Physica B: Physics of Condensed Matter 530 (2018) 43–48

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Physica B: Physics of Condensed Matter

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Effect of alkaline earth modifier on the optical and structural properties of

Cu2þ doped phosphate glasses as a bandpass filter
M. Farouk a, *, A. Samir b, M. El Okr a
a
Physics Department, Faculty of Science, Al- Azahr University, Nasr city, Cairo, 11884, Egypt
b
Engineering Mathematics and Physics Department, Faculty of Engineering at Shoubra, Benha University, 11629, Egypt

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

Keywords: Glasses of composition [16RO–3Al2O3–6CuO–20Na2O–55P2O5], where R is the alkaline earth (R ¼ Mg, Ca, Sr
Optical filters and Ba mol. %), were prepared by conventional melt quenching technique. The glass samples were characterized
Structure by X-ray diffraction, infrared spectroscopy, and spectrophotometer. XRD patterns show no sharp peaks indicating
Alkaline earth the non-crystalline nature of the prepared glasses. The density and molar volume of the glass systems were
Phosphate glass determined in order to study their structures. These results revealed that addition of alkaline earth elements leads
to the formation of non-bridging oxygens (NBOs) and expands (opens up) the structure. The infrared spectra were
analyzed to quantify the present phosphate groups. The optical absorption spectra of Cu2þ ions show the char-
acteristic broadband single of Cu2þ ions in octahedral symmetry. The band gap was estimated following two
methodologies. The first method considers the band edge of the transmission, while the second approach relays on
the estimated values of the optical constants. A decent agreement for the band gap values using the two methods
was obtained.

1. Introduction produce coloring, while Cu2þ ions create color centers with an absorption
band in the visible region and produce blue and green glasses. The color
Copper-doped phosphate glasses have interesting optical and elec- of the glass depends on the Cu2þ content, its specific coordination,
trical properties that make them suitable as color filters, solid state lasers, composition and basicity of the glass. Colors produced by Cu2þ ions in
super-ionic conductors, and non-linear optics. The primary advantage of various glasses have been interpreted in terms of ligand field theory
phosphate over other oxide glasses (e.g. silicate and borate) is their [2,5–7]. Optical Filters are being used in many applications such as
ability to accommodate high concentrations of transition metal ions and fluorescence microscopy, photography, optical device, spectroscopy,
remain amorphous. In addition, phosphate glasses enjoy a range of clinical chemistry, or machine vision inspection. Optical Filters are also
compositional and structural possibilities (ultra, meta, pyro, and ortho) suitable for life science, imaging and professional. Bandpass filters
that facilitate tailoring chemical substance and physical behavior [1]. transmit a band of wavelengths spanning the region from 1 nm to hun-
The poor chemical durability of phosphate glasses makes them dreds of nanometers in width, while adjacent wavelengths are blocked.
generally unsuitable for practical applications. It was suggested that the Band pass filters are, additionally, used in fluorescence microscopes to
chemical durability can be improved by the addition of one or more of eliminate pump light from fluorescence signal light, eye protection from
multivalent oxides such as: Al2O3, SnO, ZnO,PbO, Fe2O3, etc., which laser radiation by eliminating infrared laser light and passing only the
promotes the formation of Al–O–P, Sn–O–P,Zn–O–P, Pb–O–P, visible light, and in sunglasses to pass the visible and block UV light [8].
Fe–O–P bonds, and subsequently increases the chemical durability to a
measurable extent. A second alternative towards improving the chemical 2. Experimental details
durability of phosphate glasses is the partial replacement of oxygen by
nitrogen atoms [2–4]. In glasses, copper ions exist in more one valance The glassy system with composition
state, monovalent (Cuþ) ions, and divalent (Cu2þ) ions and may also exist [16RO–3Al2O3–6CuO–20Na2O–55P2O5], where R is the alkaline
as metallic copper (Cu0). The electronic structure of the copper atom is earth elements (R ¼ Mg, Ca, Sr and Ba mol %), were prepared by con-
3d10 4s1; the cuprous ion, having its 5 d orbitals occupied, does not ventional melt quenching method. The starting materials used in the

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

https://doi.org/10.1016/j.physb.2017.11.013
Received 19 August 2017; Received in revised form 1 November 2017; Accepted 2 November 2017
Available online 6 November 2017
0921-4526/© 2017 Elsevier B.V. All rights reserved.
M. Farouk et al. Physica B: Physics of Condensed Matter 530 (2018) 43–48

present work were reagent grade of CuO, MgO, CaO, SrCO3, BaCO3, Table 1
Na2CO3 and NH4H2PO4. All weighted chemicals were powdered finally Various physical parameters of Cu2þ doped sodium aluminum phosphate glasses.

and were thoroughly mixed in an agate mortar. Each batch was intro- Physical property MgO CaO SrO BaO
duced in porcelain crucibles in an electrical furnace at 400 ± 5  C to Density (g/cm3) ±0.02 2.60 2.64 2.80 2.99
remove water, ammonia and then melted at the 1100 ± 20  C for 1.5 h. Average molecular weight (g)±0.02 104.72 107.25 114.85 122.81
The melts were quenched between two brass plates to produce discs of Molar volume,VM, (cm3)±0.02 40.13 40.52 41.01 41.05
about 0.2 cm thickness. The prepared samples were subjected to Cu2þ-ion concentration N (x1020 ions/ 8.99 8.91 8.80 8.79
cm3)±0.02
annealing at 350 ± 5  C to remove internal stress. The glass samples Inter ionic distance (ri) (x107) cm 1.0357 1.0390 1.0433 1.0435
obtained were homogeneous with green color. X-ray diffraction (XRD) ±0.0002
spectra were obtained using a Shimadzu XD3A diffractometer. The Field Strength F (x1015cm2)±0.0001 1.1482 1.1409 1.1317 1.1311
densities of the prepared glass samples were measured by employing
Archimedes's method with toluene as an immersion fluid (ρ ¼ 1.595 kg/
m3). Infrared absorption spectra were recorded using FTIR (PerkinElmer)
in the range (400-2000 cm1). The samples were prepared using the KBr
disc technique. The absorption spectra were measured in the resolution
of 1cm1. The optical absorption spectra of well-polished glass samples
were taken at room temperature by UV–Vis spectrophotometer (JASCO
V670) with the optical resolution 0.5 nm, in the wavelength range
of 190–1100 nm.

3. Results and discussion

3.1. Physical parameters

The amorphous nature of the prepared glass samples was firstly

examined by X-Ray diffraction (XRD) at room temperature. Fig. 1 dis-
plays the obtained XRD patterns which clearly do not present sharp
diffraction peaks, confirming the non-crystalline characteristics of the
prepared glasses.
Some properties of the investigated glass system are listed in Table 1. Fig. 2. Dependence of density, and the molar volume, VM, on alkaline earth elements.
Fig. 2 hows the dependence of density and the molar volume (VM) on the
type of alkaline earth elements. The density of all glass samples increases  
ion xρNA
by increasing the atomic weight of alkaline earth elements. This is most N ¼
cm3 Mw
likely due to the fact that density is very sensitive to both the ionic size
and atomic weight of the alkaline rare earth. Generally, it is always ex- where NA is Avogadro's number, x is the mole fraction of the alkaline
pected that the density and the molar volume should show opposite earth element, ρ is the density and Mw is the average molecular weight of
trend. However, in the present work, both the density and molar volume each sample. The calculated values of N are listed in Table 1 and plotted
follow the same trend. Such an unusual behavior allows concluding that in Fig. 3. The data revealed that the Cu-ion concentration decreases,
the addition of alkaline earth causes the formation of non-bridging ox- which is most likely due to the increase of Cu–Cu spacing. With the
ygens (NBOs) and expands (opens up) the structure. This might also be evaluated magnitudes of (N), it is possible to estimate three additional
due to change of metaborate network induced by the addition of alka- parameters [9]. These are;
line earth.
  
The Cu-ion concentration (N) is the parameter of greatest interest as it 1 π 1=3
rp ðAo Þ ¼
affects different properties of the host material. The number of ions per 2 6N
cubic centimeter was calculated according to the following formula [9].

Z
F cm2 ¼ 2
rp

Fig. 1. The X-ray diffraction patterns of the glass samples. Fig. 3. Dependence of Cu2þion concentration, N, on alkali earth oxides.

44
M. Farouk et al. Physica B: Physics of Condensed Matter 530 (2018) 43–48

 13
1
ri ðAo Þ ¼
N

where rp is the Polaron radius, F is the average field strength, Z is the

valance of copper ion and ri is the inter-ionic distance. The calculated
values for each parameter are given in Table 1 and displayed in Fig. 4. It
is generally assumed that the average ion separation and the field
strength should follow an opposite trend, which is clearly observed in the
present work. Furthermore, the average Cu ion separation increases,
which can be attributed to the open structure caused by changing of the
alkaline earth elements. The field strength (F) decreases with changing
the alkaline earth elements, i.e., the results follow the common behavior,
where the average Cu–Cu distance increases producing a weaker field
around the Cu2þ ions. Therefore, changes in the physical properties of the
prepared glasses are mainly due to the change in the host matrix around
Cu2þ ions.

3.2. 3.2 FT-IR spectra Fig. 5. Infrared spectra of Cu2þ doped alkaline earth phosphate glasses.

Infrared spectroscopy is usually used to get the essential information

concerning the arrangement of the structural units of the studied glasses.
It is assumed that vibrations of structural units in the glass network are
independent of the vibrations of other neighboring units. The phosphate
units in phosphate glasses exist in the range 1400–400 cm1. The
infrared spectra of Cu2þ sodium aluminum phosphate glasses doped
alkaline earth are shown in Fig. 5.
The spectral broadening is consistent with structures having various
types of bonding. The obtained broad bands are a result of the overlap
between some individual bands. Each individual band has its own
characteristic parameters such as center, which is related to some type of
vibrations of a specific structural group, and relative area, which is
proportional to the concentration of these structural groups [10]. Fig. 6
shows the deconvoluted spectra assuming Gaussian bands. The decon-
volution data (center position c, relative area A and the corresponding
assigned vibrational modes) are given in Table 2. The band located at
around 497-507 cm-1 is assigned to the bending vibrations of O–P–O Fig. 6. Deconvolution of IR spectra of MgO glass as example.
linkages in the Q3 units [11]. The assignment of the band between 400
and 550 cm1 is difficult because of the superposition of intermediates
like MgO, CaO, SrO and BaO in the present glass system [12]. The band Table 2
around 738–750 cm-1 is attributed to symmetric stretching vibrations of Band assignments for IR spectra.

P–O–P rings in Q1 units [12]. The band near 881–978 cm1 is due to Band center c (cm1)/Relative Band assignments
the asymmetric stretching vibrations of the P–O–P linkage in Q2 area A (±3)
units [13–15]. MgO CaO SrO BaO
The observed strong band, in the region 800–1000 cm1 in the 497 507 496 501 O–P–O bending vibrations [13,14]
spectra of all the investigated glasses, which is the characteristic of linear 63 16 38 25
phosphates, suggests the presence of linear chains [12]. The band at 750 738 747 747 P–O–P symmetric vibrations [13,14]
15.3 2 8.7 3.7
881 891 891 885 P–O–P asymmetric stretching vibrations
15.1 2 3.5 6.3 [13,14].
977 966 978 975 (PO4) asymmetric stretching (Q0) [15].
34 8.9 35.7 20.7
1102 1098 1112 1104 Symmetric stretching vibrations of Q2 (PO2)
25 9.3 9.6 13 groups [13,14]
1162 1169 1165 1161 PO2  symmetric groups P– –O stretching
4 2.1 3.2 2.4 vibrations [16]
1267 1272 1270 1269 PO2 asymmetric groups P– –O stretching
25 6.1 11.8 11.5 vibrations [13,14]
1399 1417 1379 1376 Stretching modes of bridging oxygen in P–
–O
28 8.2 26 24.9 bond [13]
1527 1530 1532 1532 bending vibrations H–O–H and P–OH in the
5 4.2 7 6.5 network (bridge) [7,15,18]
1656 1648 1644 1640
12 4.1 5 3.2

1098–1112 cm1 is most likely due to the asymmetric stretching vibra-

Fig. 4. Dependence of inter ionic distance, ri, and the field strength, F, on alkaline tions of (PO3)2 groups [15]. The band at 1161-1169 cm1 is attributed
earth elements.

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M. Farouk et al. Physica B: Physics of Condensed Matter 530 (2018) 43–48

to the symmetric stretching vibrations of metaphosphate of PO2 groups

[16]. The band around 1267–1270 cm1 is associated with the asym-
metric (P–– O) stretching vibrations [13,14]. The band observed at
1376–1417 cm1 has been attributed to symmetric stretching vibrations
of bridging oxygen in P–– O bond [13]. Introduction of modifiers, such as
MgO, CaO, SrO and BaO, to the phosphate network would locate them
among the non-bridging oxygens (NBOs), sharing corners with (PO4)3
groups that connect different phosphate chains such as P4O6 5
13 , P3O10 ,
4 -1
and P2O7 [12,15]. The other two bands nearly at 1527–1532 cm and
1644–1656 cm1 are related to bending vibrations of O–H and P–OH
bonds brought by air moisture during the preparation of KBr pellets for
infrared measurements [10,11,15,17,18]. The changes in band position
are not uniform as the alkaline rare earth changes. The shift to the lowest
frequency is at calcium oxide (CaO).

3.3. Optical absorption studies

The UV transmittance is mostly influenced by heavier elements in the

glass composition, melting technology and residual impurities. Heavy
elements lead to increase in the refractive index and a decrease of
transmittance in the UV region [19]. The transmission spectra of the glass
samples in the wavelength range 190–1100 nm are shown in Fig. 7. As
observed, aluminum phosphate glass containing Cu2þ ions and doped
Fig. 7. Optical transmission spectra of Cu2þ ions doped alkaline earth phosphate glasses.
with alkaline earth, exhibit high optical transmission from about
350–650 nm. It is observed that sample containing SrO exhibits a higher
transmittance while CaO has the lower transmission. One should expect Table 3
that the addition of MgO, CaO, SrO and BrO causes fluctuations in the The optical parameters.
ligand field around the Cu2þ probe ion. This is related to changes in
RO Eopt (ev) Eopt (ev) Ee (ev) UV cut UV IR cut
polarizability of oxygen ion surrounding the Cu2þ and its dependence on mol From ASF From ε2 ±0.003 off ±3 Bandstop off ±3
the field strength of the glass network [12]. The values of UV, IR cut off % ±0.01 ±0.01 ±4
and UV bandstop are listed in Table 3. MgO 3.64 3.65 0.293 293 190–293 771
The absorption spectra of the glass samples exhibit a broad absorption CaO 3.68 3.78 0.287 290 190–290 796
band around 780 nm and it is due to 2B1g→2B2g octahedral transition of SrO 3.56 3.68 0.295 294 190–294 820
Cu2þ ions [19]. The Cu2þ ions is disturbed by an electronic hole in the BaO 3.52 3.62 0.299 295 190–295 815
degenerate orbital which has caused the tetragonal distortion according
to Jahn-teller theory, i.e., any non-linear system with the degenerate
ground state should distort in order to eliminate the degeneracy. Table 4
Therefore, the structural changes may be possible, one is elongated and The center (C), area (A), full width at half maximum (FWHM) and height of bandpass filter.

the other is compressed in the structure [12]. The band passes in optics RO mol% C (nm) A (cm2) FWHM Height
are techniques that allow to pass a band of spectral lines through a filter MgO 482.2 25563.8 263.8 81
[20,21]. The filter is characterized by parameters such as center c, CaO 485.6 28146.8 277.7 84
FWHM, height and the area of the bandpass. Table 4 shows the change of SrO 498.6 29084 274 94
these parameters with alkaline earth content (RO mol %). The center of BaO 499.9 25707.7 278.2 81.04

the bands of Cu2þ doped glass samples shows that these filters lay in the
green band. where B is a constant, Eopt is the optical band gap energy, and n may have
the following values 2, 3, 1/2 and 1/3 depending on the interband
3.3.1. Optical band gap energy (Eopt) and Urbach energy (ΔE) electronic transition (direct and indirect). The analysis of the data reveal
The optical absorption is a convenient technique to understand the that in the present case n ¼ 2, indicating an indirect transition. From the
electronic structure in glasses. The dependence of the optical band gap on plots of (αhν)1/2 as a function of photon energy (hν), the values of Eopt
the composition of glasses gives information about the structure and the can be obtained by the extrapolation of the linear region of the plots to
nature of bonds within the matrix. The absorption spectra of alkaline the hν axis for indirect transitions and are shown in Fig. 8.
earth-aluminum phosphate glasses have been recorded in the wavelength The width of the tail of the absorption spectra can also be used to
range 190–1100 nm. All investigated glasses exhibit an optical absorp- analyze possible changes in the glass structure [23]. It is worth noted that
tion band in the UV, near infrared region and the fundamental optical for lower values of the absorption coefficient α (ν)  103–104 cm1, it
absorption edge in the UV region. The absorption coefficient (α) of glass exhibits an exponential increase and is given by Refs. [24,25]:
spectrum was calculated using the equation [22]:
 
 
1 I0 hν
ΔE
αðνÞ ¼ log αðνÞ ¼ α0 exp
t I
where α0 is a constant, hν is the photon energy and ΔE is the Urbach
where t is the thickness of the sample and (I0/I) corresponds to absor-
energy, which indicates the width of the band tail of the localized states
bance near the edge. α (ν) can be related to optical band gaps for direct
in the band gap. The Urbach energy (ΔE) values of the present glass
and indirect transitions following Davis and Mott [23]:
samples were determined by taking the reciprocals of the slopes of the


hν  Eopt n linear part of the ln(α) versus hν plots as shown in Fig. 9.
αðνÞ ¼ B The obtained values of Eopt and ΔE are listed in Table 3 and plotted in
hν

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M. Farouk et al. Physica B: Physics of Condensed Matter 530 (2018) 43–48

Fig. 10. Dependence of optical band gap (Eopt) and the Urbach's Energy (ΔE) with the
content of alkaline earth.

Fig. 8. Tauc's plot for Cu2þ ions doped alkaline earth phosphate glasses.

Fig. 10. It is clear that they follow opposite trends. The values of the
optical band gap vary with the alkaline earth oxide content. The Eopt
values of these glasses are in the same range observed for another glassy
system [12]. In fact, alkaline earth additives may enhance the degree of
localization by creating defects. The addition of network modifiers, such
as alkaline earth oxides, breaks these bridges and creates non-bridging
oxygens (NBOs). The increase in Eopt for the glass samples could be
related to the increase of the cross-linking density in the glassy matrix
[25]. Urbach energy values decrease with increasing the alkaline earth
contents. The obtained smaller values of Urbach energy indicates that
Cu2þ doped alkaline earth-aluminum phosphate glasses are homoge-
neous and stable [12]. This is likely to be related to the increase in the Fig. 11. Imaginary part of the dielectric constant as a function of photon energy.
number of NBOs in the glass matrix, which means enhancement of the
degree of disorder that causes more defects or localized states in the band
gap [25,26]. ε1 ¼ n2  k2
Optical energy gaps (Eopt) were also calculated using the imaginary
part of the dielectric constant, ε2. Imaginary and real parts of dielectric ε2 ¼ 2nk
constant (ε2; ε1) are calculated by using the relations [27,28]:
1
where n is the refractive index, k is extinction coefficient and α is
2 1 þ R2
n ¼ 1
1  R2

K ¼ αλ=4π

Fig. 12. Comparison of band gap energy values which calculated from the absorption
spectrum fitting (ASF) method and imaginary part of the dielectric constant (ε2) as a
2þ
Fig. 9. Urbach plot for Cu ions doped alkaline earth phosphate glasses. function of alkaline earth.

47
M. Farouk et al. Physica B: Physics of Condensed Matter 530 (2018) 43–48

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