Thermally stimulated luminescence and electron

paramagnetic resonance studies of Eu3+-doped yttrium borate

M. Anitha
Rare Earth Development Section, Bhabha Atomic Research Center, Mumbai—400 085, India
Manoj Mohapatra, R.M. Kadam,a) and T.K. Seshagiri
Radiochemistry Division, Bhabha Atomic Research Center, Mumbai—400 085, India
A.K. Tyagi
Chemistry Division, Bhabha Atomic Research Center, Mumbai—400 085, India
V. Natarajan
Radiochemistry Division, Chemistry Division, Bhabha Atomic Research Center,
Mumbai—400 085, India

(Received 30 September 2005; accepted 22 November 2005)

Thermally stimulated luminescence (TSL) and electron paramagnetic resonance (EPR)

studies were carried out on gamma-irradiated europium-doped yttrium borate samples
in the temperature range 300–600 K. TSL studies showed the presence of two glow
peaks, a relatively weaker one at 390 K and an intense one at around 550 K.
Room-temperature EPR spectrum of irradiated samples revealed the formation of two
hole trapped radicals, namely, BO32− and O2−. Temperature variation studies showed
drastic reduction in the EPR signal intensities of these radicals around 390 and 550 K
indicating thermal destruction of O2− and BO32− radicals, respectively. The observed
TSL emission is caused by the recombination of thermally released holes from O2−
and BO32− radical ions with electrons. The energy released in electron-hole
recombination process is used for the excitation of Eu3+ ion resulting in TSL glow
peaks. TSL emission studies confirmed that Eu3+ acts as luminescent center for both
the peaks.

I. INTRODUCTION used to prepare LnBO3:Eu3+ phosphor materials with the

Rare-earth ortho-borates, RBO3 (R ⳱ Y, La, Gd and
Lu) doped with rare-earth ions (Eu3+ and Tb3+) form an
interesting class of luminescent materials, as they yield
luminescence with high efficiency under vacuum ultra-
violet (VUV) excitation.1 Therefore, ortho-borates are
potential candidates for luminescent materials to be used
in flat displays, mercury-free fluorescent tubes, plasma
display panels, and detector systems.2 Lutetium borate
doped with Ce3+ has particularly interesting characteris-
tics for applications as radiation detector. In addition to
this, yttrium aluminum borate (YAl3B4O12) and yttrium
borate have excellent nonlinear optical properties, and
their doped crystals are important for building microchip
lasers.3,4 Various synthesis methods such as solid-state
reaction, co-precipitation, microwave heating, spray py-
rolysis, sol-gel, and hydrothermal methods have been
a)
Address all correspondence to this author.
e-mail: rmkadam2003@yahoo.co.in
DOI: 10.1557/JMR.2006.0134
goal of achieving desirable properties like enhancement
of photoluminescence (PL) intensity and better chroma-
ticity.5–7 These studies indicate that LnBO3 is a good
host material with excellent luminescent properties when
doped with a suitable activator. For example, Eu3+-doped
YBO3 is shown to be a promising orange red emission
luminescent material.5 Though there is a wealth of infor-
mation available in literature on the luminescence prop-
erties of Eu3+-doped YBO3, as far as we know, there is
no report on the thermally stimulated luminescence
(TSL) study on these samples. In the recent past, TSL
and electron paramagnetic resonance (EPR) techniques
have been extensively used to investigate a number of
rare-earth doped inorganic phophors.8–10 The present pa-
per focuses on the preparation, characterization, TSL,
PL, and EPR measurements on europium-doped samples
of YBO3. TSL studies give information on the trap depth
and thermal escape probabilities, while information on
the microscopic structure and chemical nature of the
traps involved can be obtained by studying their thermal
stabilities using EPR. The complimentary nature of the
information obtained from these two techniques can be

J. Mater. Res., Vol. 21, No. 5, May 2006 © 2006 Materials Research Society 1117
 M. Anitha et al.: Thermally stimulated luminescence and electron paramagnetic resonance studies of Eu3+-doped yttrium borate
utilized for understanding the processes leading to TSL.
Further PL studies, when used in conjunction with TSL
and EPR, can shed light on the oxidation state of the
dopant ion incorporated in YBO3 lattice.
II. EXPERIMENTAL
Yttrium oxide was dissolved in concentrated nitric
acid. To this, saturated solution of oxalic acid was added
to precipitate yttrium as yttrium oxalate. The oxalate pre-
cipitate was dried and later heated at 820 K to get pure
yttrium oxide. Stoichiometric quantity of boric acid was
added to it; the mixture was ground thoroughly in a mor-
tar and annealed at 1070 K for 20 h. Europium-doped
samples were prepared in a similar way by dissolving the
required amounts of yttrium oxide and europium oxide
(Eu2O3) in concentrated HNO3 followed by precipitation
as oxalate. The europium concentration in the sample
was varied in the range 0.5–2 at.%.
X-ray diffraction patterns of the samples were re-
corded using Cu K␣ radiation (␭ ⳱ 1.5418 Å) employing
a Phillips X-ray diffractometer (model PW 1710, Eind-
hoven, The Netherlands) fitted with graphite crystal
monochromator. The x-ray diffraction patterns were col-
lected at room temperature in the range 10–65° with a 2␪
step of 0.05°. EPR studies on these samples were carried
out using a Bruker ESP-300 spectrometer (Ettlingen,
Germany) operated at X band frequency (9.5 GHz) with
100 kHz modulation frequency. Di phenyl picryl hydra-
zyl (DPPH) reference was used as the g-marker. TSL
studies were carried with a home-built unit, whereas
photo luminescence spectra were recorded using FL 900
Edinburgh fluorescence spectrometer (UK). The
YBO3:Eu3+ samples were irradiated in a 60Co gamma
source (dose rate 2.7 kGy/h) prior to TSL and EPR ex-
periments.
III. RESULTS
A. Chemical and physical characterization of
synthesized YBO3:Eu3+ polycrystalline samples
The phase purity of the material was analyzed by x-ray
powder diffraction measurements. The diffraction pat-
terns of the product obtained by solid-state reaction in-
dicated that YBO3:Eu3+ crystallizes in the hexagonal
structure (space group P63/m). There was no impurity
phase formation even in 2% Eu3+ doped YBO3 sample.
The observed lattice parameters were found to be in good
agreement with those reported in the literature11 (Card
No. 16-0277). A marginal increase in the lattice param-
eters and unit cell volume was observed with increase in
Eu3+ concentration, which is due the substitution of Eu3+
at Y3+ sites (the ionic radius of Eu3+ is 0.953 Å and that
of Y3+ is 0.893 Å)
The crystal structure of YBO3 has been investigated in
detail.12,13 Yttrium is 8-fold coordinated by oxygen
1118 J. Mater. Res., Vol. 21, No. 5, May 2006
atoms in an arrangement which can be described as a
trigonal bicapped antiprism. The oxygen atoms surround-
ing the Y3+ ions occupy two crystallographic sites: six
oxygen (O1) atoms in (4f) and two oxygen (O2) atoms in
(6h) with partial occupancy of 1/3. The Y–O (1) and
Y–O (2) distances are respectively 2.39 and 2.32 Å. Bo-
ron is 4-fold coordinated. [BO4] tetrahedra are of two
types; the first one (I) is a very regular tetrahedron with
B-O distances in the range 1.37–1.57 Å, and the second
one (II) is slightly distorted tetrahedron with two similar
short bonds (1.37 Å) and two large bonds ranging from
1.89 to 1.92 Å. The structure of YBO3 consists of a three-
dimensional (3D) network obtained by connecting [YO8]
polyhedra, wherein each [BO4] group is linked with two
adjacent [BO4] groups by O2 atoms and with two adja-
cent [YO8] groups by O1 atoms. The Y atom has unique
coordination, but two different environments can be ob-
served because of O(2) statistical distribution. Deviation
from the ideal S6 symmetry is due to existence of these
two O(2) atoms.
B. TSL studies
TSL studies were carried out on gamma-irradiated un-
doped/Eu-doped samples in the region, 300–700 K. In
undoped yttrium borate samples, a very weak TSL glow
was observed. TSL studies were carried out on gamma-
irradiated samples with 0.5%, 1%, 2%, and 2 at.% Eu
content. All the samples showed two glow peaks around
392 and 550 K (dose ⳱ 4 kGy), the TSL yield being
maximum in 1% Eu3+-doped samples. Of these, the peak
at 550 K was the most intense one. The TSL glow pattern
obtained for Eu-doped samples is shown in Fig. 1. All the
glow curves were recorded at heating rate of 2.5 K/s. The
TSL yield per unit mass of the various Eu-doped samples
when plotted as a function of dopant (Eu) concentration
clearly indicates that there is concentration quenching at
concentration of Eu beyond 1%. This is shown in Fig. 2.
Systematic gamma dose dependence study of the glow
peaks showed that intensity of both the peaks saturates
after a gamma dose of 5 kGy. To evaluate the trap pa-
rameters on the basis of the Arrhenius plot, the glow
peaks were obtained at several heating rates of 2.5, 1.5,
1, and 0.5 K/s. A plot of ln(Tm2/␤) versus 1/Tm (where ␤
corresponds to the heating rate and Tm represents the
peak temperature in K) was made, and trap depth was
calculated from the slope of the resultant graph. Least-
square fit data were used to determine the trap param-
eters, namely, trap depth and frequency factor. The trap
depth value and frequency factor obtained for the 392 K
peak are 0.56 eV, and 1.7 × 106 s−1, and that of 550 K
peak are 1.0 eV and 1.2 × 109 s−1, respectively. Alterna-
tively, the trap depth values were also evaluated by con-
ducting TSL experiments connected with the initial rise
method. The values obtained for the 392 and 500 K
peaks are 0.53 and 1.02 eV, respectively.
 M. Anitha et al.: Thermally stimulated luminescence and electron paramagnetic resonance studies of Eu3+-doped yttrium borate

FIG. 1. TSL glow curve of gamma irradiated YBO3:Eu3+ (1%) to the FIG. 2. TSL yield as a function of concentration of dopant ion.
dose of 5 kGy.

To study the spectral composition of the glow peaks,

the glow curves of the samples were recorded using
transmittance and interference filters. Spectral groups
around 585 and 600 nm were observed, which are char-
acteristic of the Eu3+ ion, as reported in literature.6

C. PL studies
PL studies were carried out on yttrium borate doped
with Eu3+ both before and after gamma irradiation. The
photoluminescence spectrum of 1% Eu doped sample
under 230 nm excitation wavelength is shown in Fig. 3.
The PL spectra consist of a number of sharp lines ranging
from 580–725 nm, which are associated with the transi-
tion from the excited 5D0 → 7FJ (J ⳱ 1, 2, 3, 4) levels
of Eu3+ activator, out of which, 5D0 → 7F1,2 transitions
(590, 610, and 625 nm) were found to be intense.6,12–14
The red emission at 610 nm (R) from 5D0 → 7F2 is an
FIG. 3. Photoluminescence excitation and emission spectra of Eu3+
electric dipole transition, while the orange emission at (1%) doped YBO3 sample at 300 K.
590 nm (O) from 5D0 → 7F1 is a typical magnetic dipole
transition. The relative intensity between them strongly
depends on the local symmetry around Eu3+ ions, and a as reported earlier.6,12–14 Similarly, the excitation spectra
lower symmetry of the crystal field around Eu3+ would obtained using 590 nm emission wavelength showed
result in a higher R/O value. The higher value of R/O broad charge transfer band around 225 nm. The depend-
observed under present investigations suggests lower ence of PL intensity of the peak at 610 nm on the dopant
crystal field symmetry around Eu3+ ions in YBO3 matrix concentration was also investigated, showing maximum

J. Mater. Res., Vol. 21, No. 5, May 2006 1119

 M. Anitha et al.: Thermally stimulated luminescence and electron paramagnetic resonance studies of Eu3+-doped yttrium borate

luminescence intensity for 1% Eu3+ ions in YBO3. Be-

yond this concentration, quenching was observed. The
concentration quenching effect was attributed to the pos-
sible non-radiative energy transfer between neighboring
Eu3+ ions, which increases the mobility of the excited
states within the host matrix and therefore increases the
probability of non-radiative de-excitation via traps.15,16
The absence of broad emission around 400 nm due to
4f 65d → 8S7/2 electric dipole transition suggested ab-
sence of Eu2+ formed in gamma-irradiated europium-
doped YBO3 samples.

D. EPR studies
Unirradiated YBO3 doped Eu3+ samples did not show
any EPR signal indicating the absence of any paramag-
netic species. Eu3+ (4f 6, 7F0) does not give EPR spec-
trum as its ground state is singlet and it is diamagnetic in
nature. However, if paramagnetic Eu2+ (4f 7, 8S7/2) ions
are formed by trapping an electron, it will provide a
strong EPR signal, which can be easily detected in the
temperature range 80–300 K.17,18 The absence of Eu2+
signal in unirradiated and gamma-irradiated europium-
doped YBO3 samples suggests that the Eu ion is present
in the trivalent state in the host matrix before and after
gamma irradiation. EPR spectrum of gamma irradiated
sample recorded at room temperature at 6.3 mW micro-
wave power showed the presence of two radicals, as
shown in Fig. 4. The first radical without any hyperfine
structure (axial symmetry, g// ⳱ 2.0295 and g⊥⳱
2.0039) was identified as O2− from the known charac-
teristics of this center from EPR studies.19,20 The g|| and
g⊥ values for this radical are very close to O2− adsorbed
on zeolites and metal oxide surfaces. However, the g||
value for O2− ion was found to be highly matrix depen-
dent and ranged between 2.015 and 2.080. The second
radical with unresolved hyperfine structure (g ⳱ 2.0023)
was attributed to BO32− from the reported g values. The
unresolved hyperfine structure could be due to hyperfine
interaction of unpaired electron of radical species with
isotope 5B11 (I ⳱ 3/2; isotopic abundance ∼81%) and
5B
10
(I ⳱ 3; isotopic abundance ∼19%). The hole
trapped borate radical was extensively studied in number
of alkali borate glasses.21–23 In the recent past, we iden-
tified the BO 3 2− radical in irradiated Tm-doped
MgB4O79 and Ce-doped SrBPO58 samples and demon-
strated the role of BO32− radical in thermally stimulated FIG. 4. Temperature dependence of the EPR spectra of O2− and
luminescence. BO32− radicals in the temperature range 300–625 K in gamma-
irradiated YBO3-doped Eu3+ sample.

IV. DISCUSSION
To establish the formation of two independent radicals
in gamma-irradiated samples unambiguously, EPR spec-
tra were recorded at room temperature by varying the
microwave power in the range 2–63 mW, as shown in
Fig. 5. It can be seen that the intensity of the O2− radical
showed an increase with increase in the microwave
power, while the intensity of the BO32− radical was al-
most independent of microwave power indicating micro-
wave induced saturation at higher powers. The EPR

1120 J. Mater. Res., Vol. 21, No. 5, May 2006

 M. Anitha et al.: Thermally stimulated luminescence and electron paramagnetic resonance studies of Eu3+-doped yttrium borate

Eu3+ sample is shown in Fig. 4. It is seen from the figure

(Fig. 6) that there was a drastic reduction in the in-
tensities of O2− and BO32− signal in the tempera-
ture range 380–400 and 530–560 K, respectively, beyond
which these radicals got thermally destroyed, releas-
ing the trapped holes. The recombination of these holes
with trapped electrons from elsewhere results in the
production of excited state of Eu3+. The excited Eu3+
emits its characteristic light (585 and 610 nm) before
coming to ground state yielding glow peaks at 390 and
550 K. The electrons trapped at anion vacancies (Ov−)
could not be detected in the present case, presumably
because of their low concentration and/or large line
widths.24,25
The photo-stimulated luminescence process in
BaFBr:Eu2+ and SrBPO5: Eu2+ is well known due to
application of these materials in digital radiogra-
phy.17,18,26 In x-ray irradiated BaFBr: Eu2+ single crys-
tals, a triple aggregate of trapped electrons at fluoride
vacancies, F(F−)/bromide vacancies, F(Br−), hole trapped
center Vk, and activator are produced. The optical stimu-
lation of electron-hole recombination leads to the emis-
sion of rare-earth activator Eu2+. However, in the present
case, triple aggregates are formed between electrons
trapped at oxygen ion vacancies (OV−), hole trapped cen-
ters O2−, BO32−, and activator ions Eu3+. On thermal
stimulation, trapped holes are released from O2− and
BO32− radicals, and they combine with electrons released
from trapped electron centers at their respective TSL
peak temperatures. The energy thus released in electron-
hole recombination process is transferred to neighboring
Eu3+ ion giving its emission. Based on these reports, the
following mechanism is proposed for the observed TSL
peaks.

FIG. 5. Microwave power variation of the EPR spectra of O2− and

BO32− radicals in the 2–63 mW range in the gamma-irradiated YBO3-
doped Eu3+ sample.

spectra recorded on annealing the gamma irradiated

europium-doped YBO3 samples in the temperature range
375–625 K also supported the formation of two indepen-
dent radicals, since the thermal stability of these two ions
was found to be different. This is discussed in next sec-
tion.
The temperature dependence of EPR spectra in the FIG. 6. Plot of intensities of (a) O2− and (b) BO32− radical ions at
range 300–625 K on the gamma-irradiated YBO3-doped different annealing temperatures.

J. Mater. Res., Vol. 21, No. 5, May 2006 1121

 M. Anitha et al.: Thermally stimulated luminescence and electron paramagnetic resonance studies of Eu3+-doped yttrium borate
On irradiation,
YBO3 → BO32−, O2−, Ov−
On heating,
O2− → O22− + h (at 390 K)
BO32− → BO33− + h (at 550 K)
(Ov−) → (Ov) + e
e + h → h␯
h␯ + Eu3+ → (Eu3+)*
(Eu3+)* → Eu3+ + h␯
It is also probable that Eu3+ traps an electron to form
Eu2+ on irradiation, and upon heating, the hole released
from hole-trapped centers combines with Eu2+ to give
(Eu3+)*, and relaxation of the latter ion to the ground
state results in the observed luminescence. However,
there was no evidence for the presence of Eu2+ either in
the photoluminescence or EPR spectra. Therefore, the
first mechanism appears to be the dominant process re-
sponsible for the observed TSL glow peaks.
V. CONCLUSION
TSL studies on Eu3+-doped YBO3 samples showed
an intense TSL glow peak at 550 K and a weak peak at
392 K, which are associated with the thermal destruction
of BO32− and O2− radical ions, respectively. The energy
released in electron hole recombination process is
transferred to the Eu3+ ion, the luminescence center,
which gets de-excited by giving emissions at 585 and
610 nm. Photoluminescence studies on samples have
confirmed the presence of Eu3+ ions at Y3+ sites. The
EPR was used to identify the hole-trapped species BO32−
and O2− formed on gamma irradiation and their role in
the observed TSL glow peaks at 550 K and 392 K, re-
spectively.
ACKNOWLEDGMENT
The authors would like to thank Dr. V.K. Manchanda,
Head Radiochemistry Division, Bhabha Atomic Re-
search Centre (BARC) for his keen interest and encour-
agement during the course of this work.
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