Optik 125 (2014) 26562660

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Optik
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Photoluminescence study in Ce3+ activated M6 B5 AlO15 (M = Sr, Ca, Ba)

and mixed host aluminoborate phosphors
V.R. Kharabe a , Abha H. Oza b , S.J. Dhoble b,
a
b

Kamla Nehru Mahavidyalaya, Sakkardara Square, Nagpur 440 009, India

Department of Physics, R. T. M. Nagpur University, Nagpur 440033, India

a r t i c l e

i n f o

Article history:
Received 4 June 2013
Accepted 2 November 2013
Keywords:
Solid state synthesis
Phosphors
Photoluminescence

a b s t r a c t
In this paper we report the modied solid state synthesis of Ce3+ activated Sr6 B5 AlO15 , Ca6 B5 AlO15
Ba6 B5 AlO15 and mixed host aluminoborate phosphors. The prepared phosphors were characterized by
photoluminescence technique. The PL excitation spectra showed the excitation peaks ranging from 300
to 400 nm and emission spectra are observed in UV-blue region of spectrum and it varied for different
hosts. This kind of emission is due to 4f6 5d 4f7 transition of Ce3+ ion. Further PLE and PL emission spectra for various compositions Ca5 Sr1 B5 AlO15 , Ca4 Sr2 B5 AlO15 , Ca3 Sr3 B5 AlO15 , Ca2 Sr4 B5 AlO15 , CaSr5 B5 AlO15
are also taken which shows Ce3+ emission at 428 nm, 425 nm, 432 nm, 427 nm, 438 nm respectively. The
calculated 2 FJ (J = 7/2, 5/2) energy gap of Ce3+ in all hosts have been calculated and obtained values for
Sr6 B5 AlO15 , Ba6 B5 AlO15 phosphors are 1888 cm1 and 1330 cm1 respectively. PL emission spectra of
mixed host aluminoborates have shown slight variations in positions of emission peaks.
2013 Elsevier GmbH. All rights reserved.

1. Introduction
A great interest in phosphors has resulted in rapid developments
in the promising display and illumination technologies. For general
lighting applications such as in UV light-emitting diodes, various photoluminescent materials including different classes such
as oxides, silicates, aluminates, aluminoborates, aluminosilicates,
nitrides, borates, etc., play vital roles. Among all these hosts studied, borate phosphors are proved to be good candidates due to their
advantages like low synthetic temperature, easy preparation, and
high luminescent brightness. Recently, compounds belonging to
aluminoborate family seem to be promising for high luminescent
efciency and good thermal stability [14]. The aluminoborates
doped with rare earth ions have attracted much attention because
of their high UV transparency and non-linear properties. In addition, borates have exceptional optical damage threshold and are
able to withstand the harsh condition in vacuum discharge lamps
or screens. Yang et al. have reported luminescent properties of
RE3+ -activated CaAl2 B2 O7 (RE = Tb, Ce) in VUVvisible region [5].
Recently, Chang et al. [6] found that Na+ ion can be substituted
into sites within the planes of the linearly coordinated O atoms
of CaAl2 (BO3 )2 O leading to the formation of a-CaAl2 B2 O7 . You and
Hong [7] investigated the luminescent properties of b-CaAl2 B2 O7
doped with Ce3+ , Gd3+ and Tb3+ ions in the UVvisible range. Li et al.

Corresponding author.
E-mail address: sjdhoble@rediffmail.com (S.J. Dhoble).
0030-4026/$ see front matter 2013 Elsevier GmbH. All rights reserved.
http://dx.doi.org/10.1016/j.ijleo.2013.11.021

[8] also reported the long-lasting phosphorescence in rare-earthdoped calcium aluminoborate glass-ceramic with a-CaAl2 B2 O7 as
crystallites. Recently lot of work is going on toward exploring new
phosphors for lamp industry applications [9,10].
Ce3+ ions are represented by a simple one-electron system. The
electronic conguration of the ground and excited states of Ce3+
are 4f1 and 5d1 , respectively. The luminescent characteristics of
Ce3+ ions are known to depend upon whether the charge compensatory vacancy is associated with Ce3+ ions in the cases of similar
aliovalent substitution [11]. There is much interest in Ce3+ -doped
ionic crystals for applications in scintillators and tunable lasers
[12]. Ce-doped YAlO3 (YAP) and LuAlO3 (LuAP) perovskites are efcient high-response scintillators for medical applications [13,14].
Ce3+ doped (Y, Lu) aluminium garnet or perovskite single crystals are fast, high light yield, chemically stable and mechanically
hard scintillators [15,16] The Ce-doped single crystalline lms (SCF)
of Y3 Al5 O12 (YAG) and Lu3 Al5 O12 (LuAG) garnets obtained by liquid phase epitaxy (LPE) are currently considered for different eld
of applications, including the laser media, scintillators for monitoring of and -particles and components of mixed ionizing
uxes as well as the screens for visualization of X-ray and visible images [16,17]. Wide-band gap uoride materials, particularly
LiCaAlF6 :Ce3+ is known as a laser material [18]. Particularly in aluminoborates uorescent spectra of CaYBO4 :Ce3+ is very weak due
to photoionization [19], SrAl2 B2 O7 :Tb3+ used as novel green phosphors were fabricated by the solgel method [20], Liang et al. have
reported photoreduction of Eu3+ ions to Eu2+ aluminoborates [21].
Also cerium can be used as a host to study their PL properties, in this

V.R. Kharabe et al. / Optik 125 (2014) 26562660

2657

context, Atchyutha Rao et al. have discussed the photoluminescent

characterizations in Sr2 CeO4 phosphor [22].
The aim of this work is to report our investigation results
on the synthesis and PL properties of the Ce3+ -activated new
UV-blue emitting M6 B5 AlO15 (M = Ca, Sr, Ba) and mixed host aluminoborate such as Ca5 Sr1 B5 AlO15 , Ca4 Sr2 B5 AlO15 , Ca3 Sr3 B5 AlO15 ,
Ca2 Sr4 B5 AlO15 , CaSr5 B5 AlO15 under UV excitation.
2. Experimental details
In the present investigation M6 B5 AlO15 (M = Ca, Sr, Ba) phosphors were prepared via solid state synthesis under reduced atmosphere (charcoal environment). For the synthesis of Sr6 B5 AlO15
(Eq. (1)), starting raw materials with AR grade of 99.99% purity
were strontium carbonate (SrCO3 Himedia, 99.9%), calcium carbonate (CaCO3 Himedia, 99.9%), barium carbonate (BaCO3 Himedia,
99.9%), boric acid (H3 BO3 , Merk, 99.9%), aluminium nitrate and
Al(NO3 )3 9H2 O ammonium cerium nitrate NH4 Ce(NO3 )2 . The mixture of reagents was unite together to obtain a homogeneous
solution. For these compositions of the metal carbonate other raw
materials were calculated using the total oxidizing and reducing valencies of the components, which serve as the numerical
coefcients so that the equivalence ratio is unity. After mixing
for about 30 min, precursor solution was transferred to a furnace preheated to anneal at 600 C for 2 h under charcoal reducing
atmosphere. Then prepared phosphors were again re-annealed at
800 C for 2 h under same atmosphere. For synthesis of Ce3+ doped
M6 B5 AlO15 (M = Ca, Sr, Ba) phosphors cerium was introduced in the
form of ammonium cerium nitrate NH4 Ce(NO3 )6 and concentrations of the Ce ions were varied from 1, 2, 5, 10 mol%. The synthesis
reaction can be described as follows:
6SrCO3 + Al(NO3 )3 9H2 O + 5H3 BO3 + NH4 Ce(NO3 )6
Sr6 B5 AlO15 : Ce + 6CO2 + 3HNO3 + NH4 + 6NO2
+ 15H2 O + 3O2

(1)

6CaCO3 + Al(NO3 )3 9H2 O + 5H3 BO3 + NH4 Ce(NO3 )6

Ca6 B5 AlO15 : Ce + 6CO2 + 3HNO3 + NH4 + 6NO2
+ 15H2 O + 3O2

(2)

6BaCO3 + Al(NO3 )3 9H2 O + 5H3 BO3 + NH4 Ce(NO3 )6

Fig. 2. Emission spectrum of Ca6 B5 AlO15 :Ce phosphor.

corresponds to the promotion of an electron from one of the surrounding ions to the 4f orbit of the central ion. This is referred to
as the charge transfer state and written as 4fn 2p1 . Ce3+ , which is
in the 4f1 conguration, shows efcient luminescence owing to the
4f5d transitions. The luminescent colors or wavelengths of these
ions change widely from near UV to the red region depending on
the nature of the host lattices. The 4f5d transition of Ce3+ ions
in solids is a parity allowed electric dipole transition (ed) and has
large oscillator strength and produces efcient broadband luminescence. It has a larger Stokes shift than that of other RE ions due to
the extended radial wave functions of the 5d state. Data on photoluminescence (PL) of Ce3+ activated M6 B5 AlO15 (M = Ca, Sr, Ba) are
presented in the results discussed below. Although the PL intensities are expressed in arbitrary units, intensities in Figs. 111 are
expressed in the same relative units and the numbers are comparable.
3.1. Photoluminescent characteristics

Ba6 B5 AlO15 : Ce + 6CO2 + 3HNO3 + NH4 + 6NO2

+ 15H2 O + 3O2

Fig. 1. Excitation spectrum of Ca6 B5 AlO15 :Ce phosphor.

(3)

The photoluminescence measurement of excitation and emission spectra were recorded in the Shimadzu RF5301PC Spectrouorophotometer tted with a sensitive photomultiplier tube.
This spectrouorophotometer provides corrected emission and
excitation spectra in the 250720 nm and 230700 nm range
respectively. The same amount of sample was used in each case.
Emission and excitation spectra were recorded using spectral slit
width of 1.5 nm.

Photoluminescence (PL) characteristics of Ce3+ activated

CaB5 AlO15 aluminoborate are presented in Figs. 1 and 2. A broad
excitation spectrum peaks at 344 nm with the highest intensity
for 5 m%. The emission spectra (at 344 nm excitation) consist of a

3. Results and discussion

Ce3+ ions are usually in the form of broad bands and play a vital
role in excitation. For Ce3+ , this is vital for emission as well. The
bands referred to fall into two groups. In the rst group, one of the
4f electrons is raised to the higher 5d levels. Transitions from conguration 4fn to 4fn1 5d are allowed. The second group of bands

Fig. 3. Excitation spectra of Sr6 B5 AlO15 :Ce phosphor.

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V.R. Kharabe et al. / Optik 125 (2014) 26562660

Fig. 4. Emission spectra of Sr6 B5 AlO15 :Ce phosphor.

Fig. 8. Emission spectrum of Ca4 Sr2 B5 AlO15 :Ce phosphor.

Fig. 5. Excitation spectra of Ba6 B5 AlO15 :Ce phosphor.

Fig. 9. Emission spectrum of Ca3 Sr3 B5 AlO15 :Ce phosphor.

Fig. 6. Emission spectra of Ba6 B5 AlO15 :Ce phosphor.

double-peaked band between 375 and 550 nm caused by the transitions from the lowest energy level of the Ce3+ 5d conguration to
the spinorbit split 2 f5/2 and 2 f7/2 levels. The peaks are located at
390 nm (25,641 cm1 ) and 421 nm (23,753 cm1 ), respectively and
the doublet splitting amounts to 1888 cm1 which is close to the
value of 2 FJ (J = 7/2, 5/2) energy gap of Ce3+ (2000 cm1 ) in most
Ce3+ -activated phosphors [23]. The result of Ce3+ concentration
dependence on emission intensity in CaB5 AlO15 material is shown

Fig. 7. Emission spectrum of Ca5 SrB5 AlO15 :Ce phosphor.

Fig. 10. Emission spectrum of Ca2 Sr4 B5 AlO15 :Ce phosphor.

Fig. 11. Emission spectrum of CaSr5 B5 AlO15 :Ce phosphor.

V.R. Kharabe et al. / Optik 125 (2014) 26562660

Table 1
Intensity compression values for all prepared phosphors (i.e. Ca6 B5 AlO15 :Ce,
Sr6 B5 AlO15 :Ce, Ba6 B5 AlO15 :Ce) and mixed host aluminoborate phosphors.
Name of phosphor

Emission
wavelength (nm)

Intensity in
arb. unit

Ca6 B5 AlO15 :Ce (10 m%)

Ca6 B5 AlO15 :Ce (5 m%)
Ca6 B5 AlO15 :Ce (2 m%)
Ca6 B5 AlO15 :Ce (1 m%)

386
421
422
420

174
540
253
213

Sr6 B5 AlO15 :Ce (10 m%)

Sr6 B5 AlO15 :Ce (5 m%)
Sr6 B5 AlO15 :Ce (2 m%)
Sr6 B5 AlO15 :Ce (1 m%)

444
438
426
424

303
388
419
399

Ba6 B5 AlO15 :Ce (2 m%)

Ba6 B5 AlO15 :Ce (1 m%)

444
445

96
44

Ca5 SrB5 AlO15 :Ce (10 m%)

Ca5 SrB5 AlO15 :Ce (5 m%)
Ca5 SrB5 AlO15 :Ce (2 m%)
Ca5 SrB5 AlO15 :Ce (1 m%)

427
428
425
424

83
257
106
41

Ca4 Sr2 B5 AlO15 :Ce (10 m%)

Ca4 Sr2 B5 AlO15 :Ce (5 m%)
Ca4 Sr2 B5 AlO15 :Ce (2 m%)
Ca4 Sr2 B5 AlO15 :Ce (1 m%)

427
425
413
422

149
260
143
82

Ca3 Sr3 B5 AlO15 :Ce (10 m%)

Ca3 Sr3 B5 AlO15 :Ce (5 m%)
Ca3 Sr3 B5 AlO15 :Ce (2 m%)
Ca3 Sr3 B5 AlO15 :Ce (1 m%)

442
432
427
421

277
316
198
23

Ca2 Sr4 B5 AlO15 :Ce (10 m%)

Ca2 Sr4 B5 AlO15 :Ce (5 m%)
Ca2 Sr4 B5 AlO15 :Ce (2 m%)
Ca2 Sr4 B5 AlO15 :Ce (1 m%)

431
427
438
427

146
359
357
128

CaSr5 B5 AlO15 :Ce (10 m%)

CaSr5 B5 AlO15 :Ce (5 m%)
CaSr5 B5 AlO15 :Ce (2 m%)
CaSr5 B5 AlO15 :Ce (1 m%)

428
425
438
423

136
234
293
275

in Fig. 2. Ce3+ ion concentration was varied from 1 mol% to 10 mol%.

It can be seen that the emission intensity increases with increase
in Ce3+ concentration but when the value of cerium concentration
is greater than 5 mol%, the intensity decreases because of concentration quenching (values as shown in Table 1). When Ce3+ content
varies from 1 mol% to 10 mol%, the peak wavelength positions
slightly vary.
Photoluminescence excitation spectra of Sr6 B5 AlO15 :Ce3+ aluminoborate for various Ce3+ concentrations gives 340360 nm
broad band excitation (Fig. 3). The broad band excitation may be
due to the charge transfer from Ce3+ ion to O2 ion. Fig. 4 shows
PL emission spectra of Sr6 B5 AlO15 :Ce3+ . It shows blue emission at
around 426 nm attributed to the 4f6 5d 4f7 transition of the Ce3+
ion. As the ionic radius of Sr2+ is larger than that of Ce3+ ion, most
of the Ce3+ ions may enter in host lattice while few may be located
at the surface only. The low-symmetry location of Ce3+ results in
the predominate emission of 5d 4f transition. Different doping
of activator ions can inuence photoluminescence characteristics
of a phosphor, usually a low doping gives weak luminescence but
excess doping perhaps causes quenching of luminescence. According to this data and PL-spectra, it is seen that the Ce3+ content not
only affects the peak height but also the peak prole. Obviously,
with increase of Ce3+ content, the emission intensity increases relatively. When Ce3+ content varies from 1 mol% to 10 mol%, the peak
wavelength positions slightly vary. In the excitation, the spectral
positions of the bands at short wavelengths remain unchanged
while the band at the longest wavelength shifts from 339 to 342 nm
as the concentration changes from 1 m% to 10 m%. The maximum
intensity observed for 2 mol% i.e. luminescence quenches at 2 m%
(as shown the intensity values in Table 1). Stokes shift calculated
for the material Sr6 B5 AlO15 is 6024 cm1 as no doublet nature is

2659

observed in emission spectra the value for doublet splitting is not

calculated for this host.
The excitation spectra of Ba6 B5 AlO15 :Ce3+ phosphor shown in
Fig. 5 consist two bands at 241 nm and 355 nm, out of these two
the phosphor was excited at 355 nm. There are no more excitation bands which is due to direct excitation of the Ce3+ ions via
transitions to the components of the Ce3+ 5d conguration. The
PL emission spectra of Ba6 B5 AlO15 :Ce3+ phosphor as shown in
Fig. 6 exhibit blue emission band centered at 444 nm. Generally,
ground state conguration of Ce3+ ion is split in two levels (as
shown in above results) i.e. 2 F5/2 and 2 F7/2 whereas the 5 d1 excited
conguration is split by the crystal eld in 25 components. The
characteristic doublet of Ce3+ ion was not observed in the emission spectrum of Ba6 B5 AlO15 :Ce3+ phosphor. The PL results were
taken for 1 m% and 2 m% concentrations and maximum intensity
is obtained for 2 m%. The stokes-shift for Ba6 B5 AlO15 :Ce phosphor
observed approximately equal to 3000 cm1 . The emission spectra give isolated broad-band under UV-region. The calculated 2 FJ
(J = 7/2, 5/2) energy gap of Ce3+ in Ba is about 1330 cm1 , which is
less than the value of 2 FJ (J = 7/2, 5/2) energy gap of Ce3+ (2000 cm1 )
in most Ce3+ -activated phosphors [23].
The PL excitation and emission spectra for all the compositions
of Ca and Sr are studied as shown in Figs. 711. List of all mix
host aluminoborates phosphors for all concentrations of cerium ion
along with their emission peaks and PL intensities are presented in
Table 1. In all the cases the observed PL intensity is maximum for
5 mol% of cerium concentration so further all the PL results will be
compared with reference to 5 m% concentration of Ce3+ ion. In all
the results below PL concentration quenching is noted for 5 m% of
Ce3+ ion.
All the mixed host have broad band PL excitation from 230 to
400 nm due to the 4f5d transition of Ce3+ ions with prominent
peak at 345 nm. The PL emission at 345 nm exhibits broad band
extending from 400 to 650 nm for all the ratios of Ca:Sr, these are
due to the transition from 5d level to the ground state of the Ce3+
ion. It is observed that the PL emission band for ratios Ca5:Sr1,
Ca4:Sr2, Ca3:Sr3, Ca2:Sr4 and Ca:Sr5 are located at 428 nm, 425 nm,
432 nm, 427 nm and 438 nm respectively. The shifting in emission
bands may be due to mismatch among the crystal structures of host
ions (Ca and Sr) and activator (Ce ion). Also the ionic radius of Ce ion
is less than the ionic radii of Ca or Sr ion which may lead to the incorporation of Ce ions at various sites for various ratios of Ca and Sr. As
Sr2+ ions progressively replace the Ca2+ ions, the enhancement in PL
emission intensity is observed up to the ratio Ca2:Sr4 it means that
Ce3+ ions are allowed in CaSr lattice in a proper way for up to this
ratio only after which intensity get reduced, however, much more
study is needed to conrm the possible reason for this. Therefore,
Ce3+ activated Ca6x Srx B5 AlO15 phosphors may prove to be good
luminescence materials for lamp industry after detailed study.
Table 1 shows the list of all prepared compounds with their
emission wavelength (nm) and PL intensity (arb. unit)
4. Conclusion
We have reported here photoluminescence characteristics of
Ce3+ activated Sr6 B5 AlO15 , Ca6 B5 AlO15 and Ba6 B5 AlO15 phosphors
prepared via modied solid state synthesis. The emission spectra
of Sr6 B5 AlO15 :Ce3+ phosphor consists of a double-peaked band
between 375 and 550 nm caused by the transitions from the
lowest energy level of the Ce3+ 5d conguration to the spinorbit
split 2 f5/2 and 2 f7/2 levels. The peaks are observed at 390 nm
(25,641 cm1 ) and 421 nm (23,753 cm1 ), and the calculated doublet splitting amounts to approximately 1888 cm1 .The emission
spectra for Ca6 B5 AlO15 :Ce3+ shows the broadband with central
peak at 426 nm. In the emission, the peak positions for lower concentrations of Ce3+ ion remains same but observed slight change

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V.R. Kharabe et al. / Optik 125 (2014) 26562660

in positions for higher concentrations. Stokes shift calculated

for the material Sr6 B5 AlO15 is 6024 cm1 . The emission spectra
of Ba6 B5 AlO15 phosphor show broad blue emission peaking at
444 nm. The characteristic doublet of Ce3+ ion was not observed
in the emission spectrum of Ba6 B5 AlO15 :Ce phosphor. Further the
stokes-shift for Ba6 B5 AlO15 :Ce phosphor calculated approximately
equal to 3000 cm1 . The emission spectra gives isolated broadband under UV-region, the calculated 2 FJ (J = 7/2, 5/2) energy gap of
Ce3+ in Ba is about 1330 cm1 .The photoluminescence spectra for
different compositions of Ca:Sr were studied and PL emission band
for ratios Ca5:Sr1, Ca4:Sr2, Ca3:Sr3, Ca2:Sr4 and Ca:Sr5 are located
at 428 nm, 425 nm, 432 nm, 427 nm and 438 nm respectively. After
detailed study these phosphors may prove good hosts for other
activators also.
Acknowledgment
One of the authors SJD is thankful to Board of Research in Nuclear
Sciences (BRNS) (sanction letter no 2011/37P/10/BRNS/144),
Department of Atomic Energy, Govt. of India for nancial assistance
during the tenure of this work.
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