RESEARCH
Influence of Nd3+ ions on TL characteristics of Li2O-MO-B2O3(MO 5 ZnO, CaO, CdO) glass system
J. Anjaiah • C. Laxmikanth • Cephas John Lyobha •
N. Veeraiah • P. Kistaiah
Received: 4 September 2014 / Accepted: 1 February 2015 / Published online: 18 February 2015
� The Author(s) 2015. This article is published with open access at Springerlink.com
Abstract Thermoluminescence (TL) characteristics of
X-ray irradiated pure and doped with Nd3? ions glasses
have been studied in the temperature range 303–573 K; all
the pure glasses have exhibited single TL peak at 382, 424
and 466 K, respectively. When these glasses are doped
with Nd3? ions no additional peaks are observed but the
glow peak temperature of the existing glow peak shifted
gradually towards higher temperatures with gain in inten-
sity of TL light output. The area under the glow curve is
found to be maximum for Nd3?-doped glasses mixed with
cadmium oxide as modifier. The trap depth parameters
associated with the observed TL peaks have been evaluated
using Chen’s formulae. The possible use of these glasses in
radiation dosimetry has been described. The result clearly
showed that neodymium (Nd)-doped cadmium borate glass
has a potential to be considered as the thermoluminescence
dosimeter.
Keywords Infra red spectra � Thermoluminescence �Borate glasses � Neodymium
Introduction
Thermoluminescence is the phenomenon of emission of
light from a solid which has been previously exposed to
ionizing radiation under conditions of increasing tem-
perature. Oxylithiumborate glasses are considered as good
materials for dosimetry applications since they are
relatively moisture resistant when compared with the pure
borate glasses. The understanding of the glass structure by
detailed studies on radiation-induced defect centres has
been an interesting subject of investigation in recent years.
Recently some recommendable work has done on ther-
moluminescence mechanisms in borate-based glasses. Nil
Kucuk and Ilker Kucuk reported the computational mod-
elling of thermoluminescence glow curves of zinc borate
crystals [1]. Haydar Aboud et al. reported the thermolu-
minescence properties of the Cu-doped lithium potassium
borate glass [2]. Influence of induced structural changes on
thermoluminescence characteristics of c-ray irradiatedPbO-Al2O3-SiO2:Dy
3? glass is reported by Sundara Rao
et al. [3]. Thermoluminescence properties of CaO-B2O3glass system doped with GeO2 is reported by T.N.H.
Tengku Kamarul Bahri et al. [4]. Thermoluminescence
study of MnO-doped borophosphate glass samples for ra-
diation dosimetry is reported by Swamy et al. [5].
It is well known that boric acid (B2O3) is one of the
good glass formers and can form glass alone with good
transparency, high chemical durability, thermal stability
and good rare-earth ion solubility [6]. The glass containing
Li2O as network modifier was seen as bubble free, highly
stable and moisture resistant, suitable for a systematic
analysis [7]. Among the three modifier oxides chosen to
mix in the present glass system, viz., CaO, ZnO and CdO;
ZnO is expected to shorten the time taken for solidification
of glasses during the quenching process and glasses
J. Anjaiah (&) � C. Laxmikanth � C. J. LyobhaDepartment of Physics, The University of Dodoma, Tanzania,
East Africa
e-mail: [email protected]
J. Anjaiah
Department of Physics, Geethanjali College of Engineering
and Technology, Keesara, Ranga Reddy District 501 301, India
N. Veeraiah
Department of Physics, Acharya Nagarjuna University,
Nagarjuna Nagar, Guntur 522 510, Andhra Pradesh, India
P. Kistaiah
Department of Physics, Osmania University,
Hyderabad 500007, Telangana, India
123
J Theor Appl Phys (2015) 9:119–125
DOI 10.1007/s40094-015-0169-5
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containing ZnO have high chemical stability and less
thermal expansion. Their wide band gap, large exciton
binding energy and intrinsic emitting property make them
as promising candidates for the development of optoelec-
tronic devices, solar energy concentrators, ultraviolet
emitting lasers and gas sensors [8]. Both ZnO and CdO are
thermally stable and appreciably covalent in character [9].
Lithium tetraborate glass system is a known and im-
portant starting material in the development of applications
of radiation dosimetry for a long period, since its effective
atomic number Zeff & 7.25 has the property of beingnearly tissue equivalent that makes it as a very promising
material in the field of personal and clinical dosimetry and
for other applications like X-ray phosphors, scintillators
and thermoluminescent detectors [5, 10–13]. However,
pure borate glasses have certain disadvantages to use in
radiation dosimetry since they are highly hygroscopic and
exhibit weak glow peak at relatively low temperatures.
Schulman et al. [14] were the first to be acknowledged
for starting the TL studies on lithium borate compounds
and since then various details on TL studies of alkali and
alkaline earth tetra borates continued up to present times
especially on magnesium and lithium borate compounds.
Several attempts were also made to enhance thermolumi-
nescence sensitivity of these glass materials by adding
different transition and rare earth or lanthanide metal ions
to these glass samples [15–20].
The study on the influence of neodymium ions on
thermoluminescence light output of these glasses is also
carried out with a view to examine the suitability of these
glasses in the radiation dosimetry.
Materials and methods
Undoped and following neodymium ion-doped glasses in
mole % are prepared by using standard melting and
quenching techniques and used for the present study [21–23].
ZnB: 30 Li2O-10 ZnO-60 B2O3,
ZnBNd: 30 Li2O-10 ZnO-59 B2O3:1Nd2O3,
CaB: 30 Li2O-10 CaO-60 B2O3,
CaBNd: 30 Li2O-10 CaO-59 B2O3:1Nd2O3,
CdB: 30 Li2O-10 CdO-60 B2O3, and
CdBNd: 30 Li2O-10 CdO-59 B2O3:1Nd2O3.
Appropriate amounts of raw materials ZnO, CaCO3, CdO,H3BO3, Li2CO3 and Nd2O3 were thoroughly mixed and
grounded in an agate mortar and melted in a platinum crucible.
The chemicals used in the work were of high purity (99.9 %).
These compositions were heated in a PID temperature-con-
trolled furnace at 450 �C for 2 h for the decarbonization fromCaCO3 and Li2CO3 and then the temperature was maintained
within the range 1,000–1,050 �C and kept the melt at this
temperature for an hour till a bubble free liquid was formed.
The crucibles were shaken frequently for the homogeneous
mixing of all the constituents. The resultant melt was poured
on a rectangular brass mould held at room temperature. The
samples were subsequently annealed at glass transition tem-
perature in another furnace to remove mechanical stress and
were polished.
The density ‘q’ of these glasses was determined by thestandard principle of Archimedes’ using xylene (99.99 %
pure) as the buoyant liquid. The glass transition temperatures
Tg and crystallization temperature Tc of these glasses were
determined (to an accuracy of ±1 �C) by differential scanningcalorimetry (DSC) traces, recorded using universal V23C TA
differential scanning calorimeter with a programmed heating
rate of 15 �C per minute in the temperature range 30–750 �C.Infrared transmission (IR) spectra for these glasses were
recorded using a Perkin Elmer Spectrometer in the
wavenumber range 400–4,000 cm-1 by KBr pellet method.
For recording thermoluminescence emission, the glasses
were irradiated with X-rays for one hour with Norelco
X-ray unit operated at 35 kV, 10 mA; thermoluminescence
output of these glasses was recorded on a computerized
Nucleonix-TL set up with a heating rate of 1 �C/s.
Results and discussion
Physical properties and characterization
From the measured values of density and the average
molecular weight �M, various other physical parameters
such as neodymium ion concentration Ni, mean neodymi-
um ion separation distance and field strength are calculated
and presented in the Table 1.
Our visual examination, absence of peaks in X-ray
diffraction spectra, existence of glass transition tem-
perature Tg and crystallization temperature Tc in differen-
tial thermal analysis curves, indicate that the glasses
prepared were of amorphous in nature.
Figure 1 represents the thermograms of pure and Li2O-
MO-B2O3:Nd2O3 glasses; the pure glasses exhibit an en-
dothermic effect due to the glass transition temperature Tg.
Presence of single transition temperature Tg at 553 �C inZnB glass, 544.7 �C in CaB glass and 537 �C in CdB glassindicates homogeneity of these glasses. At still higher
temperatures an exothermic peak Tc due to the crystal
growth followed by an endothermic effect due to the re-
melting of the glass symbolized by Tm are observed. The
glass forming ability (Hruby’s) parameters Kgl = (Tc-Tg)/
(Tm-Tc) are calculated, which give the information about
the stability of the glasses against devitrification [24, 25]
are evaluated and presented in Table 2. The highest values
of these parameters are obtained for ZnO-modifier glass
120 J Theor Appl Phys (2015) 9:119–125
123
(ZnBNd) indicating it’s relatively high glass forming
ability among the three glasses. Insets of Fig. 1 represent;
(a) the variation of Hruby’s parameter and (b) the variation
of (Tc-Tg) for Nd3? ions doped glasses mixed with dif-
ferent modifier oxides.
For the Nd3? ions doped glasses mixed with different
modifier oxides, the glass transition temperature Tg is at
548.3 �C in ZnBNd glass, 538.6 �C in CaBNd glass and533.0 �C in CdBNd glass. For all glasses with the intro-duction of neodymium ions the values of Tg and Tc-Tg is
found to decrease gradually.
Infrared spectroscopy
Figure 2 represents IR spectra of the pure as well Nd3? ions
doped Li2O-MO-B2O3 glasses. The infrared transmission
spectra of pure and praseodymium ion-doped Li2O-MO-
B2O3 glasses exhibit three groups of bands: (i) in the region
1,320–1,380 cm-1, (ii) in the region 930–1,020 cm-1 and
(iii) a band at about 710 cm-1.
It is well known that the effect of introduction of alkali
oxides into B2O3 glass is the conversion of sp2 planar BO3
units into more stable sp3 tetrahedral BO4 units and may
also create non-bridging oxygens. Each BO4 unit is linked
to two such other units and one oxygen from each unit with
a neodymium ion and the structure leads to the formation
of long tetrahedron chains. The presence of such BO4 units
in the present glasses is evident from the IR spectral
studies. The second group of bands is attributed to such
BO4 units whereas the first group of bands is identified as
due to the stretching relaxation of the B–O bond of the
trigonal BO3 units and the band at 710 cm-1 is due to the
bending vibrations of B–O-B linkages in the borate net-
work [26–29]. A weak band observed around 456 cm-1 is
Fig. 1 DSC patterns of pureand Nd3?-doped Li2O-MO-
B2O3 glasses. Insets a the
variation of Hruby’s parameter
and b the variation of (Tc-Tg)
for different modifier oxides
Table 2 Data on differentialscanning calorimetric studies of
Li2O-MO-B2O3: Nd2O3 glasses
Glass Tg (�C) Tc (�C) Tm (�C) Tg/Tm (Tc-Tg) (�C) (Tc-Tg)/Tm Kgl
ZnB 553.0 636 686.7 0.805 83.0 0.121 1.637
ZnBNd 548.3 629 685.2 0.800 80.7 0.118 1.436
CaB 544.7 625 681 0.800 80.3 0.118 1.434
CaBNd 538.6 615 678 0.794 76.4 0.113 1.213
CdB 537.0 613.8 678 0.792 76.8 0.113 1.196
CdBNd 533.0 608.5 678 0.786 75.5 0.111 1.086
Table 1 Various physicalproperties of Li2O-MO-B2O3:
Nd2O3 glasses
Property/glass ZnB ZnBNd CaB CaBNd CdB CdBNd
Refractive index, nd 1.517 1.524 1.519 1.527 1.523 1.531
Density, q (g/cm3) 2.181 3.024 2.415 3.087 2.799 3.329
Average molecular weight, �M 46.001 44.824 46.017 44.826 46.028 44.835
Nd3? ion concentration, Ni (1022/cm3) – 4.06 – 4.15 – 4.47
Inter-ionic distance of Nd3? ions, Ri (Å) – 2.91 – 2.89 – 2.82
J Theor Appl Phys (2015) 9:119–125 121
123
an indicative of the presence of ZnO4 units in the ZnB
series glass network [30, 31].
The intensity of the second group of bands (band due to
the trigonal BO4 units) is found to increase at the expense of
first group of bands (bands due to tetrahedral BO3 units) with
the introduction of Nd3? ions with the shifting of meta-
centres of first and second group of bands, respectively, to-
wards slightly lower and higher wave number for all the
glasses. No significant change in position and intensity of the
other bands are observed in the spectra of the glass by in-
troducing the neodymium ions. The summary of the data on
the positions of various bands in the IR spectra of pure and
Li2O-MO-B2O3:Nd2O3 glasses are presented in Table 3.
Thermoluminescence
Thermoluminescence glow curves of all the glasses doped
with neodymium ions are shown in Fig. 3. Pure Li2O-MO-
B2O3 (M = ZnO, CaO and CdO) glasses exhibit a glow
peak at 382, 424 and 466 K in CdB glass. When these
glasses are doped with Nd3? ions no additional peaks are
observed but the glow peak temperature Tm of the existing
glow peak shifted gradually towards higher temperatures
with a gain in the intensity of TL light output. The glow
peaks of neodymium ion-doped ZnBNd, CaBNd and
CdBNd glasses shifted to 395, 438 and 475 K, respectively.
The relative TL light outputs (area under the glow
curve) of pure and Nd3? ion-doped Li2O-MO-B2O3 glasses
are shown in the inset of Fig. 3. Pure glasses have the TL
light output intensity area under the glow curve is 502, 770
and 1,142. For the Nd3? ions doped glasses mixed with
different modifier oxides the glow peaks of neodymium
ion-doped ZnBNd, CaBNd and CdBNd glasses are 588,
1,020 and 1,252, respectively. The area under the glow
curve is also found to be maximum for CdBNd-doped glass
comparing to all other glass systems.
The trap depth parameters for these glow peaks are
computed using Chen’s formulae.
The activation energies for these glow peaks are com-
puted using Chen’s formulae [32]:
Es = 1.52 (kBTM2 /s)-1.58 (2kBTM),
Ed = 0.976 (kBTM2 /d), for the first-order kinetics.
In the above equation kB is Boltzmann constant,
s = TM-T1, d = T2-TM, lg = d/(T2-T1), where TM is theglow peak temperature and T1 (rising end) and T2 (falling
end) are the temperature at the half widths of the glow
peaks. The summary of the data on thermoluminescence
peaks with corresponding trap depth parameters of the
present glasses is furnished in Table 4. The trap depth
Fig. 2 Infrared spectra of pure(dotted line) and Nd3?-doped
(solid line) Li2O-MO-B2O3glasses
Table 3 Peak positions (cm-1) of IR spectra of Nd3?-doped Li2O-MO-B2O3 glasses
Glass Band due to B–O
bond stretching in
BO3 units
Band due to B–O
bond stretching in
BO4 units
Band due to B–O-
B linkage in
borate network
ZnB 1,378 939 710
ZnBNd 1,360 963 710
CaB 1,352 979 710
CaBNd 1,336 992 710
CdB 1,336 992 710
CdBNd 1,323 1,019 710
122 J Theor Appl Phys (2015) 9:119–125
123
parameters of pure glasses are found to be *0.422 eV andobserved to increase by doping with Nd2O3. Such value of
trap depth indicates that the lifetime (s) of electron in thesetraps is of the order of several months [5, 33].
Prior to TL measurements, the optical absorption spectra
of all the glasses before and after X-ray irradiation are
recorded. After the X-ray irradiation no additional ab-
sorption bands are observed other than those obtained in
non-irradiated glasses; however the relative intensities of
these bands are slightly affected [34].
The action of X-ray irradiation on glasses is to produce
secondary electrons from the sites where they are in a
stable state and have an excess energy. Such electrons
may traverse in the glass network depending upon their
energy and the composition of the glass and are finally
trapped, thus forming colour centres (or alternatively they
may form excitons with energy states in the forbidden
gap). The trapping sites may be the neodymium ions
which constitute the glass structure, ions of admixtures to
the main composition and the structural defects due to
impurities in the glass. Thus this process leads to the
formation of (1) boron electron centres, (2) non-bridging
oxygen hole centres and (3) boron oxygen hole centres
[35–37]. Thermoluminescence is a consequence of radia-
tive recombination between the electrons (released by
heating from electron centre) and an anti-bonding mole-
cular orbital of the nearest of the oxygen hole centres. The
observed TL peaks in the present glasses can be attributed
due to such radiation.
The Li? ions have closed structure, do not have energy
levels within 10 eV of the ground state and hence these
ions do not participate directly in luminescence but may act
as activator ions [38]. Let us assume that the Nd3? ions are
uniformly distributed throughout the sample. In the ab-
sence of Nd3? ion in the network, each electron released by
heating from electron centre would be caught by an anti-
bonding molecular orbital of the nearest of the oxygen hole
centre. The process is followed by a radiative recombina-
tion. The observed TL peak in the present glasses is at-
tributed to such radiation. If Nd3? ion is present in the glass
network, we have observed such a radiative recombination
to enhance with respect to that of corresponding pure glass
Fig. 3 Thermoluminescenceemission of pure (dotted line)
and Nd3? ions doped (solid line)
Li2O-MO-B2O3 glasses. Inset
figure represents the relative TL
light output of pure and Nd3?
ions doped glasses
Table 4 Data on various trapdepth parameters of Li2O-MO-
B2O3: Nd2O3 glasses
Glass TM (K) s (K) d (K) lg Es (eV) Ed (eV) TL light output (rel. units)
ZnB 382 30 28 0.483 0.526 0.432 502
ZnBNd 395 29 24 0.453 0.589 0.539 588
CaB 424 53 35 0.398 0.324 0.426 770
CaBNd 438 53 32 0.376 0.350 0.497 1,020
CdB 466 76 44 0.367 0.244 0.409 1,142
CdBNd 475 72 40 0.357 0.277 0.468 1,252
J Theor Appl Phys (2015) 9:119–125 123
123
indicating that the neodymium ions are acting as TL acti-
vators in all the glasses. The comparison of TL emission of
Nd3?-doped glasses shows a low percentage of enhance-
ments of TL light output for ZnBNd glasses.
The larger the number of Nd3? ions in the glass net-
work, the higher is the TL light output. Relatively larger
concentration of Nd3? ions in CdBNd glasses cause
relatively higher light output as observed (inset of Fig. 3).
Thus the analysis of the TL data of Li2O-MO-B2O3:Nd2O3glasses suggests that the CdBNd glass to be a better can-
didate for thermoluminescence emission among the three
Nd3?-doped glasses.
Conclusions
Finally our studies on properties of Li2O-MO-B2O3 glasses
doped neodymium ions indicate that (i) Differential scan-
ning calorimetric studies indicate high glass forming ability
is for ZnBNd glass. (ii) The IR spectral studies indicate
relatively less disorder in ZnBNd glass network. (iii) The
analysis of the TL data suggests that the CdBNd glass can
be used more effectively in radiation dosimetry since they
exhibit high TL light output in high temperature region.
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Influence of Nd3+ ions on TL characteristics of Li2O-MO-B2O3 (MO = ZnO, CaO, CdO) glass systemAbstractIntroductionMaterials and methodsResults and discussionPhysical properties and characterizationInfrared spectroscopyThermoluminescence
ConclusionsOpen AccessReferences