO-PZT tri-layers with different metals as

top electrode. Measurements were performed at room temperature, at a frequency of 100 kHz and
with an ac signal of 0.1 V amplitude.

(C-V) characteristics shown in Fig. 2. It can be seen that, although the tri-layer structure is
the same, the change of the metal for the top contact has a significant impact on the value
of the measured capacitance.
The shape of the C-V characteristics also suggests an AFE-like behavior. This is clearly
visible in case of Au and Cu top contacts. In case of top Pt electrode it was not possible to
raise the voltage to obtain the full butterfly shape because of the capacitors breakdown.
The results presented in Fig. 2 cannot be explained based only on a simple serial
model for the equivalent capacitance of the tri-layer. We have to admit that the change of
the metal for the top contact triggers significant changes in the characteristics of the top
PZT-electrode interface, with important impact on the capacitance. This can be related with
the presence of a Schottky-type capacitance, as recently suggested for PZT capacitors with
Pt or SrRuO3 contacts. The value of the Schottky capacitance is dependent on the built-in
potential, which is directly related to the potential barrier at the PZT-electrode interface,
and on the effective charge density near the interface. The potential barrier is dependent on
the work function difference between metal and PZT, and on the density of the interface
states. All these parameters change when the top metal is changed, thus is not surprising
that the measured capacitance differs from one metal to the other.
The zero bias capacitance has the largest value for the top Au contact, followed by Cu
and Pt. We can imagine that the equivalent capacitance of the tri-layer is given by:

1 1 1
= + (1)
C Cfix Ctop

Cfix stands for the capacitance of the tri-layer which does not change when the top metal is
changed. This includes the capacitance of the bottom Pt/PZT interface and the capacitance
of the tri-layer itself. Ctop considers only the Schottky-type capacitance related to the top
 62/[442] L. Pintilie et al.

PZT-electrode interface. At zero bias, this is given by [22]:

qε0 εst Neff
Ctop = (2)
2Vbi

Here, εst is the static dielectric constant, Neff is the effective density of fixed charges in the
depleted region near the interface and Vbi is the built-in potential considering the effect of
the polarization charges which are present near the interface. From equation (2) it can be
seen that Ctop increases when the Neff /Vbi ratio increases. The larger is Ctop the smaller will
be its effect on the measured capacitance C in (1). We may conclude that the smallest Ctop
value is for Pt top contact. One hypothesis can be that, in case of Pt, both Neff and Vbi are
small (see equation (2)). But we have to keep in mind that a larger leakage current may
lead to a lower measured capacitance, similar to the effect of a serial resistance [23].
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Therefore, current-voltage (I-V) measurements were performed at different tempera-

tures. Some results are shown in Fig. 3. The hysteresis cycle of the dc current was measured
with a delay time of 3 seconds between the voltage step and the current reading. It can
be observed that the behavior in the low temperature domain (below room temperature)
is somehow different from that above room temperature. For example, the asymmetry is
less evident at low temperatures (see the I-V characteristic at 240 K). As the temperature
increases, the negative part of the I-V characteristic becomes less and less dependent on
the top metal.
The results can be explained, at least qualitatively, considering the presence of
Schottky-type contacts at the PZT-electrode interface. In the low temperature domain,
due to a dramatic decrease of free carriers concentration, the tri-layer structure may act
as fully depleted. The leakage current in this case is dominated by bulk mechanisms, the
electrode interfaces playing a minor role. This can explain the fact that the I-V charac-
teristics are almost symmetrical in the low temperature domain. Eventually, the different
properties of the top electrode-PZT interface may lead to different positions of the Fermi
level in the structure, reflected in some differences in the magnitude of the leakage current.
The concentration of the free carriers is increasing exponentially with the temperature [24].
Therefore, in the high temperature domain the structure becomes partly depleted. At some
temperature, the depletion region will extend only over the thickness of the PZT film. The
asymmetry will be much more visible in this case, due to the different properties of the top
and bottom electrode interfaces. The negative part of the I-V characteristic is converging
towards common values for the leakage current, which is understandable if we consider
that polycrystalline PZT is most probable p-type thus, the bottom Pt-PZT interface will be
reverse biased when the minus polarity is applied on top. This interface is the same for
all studied capacitors. Therefore, the current values should be almost the same. The top
interface is reverse biased when the plus polarity is on top. The change of the metal for the
top contact should induce some changes in the value of the leakage current on the positive
part of the I-V characteristic.
The current measurements suggest that better results are obtained when Cu or Au are
used as top electrodes. The highest value for the leakage current is obtained for the top Pt
electrode. This is a little bit surprising, because Pt has the largest work function from the
three metals used as top contacts [25], but is in agreement with the results of capacitance
measurements.
Apparently, the formation of the Schottky barrier at the ferroelectric-metal interface is
not so sensitive to the work function of the metal. It could be that the interface states play
an important role in this case. The density of the interface states and the thickness of the
 Influence of the Electrode Type on PZT–BFO–PZT [443]/63
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Figure 3. Current-Voltage characteristics of PZT-BFO-PZT tri-layers with different metals as top

electrode. Measurements were performed at different temperatures (a) 240K and (b) 340K.

interface layer may differ from one metal to the other. The effect of the interface states on
the Schottky potential barrier is considered through the S factor, defined as [26]:

1
S= (3)
e2 Nδ
1+
εi ε0

N is the density of the interface states, δ is the thickness of the interface layer, and εi is
the dielectric constant in the interface layer. These quantities are hard to be measured thus
 64/[444] L. Pintilie et al.

the S factor is estimated based on an empirical equation found by Moench [27]:

1
S= (4)
1 + 0.1(ε∞ + 1)2
ε∞ is the electronic contribution to the dielectric constant of the material on which the
Schottky contact is formed. In the present case the material is always PZT, thus S factor
should not change if the top metal is changed. The potential barrier at zero bias ◦B ,
considering S factor, is given by [24]:
 
0B = S(m − χ ) + (1 − S) Eg − 0 (5)

m is the work function of the metal, χ is the electron affinity in PZT, Eg is the band
gap and 0 is the charge neutrality level in PZT. It results that, although the S factor was
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considered, still the highest potential barrier should be for Pt because it has the largest m
– χ difference. This is in disagreement with the experimental results. It could be that the
charge neutrality level is affected by the change of metal, or it could be that other factors
are affecting the formation of the potential barrier in case of ferroelectrics. We should
keep in mind that, in case of ferroelectrics, the polarization charge is also present near the
interface. This charge is requiring another charge, of opposite sign, for compensation. The
compensation charge is supplied by the ferroelectric material and the electrodes. We can
observe that Cu and Au have larger electrical conductivity than Pt. Also, the d-shell is full
for Cu and Au, while Pt has only 9 d-electrons. We may assume that Cu and Au are more
effective in compensating the polarization charges. The following scenario can be assumed:
r When the metal has large density of free electrons the compensation is performed
mainly with charges from the metal, which are then localized at the interface. The
metal-PZT contact behaves as a rectifying Schottky diode with low leakage current.
r When the metal is not able to supply full compensation charges, then the interface
properties adjust itself in order to allow a higher flow of charges in order to ensure
compensation and to keep the polarization stable. In other words, the leakage current
is increasing to supply the compensation charges for ferroelectric polarization.

Conclusions
The electric and ferroelectric properties of PZT-BFO-PZT tri-layer structure with Pt bottom
electrode and Cu, Au, Pt top contacts were studied. It was found that:
r The structure presents and AFE-like behavior no matter the metal used as top contact
r The capacitance is dependent on the top metal. The highest capacitance at zero bias
is obtained for Au.
r The leakage current is dependent on the top metal. Lower leakage currents were
obtained for top Au and Cu contacts.
The experimental results suggest the presence of Schottky-type contacts at the metal-PZT
interfaces. However, the height of the potential barrier is not obeying the theory developed
for metal-semiconductor Schottky contacts. It may be that polarization charges play a role
in the formation of the barrier, as well as the capacity of the metal to provide the necessary
compensation charges. This may be related to the occupancy level of the outer electron
shells. In any case, further experimental and theoretical studies should be performed in
order to solve the problem of metal contacts on PZT.
 Influence of the Electrode Type on PZT–BFO–PZT [445]/65

Acknowledgment
The work was financed through the CEEX contract DINAFER-44 (Romanian Ministry of
Education and Research), and through the young research grant PN2-RU-TD no.103/2007
obtained by Mrs. Stancu from the National Council of Scientific Research in Higher
Education Institutions (CNCSIS).

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