J Mater Sci: Mater Electron (2017) 28:8777–8783
DOI 10.1007/s10854-017-6604-4
Synthesis and photoluminescence properties of Eu doped
­LiBaPO4 phosphors for solid state lighting
D. N. Game1 · C. B. Palan3 · N. B. Ingale2 · S. K. Omanwar3
Received: 1 December 2016 / Accepted: 15 February 2017 / Published online: 27 February 2017
© Springer Science+Business Media New York 2017
Abstract Phosphor ­LiBaPO4: ­Eu3+ was successfully
synthesized by Pechini (citrate gel) method which is more
efficient than conventional high temperature solid state dif-
fusion reaction. X-ray diffraction analysis confirmed the
single phase formation of ­LiBaPO4 with hexagonal crystal
structure. Luminescence results showed that the phosphor
could be efficiently excited by near UV with intense exci-
tation peak at 393 nm and exhibited two bright red emis-
sion narrow bands. In the wavelength range 575–640 nm
these bands are centered at 595 and 615 nm, correspond-
ing to characteristics transitions 5D0→7F1 and 5D0→7F2
respectively of ­ Eu3+, with maximum intensity peak at
615 nm. When ­ Eu3+ in L ­ iBaPO4:Eu3+ was reduced by
the carbo-thermal reduction process to ­Eu2+ intense blue
broad emission band centered at 472 nm was obtained for
­LiBaPO4:Eu2+ phosphor when monitored at 350 nm. Hence
both of phosphors could be use in solid state lighting appli-
cation for fabrication of white light emitting diodes.
1 Introduction
White light emitting diodes (wLEDs), considered to be the
fourth generation of solid state lights and to replace tradi-
tional incandescent, halogen and fluorescent lamps have
attracted much attention and therefore have been widely
* D. N. Game
deorao.game@gmail.com
1
Cusrow Wadia Institute of Technology, Pune, India
2
Prof. Ram Meghe Institute of Technology and Research,
Badnera, Amravati, India
3
Department of Physics, Sant Gadge Baba, Amravati
University, Amravati, India
studied due to their special advantages such as high energy
efficiency, long lifetime, reliability, high luminous effi-
ciency, absence of mercury, short response time, main-
tenance as well as environmental protection [1–3]. The
combination of blue LED with yellow luminescence from
­Y3Al5O12:Ce3+ (YAG:Ce3+) phosphor material is one of
the methods to make white light [4] which suffer from the
low colour rendering index(CRI) and high colour tempera-
ture (Tc, usually above 5500 K). Another method to make
white light is to combine near ultraviolet LED and phos-
phors emitting different colors obtained with excitation
by this LED. Drawbacks in the case of earlier method can
be overcome by the use of this tri-band wLED, utilizing
RGB (red, green and blue) tricolor phosphor coatings on
the near ultraviolet (nUV) LED chip. Therefore, many red,
green and blue phosphors that can be excited by nUV light
should be developed [5]. Also, phosphors with high lumi-
nescent efficiency, stability and low cost are in demand for
application in wLED. Blue phosphor ­BaMgAl10O17:Eu2+
(BAM:Eu2+) has been intensively studied. However,
BAM:Eu2+ has two major problems namely thermal deg-
radation and UV damage, which lead to color shift and loss
in brightness.
Orthophosphate phosphors with a general formula
­ABPO4 (where A is a monovalent cation and B is a diva-
lent cation) are interesting because of their excellent
optical properties as well as thermal and hydrolytic sta-
bility. Recently, ­Eu2+ doped ­ ABPO4 phosphates have
received much attention for the potential applications in
Solid State Lighting (SSL) as new white light emission
diodes (wLEDs) phosphors, such as ­ KCaPO4:Eu2+ [6],
­KSrPO4:Eu [7], ­KBaPO4:Eu [8, 9], ­LiSrPO4:Eu2+ [10]
2+ 2+
and ­NaCaPO4:Eu2+ [11]. Therefore, many studies have
concentrated on ­ABPO4 phosphate. It was noticed that the
researchers worked with such type of materials always used
13
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8778
solid state diffusion [SSD] method for synthesis [12–16]
and Palan et al. has synthesized ­LiBaPO4 via solution com-
bustion synthesis method in which they used ammonium
nitrate [17, 18] but now a day ammonium nitrate has been
banned for its used in laboratory and such other places from
safety and security point of view. However, there were no
reports on the use of Pechini (citrate gel) method for syn-
thesis of such compound. The emphasis on Pechini (citrate
gel) method of synthesis was in view of drawbacks of SSD
[19, 20]. The main drawbacks of SSD are,
• SSD not only requires highly sophisticated equipment
but also very high temperature for diffusion process
and produces phosphors with coarse grain size having
non-homogeneous properties due to limited diffusion
lengths.
• Repeated cycles of heating and cooling, followed by
intermediate crushing/ grinding, required for the fusion
of materials produces lots of physical defects.
• This not only increases the time of reaction but also
introduce chemical impurity during crushing /grinding.
• Phosphors produced by this method are not suited for
the fabrication of thin films or coatings of LEDs for pro-
duction of wLEDs because the incorporated impurities
and physical defects produced during the reaction affect
the efficiency of phosphor.
In the light of above discussion and to overcome draw-
backs of SSD the E ­ u3+ doped ­ LiBaPO4 phosphor was
successfully synthesized by Pechini (citrate gel) method
which is low temperature thus cost effective, time saving
and producing more efficient phosphors. The phosphors
presented in this paper exhibit strong absorption below
400 nm suitable for SSL application with near UV LEDs
as a pumping source. ­LiBaPO4:Eu3+synthesized by Pechini
(citrate gel) method exhibits intense red narrow emission
bands whereas phosphor ­LiBaPO4:Eu2+ produced by carbo
thermal method shows intense blue broad emission band.
Hence these materials have potential application as red and
blue phosphors in nUV LEDs and definitely employed as
red and blue members respectively in production of tricolor
wLED using RGB phosphors in SSL.
2 Experimental
2.1 Synthesis of ­Eu3+doped ­LiBaPO4 phosphor
For synthesis of ­Eu3+ (0.001, 0.003, 0.005, 0.010 and
0.020 moles) activated orthophosphate ­LiBaPO4 phosphors
stoichiometric amount of the analytical grade precursors
Ba(NO3)2, ­Eu2O3 converted to Eu(NO3)3·6H2O and L ­ iNO3
were taken in a china clay basin and dried in a desiccator.
13
J Mater Sci: Mater Electron (2017) 28:8777–8783
­(NH4)H2PO4 was separately dried in another china basin
and mixed together with above dried precursors. The dried
precursors were then finely milled. Stoichiometric amount
of Citric acid monohydrated and Ethylene glycol along
with two drops of Glacial acetic acid were added to dried
precursors and stirred continuously. On slow heating to
140 °C for ∼1 h, above solution boils with the evolution
of pale yellowish brown fumes and the process of gelation
started. The mixture was then allowed to cool leading to
a thick pale yellow gel. The gel was further heated slowly
to 350 °C in air. The polymerization took place and a pale
yellow resin/foam was formed and was pyrolysed into stun-
ning black foam at 450 °C, which started burning at 600 °C.
The complete pyrolysis took place at 780 °C for 2 h. The
white powder so obtained was ­LiBaPO4:Eu3+ phosphor.
2.2 Preparation of ­Eu2+doped ­LiBaPO4 phosphor
Above synthesized ­ LiBaPO4:Eu3+ phosphors with dif-
ferent concentration of E ­ u3+ (0.001, 0.003, 0.005, 0.010
and 0.020 moles) was then subjected to the carbo-thermal
reduction slowly first at 600 °C for 1 h then at 980 °C for
4 h in presence of activated carbon (charcoal powder) so
as to reduce the trivalent ­(Eu3+) activator to divalent state
­(Eu2+). Thus reduced white crystalline orthophosphate
­LiBaPO4:Eu2+ phosphors were prepared.
2.3 Instrumentation
The phase purity of the prepared phosphors was inves-
tigated by a Rikagu Meniflex II X-ray diffractometer
(XRD) with Cu Kα radiation (λ = 1.54060 Å) at 40 kV
and 30 mA. The XRD patterns were collected in range of
10° ≤ 2θ ≤ 70°. Photoluminescence measurement at room
temperature was performed on a Hitachi F-7000 Spectro-
fluorimeter equipped with a 450 W Xenon lamp, in the
range 200–700 nm, with spectral width of 1 nm, spectra
were corrected using Rhodamine B standard by following
the procedure prescribe by Hitachi. Concentration quench-
ing study was carried out and chromaticity coordinates are
calculated. Surface morphology and elemental composi-
tion of phosphors was studied by using JEOL’s Scanning
Electron Microscope model JSM-6360A fitted with EDX
facility.
3 Results and discussion
3.1 Study of X‑ray diffraction (XRD) pattern
The XRD pattern of the prepared Eu doped L ­ iBaPO4
orthophosphate phosphor prepared by Pechini (citrate gel)
method is shown in Fig. 1.
J Mater Sci: Mater Electron (2017) 28:8777–8783
Fig. 1  XRD pattern of Eu doped L
­ iBaPO4 phosphor with ICDD file
According to the International Center for Diffraction
Data (ICDD 00-014-0270) as a reference, all the major
high intensity peaks are matching exactly with the stand-
ard patterns of pure L ­ iBaPO4 phosphor, though there are
few small intensity peaks in 2θ range at 25.36°, 51.2°,
66.82° and 68.62°. This indicates that the incorporated
dopant ions have not caused any significant changes
to the crystal structure of ­LiBaPO4 matrix. The doped
product crystallizes as hexagonal crystal structure with a
space group P63 volume = 391.577 Å3 and Z = 4.
Experimentally, X-ray diffraction (XRD) pattern
reveals that no other products or starting materials were
observed, implying that the ­Eu3+ ions entered into the
­LiBaPO4 structure and have almost no effect on the
­LiBaPO4 composition [21]. Though the substitution of
­Eu3+ for ­Ba2+ in ­LiBaPO4:Eu3+ phosphor is non-equiv-
alent as far as charge compensation is concern, lattice
defects created during crystal formation keep charge bal-
ance without any distortion in crystal lattice as the con-
centration of added impurity is very small. The results of
Ricardo D.S. Santos et al. indicate that the most favora-
ble energy schemes are predicted for the incorporation of
­Eu3+ ions at Ba sites in ­LiBaPO4 with ­LiBa antisite defect,
i.e., Li substitution at Ba site [22]. The Ba site preference
has been cited in the experimental work by Puppalwar
et al. [23] and Zang et al. [24] but they did not report
the preferred charge compensation defect involved in the
­Eu3+ substitution. The conclusions of these workers were
based on ion size comparisons between the Eu dopant
ions and cations at host site.
8779
3.2 Study of morphology of Eu doped ­LiBaPO4
phosphors
SEM images of as synthesized L ­ iBaPO4:Eu3+ phosphor
prepared by Pechini (citrate gel) method and L ­ iBaPO4:Eu2+
phosphor prepared by carbo-thermal reduction method
in presence of charcoal sintered at 980 °C is presented in
Fig. 2. Micrograph shows some voids in SEM image of
­LiBaPO4:Eu3+ phosphor, those are due to degassing dur-
ing the process of gelation. The obtained micrograph shows
that the particles are of irregular morphology with some
amount agglomeration. Though the accurate measurement
of particle size is not be possible but from resolution scale
one can estimate the approximate particle size of the pre-
pared phosphors as less than 1 μm to few micrometer in
range which is a suitable size for fabrication of SSL devices
[25]. From literature, it is evident that the polycrystalline
powder in which particles consisting of many crystallites
with particle size in micrometer range will find many other
applications as it can exhibit high luminescent intensi-
ties [26]. Like applications of high definition television
(HDTV), plasma display panels (PDP), cathode ray tube
(CRT), and field emission displays (FED).
3.3 Study of energy dispersive spectra of prepared
phosphors
The following energy dispersive spectrum of prepared
­LiBaPO4:Eu3+ phosphor [Fig. 3] shows prominent peaks
corresponding to elements Ba, P and O and small peaks of
13
8780
Fig. 2  SEM images of a
­Eu3+ and b ­Eu2+ doped
­LiBa0.99PO4: 0.01Eu phosphor
Fig. 3  EDS pattern of
­LiBa0.99PO4: 0.01Eu phosphor
with elemental composition
dopant element Eu. From elemental composition of pre-
pared phosphor it is clear that the elements are in appro-
priate atomic ratio. Peaks of Li is absent being low energy
element whereas some peaks indicating Pt which are due
to platinum that was being used for coating purpose during
sample preparation for scanning electron microscopy.
3.4 Photoluminescence properties (PL)
The excitation and emission spectra of the as synthesized
phosphors ­LiBaPO4:Eu3+ and ­LiBaPO4:Eu2+ were studied
in order to judge their potential as the phosphor to be used
for nUV LED based wLEDs.
3.4.1 Photoluminescence properties of ­LiBaPO4:Eu3+
Figure 4a shows combined excitation and emission pho-
toluminescence spectra of as synthesized ­LiBaPO4:Eu3+
phosphor. Excitation spectra consist of some low inten-
sity narrow bands in the wavelength range 300–400 nm,
13
J Mater Sci: Mater Electron (2017) 28:8777–8783
which can be attributed to 7F0→5DJ and 7F0→5LJ along
with high intensity excitation peak at 393 nm correspond-
ing to 7F0→5L6 transitions of E ­ u3+ ions which is well in
agreement with the emission wavelengths of nUV LED.
Like in literature elucidating the nature of the Eu lumines-
cence centers in ­LiBaPO4 which examined the lumines-
cence properties of the ­Eu3+ ions, in the present case also
it is observed that the luminescence excitation spectrum of
­Eu3+ ions in L
­ iBaPO4 (λem = 615 nm) has a low intensity
broad band centered at 244 nm, associated with the charge
transfer from the 2p orbital of ­O2− to the free 4 f orbital
of the ­Eu3+ions. Emission spectra of the as synthesized
­LiBaPO4:Eu3+ phosphor monitored at 393 nm exhibited
low intensity broad bands in wavelength rage 530–570 nm
and two high intensity red emission narrow bands in the
wavelength range 575–605 nm and 605–640 nm corre-
sponding to 5D0→7F1 and 5D0→7F2 transitions of ­ Eu3+
centered at 592 and 615 nm respectively with maximum
intensity at 615 nm in addition to this one small inten-
sity narrow peak at 580 nm and two low intensity narrow
J Mater Sci: Mater Electron (2017) 28:8777–8783
Fig. 4  a Combined excitation (a)
LiBaPO4:(0.01)Eu
and emission spectra for E ­ u3+ 50
activated ­LiBaPO4 phosphor. b Excitation for 615 nm
Combined excitation and emis-
40
sion spectra for ­Eu2+ activated
­LiBaPO4 phosphor
Intensity (a.u.)
30
20
10
0 0
200 300 400
Wavelength (nm)
bands centered at 654 nm and beyond 700 nm correspond-
ing to 5D0→7F0, 5D0→7F3 and 5D0→7F4 transitions of ­Eu3+
respectively.
3.4.2 Photoluminescence properties of ­LiBaPO4:Eu2+
Though the substitution of E ­ u3+ for ­Ba2+ in L
­ iBaPO4:Eu3+
phosphor is non-equivalent as far as charge compensation
is concern, lattice defects created during crystal formation
keep charge balance without any distortion in crystal lattice
as the concentration of added impurity is very small. This
can also be explained from the fact that excitation spectrum
of ­LiBaPO4:Eu3+ phosphors have a charge-transfer band
(CTB) [associated with transition of (2p) ­O2−→(4 f) ­Eu3+]
in the wavelength region of 200–300 nm which can be
interpreted as a spectroscopic feature of E ­ u3+ ions occupy-
ing the alkali-metal sites in the structure of the compound
[27]. Based on the above mention fact it can be presumed
that the ­Eu3+ ions occupy predominantly the alkaline-
earth metal sites in L­ iBaPO4. To confirm this presump-
tion, the ­LiBaPO4:Eu2+ phosphor solely containing ­Eu2+
ions was prepared in a reducing atmosphere by heating
­LiBaPO4:Eu3+ phosphor in presence of activated carbon at
980◦C for 4 h. It was found that the narrow bands associ-
ated with the 5D0→7FJ (J = 0, 1, 2, 3, 4) transitions in the
­Eu3+ ions [Fig. 4a] in the emission spectrum in the wave-
length range 575–640 nm disappears and broad emission
band in the wavelength range 400–600 nm, associated with
4 5
F6 D1→4F7 transitions in E ­ u2+ ions appeared (Fig. 4b).
Combined excitation and emission photolumines-
cence spectra of prepared ­ LiBaPO4:Eu2+ phosphor is
shown Fig. 4b. The excitation spectra of L ­ iBaPO4:Eu2+
phosphor sintered in reducing atmosphere, monitored
at 472 nm, exhibits a broad band, which extends from
220 to 420 nm. This high intensity band can be attrib-
uted to the 4f–5d transition of ­Eu2+ ions. The prominent
excitation peak is located at 322 nm with shouldering at
8781
3+ (b)
400 2+
LiBaPO4:(0.01)Eu
Emission for393 nm
Excitation for 472 nm
Emission for322 nm
300 Emission for350 nm
Intensity (a.u.)
200
100
500 600 700 200 300 400 500 600
Wavelength (nm)
350 nm. The emission spectra of same phosphors when
monitored at 350 nm as the excitation wavelength are
dominated by the broad and intense band in the wave-
length 400–600 nm centered at 472 nm which corre-
sponds to the allowed f-d transition of ­Eu2+. This broad
luminescence band of ­Eu2+ is due to 4F65D1→4F7 transi-
tions, which is an allowed electrostatic dipole transition.
The full width at half maximum (FWHM) of the emis-
sion band is around 85 nm.
Similarly presence of low intensity bands, in wave-
length range 450–575 nm, in emission spectra of
­LiBaPO4:Eu3+ (Fig. 4a) may be due t­o4F65D1→4F7 tran-
sitions in ­Eu2+. This indicates that some amount of ­Eu2+
ions is also present in ­LiBaPO4:Eu3+ phosphor showing
possibilities of reduction of trivalent ­Eu3+ ions to diva-
lent ­Eu2+ ions in absence of reducing medium at high
temperature. It can be concluded that some ­ Eu2+ ion
exists and the reduction of ­Eu3+ to ­Eu2+ takes place in
­LiBaPO4:Eu2+ phosphors prepared in strongly reducing
atmosphere by carbo-thermal reduction method.
Once ­Eu2+ is embedded in the structure, after the
reduction process in the sample sintering, it is hardly
oxidized in order to return to the E ­ u3+ form. The coex-
2+ 3+
istence of E ­ u /Eu has been reported in several phos-
phors. ­Eu3+ and ­Eu2+ ions also seems to be able to enter
and coexist in ­LiBaPO4 samples, such a coexistence has
also been observed by Zhang et al. [24] based on pho-
toluminescence analysis. This means that not all of the
­Eu3+ ions added to the sample are actually converted to
the desired divalent state upon heat treatment in a reduc-
ing atmosphere. The oxidation state and ionic radius of
dopant ions ­(Eu2+, ­Eu3+) are comparable to divalent cat-
ion ­(Ba2+) in the host lattice. Considering both the facts
and in the sight of above discussion it can be presumed
that these lanthanide ions in the ­LiBaPO4 phosphor lat-
tice predominantly occupies the B ­ a2+ sites.
13
8782 J Mater Sci: Mater Electron (2017) 28:8777–8783

3.5 Effect of concentration of Eu ions on emission

intensity of prepared phosphors

Figure 5 shows the graphs between emission inten-

sity and dopant concentrations in ­ LiBaPO4:Eu3+ and
2+
­LiBaPO4:Eu . The emission intensity increases with
increasing of Eu concentration, and reaches the maxi-
mum at about 1 mol%. The positions of the emission.
Concentration quenching occurs, when the Eu con-
centration is beyond 1 mol%. Qiu et al. [28] showed that
the probability of energy transfer among the Eu ions
increases to a certain extent with the increase in Eu ion
concentration in the host matrix. Blasse proposed the
critical energy transfer distance ­(Rc) to realize the mech-
anism of energy transfer in phosphors whereby R ­ c is
approximately equal to twice the radius of a sphere with
the volume as shown in the following equation [29–31].
( )1
3V 3
Rc ≈ 2
4𝜋xc N ­ iBaPO4: ­Eu3+ and ­LiBaPO4:Eu2+
Fig. 6  Chromaticity diagrams of L
In which ­ Xc is the critical concentration, N is the phosphors
number of cations in the unit cell and V is the volume
of the unit cell. The unit cell volume V of ­LiBaPO4 is
due to multipole–multipole interaction which is respon-
0.391577 ­nm3, the critical concentration Xc is 0.01,
sible for the energy transfer of forbidden transitions [31].
resulting from the maximum intensity of ­LiBa1 − xPO4:
xEu at x = 0.01 and the number of host cations in the unit
3.6 Study of colour chromaticity
cell of ­LiBaPO4 is 4. Based on the above values, the criti-
cal distance of energy transfer R ­ c is calculated as 2.7 nm
In general, color is represented by means of color coordi-
i.e., 27 Å. As R
­ c is more than 5 Å exchange interaction is
nates. The chromaticity diagram established by the Com-
not responsible for non-radiative energy transfer process
mission Internationale de l’Eclairage (CIE) in 1931 is a two
between different E ­ u3+ ion in the host. Similarly radiation
dimensional graphical representation of any color perceiva-
reabsorption is possible only if there is overlapping of
ble by the human eye on an x–y plot. Hence, in our present
excitation and emission spectra. Thus, in view of PL and
work, the chromaticity coordinates of ­LiBaPO4:Eu3+ and
PLE spectra of L ­ iBaPO4: Eu, radiation reabsorption is
­LiBaPO4:Eu2+ phosphors (Eu = 1 mol %) has been calcu-
unlikely to occur. As a result energy transfer between dif-
lated from their corresponding emission spectra as (0.562,
ferent Eu ions in ­LiBaPO4 phosphor may have happened
0.363) and (0.164, 0.232) shown in Fig. 6a, b respectively,
demonstrate better colour purity.

Fig. 5  Effect of dopant concen- (a) 50 (b) 400

tration a ­LiBaPO4: ­Eu3+ and b
­LiBaPO4:Eu2+
40
300
Intensity (a.u.)

Intensity (a.u.)

30 0.001 Eu
0.001 Eu 0.003 Eu
0.003 Eu 200 0.005 Eu
0.005 Eu 0.01 Eu
20 0.02 Eu
0.01 Eu
0.02 Eu
100
10

0 0
550 600 650 400 500 600
Wavelength (nm) Wavelength (nm)

13
J Mater Sci: Mater Electron (2017) 28:8777–8783
4 Conclusions
Photoluminescence measurements showed that ­Eu2+ doped
orthophosphate exhibited intense broad band emission
peaking at 472 nm under nUV excitation whereas ­Eu3+
doped orthophosphate showed two narrow-bands of intense
red emission peaking at 595 and 615 nm under nUV exci-
tation. Thus blue and red LEDs can be fabricated by pre-
coating above synthesized phosphor on nUV LED source.
Similarly wLEDs can be fabricates using these phosphors
along with green emitting phosphor like ­NaCaPO4:Eu2+
by coating onto 395 nm-emitting InGaN chips. Thus it
indicates that the above synthesized orthophosphate phos-
phors are potential and promising candidate for fabrica-
tion of nUV based wLEDs. Since the width of the emis-
sion peak of an LED is much broader than the absorption
line of ­Eu3+, the overlap is actually quite low (and too low
for applications). Whereas absorption band of ­Eu2+ is quite
broad showing very good overlapping with emission peak
of LED thus the emission intensity of L ­ iBaPO4:Eu2+ is
very high in comparison with L ­ iBaPO4:Eu3+. This is the
2+
major advantage of E ­ u over E ­ u3+ as far as SSL applica-
tions are concerned.
Some ­Eu2+ ion that exist in ­ LiBaPO4:Eu3+ phos-
phor and the reduction of ­Eu to ­Eu2+ taken place in a
3+
­LiBaPO4:Eu3+ phosphors can be stabilized by providing
strongly reducing atmosphere using reducing agent, like
activated charcoal in carbo-thermal reduction method in
present case. From the luminescence examination finally it
can be concluded that the both ­Eu2+ and ­Eu3+ ions co-exist
in ­LiBaPO4 and occupy predominantly the alkaline-earth
metal sites.
Acknowledgements Author, DNG, is thankful to the Head of the
Department of Physics, Sant Gadge Baba Amravati University, Amra-
vati for providing all the necessary research facilities and also to the
Principal, Cusrow Wadia Institute of Technology, Pune for his con-
stant encouragement and guidance.
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