Journal of Luminescence 155 (2014) 269274

Contents lists available at ScienceDirect

Journal of Luminescence
journal homepage: www.elsevier.com/locate/jlumin

Enhancing photoluminescence with Li-doped CaTiO3:Eu3 red

phosphors prepared by solid state synthesis
Yibing Wu a,b,n, Zhuo Sun b, Kaibin Ruan a, Yong Xu a, Hong Zhang a
a

College of Mechanical and Electronic Engineering, Fujian Agriculture and Forestry University, Fuzhou, Fujian 350002, People's Republic of China
Engineering Research Center for Nanophotonics and Advanced Instrument, Ministry of Education, Department of Physics, East China Normal University,
Shanghai 200062, People's Republic of China
b

art ic l e i nf o

a b s t r a c t

Article history:
Received 16 February 2014
Received in revised form
16 June 2014
Accepted 25 June 2014
Available online 7 July 2014

Red phosphors of Li-doped CaTiO3:Eu3 that enhance photoluminescence have been synthesized by a
solid-state method, and their structure and morphology were conrmed by X-ray diffraction (XRD) and
scanning electron microscopy (SEM). The luminescence property was measured using photoluminescence excitation (PLE) and photoluminescence (PL) spectra, respectively. The effect of sintered
temperature and Eu3 and Li concentration in as-prepared series phosphors was studied. Results
indicate that the optimal luminescence properties of CaTiO3:Eu3 (CTE) phosphors are typically
obtained at 1300 1C with 12 mol% of Eu3 concentration, and the emission intensity can be greatly
enhanced by the incorporation of Li into the CTE phosphors, attributing that Li not only compensates
positive charge defect by replacement of Ca2 with Eu3 , but also plays a role of ux, which could
enhance the crystallinity of the phosphors. The intensity of the optimal Li-doped CaTiO3:Eu3 phosphor
(CLTE) is 2.3 times of that of CTE. PL spectrum showed that CLTE phosphor was efciently excited by
near-ultraviolet light at wavelength around 398 nm and emitted intensive red light with a peak around
616 nm corresponding to the 5D0-7F2 transition of Eu3 . Furthermore, this phosphor has very good
thermal stability and high color purity, implying the potential to be a promising red phosphor in white
light emitting diodes.
& 2014 Elsevier B.V. All rights reserved.

Keywords:
LED
CaTiO3
Phosphors
Li-doped

1. Introduction
Due to their excellent properties, such as high color rendering
index, low power consumption, long lifespan, high luminescence
efciency and environmentally-friendly characteristics, white
light-emitting diodes (WLEDs) have recently attracted much
attention [13]. They may be able to replace traditional light
sources (such as incandescent and uorescent lamps) and have
shown many other potential applications as the next generation
light source including indicators, neon lamps, decorative lamps,
backlights for cellular phones and liquid crystal displays [4,5].
Among different types of WLEDs, the tricolor phosphor converted
WLEDs have been widely studied for their high color rendering
index and tunable color temperature [6]. The current phosphor
materials of choice for solid state lighting based upon near
ultraviolet (NUV) GaN-LEDs include Y2O2S:Eu3 for red, ZnS:
Cu ,Al3 for green and BaMgAl10O17:Eu2 for blue [7]. However,
n
Corresponding author. College of Mechanical and Electronic Engineering, Fujian
Agriculture and Forestry University, Fuzhou, Fujian 350002, China. Tel.: 86
59983789346.
E-mail address: ab@fafu.edu.cn (Y. Wu).

http://dx.doi.org/10.1016/j.jlumin.2014.06.051
0022-2313/& 2014 Elsevier B.V. All rights reserved.

compared to the green and blue phosphors, the red phosphors

have much lower efciency [8]. Moreover, sulde-based phosphors are chemically unstable at atmospheric conditions and are
environmentally unfriendly. Therefore, it is of paramount importance to nd a desirable red emitting phosphor, with good thermal
stability, environmentally friendly and strong luminescent intensity, which can be successfully excited by the NUV light.
Rare-earth ions-doped titanates have attracted lots of attentions because of their promising luminescent properties, friendly
environment and the well-known chemical stability, which can be
used as LEDs [912]. There are some researches on CaTiO3-based
phosphor materials, but most studies have focused on Pr3 -doped
long persistent phosphorescent phosphors [1315], which are
excited by UV in the range of 150300 nm. However, this type of
phosphor cannot match the promising InGaN-based chips.
Although the Eu3 -doped CaTiO3 phosphor that exhibits strong
red luminescence have been synthesized according to the literature [1619], the researches on CaTiO3:Eu3 are still inadequate,
and their applications were restricted due to the low luminous
intensities in these perovskite-type hosts, more detailed research
need to be done. In addition, when a Ca2 ion is substituted by
an Eu3 in the CaTiO3 lattices, there will be a positive charge

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Y. Wu et al. / Journal of Luminescence 155 (2014) 269274

defect [20]. Such charge defects hamper the process of energy

transfer from the host to Eu3 . However, it can be compensated
by the negative charge defect when a Ca2 ion is substituted by a
Li ion, consequently leading to the reinforcement of the optical
performances.
Based on these observations, we prepared the Li-doped CaTiO3:
Eu3 red phosphors via solid state synthesis in this work and
characterized the formation, morphology and PL properties of
them. The inuence of Eu content, Li content and sinter temperature on luminescent intensity was discussed in detail, and the
reasons for the enhancement of luminescence were explained
as well.

2. Experimental
Ca1  xTiO3:xEu3 and Li-doped Ca0.88  xLixTiO3:12%Eu3 series
red phosphors were prepared via the solid state synthesis. The
starting materials were calcium carbonate (CaCO3, Aldrich, 99.0%),
titanium dioxide (TiO2, Aldrich, 99.8%), europium oxide (Eu2O3,
Aldrich, 99.9%), and lithium carbonate (Li2CO3, Aldrich, 99.8%). For
homogeneous mixing of small amount of activators, the stoichiometric weights of materials were ball-milled thoroughly in ethanol
(99%) for 3 h, and were dried at 120 1C for 12 h. The powder
mixture was packed into an alumina crucible and heated in a
mufe furnace at a constant rate (400 1C h  1) from room temperature to a temperature in the range of 9001400 1C, and held at
high temperature for 4 h. The materials were cooled to room
temperature again and then crushed into ne powders.
The X-ray diffraction (XRD) patterns of the powder samples
were identied by X-ray diffractometer (Model Ultima IV, Rigaku,
Japan) using Cu K radiation ( 0.15406 nm) at 35 kV and 25 mA.
The microstructures and morphologies of the samples were
observed using a scanning electron microscope (SEM) (Model
S-4800, Hitachi, Japan). Particle size of the samples was determined with a laser scattering particle size analyzer (Model LA950V2, Horiba, France). Fluorescence spectra were measured using
a uorescence spectrophotometer (Model Fluoromax-4, Horiba,
France).

3. Results and discussion

3.1. XRD characteristics
Fig. 1(a) shows the XRD patterns of the Ca0.88TiO3:12%Eu3
(CTE) samples sintered at different temperatures for 4 h. The
diffraction peaks of the obtained powders are in good agreement
with the JCPDS Card no. 22-0153 of orthorhombic CaTiO3, and the
intensity of the diffraction peaks gets higher and sharper with the
increase of temperatures. But when temperature reaches 1400 1C,
the intensity does not increase again. Meanwhile, we also noticed
that there are some weak impurity peaks for the sample sintered
at 1000 1C in Fig. 1(a), where the asterisks, red hearts and the
diamond symbols are corresponded to Eu2O3, TiO2 and Eu2Ti2O7,
respectively. With the increase of temperatures, the impurity
peaks of Eu2O3 and TiO2 disappear and the phase for Eu2Ti2O7
becomes weaker. Therefore, the optimum reaction temperature is
1300 1C for phase formation. The strongest reection of CTE was
centered at 2 33.170, which corresponds to the crystalline plane
with Miller indices (121). The crystallite size was estimated using
the diffraction peaks by the WilliamsonHall equation [21]:

cos k=L sin ;

where is the full-width-at-half-maximum (FWHM) of the

diffraction, is the Bragg angle, is the lattice strain associated

Fig. 1. (a) XRD patterns of Ca0.88TiO3:12%Eu3 phosphors sintered at different

temperatures; (b) XRD patterns of Ca1  xTiO3:xEu3 phosphors sintered at 1300 1C;
and (c) XRD patterns of Li-doped Ca0.88  xLixTiO3:12%Eu3 phosphors.

with the nanoparticles, k is a constant, (0.15406 nm) is the

wavelength of the X-rays used to characterize the compounds, and
L is the average thickness of the crystal in a direction normal to the
diffraction plane hkl, where L is often used to estimate the
crystallite size instead of the size of the polycrystalline aggregate.
The FWHM was corrected for the instrumental broadening using a
standard Si sample. The value of L for as-prepared CTE phosphors
sintered at 1000 1C, 1100 1C, 1200 1C, 1300 1C and 1400 1C calculated from Eq. (1) was approximately 42 nm, 48 nm, 52 nm, 55 nm
and 47 nm, respectively, showing that the crystallite size increased

Y. Wu et al. / Journal of Luminescence 155 (2014) 269274

with the increase of sintered temperature at the range from

1000 1C to 1300 1C, which was due to higher crystallinity.
Fig. 1(b) displays the XRD patterns of Ca1  xTiO3:xEu3 sintered
at 1300 1C with different Eu3 concentrations. We can see from
this gure that the co-doped Eu3 ion had little inuence on the
host structure, and nearly all of the peaks could be attributed
to orthorhombic CaTiO3 phases, indicating that Eu3 ions might
easily replace Ca2 ions in the host because of the approximate
radii of them. There is impurity phase of Eu2Ti2O7 which appears
in the sample of 10 mol% and 12 mol% of Eu3 , but it is very weak.
When the Eu3 content is greater than 12 mol% (x 0.12) in the
Ca1  xTiO3:xEu3 series, the crystallinity became worse and the
peaks of the impurity phase of Eu2Ti2O7 became obvious. So
the optimum concentration of Eu3 ion in the Ca1  xTiO3:xEu3
series phosphor is 12 mol%.
Fig. 1(c) shows the XRD patterns of Ca0.88  xLixTiO3:12%Eu3
phosphors with different Li concentrations (0 mol%, 4 mol%,
8 mol% and 12 mol%). The Li-doped Ca0.88  xLixTiO3:12%Eu3 phosphors showed improved crystallinity compared to CTE, as evidenced by relatively high and sharp peaks in the XRD patterns,

271

indicating that the Li content incorporated into the CaTiO3 lattice

serve as a self-promoter for the better crystallization. As Li content
increased from 4 mol% to 8 mol%, the crystallinity was improved.
However, the crystallinity became worse when the concentration
of Li is greater than 12 mol%. What is more, the impurity phase of
Eu2Ti2O7 disappears in the sample of 8 mol%. So the optimum
concentration of Li in the Ca0.88  xLixTiO3:12%Eu3 series phosphors is 8 mol%. The L value of Li-doped Ca0.80Li0.08TiO3:12%Eu3
(CLTE) phosphors was estimated to be approximately 57.6 nm,
using the diffraction peaks and WilliamsonHall equation Eq. (1),
which shows that Li is not only a charge compensator, but also
plays the role of ux, enhancing the crystallinity.
3.2. SEM (surface morphology)
SEM offers an important tool for the characterization of
materials and to study the texture, topography and surface
features of the prepared phosphors. Fig. 2(a)(e) exhibits the
scanning electron microscope (SEM) images of CTE phosphors
sintered at different temperatures via the solid-state reaction

Fig. 2. SEM image of CTE phosphors sintered at different temperatures (a) 1000 1C, (b) 1100 1C, (c) 1200 1C, (d) 1300 1C, (e) 1400 1C; and (f) SEM image of CLTE phosphors
sintered at 1300 1C.

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Y. Wu et al. / Journal of Luminescence 155 (2014) 269274

Fig. 3. Particle size distribution of CLTE phosphors.

method. When the CTE phosphors sintered at 1000 1C, 1100 1C and
1200 1C, the shape of the grain was spherical. But the particles of
CTE phosphors became aggregate and irregular when the temperature reached 1300 1C. On the other hand, according with the
result of XRD, it was obvious that the particle size increased with
sintering temperature. Fig. 2(f) shows the SEM image of
Li-doped Ca0.80Li8TiO3:12%Eu3 (CLTE) phosphors sintered at
1300 1C. We see from these gures that the particles of CLTE
phosphors are larger and more irregular than that of CTE phosphors sintered at same temperature (Fig. 2(d)). The average
particle sizes of CET and CLTE are around 3 and 4 mm, respectively.
This result shows that the particle size increased after Li was
doped into CaTiO3:Eu3 . Thus, Li doping enhances the crystallinity and the growth of CaTiO3 particles, as shown in the XRD and
SEM results. Quantitative analysis of the sample particle size was
also determined by laser light scattering methodology. Fig. 3
shows the particle size distribution of CLTE phosphor. CLTE
phosphor had only one maxima around 3.5 mm with a shoulder
near 10 mm, and the average size of the phosphor is 4 mm. Results
from the laser scattering particle size distribution analysis displayed good correspondence with the SEM image analysis of the
CLTE sample.
3.3. Photoluminescence properties
Fig. 4 shows the excitation and emission spectra of a CTE
phosphor sintered at 1300 1C for 4 h via the solid state synthesis.
The as-prepared phosphor exhibits strong red luminescence under
NUV excitation. The excitation spectrum of the phosphor is
recorded in the range from 350 nm to 500 nm monitored at
616 nm as shown in the left part of Fig. 4. The sharp lines in the
355470 nm range are associated with intra-congurational 4f4f
transition of Eu3 in the host lattices, and the excitation peaks
located at 362, 398, 417 and 465 nm correspond to 7F0-5D4,
7
F0-5L6, 7F0-5D3,and 7F0-5D2 transitions, respectively[20]. The
transitions within the Eu3 , 4f6 conguration in longer spectral
region with 7F0-5L6 (398 nm) is the most prominent group. The
PLE spectra reveals that the CTE phosphor is suitable for being
excited by commercial GaN-based NUV LED, showing great potential in making WLEDs.
The emission spectrum of the CTE phosphor excited by 398 nm
irradiation is shown in the right part of Fig. 4. The emission
spectrum of the samples exhibits four obvious maxima allocated at
594, 616, 655 and 696 nm, being assigned to transitions from the
excited 5D0 state to 7FJ (J 0,1,2,) levels of the Eu3 , respectively

Fig. 4. Emission spectra and excitation spectra of CTE and CLTE phosphors sintered
at 1300 1C.

Fig. 5. PL spectra of Ca0.88TiO3:12%Eu3 phosphors sintered at different temperatures and PL intensity as a function of sintered temperature in the inset.

[2]. The most intensive band at 616 nm is due to the 5D0-7F2

transition. The 5D0-7F1 band at 595 nm is a magnetic dipole one
and hardly varies with the crystal eld strength around the Eu3 ,
but the electric dipole transition 5D0-7F2 is very sensitive to the
local environment around the Eu3 , and a large probability of this
transition has been postulated to be due to an increase in
covalence and a decrease of symmetry.[8,2223] The asymmetry
ratio R I(5D0-7F2)/I(5D0-7F1) of CTE sample is calculated as
2.32, indicating that the Eu3 ions of sample occupy low symmetry sites, which would increase the emission strength of the
electric dipole transition.
Fig. 5 shows emission spectra of Ca0.88TiO3:12%Eu3 (CTE)
phosphors sintered at difference temperatures and PL intensity
as a function of sintered temperature in the inset. The fact that the
emission peaks were stable at the same position suggests that
changing the sintered temperature did not affect radioactive
transitions of Eu3 ions in the hosts. The emission intensities of
the samples excited at 398 nm increased with sintering temperature when it is lower than 1300 1C. However, when the sintered
temperature was higher than 1300 1C, the emission intensity
started decreasing. So the highest emission intensity of CTE
phosphors was observed with the sample sintered at 1300 1C.

Y. Wu et al. / Journal of Luminescence 155 (2014) 269274

Fig. 6. PL spectra of Ca1  xTiO3:xEu3 series phosphors sintered at 1300 1C and PL

intensity as a function of Eu3 concentration in the inset.

Fig.7. PL spectra of Ca0.88  xLixTiO3:12%Eu3 series phosphors sintered at 1300 1C

and PL intensity as a function of Li concentration in the inset.

This can be due to the increased crystallinity of the samples, which

has been proved by the XRD analysis.
Fig. 6 showed emission spectra of Ca1  xTiO3:xEu3 phosphors
with different doped concentrations of Eu3 and PL intensity as a
function of Eu3 content in the inset. All samples showed broad
emission peaks in the range from 585 to 630 nm with the
maximum intensity at about 618 nm. The emission intensity of
the samples increased monotonically with the Eu3 content at low
Eu3 doped concentration. But when the Eu3 content was higher
than 12 mol%, the emission intensity decreased dramatically due
to concentration quenching. This may be caused by two reasons:
rstly, the activation of Eu3 might not completely occur in the
matrix of the CaTiO3 host material at high doping concentration
and there appeared impurity phase of the Eu2Ti2O7 from XRD
result, which would deteriorate the luminescent properties and
result in the decrease of PL properties. Secondly, concentration
quenching usually occurs as a result of non-radioactive energy
transfer among luminescent centers. The probability of energy
transfer between two activator ions is inversely proportional to
the n power of R (n 6, 8, or 10), where R is the distance between
the activator ions [16]. With increasing Eu3 concentration, the
distance between Eu3 ions decreased, the probability of energy
transfer among them would increase dramatically, which

273

Fig. 8. CIE parameters and color purity of the CTE and CLTE phosphors.

ultimately caused the quenching. The optimal concentration for

obtaining the highest PL intensity of CTE was 12 mol% of Eu3 ,
which can be produced for use in LEDs.
Fig. 7 shows emission spectra of CLTE phosphors with different
doped concentrations of Li sintered at 1300 1. The inset shows
the PL intensity as a function of Li concentrations. On the one
hand, the emission peak positions are located at the same
wavelengths as that in Fig. 7, suggesting that the mechanism of
light emission remains when Li is introduced. On the other hand,
the emission intensities increased with concentration of Li, and
the optimal content for obtaining the highest PL intensity of CLTE
was 8 mol% of Li, while the intensity of CLTE is 2.3 times of that of
CTE. This illustrates that Li-incorporation can greatly promote the
luminous efciency of CTE. It is clear that Eu3 ion has one more
positive charge than Ca2 ion; therefore, one-by-one replacement
of Ca2 by Eu3 made accumulation of positive charge. Such
positive charge defect may hamper the process of energy transfer
from host to Eu3 , but it can be compensated by the negative
charge defect when some Ca2 ions are substituted by Li ions,
consequently leading to the reinforcement of the optical performances [24]. In addition, Li2CO3 may act as the role of solid ux in
the experiment, and stimulate the host lattice formation and grain
growth, leading to higher oscillator strengths for the optical
transitions[15,25], thus the PL intensity was improved. When the
content of Li exceeds 8 mol%, there is a gradual decrease in the PL
intensity due to concentration quenching. It seems that a higher
level of substitution by Li would slightly distort the orthorhombic structure due to the smaller ionic radius of Li compared to
Ca2 . This distortion might have a signicant inuence on crystallization of the CLTE, so the crystallinity became worse as shown in
Fig. 1(c), which lead to decrease the intensity of luminescence.
However, further studies are needed to reveal the details of the
mechanism.
The red emission can be further conrmed by the CIE (Commission international de LEclairage 1931 chromaticity) coordinates from their emission spectra. Fig. 8 shows that the CIE
chromaticity coordination of CTE and CLTE phosphor excited by
398 nm is (x 0.640, y0.359) and (x 0.649, y 0.350), respectively. That is to say, chromaticity coordinate of Li-doped CLTE
phosphors is closer to the chromaticity coordinate of the standard
red light, which is (x 0.67, y 0.33). Color purities of CTE and
CLTE are 99.8% and 99.9%, respectively. The color purity is the
weighted average of the (x, y) coordinates relative to the coordinates of the illuminant and the coordinates of the dominant

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Y. Wu et al. / Journal of Luminescence 155 (2014) 269274

CaTiO3:Eu3 , where Li does not only compensate positive charge

defect by the replacement of Ca2 , but also plays a role of ux.
The intensity of the optimal Li-doped CaTiO3:Eu3 phosphor, Ca0.8
Li0.08TiO3:12%Eu3 (CLTE), is 2.3 times of that of Ca0.88TiO3:12%
Eu3 (CTE). In addition, color purity of CLTE is higher. The CIE of
CLTE was closer to the NTSC red than that of CTE, and this
phosphor has excellent thermal stability compared with the
commercial Y2O3S:Eu3 . Therefore, these properties made asprepared Li-doping CaTiO3:Eu3 phosphors a promising red phosphor to be used for tricolor WLED.

Acknowledgments
The nancial support from the Natural Science Fund of Science
and Technology, Department of Fujian Province (No. 2011J05122),
and the Department of Education, Fujian Province (No. JB12067)
for this work is greatly appreciated.

Fig. 9. The luminous intensities of CLTE with raised temperatures.

wavelength [26]
q
xs xi 2  ys  yi 2
Colorpurity q100%
xd xi 2  yd  yi 2

References
2

where (xs, ys), (xi, yi) and (xd, yd) are the color coordinates of the
sample phosphors, the illuminant and the dominant wavelength,
respectively.
Fig. 9 shows the luminous intensity changes of CLTE with
raising temperatures. When the temperature was increased to
80 1C, the luminous intensity of CLTE only dropped to 91%. When
the temperature was increased to 120 1C, the luminous intensity of
CLTE still remained 80%, indicating that the Li-doped CET phosphor has very good thermal stability compared with the commercial Y2O3S:Eu3 . Because of these performances, CLTE phosphor
could be a potential candidate for tricolor while LEDs.
4. Conclusions
In this work, the Li-doping CaTiO3:Eu3 red phosphors with
different mole radios of Eu3 and Li to Ti were synthesized by
the conventional solid-state reaction method, and their formation,
morphology and PL properties were discussed as well. The asprepared phosphors show emission peaks from 580 to 700 nm and
the maximum emission wavelength is at 616 nm under the nearultraviolet excitation (398 nm). Results indicate that sintered
temperature and Eu3 content have a great inuence on the
luminescence characteristics of the CaTiO3:Eu3 phosphors, and
the optimal luminescence properties of CaTiO3:Eu3 phosphors
are typically obtained at 1300 1C with 12 mol% of Eu3 concentration. Furthermore, the red emission photoluminescence intensity
can be greatly enhanced by the incorporation of Li into the

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