Journal of Luminescence 229 (2021) 117701

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Journal of Luminescence
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NIR photoluminescence studies of Nd3+doped B2O3–BaF2–PbF2–Al2O3

glasses for 1.063 μm laser applications
P. Rekha Rani a, M. Venkateswarlu a, *, K. Swapna a, Sk Mahamuda a, Rupesh A. Talewar a, Ch.
B. Annapurna Devi b, A.S. Rao c
a
Department of Physics, Koneru Lakshmaiah Education Foundation, Vaddeswaram, 522502, Guntur (Dt.), A.P, India
b
Department of Physics, Vignan’s Lara Institute of Technology & Science, Vadlamudi, Guntur, Andhra Pradesh, 522 213, India
c
Department of Applied Physics, Delhi Technological University, Bawana Road, New Delhi, 110042, India

A R T I C L E I N F O A B S T R A C T

Keywords: This paper describes the preparation and characterization of various concentrations of Nd3+ doped
Borate glass B2O3–BaF2–PbF2–Al2O3 (BaPbAlFB) glasses in detailed. The glasses used in the present work are synthesized by
Nd3+ ions using melt quenching process and characterized by measuring the absorption, photoluminescence (PL) and PL
Optical properties
decay spectral profiles. The energies of the absorption spectral profiles called oscillator strengths are evaluated
NIR emission
Laser properties
from the absorption spectra and subjected to Judd-Ofelt (J-O) theory to evaluate the J-O intensity parameters
using least squares fit method. Under 808 nm diode laser excitation, the BaPbAlFBNd glasses exhibit three
emission bands at near-infrared region around 887, 1063, 1336 nm from 4F3/2 → 4I9/2, 4I11/2 and 4I13/2 radiative
transitions respectively. Among the three emissions, the one observed at 1063 nm is found to be more intense
relatively. The lifetime of 4F3/2 transition has been estimated experimentally through decay measurements
recorded under 808 nm excitation wavelength. Among all the BaPbAlFB glasses investigated, the one with 1.0
mol% of Nd3+ ions is showing relatively high fluorescence quantum efficiency. The measured saturation intensity
(IS) values shows relatively the low threshold values. The obtained results endorsed the potentiality of BaP­
bAlFBNd1.0 glass for the fabrication of fiber amplifiers and solid-state lasers that can act in NIR region at 1063
nm wavelength.

1. Introduction materials [2]. RE ions doped glasses are not only the subject matter for
infrared radiation and also used in different areas such as high gain laser
In recent years, solid-state lasers are considered as the most signifi­ system, optical communication system, NIR-to-visible emission, medi­
cant sources of radiation because of their appreciable characteristics cine, industry, surveillance, optical switching and data storage devices
than the other laser systems. Solid-state lasers have many advantages in [5].
various fields such as industries tool in several mass production pro­ Of many RE active ions, neodymium (Nd3+) ion is one of the
cesses; source of radiation for therapeutic, aesthetic, and surgical pro­ prominent one because of its spectroscopic importance as it possesses
cedures; diagnostic instrumentation in research fields. Solid state lasers huge number of manifold absorption energy levels from UV–vis to NIR
also functions as a target designators, infrared countermeasure systems spectral region for effective optical pumping and emission. It can also
and range finders in armed forces etc., [1]. These several features and perform with greater efficiencies under normal temperatures. Moreover,
advantages made the solid-state lasers as superior laser material among Nd3+ ions owns a great importance due to their spectacular features in
all the existed laser systems. Usually, glasses and crystalline materials prominent area namely, fiber-optic telecommunication system for
activated with rare earth (RE) ions perform a great role in exhibiting tunable and femtosecond and picosecond pulse width (ultrafast) lasers
lasing action. This is because of the existence of the 4fn electronic level [6,7]. Glasses doped with Nd3+ ions are well-known for its adoptability
structures existing in RE ions possess huge number of long-lasting in­ in different areas including solid-state lasers, microchip lasers, gener­
termediate levels to get more populous [2–4]. In fact, glasses are the ating the electricity through laser inertial nuclear fusion energy power
most adaptable materials for solid state lasers than the crystalline plants and planar waveguides [8,9]. Usually at wavelengths around

* Corresponding author.
E-mail address: [email protected] (M. Venkateswarlu).

https://doi.org/10.1016/j.jlumin.2020.117701
Received 28 April 2020; Received in revised form 6 October 2020; Accepted 13 October 2020
Available online 15 October 2020
0022-2313/© 2020 Elsevier B.V. All rights reserved.
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

1800, 1350, 1064 and 880 nm, Nd3+ ions can offer effective lasing ions spectral properties in fluoride glasses with phosphates as additives.
emission. Among them, the luminescence of Nd3+ ions doped glasses at Pingsheng Yu et al. [20] reported the spectroscopic investigations on
~1300 nm has greater importance in the field of optical fiber amplifiers Nd-doped Bi2O3-GeO2/SiO2 glasses. Xue Wang et al. [18] detailed
especially in NIR region. In fact, Nd3+ ions can operate with high extent about the influence of Al2O3 and La2O3 host glass on spectroscopic
of gain cross-sections in 4 level mode laser systems. This is the main properties of Nd doped sol-gel silica glasses. Devarajulu Gelija et al. [21]
motive for the usage of Nd3+ ion as active ions in glasses and crystals to studied 2.0 μm emission in SiO2–Al2O3–Na2CO3–SrF2–CaF2 glass system
generate solid-state lasers in NIR region around 1064 nm under 808 nm co-doped with Nd3+/Ho3+ ions for laser applications in mid-infrared
excitation wavelengths [10]. To overcome the unfavourable effect of region. The present work focus on the photoluminescence assessment
non-radiative degradation and for better lasing emission, it is essential of barium lead alumino fluoro borate glass activated with Nd3+ ions to
to have a longer fluorescence lifetimes for Nd3+ ion at 4F3/2 level in NIR perceive highly intensified NIR lasing output. Additionally, Judd-Ofelt
region around 1064 nm. Already several investigations have been done (J-O) calculations are accomplished theoretically to report the oscil­
on this intense emission at 1064 nm for high-power and high gain laser lator strength, three J-O intensity parameters and quantum efficiency of
systems [11]. But it is a requisite to develop a suitable host material for the RE ion in the present glass system. Laser properties such as satura­
Nd3+ ions which explores the most conducive features like less phonon tion intensity, stimulated emission, absorption and gain cross-sections
energy and low OH- content, as these may minimizes the excitation are evaluated and discussed.
(non-radiative losses) owing to multi-phonon relaxation to achieve
many more applications in NIR well as in visible region. 2. Material and characterization
In fact, an ideal host glass must accomplish and satisfy some de­
mands particularly extensive spectral transitions from UV to mid-IR, 2.1. Synthesis
excellent mechanical strength, outstanding thermal and chemical sta­
bilities, high non-linear refractive index and relatively least phonon A series of neodymium doped BaPbAlFB glasses with chemical
energy, which minimizes the multi-phonon non-radiative probabilities composition (65-x)B2O3 +10PbF2 + 20BaF2 + 5Al2O3 + xNd2O3, (where
and inevitably enhance the quantum yields. After an assessment, the x = 0.5, 1.0, 1.5, 2.0 and 2.5 mol%) were prepared by using the con­
host glasses such as chalcogenides, borates, fluoro zirconates, fluorides, ventional melt-quench process. An appropriate amount of raw materials
silicates and tellurites have been a topic of discussion for many people are weighted up to 10 gm by using a sensitive electronic weighing ma­
working in this fascinating area of research. Among many glassy mate­ chine and grinded thoroughly for 1 h to obtain fine powder. The pow­
rials, borate glasses have their own identity because of their high bond ders collected in a silica crucible at 1150 ◦ C for 25 min and stirred
strength and high thermal stability in comparison with silicates, phos­ continuously to get transparent viscous melt. Such viscous melts were
phates etc. and also among several oxides glasses, borate glass possesses poured for quenching process on a preheated brass mould and pressed
several practical advantages because of its remarkable features such as quickly with another brass mould. Further, to eradicate the internal
easy incorporation of RE ions, outrageous transparency, moderate stresses, the glass samples are annealed at 400 ◦ C for 3 h, and cooled
melting point and outstanding thermal stability. Nevertheless, a borate down slowly to attain room temperature (28 ◦ C). Finally, these samples
glass solely exhibits maximum phonon energy (1300 cm− 1) which pro­ have been allowed for spectral measurements and their respective im­
motes non-radiative decays and lowers the emission intensity of the RE ages are presented in Fig. 1.
ion. Hence, it is mandatory to add a suitable modifier to borate glass
network to annihilates the high phonon energy of the borates and up­ 2.2. Characterization
grade the physical and spectroscopic characteristics of the glass
network. Among various modifiers, lead fluoride (PbF2) and barium Table 1, represents experimentally measured density and refractive
fluoride (BaF2) have their significance in eradicating high phonon en­ index for the titled glasses. Densities are measured experimentally by
ergies [12]. Therefore, addition of modifiers (PbF2 and BaF2) not only employing Archimedes’ method using water as an immersion liquid.
supress the high phonon energy, but also originates a dynamic shift of a Refractive indices are measured by using Brewster’s angle method
few BO3 triangles to BO4 tetrahedra and leads to emerge several cyclic (employing 650 nm wavelength line of He–Ne laser). The absorption
units such as di-borate, tri-borate, tetra-borate or penta-borate groups, spectra of the as prepared glasses were recorded using JASCO model
which modifies the boron coordination and results in the modification of V670 spectrophotometer with 0.1 nm spectral resolution at room tem­
structural and spectroscopic properties by creating non-bridging oxygen perature (300 K). The photoluminescence (PL) excitation, PL and PL
atoms in the glass network [13,14]. Moreover, addition of fluorides has decay spectral measurements were recorded using an Edinburgh FLS-
its own significance because glasses contain fluorides exhibits low 980 fluorescence spectrometer (under 808 nm excitation of diode
phonon energy quite useful for lasers, fibres and mid-IR region optical laser) coupled with InGas detector having 0.02 nm wavelength accuracy
communication system [15]. Especially fluorides offers laser generation and 0.05 nm minimum step size.
with maximum quantum efficiency and least non-radiative decay rates.
Also, in fluoride glasses, the effect of temperature is very less on the 3. Results and discussion
refractive index (dn/dt is negative). This is the most distinctive property
of fluorides, which makes them as an outstanding material in the tele­ 3.1. Absorption spectral studies and Judd-Ofelt analysis
communication system [16]. Aluminium trioxide (Al2O3) being an in­
termediate, added to a glassy network can intensifies fluorescence, In UV–vis–NIR region, the absorption spectra of various concentra­
allows the uniform distribution of RE ions and minimizes the transition tions of Nd3+-BaPbAlFB glass compositions are recorded in between 350
temperature of glass [17]. In spite of this, inclusion of Al2O3 improves and 950 nm spectral range and is shown in Fig. 2. The details of ab­
the fluorescence quantum yield remarkably, which elucidate that Al3+ sorption transitions along wavelength location for the titled glass are
ions counteract the congregation of RE dopants in the glass network, given in Table 2. As shown in Fig. 2, the absorption spectra of titled
consequently lowers the cross-relaxation and energy migration between glasses comprises nine peaks located at 383, 458, 506, 558, 615, 658,
the ions [18]. 715, 803 and 873 nm corresponding to the transition from 4I9/2 ground
Over the past few years, several investigations have been conducting state to various (2P, 2D)3/2, 4G11/2, 4G9/2, 4G5/2+ 2G7/2, 2H11/2, 4F9/2,
to understand photoluminescence studies of Nd3+ ions doped with 4
F7/2+4S3/2, 4F5/2+2H9/2 and 4F3/2 excited states of Nd3+ ions. It can be
various types of host glasses. Recently, W. C. Wang and his team re­ noticed from Fig. 2 that, different concentrations of Nd3+ ions doped
ported about the optical properties of Nd3+ ions doped fluoro-sulfo- BaPbAlFB glasses resembles to each other in their band positions and
phosphate glasses [19]. E. Kolobkova et al. [16] described the Nd3+ show changes in their intensities and peak width. The transition 4I9/2 →

2
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

Fig. 1. Photographic pictures of various concentrations of Nd3+ ions doped BaPbAlFB glasses.

Table 1
Few crucial physical parameters of Nd3+ ions doped BaPbAlFB glasses.
Physical parameter BaPbAlFB BaPbAlFB BaPbAlFB BaPbAlFB BaPbAlFB
Nd0.5 Nd1.0 Nd1.5 Nd2.0 Nd2.5

Density 2.98 3.01 3.04 3.07 3.10

Refractive index 1.88 1.89 1.90 1.91 1.92
Ion concentration, (x1020) ion/cm3 0.84 1.04 2.52 3.35 4.17
Inter ionic distance, A 56.2 32.1 14.8 11.8 8.80
◦

Average molecular weight 106.2 107.6 108.9 110.3 111.7

Optical basicity 0.426 0.428 0.430 0.433 0.435
Molar refraction 19.8 20.0 20.2 20.4 20.6
Molar electronic polarizability 7.89 7.97 8.04 8.12 8.19
Oxide ion polarizability, Å3 3.42 3.44 3.46 3.49 3.51
Indirect bandgap 3.74 3.69 3.63 3.58 3.54

Table 2
Absorption transitions, corresponding wavelength & energy, experimental (fexp)
(10− 6) & calculated oscillator strengths (fcal) (10− 6), rms deviation (δrms) (10− 6)
and bonding parameter of 1 mol% of Nd3+ ions doped BaPbAlFB glass with
comparative studies.
Transition λ (nm) Energy (cm− 1) BaPbAlFBNd1.0 BBZPANd10 LPBTN1
4
I9/2
fexp fcal fexp [26] fexp [10]

(2P,2D)3/2 383 25,839 1.829 0.163 – –

4
G11/2 458 21,598 0.614 0.310 – –
4
G9/2 506 19,762 2.885 2.448 2.73 1.46
4
G5/2+ 2G7/2 558 17,921 18.80 19.82 25.07 39.40
2
H11/2 615 16,260 0.355 0.215 0.27 0.28
4
F9/2 658 15,197 1.317 0.900 1.98 1.38
4
F7/2+4S3/2 715 13,986 9.145 9.687 10.84 15.42
4
F5/2+2H9/2 803 12,453 8.014 8.626 13.13 12.57
4
F3/2 879 11,376 3.912 5.503 1.22 3.55
Δrms 0.75 0.59 0.34
δ 1.98 – 0.07

where, ϑC and ϑa is the wavenumber of a specific transition of Nd3+ ion

Fig. 2. Absorption spectra of Nd3+ ions doped BaPbAlFB glasses.
and wave number of the aqua ion respectively. The values obtained for δ
2 reveals the nature of the bonding between RE ions and the surrounding
H11/2 observed at 615 nm (16, 260 cm− 1) is hypersensitive in nature,
ligand ions. If δ value is positive, then the nature of bonding is consid­
because of its maximum intensity and fulfills the selection rules |ΔL| ≤
ered as covalent otherwise it is considered as ionic in character. Based on
2, |ΔS| ≤ 0 and |ΔJ| ≤ 2. The hypersensitive electric dipole transitions
the estimated values that are given in Table 2, it is noticed that present
are very sensitive to the neighborhood environment around the RE ions.
glass system possesses positive values indicating covalency nature of
In general, the positions of these transitions depend on RE ion embedded
bonding between RE ions and the surrounding ligands.
into the host glass network.
It is well known that, Judd-Ofelt theory (J-O) [23,24] applied to the
The interaction existing between 4f orbital’s of RE ions and oxygen
energies of the absorption spectral features called oscillator strengths is
ligands in the host matrix (interaction between Nd and O in the present
most successful in understanding the radiative properties of RE doped
case) is termed as Nephelauxetic effect [22]. The information pertaining
glasses. Using J-O theory, the experimental oscillator strengths (fexp) are
to Nephelauxetic effect is quite useful in understanding the nature of
obtained from the following formula [25];
bonding existing between the doped RE ions and oxygen ligands present
in the host material. The Nephelauxetic ratio (β) and bonding parameter 4.318 × 10− 9
fexp = α(ϑ)dϑ (3)
(δrms ) values are evaluated by using the following expressions; N

β=
ϑC
(1) here, N is the concentration of Nd3+ ions, α is the absorption coefficient
ϑa (cm− 1). The fexp value obtained for 1 mol% of Nd3+ ions in BaPbAlFB
( ) glass is given in Table 2. The calculated oscillator strength (fcal) is rep­
δ=
1− β
× 100 (2) resented by the following formula;
β

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P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

8π2 mc (n2 + 2)
2 long chain order of glass network structure and leads to produce NBOs.
(4)
′ ′ ′
fcal [(S, L)J; (S , L )J ] =
3hλe2 (2J + 1) 9n
Sed Further, increase in the number of NBOs takes place by increasing the
concentration of Nd3+ ions. This describes the existence of free O− 2 ions
here, (S, L)J, and (S′ , L′ )J’ represents the ground state and excited states which indicates the increase in the donor ability of the oxygen ions in
of an induced electric dipole absorption transitions respectively; m & e the glass network and this is known as optical basicity. Hence, Table 1
are mass and charge of an electron respectively; c is velocity of light in represents the increase in the indirect optical bandgap and optical ba­
vacuum; n is the index of refraction of the medium and λ is the wave­ sicity values along with the concentration of Nd3+ ions. Further, the
length of the transition. The root mean square error (Δrms) which de­ optical basicity values depend on degree of polarizability which can be
scribes the validation of J-O theory by predicting the degree of ability of calculated by using the measured refractive index values with the help of
the fit is given by. the following equation.
[∑ ( ( )
)2 ]12 3
fexp − fcal αm = Rm (7)
Δrms = (5) 4π N
p− 3
here, N represents the number of ions per mole, Rm denotes the molar
where p represents number of transitions related in the calculations of J- refraction and its values are presented in Table .1. Here the molar
O parameters. The fexp, fcal and rms deviation values observed for BaP­ electronic polarizability values are increasing with respect to the in­
bAlFBNd1.0 glass are shown in Table 2 along with values reported for crease in the Nd3+ ion concentration as the donor capability of oxygen
other glasses in literature for comparison [10,26]. ion are increased along with increasing the concentration of Nd3+ ions.
For multicomponent glasses, the oxide ion polarizability (α2−0 ) can be
calculated by using the following relation.
3.2. Optical bandgap, refractive index, oxide ion polarizability and [ ]
basicity values analysis Rm
−
∑
α
2.52 cat
α2−0 (n0 ) = (8)
Optical bandgap studies are useful in scrutinizing the electronic band N02−
structure of amorphous materials. According to Davis and Motto, the
optical bandgap of the RE doped glasses can be evaluated by using the where, αcat is the cation polarizability, N denotes the number of oxide
following expression. ions. From the values listed in Table .1 it is conspicuous that, optical
( )n basicity and oxide ion polarizability values are linearly increasing with
αhν = α0 hν − Eg (6) Nd3+ ion concentration because of the stronger electron donor ability of
the oxide ions.
here, α0 is known to be an independent constant and named as band The J-O parameters elucidate the structural properties of the glass
tailing parameter, Eg is the optical energy gap located among the network like rigidity and bonding nature. The obtained J-O parameters
localized states in the electronic band structure of the amorphous ma­ for BaPbAlFBNd1.0 glass are presented in Table 3 along with values
terials and another constant n called power factor whose values differ for reported in literature for various other Nd3+ ions doped glasses [19,
various transitions modes. The value of n equal to ½, 2, 3/2 and 3 rep­ 27–31]. The J-O parameters obtained for BaPbAlFBNd1.0 glass are
resents the direct allowed, indirect allowed, direct forbidden and indi­ following the trends Ω2˃ Ω6˃ Ω4. Here, higher values of Ω2 represents the
rect forbidden transitions respectively. The bandgap values calculated non-symmetry of crystal field around Nd3+ ion site and also more
from indirect bandgap spectra with the help of Tauc plot, plotted in covalency between Nd3+ and oxygen ions i.e., Nd–O. The Nd–O bonds
between (αhν)1/2 and hν are shown in Fig. 3 and the values are listed in with more covalency indicates the existence of multitudes of NBOs. It is
Table 1. From Table 1, it is noticed that, the indirect optical bandgap found from Table 3 that, the Ω2 value of BaPbAlFBNd1.0 glass is greater
values are decreasing with increase in the concentration of Nd3+ ions. than few other host glasses, indicating more asymmetry of crystal field
This is because of the addition of network modifier such as PbF2 and around Nd3+ ions in BaPbAlFBNd1.0 glass when compared with few
BaF2 to the glass network. Such network modifiers tends to shatters the other glasses. Another crucial parameter which describes emission in­
tensity of 4F3/2 → 4I11/2 transition of Nd3+ ions around 1063 nm in NIR
region is termed as spectroscopic quality factor [χ], which can be
evaluated by taking the ratio of Ω4 and Ω6 values. If χ > 1, the intensity
of 4F3/2 → 4I11/2 transition found to be more than that of 4F3/2 → 4I9/2
transition in host glass. As shown in Table 3, the χ value obtained for
BaPbAlFBNd1.0 glass is 0.91 and is comparable with the value reported
in literature.
The radiative parameters of 4F3/2 levels of the Nd3+ ions are calcu­
lated with the help of Ωλ values and index of refraction of the BaP­
bAlFBNd glasses. The following expressions are used to estimate various

Table 3
Comparison of Judd-Ofelt intensity parameters Ωλ(λ = 2, 4, 6)(10− 20 m2),
spectroscopic quality factor (χ) of Nd3+ ions doped BaPbAlFB glasses along with
reported values.
Samples Ω2 Ω4 Ω6 Trend χ = Ω4/Ω6 Reference

BaPbAlFBNd1.0 5.77 3.68 4.01 Ω2 > Ω6 > Ω4 0.91 Present work

FPS30Nd1.0 3.16 3.00 3.72 Ω6 > Ω2 > Ω4 0.94 [19]
BSKNLNd10 9.93 8.05 8.35 Ω2 > Ω6 > Ω4 0.96 [27]
PNbKANd1.0 9.83 4.98 4.52 Ω2>Ω4 > Ω6 1.10 [28]
PZNd1.0 5.46 3.22 4.29 Ω2>Ω6 > Ω4 0.75 [29]
SPB1 4.81 1.97 3.94 0.50 [30]
Fig. 3. Indirect bandgap spectra of various concentrations of Nd3+ ions doped
Ω2 > Ω6 > Ω4
LHG-8 4.40 5.10 5.60 Ω6 > Ω4 > Ω2 0.91 [31]
BaPbAlFB glasses.

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P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

radiative parameters possessed by the titled glasses and are listed in

Table 4 [32,33].
The radiative transition probability (AR) is given by
[ 2
]
′ , 64π4 ϑ3 n(n2 + 2) ′ ′ 3 ′ ′
AR (ψ J → ψ J ) = Sed (ψ J → ψ J ) + n Smd (ψ J → ψ J )
3h(2J + 1) 9
(9)
The radiative lifetime (τr ) is given by
1
τr (ψ J) = ∑ (10)
′ ′
ψ J AR (ψ J→ψ ′ J ′ )

The total radiative transition probability (AT) is represented by

∑
(11)
′ ′
AT ψ (J) = AR (ψ J → ψ J )
ψ ′ J′

According to J-O theory, the branching ratio(βR) is given by

′ ′
AR (ψ J, ψ J )
(12)
′ ′
βR (ψ J → ψ J ) =
Aτ ψ J

3.3. Photoluminescence excitation and emission spectral analysis Fig. 4. PLE and PL spectrum of 1 mol% of Nd3+ ions doped BaPbAlFB.

3.3.1. (a) NIR emission spectral analysis decreases showing concentration quenching effect. Increase in Nd3+ ion
Fig. 4 represents the combined spectra of PLE and PL of BaP­ concentration decreases the distance between Nd3+-Nd3+ ions and
bAlFBNd1.0 glass. The PLE spectra are recorded 200–850 nm spectral thereby increases the interaction between them. This increase in inter­
range fixing emission wavelength at 1063 nm. The obtained PLE spec­ action of Nd3+-Nd3+ ions causes the migration of energy between the
trum shows ten peaks located at 240, 359, 432, 475, 528, 586, 626, 685, active ions through cross-relaxations [34]. Usually the intensity of the
740, 823 nm and their corresponding transitions are situated at 2F7/2, peaks depends upon the interionic separation among Nd3+-Nd3+ ions
4
D3/2, 2P1/2, 2G9/2, (4G9/2, 4G7/2), 2G7/2, 2H11/2, 4F9/2, 4S3/2, 4F5/2 and Nd3+ ions concentration. If the interionic separation among
respectively. Fig. 4 represents the PL spectra of all compositions of Nd3+ Nd3+-Nd3+ ions values approaches to ~15 Ao and the concentration of
ions doped BaPbAlFB glasses pumped at 808 nm laser diode excitation Nd3+ ions is greater than 12 × 1019 ions/cm3, then there will be a
wavelength. Three peaks are identified at 887, 1063, 1336 nm origi­ decrease in intensity of the peaks and the cross relaxation mechanism
nated from 4F3/2 → 4I9/2, 4F3/2 → 4I11/2 and 4F3/2 → 4I13/2 transition would initiated leading to concentration quenching [35]. Table 1 shows
states respectively. Among all the peaks, the transition 4F3/2 → 4I11/2 inter ionic distance along with Nd3+ ion concentration values for all the
centred at 1063 nm, comprised maximum intensity than the remaining as prepared glasses. From Table 1 it is conspicuous that, beyond 1 mol%,
two peaks. Fig. 5, clearly shows the effect of concentration of Nd2O3 ions Nd3+ ion doped in BaPbAlFB glass, the criteria for concentration
on intensity of the emission peaks. The intensity of emitted peaks in­ quenching gets fulfilled. Hence beyond 1 mol%, in Nd3+ ion doped
creases along with concentration of Nd3+ ions up to 1.0 mol% and BaPbAlFB glass cross relaxation mechanism got initiated. Furthermore,
the emission peak originated from 4F3/2 → 4I11/2 state at 1063 nm
Table 4 wavelength is having lot of significance as a potential laser emission
Transition probabilities (AR) (s− 1), total transition probability (AT) (s− 1), wavelength. This prominent wavelength is obtained by the mechanism
branching ratio (βR and βexp) and radiative lifetimes (τR) (μs) for the observed of lasing action in 4 level laser systems. Fig. 7 represents the partial
emission transitions of Nd3+ ions doped BaPbAlFB glasses.
energy level diagram highlighting PLE, PL and cross relaxation mecha­
Sample name Transition AR AT βR βexp τR nism observed in Nd3+ doped BaPbAlFB glasses. The lasing action takes
4
BaPbAlFBNd0.5 F3/2 → 4I9/2 266.13 1335.67 0.199 0.196 509
4
F3/2 → 6I11/ 846.30 0.633 0.624
2
4
F3/2 → 212.70 0.159 0.160
6
H13/2
4
BaPbAlFBNd1.0 F3/2 → 4I9/2 520.82 2526.20 0.206 0.214 272
4
F3/2 → 6I11/ 1588.98 0.629 0.667
2
4
F3/2 → 396.78 0.157 0.161
6
H13/2
4
BaPbAlFBNd1.5 F3/2 → 4I9/2 439.41 2102.75 0.209 0.213 312
4
F3/2 → 6I11/ 1318.58 0.627 0.618
2
4
F3/2 → 328.52 0.156 0.162
6
H13/2
4
BaPbAlFBNd2.0 F3/2 → 4I9/2 381.70 1882.95 0.202 0.207 401
4
F3/2 → 6I11/ 1188.84 0.631 0.637
2
4
F3/2 → 297.69 0.158 0.159
6
H13/2
4
BaPbAlFBNd2.5 F3/2 → 4I9/2 302.39 1517.28 0.199 0.120 559
4
F3/2 → 6I11/ 961.53 0.633 0.635
2
4
F3/2 → 241.42 0.159 0.161
6 Fig. 5. NIR emission spectra of different concentrations of Nd3+ ions doped
H13/2
BaPbAlFB glasses at 808 nm excitation wavelength.

5
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

place at 808 nm excitation due to the immediate falling of Nd3+ ions

from 4F9/2 excited state to 4F3/2 meta-stable state due to fast
non-radiative relaxation as shown in Fig. 7. This process leads to the
origination of peaks at 887 nm, 1063 nm and 1336 nm through radiative
transitions 4F3/2 → 4I9/2, 4F3/2 → 4I11/2 and 4F3/2 → 4I13/2 respectively.

3.3.2. (b) up-conversion (UC) spectral analysis

Fig. 6 depicts the UC spectra of different concentrations of Nd3+ ions
doped BaPbAlFB glasses under 585 nm excitation wavelength. The
observed luminescence spectra exhibits strong fluorescence in visible
region at 491 nm wavelength. The UC process may be associated with
the excited state absorption (ESA) from 4F3/2 to 2K15/2 levels. Fig. 7
represents the possible UC mechanisms in the as prepared glasses. In the
first step, Nd3+ ions in the ground level (4I9/2) gets excited directly by
absorbing the 585 nm photons to the excited 4G5/2 level and then relaxes
non-radiatively to the metastable 4F3/2 level. The cross-relaxation pro­
cess between the 4G5/2 and 4F3/2 levels causes the population of the 2K15/
3+
2 level by absorbing a second photon. Finally, the excited Nd ions at
2
K15/2 state can decay non-radiatively to the next lower energy level
4
G9/2 ground levels and causes the UC emission at 491 nm (4G9/2 → 4I9/
Fig. 7. Energy level diagram of Nd3+ ions doped BaPbAlFB glasses.
2).These transitions result in the visible UC luminescence at around 491
nm wavelength as shown in Fig. 7 [36,37].

3.4. Photoluminescence decay spectral analysis

The decay profiles recorded for 4F3/2 fluorescence level observed at

1063 nm for Nd3+ ions in BaPbAlFB glasses are shown in Fig. 8 under
808 nm excitation wavelength. From 0.5 to 1.0 mol% of Nd3+ in BaP­
bAlFB glasses the decay curves show single exponential nature and
thereafter (from 1.5 to 2.5 mol% of Nd3+ ions) changed to bi-
exponential nature. The main cause for this is migration of energy
among the Nd3+ ions. The experimental decay lifetimes are estimated
with the help of the following formulae and are given in Table 5 [38].
∫
I(t)
τexp = dt (single ​ exponential) (13)
IO

A1 τ21 + A2 τ22
τexp = (bi − exponential) (14)
A1 τ 1 + A2 τ 2

here, I(t) and Io are the emission intensities at t = t and t = 0 respec­

tively, A1 and A2 are constants, τ1 and τ2 are the short and long decay Fig. 8. Decay curves of the 4F3/2 level of Nd3+ ions in BaPbAlFB glasses.
times, respectively. From the data given in Table 5, it can be observed

Table 5
Radiative (τR) (μs) & measured lifetimes (τexp) (μs), quantum efficiency (η), non-
radiative relaxation rate (WNR) and saturation intensity (IS) (x108) W/m2 of
Nd3+ ions doped BaPbAlFB glasses along with reported values for other glasses.
Sample τR τexp η (%) WNR IS References

BaPbAlFBNd0.5 509 350 69 892 4.18 Present work

BaPbAlFBNd1.0 272 245 90 405 3.22 Present work
BaPbAlFBNd1.5 312 179 57 2381 5.37 Present work
BaPbAlFBNd2.0 401 139 35 4700 7.76 Present work
BaPbAlFBNd2.5 559 85 16 9975 15.8 Present work
LBZNd1.0 597 412 69 752 – [9]
LiPbAlBNd1.0 147 113 77 2046 5.51 [22]
BSGdCaNd0.5 600 385 57 – 3.98 [32]
PKAlCaFNd1.0 220 154 70 1940 2.41 [42]
TZNLNNd1.0 154 136 88 859 3.20 [43]

that, τexp values are decreasing with increase in Nd3+ ions concentration
in the titled glasses due to self-quenching mechanism. In self-quenching
mechanism, energy transfer takes place among the excited state Nd3+
ions (donors) and ground state Nd3+ ions (acceptors) through cross
relaxation process and depopulates the 4F3/2 emitting level through non-
Fig. 6. Up-conversion spectra of various concentrations of Nd3+ ions doped radiative (NR) mechanism [39]. Further, one of the significant param­
BaPbAlFB glasses at 585 nm excitation wavelength. eter, quantum efficiency (η) which estimates the lasing capability of the

6
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

as prepared samples can be estimated by using the relevant equation as ∫

I(λ)dλ
given below. ΔλP = (18)
IP
τ
η = exp (15)
τR here, I(λ) and IP denotes the intensities at emission wavelength λ, and
Table 5 shows the obtained η values for BaPbAlFBNd glasses doped emission peak wavelength λP. Table 6, represents the calculated σSe
with various concentrations of Nd3+ ions. The NR energies are explained values of the as prepared glasses. From Table 6, it is identified that the 1
by NR transition rate (WNR) calculated using the following equation and mol % of Nd3+ ions doped BaPbAlFB glass acquires maximum value of
are given in Table 5; σSe (7.23 × 10− 20 cm2) at 1063 nm when compared with the reported
values [44–48]. Relatively higher value of σSe observed for BaP­
WNR =
1
−
1
(16) bAlFBNd1.0 glass speaks its suitability to produce efficient NIR laser
τexp τR emission at 1063 nm. Further the remaining pre-eminent parameters
From Table 5 it is observed that, BaPbAlFBNd1.0 glass possesses such as gain bandwidth (σSe × ΔλP), which states the performance of the
lowest value of WNR than the remaining glasses, indicating potentiality optical amplification, optical gain (σSe × τR) represents the laser
of that glass to give intense radiative laser emission at 1063 nm. Ac­ threshold values, are evaluated and are given in Table 6. Here, BaP­
cording to Dexter [40], the non-radiative relaxation rate is proportional bAlFBNd1.0 glass possesses low gain bandwidth and high optical gain,
to the squared concentration. Fig. 9 indicates the NR relaxation rates which describes the suitability to attain high gain laser performance.
that varies consistently with the squared concentration (N) from BaP­ Therefore, BaPbAlFBNd1.0 glass might be a suitable one for broadband
bAlFBNd1.5 glasses, because of the migration of energy among optical amplification at 1063 nm (4F3/2 → 4I11/2).
Nd3+-Nd3+ ions pair through dipole–dipole interaction [41]. Table 5, Further, the branching ratios of both experimental and radiative
depicts τR, η and WNR values along with τexp for all the as prepared (βexp and βR) are noted in Table 4. From Table 4, it can be identified that
glasses along with literature values [9,22,32,42,44]. From the data βexp and βR values are greater than 0.50 for 4F3/2 → 4I11/2 transition. It is
shown in Table 5, it is conspicuous that, BaPbAlFBNd1.0 glass possesses well known that, branching ratio values greater than 0.5 indicates
relatively highest quantum efficiency than the other glasses of the pre­ favourable condition to get efficient lasing action. Therefore looking at
sent work and glasses reported in literature. the values of branching ratio reported in Table 4 it is contemplated that,
BaPbAlFBNd1.0 glass is quite suitable to produce prospective NIR laser
3.5. Laser quality parameters analysis emission at 1.06 μm. Another way to calculate radiative branching ratios
(βR*) with the help of spectroscopic quality factor (χ) followed by T. S.
Stimulated emission cross-sections (σse), effective bandwidths (ΔλP), Lomheim and L. G. De Shazer procedure [49] is as follows;
figure of merit (σsexτexp), gain bandwidths (σsex ΔλP), branching ratios ( ) (0.3194 + χ ) + 0.07671
(β), optical gains (σsex τR) and saturation intensities (Is) are the laser β*R 4 F3/2 → 4 I9/2 = (19)
(0.4247 + χ ) + 0.4567
quality parameters used to explain the reliability of the as prepared
glasses for practical laser applications. The stimulated emission-cross ( ) (0.10534 + χ ) + 0.2874
β*R 4 F3/2 → 4 I11/2 = (20)
section (σse) is one of the most prominent parameter used to under­ (0.4247 + χ ) + 0.4567
stand the lasing potentiality of a glassy material doped with RE ions. The
following expression is employed to estimate σse value; ( ) 0.0902
β*R 4 F3/2 → 4 I13/2 = (21)
(0.4247 + χ ) + 0.4567
λ4p
σ se = AR (17) It is also proposed that the ratio between βR* 4F3/2 → 4I11/2 and βR*
8π cn2 Δλ
4
F3/2 → 4I13/2 has a linear relation with χ-parameter in accordance with
P

here, λP represents the peak emission wavelength and ΔλP is the fluo­ the below equation
rescence effective line width, which is expressed by

Table 6
Emission peak wavelength (λP) (nm), effective band widths (ΔλP) (nm), stimu­
lated emission cross-sections (σse) (x10− 20) (cm2), gain bandwidth (σse x Δλp)
(10− 28) (cm3) and optical gain parameters (σse x τR) (10− 25) (cm2s) for the
emission transitions of Nd3+ ions doped BaPbAlFB glasses.
Spectral BaPbAlFB BaPbAlFB BaPbAlFB BaPbAlFB BaPbAlFB
parameters Nd0.5 Nd1.0 Nd1.5 Nd2.0 Nd2.5
4
F3/2 → 4I9/2

λp 887 887 887 887 887

Δλp 14.8 15.6 15.1 12.3 11.6
σse 1.40 2.57 2.34 2.22 1.94
σse x Δλp 0.20 0.40 0.33 0.28 0.22
σse x τR 71.2 69.9 73.0 89.0 108.4
4
F3/2 → 6I11/2
λp 1063 1063 1063 1063 1063
Δλp 32.45 34.8 33.8 33.6 33.5
σse 4.18 7.23 6.11 5.48 4.40
σse x Δλp 1.35 2.51 2.06 1.84 1.47
σse x τR 212.5 196.6 190.6 219.2 245.9
4
F3/2 → 6H13/2
λp 1336 1336 1336 1336 1336
Δλp 4.40 5.37 3.88 3.14 2.95
σse 0.19 0.36 0.33 0.31 0.29
σse x Δλp 0.84 1.56 1.28 1.15 1.00
Fig. 9. Non-radiative relaxation rate (WNR) dependence on square of the con­
σse x τR 9.67 9.79 10.29 12.4 16.2
centration of Nd3+ doped BaPbAlFB glasses.

7
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

β*R (4F3/2→4I11/2)
= 1.167χ + 3.185 (22)
β*R (4F3/2→4I13/2)

For all the BaPbAlFBNd glass samples, the calculated ratio (R[βR* ])
of βR* (4F3/2 → 4I11/2) and βR* (4F3/2 → 4I13/2) is identified as nearer to
those acquired from R[Q] = (1.167 × Q) + 3.185 and are displayed in
Table 7.
The absorption and emission cross-sections are playing a significant
role in optical amplifiers and fiber lasers. The absorption cross section
(σabs) can be estimated using the below equation [50].
OD(λ)
σ abs (λ) = 2.0303 (23)
Nl

here, OD(λ) denotes the optical density and N represents the Nd3+ ion
concentration. By using the Fuchtbauer-Ladenburg formula [51] and
calculated σ abs values, stimulated emission cross-section (σecs) can be
evaluated as follows.
⎡ ⎤
hc
zl ⎢Ezl − λ ⎥ Fig. 10. Computed absorption and emission cross-sections of Nd3+: 4F3/2 →
σ ecs (λ) = σabs (λ) exp⎣ ⎦ (24)
4
zu KT I11/2 transition in BaPbAlFB glasses.

where Zl and Zu denotes partition functions pertaining to lower and

upper manifolds respectively [52]. Ezl denotes energy gap existing in
between the lowest Stark levels of two manifolds. The σabs and σecs
values obtained for 4F3/2 → 4I11/2 transition of BaPbAlFBNd1.0 glass are
5.84 × 10− 20 cm− 20 and 7.79 × 10− 20 cm− 2 respectively. The σabs and
σecs values obtained in the present work are shown in Fig. 10. The gain
cross-section spectra G(λ) which estimates laser wavelength probability,
is determined by absorption and emission cross-sections values with the
help of the given equation.
G(λ) = γ N σecs (λ) − (1 − γ)N σacs (λ) (25)

where, γ represents the population inversion rate for 4F3/2 → 4I11/2 laser
emission. This γ value increased from 0 to 1.00 in 0.1 step comprise the
evaluated gain cross-section spectra versus the wavelength as shown in
Fig. 11. It is clear from Fig. 11 that, there appears a positive gain at γ =
0.2, which denotes the low pumping threshold.
At the operating time of cw laser material, low threshold values are
favourable for the pump input power. In this the threshold value varies
uniformly with IS and non-uniform with σ se and τexp . Therefore, IS is Fig. 11. Gain cross-sections with various γ values corresponding to Nd3+: 4F3/2
determined by the following equation [53]. → 4I11/2 transition in BaPbAlFB glasses.
hc
IS = (26) variation of saturation intensity with concentration of Nd3+ ions in
λp σse τexp
BaPbAlFB glasses. Fig. 13 show comparison of η, σse and Is values ob­
As per the aforementioned equation, higher the product of σ se and tained in the present work with the values reported in literature. As
τexp results in the lowering of the Is values; this leads to the low laser shown in Fig. 13, the value of Is obtained for 1 mol% of BaPbAlFBNd
threshold values. Table 5, shows the IS value along with other radiative glass is 3.22Х108 W/m2, which is minimum than the other Nd3+ ions
properties of the BaPbAlFBNd glasses along with the other Nd3+-doped doped glasses reported in literature [22,43,54]. This clearly indicates
host glasses. As per the data given in Table 5, the value of laser threshold the superiority of BaPbAlFBNd1.0 glass for NIR lasing applications.
is minimum for 1 mol% of Nd3+ ions in BaPbAlFBNd glass and increases
with increase in Nd3+ ion concentration showing superiority of BaP­
bAlFBNd1.0 glass for 1063 μm laser emission. Fig. 12 shows the 3.6. Figure of merit for gain and bandwidth analysis

Figure of merit for gain and bandwidth denoted by FOM (G) and
Table 7 FOM (B) respectively are important parameters used to estimate the
Comparison of Lomheim-Shazer branching ratios (βR*) of 4F3/2 → 4I11/2 and 4F3/ efficiency of an optical fiber [55]. The FOM (G) used to evaluate the
4
2 → I13/2 transitions, their ratio (R[βR*]) and the linear relation of quality factor threshold power of a glass material and can be calculated by using the
(R[χ]) in BaPbAlFBNd glass samples. given equation [56].
Glass χ βR*(4F3/2 → βR*(4F3/2 → R Rχ FOM(G) = σ se τexp (27)
4 4
I11/2) I13/2) (βR*)

BaPbAlFBNd0.5 0.90 0.4532 0.096 4.720 4.235 Table 8 gives the calculated FOM (G) value for BaPbAlFBNd1.0
BaPbAlFBNd1.0 0.91 0.4544 0.097 4.684 4.246 including other reported values [57–59]. To accomplish high gain laser
BaPbAlFBNd1.5 0.88 0.4521 0.095 4.758 4.223 medium, maximum should be the FOM value. Hence the FOM value is
BaPbAlFBNd2.0 0.87 0.4495 0.093 4.833 4.200 uniformly varies with the slope efficiency and inversely varies with the
BaPbAlFBNd2.5 0.86 0.4457 0.089 5.007 4.188
threshold pump power [60]. While the FOM for bandwidth can be

8
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

Table 8
Spectroscopic figure of merit [FOM(G)] for 4F3/2 → 4I11/2 transition in BaP­
bAlFBNd1.0 glass along with various Nd3+ ions doped host glasses.
24
Sample Wavelength FOM(G) (X10− s Reference
(nm) cm2)

BaPbAlFBNd1.0 1063 17.71 Present

work
Fluorophosphate 1053 13.33 [57]
49.5GeO2-40Sb2O3–10BaO- 1064 6.044 [58]
0.5Nd2O3
BGG 1054 4.56 [59]

4. Conclusions

Optical absorption and spectroscopic studies of BaPbAlFB glasses

activated with Nd3+ ions have been analyzed using absorption, PLE, PL
and PL decay investigations. Absorption spectral data is used to estimate
oscillator strength, bonding parameters and nephelauxetic ratio needed
to predict radiative properties and bonding nature in the as prepared
glasses. The Ω2 J-O parameter evaluated reveals the nature of bonding
Fig. 12. Saturation intensity (Is) of 4I11/2 transition at various concentrations of between neodymium and oxygen ligands in the as prepared glass is
Nd3+ ions doped glasses. covalent in nature. Correlation of absorption and emission spectral data
allows to estimate emission cross-sections, branching ratios and spec­
troscopic quality factor (Ω4/Ω6). The PL decay profiles of recorded for
4
F3/2 level under 808 nm excitation were used to estimate experimental
lifetimes. The experimental lifetimes are gradually decreasing with in­
crease in Nd3+ ion concentration. The laser quality parameters namely
quantum efficiency, saturation intensity, figure of merit, absorption
cross-section, emission cross-section and gain cross-section have been
evaluated. All the results observed finally reveals the suitability of
BaPbAlFBNd1.0 glass for potential NIR laser application at 1.063 μm.

Credit author statement

Author contributions:P. Rekha Rani synthesized and performed ex­

periments. Dr. M Venkateswatlu performed JO calculations and super­
vised in understanding those results along with Dr.K. Swapna, Dr. Sk.
Mahamuda, Dr. Ch.B. Annapurna Devi and Dr. A.S Rao, analyzed the
results and wrote the manuscript as well as participated in revising it
critically for important intellectual contents to be published. All authors
discussed the results and contributed to the final manuscript.

Declaration of competing interest

Fig. 13. Comparative studies of η, σse, Is values of BaPbAlFBNd1.0 glass with
other host glasses.
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
determined from the σse and fluorescence effective line width values by the work reported in this paper.
using the following relation.
FOM(B) = σse Δλp (28) Acknowledgements

here, the calculated FOM (B) values for Nd3+ ions doped BaPbAlFB The authors, Dr. K. Swapna (File Number: ECR/2015/000335), Dr.
glasses are 1.35, 2.51, 2.06, 1.84 and 1.47 respectively. Among them, Sk. Mahamuda (File Number: ECR/2016/000376) and Prof. A. S. Rao
BaPbAlFBNd1.0 glass acquired maximum value than the remaining (EMR/2016/007766) are thankful to Department of Science and Tech­
glasses at 1063 nm wavelength; this shows the suitability of BaP­ nology (DST), Govt. of India, New Delhi for the award of major research
bAlFBNd1.0 glass in the applications of C-band telecommunication and projects to them under DST-SERB. The authors are also very much
amplifier applications. Further, BaPbAlFBNd1.0 has maximum values of thankful to Prof. C. K. Jayasankar, S. V. University, Tirupati for
FOM(G) than the other reported values. This speaks the superiority of extending his research lab facilities. The authors also thank Department
BaPbAlFBNd1.0 glass for 1063 nm NIR applications. of Science and Technology (DST), Govt. of India, for the award of DST-
FIST Level-1 (SR/FST/PS-1/2018/35) scheme to Department of Physics,
KLEF.

9
P.R. Rani et al. Journal of Luminescence 229 (2021) 117701

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