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: anjaiah.juluru@gmail.com

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

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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

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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