JOURNAL OF RARE EARTHS, Vol. 33, No. 4, Apr. 2015, P.

391

Piezoelectric and upconversion emission properties of Er3+-doped

0.5Ba(Zr0.2Ti0.8)O3-0.5(Ba0.7Ca0.3)TiO3 ceramic
DAI Junli (᠈৯Б), DU Peng (ᴰ吣), XU Jiadan (ᕤՇЍ), XU Chaoxiang (ᕤ䍙⼹), LUO Laihui (㔫ᴹ᜻)*
(Department of Microelectronic Science and Engineering, Ningbo University, Ningbo 315211, China)

Received 2 July 2014; revised 17 December 2014

Abstract: In this investigation, the ferroelectric, piezoelectric properties, and upconversion (UC) emissions of Er3+-doped
0.5Ba(Zr0.2Ti0.8)O3-0.5(Ba0.7Ca0.3)TiO3 (BZT-BCT) were investigated. The results showed that the ferroelectric and piezoelectric per-
formances of BZT-BCT ceramics decreased with the increment of Er doping content. Under the excitation of 980 nm light, all sam-
ples exhibited strong green UC emissions. A maximum green UC emission was observed in BZT-BCT:0.015Er. The variation of the
UC emission with Er doping content did not coincide with that of electrical properties of the ceramics. The relation between the UC
emission and piezoelectric properties was discussed.

Keywords: multifunction; upconversion; ferroelectric; ceramic; rare earths

In recent years, UC emission properties of rare-earth
(RE)-doped materials have attracted considerable atten-
tion due to their wide applications in UC laser, bio- im-
aging in vivo, temperature sensor and so on[1–3]. Ferro-
electrics are electrical multifunctional materials, they
show excellent piezoelectric, ferroelectric, and pyroelec-
tric performances. In modern industry, multifunction is
an essential characteristic of smart materials. It is well
accepted that more multifunctional properties, such as
mechanoluminescence and electroluminescence, can be
realized by RE doping in ferroelectrics[4,5]. Wang et al.[5]
reported that electro-mechano, mechano-optic and elec-
tro-optic coupling could be realized in the Pr doped Ba-
TiO3-based ceramics. In addition, it seems that there is
inner relation between the photoluminescence and di-
electric properties in the RE doped ceramics[4,6–8]. For
example, Zhou et al.[9] have revealed that the strongest
red emission in the Pr3+-doped Na1/2Bi1/2TiO3 (NBT)-
based ceramic was observed at the composition where
the ceramics had the largest piezoelectric response and
the strongest ferroelectric properties. Furthermore, the
dielectric properties of the ferroelectrics were enhanced
by RE-doping[10,11]. Wu et al.[10] reported that the dielec-
tric, ferroelectric, and piezoelectric properties of NBT
ceramics were improved by doping Er2O3. It was also
reported that the photoluminescence of the RE-doped
ceramics could be tuned by the physical treatment, such
as application of electric field, and poling. Hao et al. re-
ported that the enhancement and modulation of UC
emission was realized by applying a relatively low volt-
age upon Yb/Er co-doped BaTiO3 thin films in an in-situ
and real-time manner[12]. Furthermore, we also demon-
strated that the red emissions of the Pr-doped ferroelec-
tric NBT-based ceramics were enhanced by a simple
treatment electric field poling[13].
So far, the lead zirconate titanate (PZT) ferroelectric
ceramics are widely used due to their excellent piezo-
electric and ferroelectric properties. However, due to the
pollution of lead, it is necessary to search new lead-free
ferroelectric ceramics to replace the lead-based ceramics.
0.5Ba(Zr0.2Ti0.8)O3-0.5(Ba0.7Ca0.3)TiO3 (BZT-BCT) ce-
ramic was reported to have the largest piezoelectric re-
sponse in the lead-free ceramics[14], showing a d33 of 620
pC/N. This value is even higher than that of soft lead-
containing PZT ceramics. RE Er acting as an important
inorganic luminescence activator has been extensively
investigated due to its unique energy level characteristic
in UC emissions[15,16]. Therefore, in the present work,
BZT-BCT ceramics doped with different Er ion concen-
trations were prepared to investigate on the effect of Er
doping content on the dielectric properties and UC emis-
sion intensities.
1 Experimental
According to our previous results, the UC emissions in
ABO3 perovskite with A-site substitution by Er3+ were
stronger than that in the counterpart with B-site substitu-
tion[11]. Thus, the Er3+ ions were designed to occupy the
A sites by substituting Ba2+ and Ca2+ ions in proportion

Foundation item: Project supported by National Natural Science Foundation of China (61378068)
* Corresponding author: LUO Laihui (E-mail: llhsic@126.com; Tel.: +86-574-87600953)
DOI: 10.1016/S1002-0721(14)60431-2
392 JOURNAL OF RARE EARTHS, Vol. 33, No. 4, Apr. 2015

according to chemical formula 0.5(Ba(1–3x/2)Erx)(Zr0.2Ti0.8) (Ocean Optics USB4000) under the excitation of a 980
O3-0.5(Ba(0.7–3x/2)Ca(0.3–3x/2)Erx)TiO3 (0”x”0.03). The ce- nm diode laser.
ramics were prepared by a conventional solid-state reac-
tion method. High-purity powders of CaCO3, BaCO3,
2 Results and discussion
TiO2, ZrO2, and Er2O3 were used as raw materials. To
prepare the BZT-BCT:xEr, the raw powders in the The XRD patterns of BZT-BCT:xEr ceramics with 0”
stoichiometric ratio were mixed in alcohol by agate balls x”0.03 are shown in Fig. 1(a). It can be clearly seen that
for 10 h, and then dried and calcined at 1200 ºC for 4 h. all samples possess pure perovskite structure and no
After remilling, mixing thoroughly with a PVA binder secondary impure phase is observed within the XRD de-
solution, the powders were pressed into pellets, and the tection resolution. This result suggests that the Er3+ ions
pellets were finally sintered at 1450 ºC for 4 h in air. For have diffused into the BZT-BCT host. The zoomed XRD
carrying out the dielectric measurement, all the sintered patterns of BZT-BCT:xEr located at 2ș~45º and ~66º are
pellets were ground to ~1 mm in thickness and silver shown in Figs. 1(b) and (c), respectively. As can be seen,
electrode was coated on both sides. peaks at 2ș~45º and ~66º respectively split into (002)/
The crystal structure of the ceramics was checked by (200) and (220)/(202) double peaks. It is believed that
using an X-ray diffraction (XRD) analyzer (Bruker D8 the split (002)/(200) and (220)/(202) peaks are assigned
Advance) with Cu KĮ radiation. The morphology of sin- to the coexistence of tetragonal and rhombohedral
tered powders was investigated by a scanning electron phases[17]. Furthermore, both Figs. 1(b) and (c) show that
microscope (SEM) (Hitachi SU-700). The polarization vs. the diffraction peaks slightly shift to larger angle, which
electric field (P-E) hysteresis loops were obtained at 1 indicates that the lattice of the BZT-BCT:xEr ceramics
Hz by the RT Premier II ferroelectric workstation. The shrinks. The smaller Er3+ (0.122 nm, 12 Coordinate) oc-
strain vs. electric field (S-E) hysteresis loops were inves- cupies the larger Ba2+ (0.161 nm, 12 Coordinate) and
tigated by an MTI-2100 optical sensor. The UC emis- Ca2+ (0.134 nm, 12 Coordinate) ions. As a result, the lat-
sions were recorded by using a spectrofluorometer tice shrinks.
(Ocean Optics USB4000) under the excitation of a 980 The representative surface morphology of BZT-BCT:
nm diode laser. xEr ceramics with x=0, 0.006, 0.015 and 0.03 is pre-
According to our previous results, the UC emissions in sented in Fig. 2. From Fig. 2(a), one can know that the
ABO3 perovskite with A-site substitution by Er3+ were
stronger than that in the counterpart with B-site substitu-
tion[11]. Thus, the Er3+ ions were designed to occupy the
A sites by substituting Ba2+ and Ca2+ ions in proportion
according to chemical formula 0.5(Ba(1–3x/2)Erx)(Zr0.2Ti0.8)
O3-0.5(Ba(0.7–3x/2)Ca(0.3–3x/2)Erx)TiO3 (0”x”0.03). The ce-
ramics were prepared by a conventional solid-state reac-
tion method. High-purity powders of CaCO3, BaCO3,
TiO2, ZrO2, and Er2O3 were used as raw materials. To
prepare the BZT-BCT:xEr, the raw powders in the
stoichiometric ratio were mixed in alcohol by agate balls
for 10 h, and then dried and calcined at 1200 ºC for 4 h.
After remilling, mixing thoroughly with a PVA binder
solution, the powders were pressed into pellets, and the
pellets were finally sintered at 1450 ºC for 4 h in air. For
carrying out the dielectric measurement, all the sintered
pellets were ground to ~1 mm in thickness and silver
electrode was coated on both sides.
The crystal structure of the ceramics was checked by
using an X-ray diffraction (XRD) analyzer (Bruker D8
Advance) with Cu KĮ radiation. The morphology of sin-
tered powders was investigated by a scanning electron
microscope (SEM) (Hitachi SU-700). The polarization vs.
electric field (P-E) hysteresis loops were obtained at 1
Hz by the RT Premier II ferroelectric workstation. The
strain vs. electric field (S-E) hysteresis loops were inves- Fig. 1 XRD patterns of BZT-BCT:xEr ceramics (a), the zoomed
tigated by an MTI-2100 optical sensor. The UC emis- XRD patterns from 44º to 48º (b) and the zoomed XRD
sions were recorded by using a spectrofluorometer patterns from 64º to 68º (c)
DAI Junli et al., Piezoelectric and upconversion emission properties of Er3+-doped … 393

Fig. 2 Typical SEM micrograph of BZT-BCT:xEr ceramics

(a) x=0; (b) x=0.006; (c) x=0.015; (d) x=0.03

grain size of pure BZT-BCT is very inhomogeneous. The
largest grain reaches as high as ~30 ȝm, meanwhile the
smallest one is only 3~4 ȝm. It can be seen that no obvi-
ous pores were observed, which indicates that all sam-
ples were densely sintered. With the increment of Er
doping x from 0 to 0.03, the morphology of the grain
changes little.
Fig. 3(a) displays several typical P-E hysteresis loops
of BZT-BCT:xEr ceramics at room temperature under
the maximal electric field of 50 kV/cm. It is obvious that
well saturated and square-like loops are obtained for all
the studied compositions. The remanent polarization Pr
and the coercive field Ec as a function of Er content x are
shown in Fig. 3(b). It is found that pure BZT-BCT ceram-
ics possess the largest Pr (~15.1 ȝC/cm2) and the smallest
Ec (~3 kV/cm). Pr of BZT-BCT:xEr ceramics decreases
gradually, whereas Ec increases until x=0.015. Similar
result is also observed by Li et al.[18] in (Ba0.99Ca0.01)
(Ti0.98Zr0.02)O3 ceramics. The decreased Pr and increased
Ec indicate that moderate Er doping plays a hard effect
on the ceramics. When the Ca2+ and Ba2+ are substituted
by Er3+, charge defects are created. The charge defects
will pin the domain switching. As a result, polarization of
the ceramics is decreased, and Ec is increased by Er3+
doping. However, Pr and Ec change little when Er content
x>0.015. This result might be caused by that excessive Er
doping addition does not diffuse to the lattice of BZT-
BCT due to the difference of the ion radius and valence
between Er3+ and A-site ions (Ca2+, and Ba2+). As a result,
the excessive Er3+ may accumulate at the grain bounda-
ries in the ceramics, which will degenerate the photolu-
minescence properties.
To investigate the piezoelectric properties of the BZT-
BCT:xEr ceramics, the strain behavior of BZT-BCT:xEr
ceramics was measured. Bipolar electric field vs. strain
curves of BZT-BCT:xEr ceramics at room temperature
with the largest electric field of 20 kV/cm are shown in
Fig. 4(a). From Fig. 4(a), it can be seen that all samples
show a butterfly-shaped curve. The maximum strain of
BZT-BCT:xEr ceramics is around 0.11%, which is ob-

Fig. 3 Typical P-E hysteresis loops of BZT-BCT:xEr ceramics

at room temperature (a) and variations of Pr and Ec with Fig. 4 Bipolar (a) and unipolar (b) strain loops of the BZT-
the Er content x for the BZT-BCT:xEr ceramics (b) BCT:xEr ceramics at room temperature
394
tained at x=0. The largest strain of BZT-BCT:xEr ce-
ramics under 20 kV/cm decreases with the Er content in-
crement until x=0.015, and then changes little. The strain
behavior as a function of Er content is consistent with
that of ferroelectric properties, as mentioned in Fig. 3(b).
Fig. 4(b) shows the unipolar strain of the ceramics. All
the ceramics illustrate a low hysteresis behavior. The low
hysteresis of the ceramic is favorable to its application in
piezoelectric actuator. The effective piezoelectric coeffi-
cient d33 can be calculated by the following equation:
d33=Smax/Emax, where Smax is the maximum strain under
the maximal applied electric field Emax. The calculated
d33 of pure BZT-BCT reaches ~540 pm/V.
In order to study the UC emission properties of the
BZT-BCT:xEr ceramics, the UC emission spectra under
the excitation of 980 nm were measured, as shown in Fig.
5(a). Under the excitation of 980 nm light, a strong UC
emission is observed, as shown in the inset of Fig. 5(a).
The UC emission spectra include two parts, that is, the
strong green emission located at around 530 and 550 nm
from the mixed levels (2H11/2, 4S3/2)ĺ4I15/2, and the rela-
tively weak red emission located at ~660 nm from
4
F9/2ĺ4I15/2. All UC emission bands coincide well with
the earlier reports[11,19]. As can be seen, there is no obvi-
ous shift for the emission peaks, and UC emission inten-
sities of BZT-BCT:xEr ceramics have a significant change
with the increment of Er content. The green (550 nm)
and red (660 nm) emission intensities as a function of Er
Fig. 5 Upconversion emission spectra of BZT-BCT:xEr ceram-
ics under the excitation of 980 nm (a) and the green and
red emission intensities as a function of Er doping con-
centration (b) (The inset is the photograph of BZT-BCT:
0.002Er excited under 980 nm laser)
JOURNAL OF RARE EARTHS, Vol. 33, No. 4, Apr. 2015
content x are shown in Fig. 5(b), where the emission in-
tensities were determined by integrating the area below
the UC emission curve. From Fig. 5(b) one knows that
the green emission intensity linearly increases when Er
content x”0.006. With further increasing of the Er doping
content (x”0.015), the green light intensity increases con-
tinuously. However, the increasing rate decreases. It is
also found that the variation of red emission intensity
with Er content x”0.015 is similar with that of green
emission. The variation of increasing rate with the Er
content may be caused by the change of UC mechanism
due to the variation of Er content. As we know, the UC
emission of Er is a two-photon process. Excited state
absorption (ESA) and energy transition (ET) may take
place during UC process[11]. The intensities of the green
emission show a decreased trend as x further increases to
>0.015, while the red one increases continuously until
x=0.025. The interaction of cross relaxation (CR) and ET
process should be responsible for the inconsistence of
variation of the green and red emission intensity with the
Er content when Er doping content in the range of
0.015”x”0.025. The reason will be discussed later. As Er
content increases to x>0.025, both the green and red light
intensities reduce dramatically, which is caused by the
concentration quenching.
The mechanism of UC emission of Er3+-doped materi-
als has been extensively studied[11,20,21]. The simplified
energy level diagrams of Er3+-doped BZT-BCT are shown
in Figs. 6(a) and (b). Under the excitation of 980 nm light,
electrons populating at ground state are excited to 4I11/2
level through the ground state absorption (GSA) process,
as shown in Fig. 6(a). After that the multiphonon relaxa-
tion (MPR) process happens and electrons are partly de-
cayed to 4I13/2 level. Then the same laser pumps the elec-
trons from 4I13/2 and 4I11/2 to 4F9/2 and 4F7/2 respectively.
Subsequently, the electrons located at 4F7/2 level nonra-
diatively relax to the mixed 2H11/2, 4S3/2 and 4F9/2 levels
by MPR process. Finally, the electrons relax to the
ground state. As a result, the green and red emissions are
observed. It should be noted that levels 2H11/2, 4S3/2 are
Fig. 6 Energy level diagrams for the proposed UC mechanism
(a) ESA UC process; (b) ET process
DAI Junli et al., Piezoelectric and upconversion emission properties of Er3+-doped …
two thermally coupled levels, and at low temperature the
530 nm emission light was not observed[22]. It is well
known that the CR process: (2H11/2, 4S3/2ĺ4I9/2)+(4I15/2ĺ
4
I13/2) would take place when the Er3+ ion concentration
reaches a certain degree as shown in Fig. 6(b)[11,16]. The
4 Wong Magna Foundation in Ningbo University and Natural Sci-
I9/2 and 4I13/2 levels are populated due to the CR process.
It is clear that the level 4I9/2 could partly nonradiatively
relax to the lower levels 4I11/2 and 4I13/2 or partly radia-
tively decays to the ground state[11,16,20,23]. The electrons
located at 4I13/2 level could not only radiatively decay to
the ground state, but also follow an UC promotion to the
4 terial is more than the sum of its parts. Nat. Mater., 2012,
F9/2 level through ET process: (4I13/2+4I11/2)ĺ(4F9/2+4I15/2)
by the neighboring Er3+ ions. The CR and ET processes
take place simultaneously. The interaction of CR and ET
leads to that the red emission from the 4F9/2 level is en-
hanced, while the green emission from the mixed 2H11/2,
4
S3/2 levels decreases when the Er3+ ions reach a certain
concentration. In this process, this phenomenon happens
when 0.015”x”0.025, as shown in Fig. 5(b).
The above results demonstrate that the piezoelectric
and ferroelectric properties of BZT-BCT ceramic were
weakened by RE Er doping. This result is contrary to that
of RE doped NBT-based ceramics. In terms of RE doped
NBT-based ferroelectric, enhanced piezoelectric proper-
ties were observed by the doping of RE ions[10,24,25]. The
Na and Bi elements evaporate during sintering, and the
oxygen vacancies are formed due to the evaporation of
Na and Bi ion. The oxygen vacancies are one of the main
causes of the degradation of piezoelectric properties in
ferroelectrics[10]. And oxygen vacancies are reduced by
compensating the evaporated elements by RE ion doping.
As a result, the piezoelectric properties of RE doped
NBT-based ferroelectric are increased. In the present
process, the ions in BZT-BCT ceramics do not volatilize
during sintering. That is to say, no oxygen vacancy is
created. However, the trivalent Er ions occupy the A sites
by substituting bivalent Ca and Ba ions, which will cre-
ate the vacancies of Ba and Ca ions to meet the charge
compensation mechanism. This leads to the decreased
ferroelectric and piezoelectric properties, as shown in
Figs. 3 and 4.
3 Conclusions
In summary, the BZT-BCT:xEr ceramics were pre-
pared by the solid-state reaction technique. The ferro-
electric and piezoelectric properties decreased gradually
when the Er content x”0.015. When x was over 0.015,
the ferroelectric and piezoelectric properties did not have
significant change with further increase of Er content.
Under the excitation of 980 nm light, the BZT-
BCT:0.015Er ceramic exhibited the maximal UC emis-
sion intensity. The maximal UC properties were not ob-
served at the same composition where maximal piezo-
electric properties were observed. Our results demon-
395
strated that the relationship between the piezoelectric and
photoluminescence properties in RE doped ferroelectric
ceramics might depend on the host materials.
Acknowledgements: The work was also supported by the K.C.
ence Foundation of Ningbo (2012A610178).
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