Ceramics International 43 (2017) 15635–15644

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Ceramics International
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Preparation and study of optical, thermal, and antibacterial properties of MARK

vanadate–tellurite glass
⁎
N. Elkhoshkhanya, , Ali Redaa, Amira M. Embabyb
a
Department of Material Science, Institute of Graduate Studies and Researches, Alexandria University,163 Horreya Avenue, Shatby 21526, Egypt
b
Department of Biotechnology, Institute of Graduate Studies and Research, Alexandria University, Egypt, 163 Horreya Avenue, Shatby 21526, Egypt

A R T I C L E I N F O A BS T RAC T

Keywords: The present study highlights the formulation, the properties (physical, optical and thermal), and the
Vanadate–tellurite Glass antibacterial potential of vanadate–tellurite Glass System. The quaternary sample system (90-X) TeO2− 5
Optical properties CaO −5 Na2O- X V2O5) where x = 5, 10, 15 and 20 mol% was prepared via conventional melt cast-quenching
Thermal properties technique. Thermal stability, fragility and crystallization kinetics like activation energy and Avrami number
Antibacterial properties
have been estimated. The optical properties were investigated in terms of Cut-off wavelength λc, Urbach energy
ΔE, optical band gap Eopt, refractive index and molar refractive. A broad spectrum antibacterial activity of
vanadate–tellurite glass was confirmed against two Gram +ve bacteria (e.g., Enterococcus faecalis and Listeria
monocytogenes) and three Gram -ve bacteria (e.g. Pseudomonas aeruginosa, Escherichia coli and Salmonella
entericaserovar Typhimurium). The antibacterial potential of V2O5 incorporated in tellurite glass increased
significantly (P < 0.01) with increasing the concentration of V2O5 from 5 to 20 mol% in TVCN for all tested
bacterial pathogens. This study provide new antibacterial, semiconductor glass has high refractive index and
good thermal stability (≃ 100 °C) can be used in biomedical applications and attract growing attention in this
field.

1. Introduction
Glasses based on tellurium dioxide are one of most important
considerable attention among the oxide glasses like silicates and
phosphates because of their various unique and gorgeous physical and
chemical properties like high refractive index(1.8–2.3), dielectric con-
stant (13–35), high thermal expansion coefficient(120–170 ×10−7°C−1),
low glass transition temperature Tg (< 300 °C), high thermal stability,
low melting temperature (< 1000 °C), small phonon energy (640–
790 cm−1)and higher optical transmission in the infrared (IR) region
(0.4–6 µm)which is valuable to design near-IR and mid-IR lasers and
amplifiers [1–13]. Tellurite based glasses have been widely studied in
their physical, elastic, optical, electrical and thermal properties [14,15].
These intelligent properties would be useful in a broad range of
applications in medical, civil, photonic and military areas like erasable
optical recording media, optical waveguides, optical switching devices,
fiber laser, optical amplifier, windows of the laser radar, Raman
amplification, gas sensors, 3D-display devices, and thermal imaging
[16–25]. A plethora of reports highlighted the effect of adding transition
metals such as V2O5 that help improves the semi-conducting properties
of the glass. Additionally, the change in the thermal and the optical
properties has been studied [26–31]. The vanadium element has several
oxidation states. Trivalence (V+3), tetra valence (V+4) called (vanadyl),
and pent valence (V+5) called (vanadate), the V+4 and V+5 being the most
common. Vanadia (Vanadium pentoxide, V2O5) is a strong oxidant. It
has been reported that Vanadia have many applications in a variety of
fields including industrial exploitation like (batteries and solar cells),
biological like (biosensor to detect biological macromolecules) and
pharmacological [32,33]. Antibacterial activity of metals has been
reported since antiquity. Non-essential metals ions such as silver ion ,
copper ion, vanadium ions and zinc ion demonstrated high potential
toxicity towards the majority of bacteria [34]. A great attention has been
paid to broad spectrum antibacterial agents with high antibacterial
potential against both Gram -ve and Gram +ve bacteria. Antibacterial
and antimicrobial potential of vanadium, V2O3, VO2, and V2O5 have
been studied and found that antibacterial activity increased with higher
vanadium valence (V2O5) [35]. A plethora of reports studied antibacter-
ial and cytotoxicity activity of vanadia V2O5 and results show excellent
antibacterial potential where a marked decrease in the colonies of
bacteria with increasing V2O5 concentration. This antibacterial activity
was due to reactive oxygen species (ROS) generated within the cells and
thus cause oxidative stress and damage [35–38].

⁎
Corresponding author.
E-mail address: Elkhoshkhany@alexu.edu.eg (N. Elkhoshkhany).

http://dx.doi.org/10.1016/j.ceramint.2017.08.120
Received 6 August 2017; Received in revised form 17 August 2017; Accepted 18 August 2017
Available online 19 August 2017
0272-8842/ © 2017 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
N. Elkhoshkhany et al.
In 2017, a priority list of twelve bacteria that considered priorities
in immediate need for new antibiotics has been issued by World Health
Organization (WHO). Staphylococcus aureus, E.faecium, P.aeruginosa
Salmonella spp, and E.coli are among bacteria in the WHO priority list
that poses the highest risk to human health. In this context, the
literature of review has discussed the significantly improved antibac-
terial activity against E. coli and S.aureus upon adding V2O5 to TiO2–
Nanoparticles, polyaniline, Ag modified nano tubes, and titanium nano
composite thin film [39–41].
The objective of the present research is preparing promising
vanadate–tellurite glass with good optical, thermal, and antibacterial
properties which can be used in biomedical applications.
2. Experimental
2.1. Glass preparation
All glass samples prepared from chemically highly pure grade
chemicals in the powder form. TeO2 (99.999% purity, Aldrich),
Calcium oxide (CaO) as Calcium carbonate (CaCO3) (99.99% purity,
Loba), Sodium oxide (Na2O) as sodium carbonate (Na2CO3) (99.99%
purity, Sigma), and Vanadium pent oxide (V2O5) (99% purity, Loba)
were introduced. The appropriate amount of the starting materials of
each batch equivalent to 10.0 g glass was accurately weighed according
to the formula (90-X) TeO2− 5 CaO −5 Na2O- X V2O5) where x = 5, 10,
15 and 20 mol% then ground in a mortar to ensure the homogeneity.
Then transferred to platinum crucibles and were melted under
controlled conditions in a muffle furnace at (800–850 °C) for 25 min
to obtain a homogeneously mixed melt. During melting, the melt was
manually stirred by swirling to get free of gas bubbles and obtaining
homogeneity. The melt was rapidly quenched by pouring it into a
preheated stainless-steel mold. Then, samples annealed at 250◦C for
2 h, after that slowly cooled down to room temperature to relieve the
mechanical strains.
2.2. XRD measurements
Samples were identified by X-ray diffraction technique (XRD) to
ensure the glassy state which is commonly used in verifying the
amorphous state of glassy materials. X-ray diffractometer with Cu
radiation for finely grounded glass samples was used. The voltage and
current settings of the instrument are 40 kV and 30 mA respectively.
Scans were performed with a step size of 0.02 deg. and a step time of
0.3 s over an angular range 2 deg. from 4 to 100.
2.3. Physical measurements
Density (ρ) of the samples was determined by the standard
principle of Archimedes using Toluene (99.9%) at room temperature,
as the buoyant liquid. using Eq. (1) [42]
Wa
ρ=( )ρ (g·cm−3)
Wa − Wx x (1)
Where Wa is the weight of glass in the air, Wx is the weight of the glass
in Toluene, ρx is the density of Toluene. The density of Toluene at room
temperature is 0.864 g cm−3. Density obtained by three repeated
measurements showed an estimated error was ± 0.002 g cm−3.
The Molar volume was calculated using the Eq. (2) [42]
ΣMT
Vm = (cm3.mol−1)
ρ (2)
Where MT is the total molecular weight of the multi-component glass
system given as (Eq. (3):
MT = x iZ i (3)
Where xi and Zi are the mole fraction and the molecular weight of the
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Ceramics International 43 (2017) 15635–15644
oxides respectively.
Another important physical parameter Oxygen packing density
(OPD) of the samples calculated using Eq. (4) [43]
1000C*ρ
OPD = (mol. L−1)
MT (4)
C is the number of oxygen atoms per each composition.
The oxygen molar volume of glass vo calculated using Eq. (5) [43]
Σx izi 1
Vo = * (cm3.mol−1)
ρ Σx in i (5)
Where ni is the number of oxygen atoms in each correspondent oxide.
The average bond stretching force constant F is given by Eq. (6)
[44]
∑ (xn f f)i
F= (N/m)
∑ (xn f )i (6)
Where, n f and f are the coordination number of cation and the
stretching force constant of oxide respectively. Now for more quanti-
tative analysis, we calculated nb , the number of bonds per unit volume
of the glass given by Eq. (7) [45]
NA −3
nb = ∑ (n f ) i * (m )
vm (7)
Where, NA is Avogadro's number.
2.4. UV/VIS absorption measurements
All Polished glass samples measured at room temperature by
(Thermo-scientific, evolution 300UV–VIS Spectrophotometer) in the
range of wavelength from 200 to 800 nm.
2.5. Differential thermal analysis measurements
Differential Scanning Calorimetry DSC (TA Instruments, SDT
Q600) discuss the thermal properties of the glass samples.
Differential scanning Calorimetry (DSC) was carried out on the samples
in the temperature from room temperature at four different heating
rates 10, 15, 20, and 25 °C/min up to about 700 °C in a nitrogen
atmosphere at a flow rate of 15 Psi to find glass transformation
temperature Tg , onset crystallization temperature Tx , crystallization
peak temperature TC, and melting temperature Tm. The samples finely
grounded and placed in an open platinum pan for measurements.
2.6. Antibacterial activity
2.6.1. Bacterial strains
Five different bacterial strains were used to test the antibacterial
activity of Tellurite Glass. The following bacteria species of American
Type Culture Collection (ATCC) were used in this study Salmonella
enetricaserovar Typhimurium (ATCC14028), Escherichia coli
(ATCC10536), Enterococcus faecalis (ATCC29212), Pseudomonas
aeruginosa (ATCC27853), and Listeria monocytogenes (ATCC7644).
2.6.2. Growth medium
Nutrient broth (NB, Oxoid) was used for activation and growing of
all tested bacterial strains. Nutrient agar (NA) is NB containing1.5%
(w/v) agar. NA is used during the course of testing antibacterial activity
of glass samples.
2.6.3. Bacterial growth conditions
For activation and preparation of seed cultures purposes, all
bacterial strains were grown in 20 ml NB in 100 ml Erlenmeyer flask
at 37 °C for 18 h with an agitation speed of 150 rpm (Brunswick
Incubator Shaker, USA). While, for testing the antibacterial properties
of V2O5-Tellurite Glass System, NA medium, poured in sterilized
N. Elkhoshkhany et al. Ceramics International 43 (2017) 15635–15644

plastic Petri-dishes, was used. Then, all inoculated plates were in-
cubated at 37 °C for 18 h.

2.6.4. Agar disk diffusion assay

The agar disk diffusion assay (halo zone test) was used in this study
to evaluate the antibacterial properties of V2O5-Tellurite Glass System.
Four different synthesized TVCN, glass samples incorporated different
concentrations of V2O5, (TVCN 5, TVCN 10, TVCN 15, and TVCN 20)
were tested. A seed bacterial culture from each tested bacterial strain
was prepared. A single colony of 18 h actively growing a culture of each
bacterial strain was picked to inoculate 20 ml NB in 100 ml Erlenmeyer
flask. The inoculated broth medium (NB) was incubated at 37 °C for
18 h with an agitation speed of 150 rpm. Next day, 2.5 ml of each
growing culture for each bacterial strain were withdrawn aseptically to
inoculate 200 ml NA in 500 ml Erlenmeyer flask, separately. The
inoculated NA was poured in sterilized 25 ml Petri-dishes. After agar
solidification, a sample of V2O5-Tellurite Glass System included in
TVCN has overlaid as epically on the surface of the agar plates. Then all
agar plates were incubated in JSGI −100T incubator at the upright
position at 37 °C for 24 h. Next day, all plates were checked for halo Fig. 1. X-Ray diffraction patterns of the prepared samples.
zone appearance around each tested concentration of TVCN. Each
concentration included TVCN was tested 3 times and the average of the increasing V2O5 mol% and creating of non-bridging oxides (NBOs)
three readings taken. [48,52].

2.7. Statistical analysis

3.3. UV/VIS absorption spectra
Statistical analysis of the obtained data was carried out using the
The ultraviolet light absorbance of the vanadate–tellurite glass
overlapping rule of Standard error (SE) bar [46].
samples as a function of wavelength is shown in Fig. 3. The absorption
edge of glass samples can be identified. The fundamental absorption
2.8. pH measurements
edge shifts to higher wavelength with increasing the highly
polarizableV2O5 content in the glass samples. The cut-off wavelength
The change in pH of the deionized water during the dissolution of
λc increases from 256 nm to 277 nm due to the decrease of the bridging
vanadium tellurite glass samples was measured by pH meter (Jenway
oxygen which flavors non-bridging oxides (NBOs) formation [53]. The
3510, UK) calibrated using pH buffer solution 4.00 ± 0.01 and 10.00 ±
optical absorption coefficient α(ν) for each photon energy is calculated
0.02 (Scharlau) every 30 min and up to 270 min [47].
by Beer–Lambert law as shown in Eq. (8) [14]
3. Results and discussion 2 : 303 × abs(λ)
α(ν) =
d (8)
3.1. X-ray diffraction for glass samples
Where d is the glass thickness and Abs (λ) is the film absorbance. The
absorption coefficient α(ν) also depends on photon energy (hν) from the
The X-Ray diffraction patterns of the synthesized glass samples
Davis and Mott Eq. (9) [54]
(TVCN5, TVCN10, TVCN15, and TVCN20) show only broad peaks at
low angles and no sharp peak. This type of peaks is the characteristic of B×(h ν − Eopt)n
α(ν) =
amorphous nature of the glass samples in the studied composition hν (9)
range as demonstrated in Fig. 1.
Where, B, n are constant and Eopt the optical energy band gap. Where,
n is equal to 1/2 for directly allowed transitions, 2 for indirect allowed
3.2. Physical measurements
transitions [55]. Band gap values can be obtained from Eq. (9) by the
plot of (αhυ) 2 cm2ev2 and (αhυ) 1/2 cm−1/2ev1/2 against hυ as a
The density of a glass is the main property that has the capacity to
function of V2O5 mol% as shown in Figs. 4 and 5. The optical energy
evaluate the compactness. The values of density, molar volume, and
band gap values determined by extrapolating the linear parts of curves
OPD were displayed in Table 1. Density, molar volume and OPD of the
to (αhυ) 2 = 0 and (αhυ)1/2 = 0 for direct and indirect allowed
glasses varied from 5.15 to 4.72 g cm−3, 30.11–33.54 cm3 mol−1 and
transitions, respectively. The range of the energy gap decreases from
74.7–80.51 mol L−1, respectively with increasing V2O5 from 5 to
3.23 to 2.70 eV and from 3.51 to 2.98 eV with an accuracy of ± 0.01 eV
20 mol% as shown in Fig. 2. The decrease in density is due to the
for direct and indirect transition respectively as the concentration of
decrease in the atomic weight and the increase in the atomic radii
V2O5 mol% increase. The change in optical band gap is caused by the
where (Mw (V) = 50.94 g mol−1 and Mw (Te) = 127.60 g mol−1,r (V) =
change in the local configuration of glass structure where the top of the
1.6 Å and r (Te) = 1.34 Å). The increase in the molar volume is
valence band gets raised because of the formation of more non-
attributed to the rearrangement of the lattice due to the substitution of
bridging oxygen's (NBO's) [26,48, 49,56]. Direct band gaps are less
TeO2 by V2O5 which leads to increase the oxygen content and
than indirect band gaps for all glass samples. The relation between the
formation excess of free volume. OPD increases due to increases in
molar refractive index (n) and the band gap energy is given by Eq. (10)
the number of oxygen atoms per unit composition, which make glass
[57]
network more opened (excess of non-bridging oxides (NBOs)). These
behaviors of density, molar volume, and OPD agreed with previous ⎛ n2−1 ⎞ E
studies [48–51]. The average bond stretching force constant F increase ⎜ 2 ⎟ = 1− OPT
⎝ n +2 ⎠ 20 (10)
while the number of bonds per unit volume of the glass (nb ) and the
oxygen molar volume values (Vo) demonstrated a decrease with It is found that the molar refractive index (n) increase from 1.99 to

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Table 1
Physical data for glass samples measured at room temperature.

Sample code Composition ρ g cm−3 ( ± 0.002) Vm cm3/mol ( ± 0.002) OPD mol. L−1 Vo cm3/mol F N/m nb × 10 28 m−3

TVCN5 85TeO2–5CaO –5Na2O –5V2O5 5.15 30.11 74.71 13.38 219.4 8.30
TVCN10 80TeO2–5CaO –5Na2O –10V2O5 4.95 31.55 76.08 13.14 222.8 8.02
TVCN15 75TeO2–5CaO –5Na2O –15V2O5 4.76 33.05 77.16 12.96 226.2 7.74
TVCN20 70TeO2–5CaO –5Na2O –20V2O5 4.72 33.54 80.51 12.42 229.5 7.72

Fig. 2. Variations of density and molar volume against V2O5 (mol. %) for all glass Fig. 5. Plot of (αhυ) 2
against photon energy (hυ) for all glass samples.
samples.

Fig. 6. Plot of ln(α) as a function of photon energy (hυ) for all glass samples.
Fig. 3. Optical absorption spectra for all glass samples.

[BO]. In addition, the polarity of bridging oxygen (BO) is less than that
of non-bridging oxygen (NBO) [58,59].
The molar refractive (Rm) is given by Lorentz–Lorenz equation as
shown in Eq. (11) [60]
⎛ n2−1 ⎞
R m = Vm × ⎜ 2 ⎟cm3
⎝ n +2 ⎠ (11)
⎛ n2 − 1 ⎞
where the quantity ⎜ 2 ⎟ is called the reflection loss [60].
⎝ n +2 ⎠
It is found that the molar refractive (Rm) increases from 18.01 to
22.21 and 17.50–20.59 for direct and indirect transitions respectively.
Urbach energy ΔE, the width of localized states, is used to characterize
the degree of disorder in amorphous and crystalline materials. The
fundamental absorption edge follows an exponential law introducing
the Urbach energy as shown in Eq. (12) [61].
1/2
Fig. 4. Plot of (αhυ) against photon energy (hυ) for all glass samples.
hυ
α(ν) = αᵒ e( ΔE ) (12)

2.11 and 1.94–2.04 for direct and indirect transitions respectively. This Where αᵒ is a constant, ΔE is the Urbach energy indicates the width of
increase in the refractive index is due to high polarizable V+5 that can the band tails of the localized states and ν is the frequency. For many
form non-bridging oxygen [NBO] by breaking the bridging oxygen amorphous systems, Urbach assumes that the absorption coefficient is

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Table 2
Cut-off wavelength λc, direct optical energy gap (E)D, refractive index (n)D, Molar refraction (Rm)D, indirect optical energy gap (E)In, refractive index (n)In, Molar refraction (Rm)In, and
Urbach energy (ΔE) of glass system.

Sample λc (nm) E (eV)D ( ± 0.01) (n)D (Rm)D E (eV)In ( ± 0.01) (n)In (Rm) In ΔE (eV) ( ± 0.01)

TVCN5 256 3.23 1.99 18.01 3.51 1.94 17.50 0.189

TVCN10 271 3.00 2.04 19.33 3.22 2.00 18.89 0.191
TVCN15 274 2.91 2.06 20.44 3.30 1.98 19.62 0.205
TVCN20 277 2.70 2.11 21.21 2.98 2.04 20.59 0.221

an exponential function of photon energy. The exponential behavior
corresponding to Eq. (12) was also demonstrated for the present glass
and was displayed in Fig. 6. The values of the (ΔE) are calculated from
the slopes of the linear regions of those curves as shown in Fig. 6 and
the values were presented in Table 2. The values of ΔE found to lay in
between 0.189 and 0.221 eV for vanadate–tellurite glass samples. ΔE
values lie in the amorphous semiconductors range 0.046–0.66 eV [62].
It is clear from these values that the widths of the band tails of the
localized states depend upon the concentration of the modifier. Present
findings are consistent with XRD results, where no continuous sharp
peaks were observed which reflected the amorphous nature. Further, it
indicated long-range atomic arrangement absence and the periodicity
in the glassy systems. It's found that with increasing V2O5 content the
Urbach energy increased. Thus, the presence of vanadium ions
introduced more randomness in the glass structure. TVCN20 had the
highest Urbach energy and lowest band gap, which indicated that the
formation of more NBOs created more disorder and randomness,
thereby also decreasing the band gap in between the conduction and
the valence band [48,63].
3.4. DSC measurements
The Differential Scanning Calorimetry (DSC) curves for all glass
samples were shown in Figs. 7 and 8. All glasses exhibited endothermic
effects due to a glass transition temperature (Tg ). At higher tempera-
tures, exothermic peaks (TC1, TC2 ) due to the crystal growth, the first
exothermic peak may be attributed to nucleation processes followed by
the formation of a crystalline phase having a low internal free energy.
The second peak at a higher temperature is attributed to form of more
relaxed crystalline phase followed by an endothermic effect due to the

Fig. 7. Plot DSC curves of different rates 10, 15, 20 and 25 °C/min of (TVCN5) glass sample.

Fig. 8. Plot DSC curves of rate 25 °C/min for all glass samples.

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S = Tx − Tg (13)

Tc − Tg
Kg = .
Tm − Tc (14)

0.151−χ
F= Whereχ = ∆Tg /Tg and , ∆Tg = Tgend − Tgonset
0.151+χ (15)

It is found that the value of Tg decreases from 299.5 °C to 279.4 °C

which attributed to the decrease degree of polymerization and decrease
in number of bonds per unit volume (nb ).The thermal stability (S)
increased from 95.7 °C to 111.9 °C and Kg increased from0.53 to 0.85
with the increase of V2O5 mol% [29,30,49]. Thermodynamic fragility is
found to decrease from 0.60 to 0.23. This decrease in fragility due to
the glass network getting loose packed which lead to increasing the
degree of the disorder and it was confirmed by the increasing in the
molar volume(Vm) and increase forming of non-bridging oxygen's [67].
The relation between Tg and the heating rate Ø is given by the Eq. (16)
Fig. 9. Plot of (Tg ) as a function of (ln(Ø)) for all glass samples.
[68]
Tg = A + B ln(Ø) (16)

Where A and B are constants and at a temperature T as shown in Fig. 9.

Activation energy of transition (Et ) is calculated by Ozawa's formula
[69] as given in the following Eq. (17)
−Eto
ln(Ø) = +Const.
RTg (17)

Where, Activation energy (Eto ) is given by slope of the plot ln(Ø)against

1
( T ) as shown in Fig. 10 and Kissinger's formula [70] as given in the
g
following Eq. (18)
Ø −Etk
ln( )= +Const.
Tg 2 RTg (18)
Ø
Where, Activation energy (Etk ) is given by slope of the plot ln( )against
Tg2
1
(T ) as shown in Fig. 11. The activation energy of crystallization (Ec) for
g
Fig. 10. Plot of (ln(Ø)) as a function of (1000/Tg ) for all glass samples. the second peak of crystallization can be calculated using Ozawa's (EcO)
[71]and Kissinger's (EcK) [70] formulas as given in the following Eqs.
(19 and 20) respectively.
−ECo
ln(Ø) = +Const
RTC (19)

Ø −ECk
ln( )= +Const.
Tc 2 RTC (20)

Where, Activation energy (ECo ) is given by the slope of the plot

1
ln(Ø)against (T ) as shown in Fig. 12 and Activation energy (Eck ) is
C
Ø 1
given by the slope of the plot ln( )against ( T ) as shown in Fig. 13. The
Tc 2 c

Fig. 11. Plot of ln(Ø/Tg 2 ) as a function of (1000/Tg ) for all glass samples.

re-melting of the glass which is denoted by Tm are also observed [29].

The glass stability against crystallization (S), and glass-forming ten-
dency (Kg) are the useful parameters. The thermal stability (S) of the
glass samples was determined as showing in Eq. (13) [64]. Glass-
forming tendency (Kg) is calculated as showing in Eq.(14) [65], the
thermodynamic fragilities F can be calculated by using Eq. (15) [66]. Fig. 12. Plot of ln(Ø) as a function of (1000/Tc ) for all glass samples.

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µ is the volume fraction crystallized in time t and calculated by µ

= AT where A is the total area of the exothermic crystallization peak
A
and AT is the partial area between temperature just starts crystal-
lization Ti and selected temperature. By plotting ln(−ln(1 − μ))
versus ln (Ø ) as shown in Fig. 14, the value of the slope equal
to n, and found to be ≥ 1 that meant the crystal growth mechanism
was one dimensional crystal growth from the surface to the inside
so, the crystallization peaks were broadened with increasing
V 2O 5 content [72]. All thermal and kinetics parameters listed in
Table 3.

3.5. Antibacterial properties

Fig. 13. Plot of ln(Ø/Tc 2 ) as a function of (1000/Tc ) for all glass samples.
Fig. 14. Relation between ln (- ln (1-µ)) and Ln (Ø) of glass samples.
values of (Et ) and (Ec) decrease with increasing V2O5 mol% due to the
decrease in density and number of bonds per unit volume (nb )) and
increase of molar volume and formation of non-bridging oxygen's with
increasing V2O5 mol% [29,49]. The order of crystallization n (Avrami
number) for the prepared glass systems will be calculated using Eq.
(21) [71].
d[ln(−ln(1−μ))]
=n
d[ln(Ø)]
An antibacterial activity of a substance is an indication of its
ability to kill bacteria or inhibit their growth. In this context, four
different concentrations of TVCN combinations were tested against
the following bacterial strains: S.entericaserovar Typhimurium,
E.coli, P.aeruginosa, L. monocytogenes and E. Faecalis by using
the halo zone test (agar disk diffusion assay) [73]. The antibacterial
effect is indicated by the clear zone (zone of no bacterial growth)
around each glass disk. The average of three reading of halo zone of
growth inhibition was demonstrated in Table 4. Data revealed that
there was an inhibitory effect of TVCN on the growth of all tested
bacterial strains after 24 h at 37 °C Fig. 15. In general, the inhibition
zone increased significantly (P < 0.01) by increasing the concentration
of V2O5 mol% as demonstrated from Fig. 16 for all tested bacterial
strains as shown in Table 4. The highest inhibition zone was observed
at 20% mol of V2O5 for all tested bacterial strains as illustrated from
Fig. 15. TVCN5 exhibited antibacterial effect on all tested bacterial
strains in the following order: L.monocytogenes > E.coli >
P.aeruginosa > E.faecalis > S.enetrica serovar Typhimurium Fig. 16.
Conversely, the other concentrations of TVNC10 to TVNC20 showed
antibacterial effect in the following order: L.monocytogenes >
P.aeruginosa > E.coli > E.faecalis > S.enterica serovar Typhimurium
Fig. 16. Generally, all TVCN samples exhibited their highest anti-
bacterial effect on L.monocytogenes in comparison with the other
tested bacterial strains. So far, V2O5 is not reported yet as an
antibacterial agent in combination with any type of glass.
Antibacterial potential of tellurite glass and non-tellurite glass
incorporated with metals against S. enterica serovar Typhimurium
(21) had not been reported yet. The present manuscript handles a novel

Table 3
Glass transition temperature (Tg ), crystallization temperature (TC1, TC2 ), and onset of crystallization temperature (Tx1, Tx2 ), thermal stability (S), Glass-forming tendency (Kg), Activation
energy of glass transition (Et ), activation energy of crystallization (Ec), and order of crystallization of the TVCN glass samples.

Sample Tg ± 1 °c Tx1 °c ± 1 °c Tc1 °c ± 1 °c Tx2 °c ± 1 °c F Tc2 °c ± 1 °c Tm °c ± 1 °c S °c kg Eto KJ Etk KJ ECo KJ ECk KJ n

mol−1 mol−1 mol−1 mol−1

TVCN5 299.5 337.4 343.2 395.2 0.60 419.3 645.2 95.7 0.53 439.25 438.11 283.46 282.07 1.28
TVCN10 291.2 – – 384.8 0.50 410.9 613.6 93.6 0.59 387.70 386.57 249.00 247.63 1.37
TVCN15 284.1 326.3 348.6 381.5 0.48 410 568.6 97.4 0.79 363.44 362.33 201.66 200.29 1.01
TVCN20 279.4 363.3 373.8 391.3 0.23 417 578.4 111.9 0.85 297.38 296.28 148.00 146.62 1.14

Table 4
Diameter of inhibition zone (cm) of all glass samples against different bacterial strains.

Sample Inhibition zone (cm) of bacterial strain

E.coli E.faecalis S. entericaserovar Typhimurium P.aeruginosa L.monocytogenes

TVCN5 3.35 3.07 2.12 3.17 4.20

TVCN10 3.63 3.43 2.42 3.93 4.90
TVCN15 3.83 3.63 2.63 4.32 5.26
TVCN20 4.10 3.85 2.82 4.87 5.87

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N. Elkhoshkhany et al. Ceramics International 43 (2017) 15635–15644

Fig. 15. Agar disk diffusion plate assay for different bacterial inhibition at 37 ͦ C for 24 h Where, a) inhibition zone of E. faecalis growth in TVCN5 andTVCN15 b) inhibition zone of L.
monocytogenes growth TVCN5 andTVCN10c) inhibition zone of P.aeruginosa in TVCN10 andTVCN15 d) inhibition zone of S. enteric serovar Typhimurium growth in TVCN5
andTVCN15 e) inhibition zone of E.coli growth in TVCN10 andTVCN20.

subject that would make the evaluation of present findings is
important. To the best of knowledge, present data concerning the
antibacterial activity of all TVCN is considered the first finding
verifying its antibacterial potential against broad spectrum Gram-ve
bacteria (e.g., S.enetrica serovar Typhimurium, E.coli, and
P.aeruginosa) and Gram +ve bacteria (e.g., E.faecalis and
L.monocytogenes). The marked decreases in colonies of bacteria with
increasing V2O5 mol% concentration is attributed to produce reactive
oxygen species (ROS) and antioxidant depletion due to redox-activity
of vanadium ion where vanadate (v5+) reduced to vanadyl (v4+) then
again to oxidized vanadate (v5+) which would lead to oxidative stress,
damage to bacterial DNA and inhibit the particular enzyme activities
which are vital for cell growth [34–36].
3.6. pH measurements
pH one of the important factor controlling antibacterial potential
[74]. The pH changes measured of glasses samples in deionized water
at 37 °C for different time are listed in the Table 5 and Fig. 17 a fast
drop in pH was seen after 3 h of dissolution and then the pH decreased
slowly with increasing time. It was found that the magnitude of the pH
drop increases with the increase in glass dissolution rate and vanadium
mol%. It is well known that growth of bacteria depends on acidity or
alkalinity of the medium. The pH affects the rate of enzyme action and
plays a role in determining the ability of bacteria to grow or survive in
particular environments [75]. The optimum range for bacteria grows in
the pH range between 6.7 and 7.5.

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N. Elkhoshkhany et al. Ceramics International 43 (2017) 15635–15644

Fig. 16. Diameter of inhibition zone (cm) of all tested bacterial strains upon using different concentrations of V2O5 incorporated in all glass samples. Results are averages of three
readings with ± SE bars.

Table 5 (D) The thermal stability (S), and glass factor tendency (Kg) were
pH values ( ± 0.02) of glass samples in different times. found to increase and the thermodynamic fragilities F decrease
with the increasing of V2O5 mol% while, generally activation
Sample PH ( ± 0.02) at different dissolution time (min)
energies decreased due to the formation of non-bridging oxygen
30 60 90 120 150 180 210 240 270 NBO's.
(E) The antibacterial potential of V2O5 added in all TVCN increased
TVCN5 4.84 4.93 5.00 4.89 4.78 4.69 4.78 4.72 4.71 significantly (P < 0.01) by increasing the concentrations of V2O5
TVCN10 5.06 5.12 5.13 5.08 5.01 4.87 4.86 4.86 4.84
TVCN15 5.36 5.66 5.55 5.34 5.14 4.86 4.85 4.90 4.88
from 5 to 20 mol% for all tested bacterial pathogens. All TVCN
TVCN20 5.58 5.80 5.65 5.49 5.25 5.03 4.98 4.96 4.94 showed the highest antibacterial effect on L.monocytogenes in
comparison with the other tested bacterial strains.
(F) It was found that the magnitude of the pH drop increases with the
increase in glass dissolution rate and vanadium content.

References

Fig. 17. variation of pH with time for all glass samples.
4. Conclusion
In the present study, physical, optical, thermal, and antibacterial
properties of (90-X) TeO2− 5 CaO −5 Na2O- X V2O5) where x = 5, 10,
15 and 20 mol% samples were investigated to unravel the impact of
V2O5 on the samples' properties. The following conclusions could be
outlined:
(A) All samples showed only broad peaks at low angles without sharp
peaks indicating the form of glass structure.
(B) The observed decrease in the density and the increase in the molar
volume are ascribed to the replacement of Te heavy atom by the
light atom V.
(C) Optical measurements proved that optical energy band gap
decreased and Urbach energy increased with V2O5 mol% in-
creases, so the vanadium ions act as a network modifier, and
introduces opening structure due to the formation of more NBO's
and making more bonding defects.
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