Optical

study of gamma irradiated sodium metaphosphate glasses containing divalent metal oxide MO (ZnO or CdO)

E. Nabhana

W.M. Abd-Allahb, ⁎
wesamomar2007@yahoo.com

F.M. Ezz-El-Dinb

a
Physics Department, Faculty of Science, Al-Azhar University (Girls), Egypt

b
Radiation Chem Department, National Center for Radiation Research and Technology, Atomic Energy Authority, Egypt

⁎
Corresponding author at: National Center for Radiation Research and Technology, Nasr-City, Cairo, Egypt.

Abstract
Sodium metaphosphate glasses containing divalent metal oxide, ZnO or CdO with composition 50 P2O5 – (50 − x) Na2O – x MO (ZnO, or CdO) where x = 0, 10, 20 (mol%) were prepared by conventional
melt method. UV/visible spectroscopy and FTIR spectroscopy are measured before and after exposing to successive gamma irradiation doses (5–80 kGy). The optical absorption spectra results of the samples
before irradiation reveal a strong UV absorption band at (∼230 nm) which is related to unavoided iron impurities. The effects of gamma irradiation on the optical spectral properties of the various glasses
have been compared. From the optical absorption spectral data, the optical band gap is evaluated. The main structural groups and the influence of both divalent metal oxide and gamma irradiation effect on
the structural vibrational groups are realized through IR spectroscopy. The FTIR spectra of γ-irradiated samples are characterized by the stability of the number and position for the main characteristic band
of phosphate groups. To better understood the structural changes during γ-irradiation, a deconvolution of FTIR spectra in the range 650–1450 cm−1 is made. The FTIR deconvolution results found evidence
that, the changes occurring after gamma irradiation have been related to irradiation induced structural defects and compositional changes.

Keywords: Sodium metaphosphate glass; UV–visible spectra; IR spectra; Deconvolution; Optical band gap; Gamma ray

Introduction
The short range structure of glassy P2O5 consists of a network of Q3 tetrahedral units where three of the oxygens are bridging (P-O-P) and one non-bridging (P

O),with the addition of alkali oxide(Na2O) to P2O5, the conversion of is P-O-P bridging to P-O-M+, non-bridging oxygens takes place, which indicate the formation of Q2 tetrahedral with two non-bridging oxygen
atoms. Thus the addition of alkali oxide to vitreous P2O5 results in the creation of non-bridging oxygens at the expense of bridging oxygens. As alkali oxide is added to P2O5, the phosphate structural groups pass from
Q3 to Q2 to Q1 to Q0 as the molar ratio of alkali oxide to P2O5, R = M2O/P2O5, passes from 0 to 1 to 2 and finally to 3. These modifications are similar to those taking place in a silicate network upon the addition of alkali
earth oxides, such as Na2O to P2O5, results in the conversion of the three dimensional network, to linear phosphate chains. This linear chain structure due to the cleavage of P–O–P linkages and the creation of NBOs in
the glass [1]. Recently, Phosphate glasses are technologically important because they generally have a high thermal expansion coefficient and high refractive indices, low melting temperature, low glass transition
temperature, low thermo-optical coefficient and large emission. Thus, they are suitable for many applications such as glass to metal seals [2–4], biomedical engineering. However, their relatively poor chemical
durability makes them unsuitable for practical applications. The addition of one or more of divalent oxides like ZnO or CdO leads to improvement in the chemical durability, mechanical properties, and thermal
expansion by increasing the strength of bonds and the compaction of the phosphate glass system, these cations can enter the glass network either network former or network modifier [5]. It is important to study the
interaction of gamma ray with a glass system as it may be lead to various changes in the structural, optical and electrical properties of the glasses [6]. The radiation interaction with the host glass may cause the
displacement of lattice atoms or electronic defects which involve changes in the valence state of the lattice or impurity atoms. Also, it may involve ionization and charge trapping and/or radiolysis or photochemical
reactions as high energy radiations change in the optical properties of the glasses in a way that the appearance of new absorption bands in visible and ultraviolet part of the spectrum takes place. This is may be due
to different kinds of defect centers generated as a result of creation and capture of electron and hole pair during the irradiation process [7,8].
 The main objective of this work is to evaluate the effects of ZnO or CdO on optical study and also study the effect of gamma irradiation on the measured spectral properties and justify the induced defects
generated, so as to explore its use for nuclear industry.

Experimental
Preparation of the glasses
Sodium metaphosphate glasses prepared from P2O5 was introduced in the form of pure ammonium hydrogen phosphate (NH4H2PO4), sodium oxide was introduced in the form of its respective anhydrous sodium carbonate

Na2CO3 (Analar quality) and MO was added in the form of its respective pure oxide. The composition (50 − x) Na2O – 50 P2O5 – x MO (ZnO, or CdO), where x = 0, 10, 20 mol%. The composition of the studied glasses as shown in Table

1. The batches were melted in silica crucibles from 900– to 1100 °C ± 20 °C (depending on composition) for two hours in the electrically heated furnace and each melt was stirred by rotating the crucible several times every 30 min.

The homogeneous melts were cast into preheated stainless steel molds. Then the prepared samples were immediately transferred to an annealing furnace regulated at 220 °C. The muffle after one hour was left to cool to room

temperature at rate of 25 °C/h.

Table 1 Chemical composition of investigated glass (mol%).

Glass sample Composition

P 2O 5 Na2O ZnO CdO

G1 50 50 – –

G2 50 40 10 –

G3 50 40 10

G4 50 30 20

UV–visible absorption measurements

The optical absorption of highly polished samples measured against air at room temperature 25 °C. Optical absorption measurements before and after successive gamma irradiation were carried out with a recording double-

beam spectrophotometer (type Unicam spectrometer made in England), covering the range from 190 to 1000 nm.

Infrared absorption spectra measurements

The FTIR absorption spectra were registered at room temperatures using a JASCO FTIR 6200 spectrometer. IR absorption spectra were measured immediately after preparing the disks of KBr and glass samples. The FTIR

spectra were recorded in the wavenumber range of 400–4000 cm−1. A quantitative analysis of the infrared spectrum has been carried out by a careful deconvolution of the absorption profiles utilizing the “peak fit” program. IR spectra

were corrected for the dark current noises and background using two- point bas line correction. Many trials have been carried out using different band shapes, but has fit obtained was been found to be Gaussian shape. The position of

each band, its width and intensity are parameters adjusted automatically by the program, on the basis of the minimization of the deviations between experimental and simulated spectrum.

Irradiation facility
Glasses were subjected for different doses using an Indian 60Co gamma-rays cell (2000 Ci) with a dose rate 4.26 kGy/h. The samples were placed in a manner that each glass sample was subjected to the same irradiation dose.

Results and discussion

Absorption spectra before irradiation
Fig. 1 Illustrate the UV–visible absorption spectrum of samples (G1–G3) before irradiation. The spectra were recorded from (200-800 nm), reveal a strong UV absorption band centered at (230 nm), and no visible absorption is

observed. The observed UV absorption band (230 nm) can be assumed to originate from the presence of trace unavoidable iron impurity species (Fe3+ and Fe2+) in the raw materials used to prepare the studied glasses [9–11] Iron can

exist in the 2+ and 3+ states in glasses, depending upon the conditions of preparation. The two iron states have strong charge transfer bands with different absorption coefficients, being more than one order of magnitude higher for
Fe3+ than for Fe2+ [6]. Also, The broadness of the extending band (200 → 300 nm) in the present study is attributed to the possible presence of more than one site of both iron species Fe2+ and Fe3+ ion [12]. Thus we can assert the

intense charge-transfer absorption near 230 nm in glass is related to Fe3+ ions. This result is supported by recent investigations done by several publications [13,14]. They have concluded that these glasses exhibit characteristic charge

transfer ultraviolet absorption bands because of the presence of transition metal ions (e.g. Fe3+, Cr6+, etc.) even if present in the ppm level. With careful examination of UV/visible spectra, there is an obvious difference between G2 and

G3 is observed in UV–visible spectra of the glasses. Thus, the observed increase in the intensity of G2 than G3 at (250 nm) may be assumed to the function of G2 which increase the absorption trace iron impurities than the G3 which

causes retardation of the absorption of iron ions leading to the observed decrease in the intensity retarded the effect of iron impurities so, its intensity decrease.

Fig. 1 Optical absorption spectra of the sodium metaphosphate glass containing divalent metal oxide.

Effect of gamma irradiation on absorption spectra of base sodium metaphosphate glass

Fig. 2a Shows the UV–visible spectrum of base sodium metaphosphate glass (G1) after gamma irradiation. The spectrum before irradiation reveals a prominent band at 230 nm in UV region and, no absorption bands is

observed in visible region. On subjecting this glass G1 to three successful doses 30, 50 and 80 kGy, visible band is induced at (500 nm) and increase in the intensity with increase the irradiation dose. Möncke and Ehrt [11] have

reached to the identification of this band (500 nm) by the deconvolution method induced bands in phosphate glasses. There are three bands that observed in the visible region, which are assigned to a phosphate-bonded oxygen hole

centers (POHCs), and other three bands are related to oxygen hole centers (OHCs), and further three bands within the UV region, which are related to electron centers (PECs). Experimental optical results indicate that the induced

bands in the G1 after irradiation extend in both the UV and visible regions. It seems that the induced bands in the UV region are correlated mainly with defects generated through photochemical reactions with trace iron impurities

while the induced visible bands 500 nm are due to the effect of gamma irradiation on the host phosphate glass itself and causing the formation of positive hole centers of POHCs and OHCs as mentioned by F.H. ElBatal et al. [15].

Fig. 2 Optical absorption spectra of sodium metaphosphate glasses and sodium metaphosphate containing divalent metal oxide after gamma irradiation.
Effect of gamma irradiation on absorption spectra of divalent metal oxide doped sodium metaphosphate glasses
Fig. 2(b, c) Illustrate the optical absorption spectra of G2, G3 glasses respectively after gamma irradiation. The optical spectra reveal the following spectral features:

The UV–visible spectra of (G2, G3) on subjecting these glasses to different doses of gamma irradiation, the broad visible band is identified at (500 nm). The induced broad visible band at (500 nm) which are observed at (G2,

G3) may be attributed to the effect of gamma irradiation on the host phosphate glass itself and the formation of phosphorus oxygen hole center (POHC) and OHCs as mentioned before. However, the increase in the intensity of the

broad visible band (400–500 nm) in G2 than G3, may be due to increase in the number of phosphorus non-bridging oxygen hole center (NBOHC) as suggested by various authors [16,17] .On the other hand the minor change in G3 may

be due to many reasons:

The UV induced defects of G3 doped glass reveal very low intensity bands indicating the possible retardation effect of Cd2+ions. It seems that some of the Cd2+ ions capture positive holes and Cd 3+ or (Cd2+) + ions The visible

induced defect shows an induced broad band at 500 nm and with progressive irradiation doses reveals the obvious resolution of induced visible band which seem to be due to combined effect of induced defect obtained from both Cd

ions and phosphate network. The very weak bands due to Cd2+ are mainly located in the UV region and interfere with ultraviolet iron impurities bands [18], this effect may be explained by assuming that Cd2+ ions compete with iron

impurities for capturing electrons and this seems to cause the obvious retardation [19].

Optical energy gap

The study of optical absorption is a useful method for the investigation of optically induced transition and for the provision of information about the picture of the band structure and energy gap of non-crystalline materials, the

optical transition is preferred to be indirect transition due to lack of translation symmetry where the wave vector (momentum) is not defined. Energy gab can be calculated by the following (1) equation is given by Davis and Mott [20].

(1)

Where hν is the incident photon energy, B is the band tailing parameter constant, Eg is the optical band gap energy, and α is the absorption coefficient determined by the formula (α = 2.303 × Absorbance/glass thickness) in

units of cm−1. The optical band gap value can be determined from extrapolating the linear region of the curve to the hν axis where (αhν)1/2 = 0 and the values were calculated for all samples before and after irradiation. Fig. 3 as shown

the relation between the optical energy gap and doses of gamma irradiation for G1,G2 and G3. It can be observed from results, that most values of Eg decrease under the influence of replacement of Na2O with M (ZnO or CdO) for the

glass samples in indirect transition, Although the replacement of Na2O with the divalent metal oxides CdO or ZnO decrease the non-bridging oxygen NBOs, which form defects levels higher than the valance band and so Eg increase. In

other hand as NBOs decrease lead to the crosslink density increase and causes compaction. This compaction will cause the energy levels to be closely spaced and so the energy gap will decrease. However, there is significant decrease

in the band gap after 30, 50 and 80 kGy in all samples comparison to unirradiated glass composition for G1, G2 and G3 respectively. As shown previously in Fig 3 and also in Fig. 4 represented G3 for example. This can be understood

and take into consideration that radiation causes the following effects:

Fig. 3 The relation between energy gap and doses of gamma irradiation for G1, G2, G3.
Fig. 4 Indirect optical band gap determination for G3.

(i) Increase in degree of disorder of the amorphous phase after irradiation.

(ii) The defect centers formed by charge trapping of the radiolytic, the valence and conduction bands.

(iii) Induce transitions between the valence band and the defect levels or from the defect levels to exited states or the conduction band.

In principle, the optical band of defect center could be extremely narrow and well defined, but site-to-site variation arising from the random nature of the glass invariably causes a distortion in the energy level positions and

broadening of the band. In addition, the measured spectrum usually consists of one or more broad bands due to different color centers, and the bands often overlap. However, the observed slight increase in Eg of G3 glass after

irradiation, may be referred to the larger radius of Cd2+(0.91 Å) than Zn2+ (0.70 Å),which This mean the probability of saturation of some induced defects which are formed during irradiation is higher in glass containing Zn2+ions than

in the glass containing Cd2+ ions [21].

Infrared absorption spectra

Effect of gamma irradiation on the IR spectra
The FT-IR spectra of the sodium meta phosphate glasses undoped and doped with the divalent metal oxides have been studied in a previous work without studied the effect of gamma irradiation [22]. Fig. 5 Shows the IR spectra

of G1,G2,G3 and G4 before and after gamma irradiation with different doses (30, 50, and 80 kGy). The FT-IR results can be realized and interpreted from Fig. 5 based on the concept of the free independent vibration of various

structural groups the following assignments are introduce for sodium metaphosphate glasses.

a) The two bands at about 1280 and 1180 cm−1 are related to O-P-O groups asymmetric and symmetric respectively [22].

b) The two bands at about 1100 and 1000 cm−1 are related to P-O- groups, non bridging oxygen portion of PO4 in Q1 tetrahedra, P-O− asy and P-O− sym respectively in PO4 tetrahedra in the chain structure [1,23].

c) The band at 880 cm−1 is attributed to different metaphosphate groups [2].

d) The characteristic absorption bands of cyclic phosphates in the region 720–780 cm−1 centered at about 750 cm−1 symmetric stretching vibrations of P-O-P rings [24].

e) The bands in the range 500–400 cm−1 assigned to the bending vibration of O–P–O units, δ(PO2) modes of (PO2)n chain groups, and the band at about 500 cm−1 is related as a fundamental frequency of (PO4)3− [25].
Fig. 5 Infrared absorption spectra of sodium metaphosphate undoped and doped after gamma irradiation.

In Fig. 5 after sample G1 is exposed to first dose 30 kGy, its spectra and its peak seem to remain in the same position except the intensity of the absorption peak slightly decreases in all frequency range (400–1600) cm−1.

However, at 50 and 80 kGy, the intensity of the absorption peak suddenly increase in all frequency range (400–1600) cm−1, especially at two bands 1280 cm−1 related to PO2 asy and 1100 cm−1 which is related to P-O- and non bridging

oxygen in PO4 tetrahedra in comparison to unirradiated sample. The increase in the intensity of this band strongly reflects the changes taking place in the glass structure after interaction with gamma irradiation [26]. From this, it can

be seen that the parent glass G1 is slightly affected by 30 kGy, while, it is strongly affected by dose of 50 and 80 kGy, which cause an increase in the non bridging oxygen. The IR spectra of the glass sample G2 with the replacement of

Na2O with 10 mol% ZnO before and after irradiated with different irradiation doses (30, 50 and80 kGy) from the figure it can be seen that the assignment of the bands before and after irradiation are similar except that the band at

1000 cm−1which is related to the phosphate non bridging oxygen portion of PO4 tetrahedra in Q1 tetrahedra and the, P-O- sy is very weak compared with that of the sodium-metaphosphate. It is clear that after irradiation with gamma

rays the sample is not affected by the gamma ray with the dose of 30and 50 kGy while there are changing in the relative intensity of the bands with 80 kGy. The IR spectra of the glass sample G3 before and after irradiation with

different radiation dose (30, 50 and 80 kGy) from the figure it can be seen that the relative height of band and their positions don’t change with the replacement of Na2O with 10 mol% CdO before and after irradiation. Experimental

data indicate that the IR spectra of all glasses after gamma irradiation reveal the same main vibrational bands with nearly no changes in their numbers or positions. This indicates general stability of such glasses towards gamma

irradiation due to the presence of heavy metal cations [27]. The IR spectra of the glass sample G4 with the replacement of Na2O with 20 mol% ZnO before and after irradiated with different irradiation doses (30, 50 and80 kGy) from

the figure it can be seen that the position and assignment of the bands are similar before irradiation, except that the band at 1000 cm−1which is related to, the phosphate non bridging oxygen portion of PO4 tetrahedra in Q1 tetrahedra

and also the P-O− sy is very weak compared with that of the parent glass. Moreover, there is a broadening in the bands as the Na2O is replaced by 20% ZnO. It has established that the gamma irradiation on the IR spectra of phosphate

glasses, produces minor changes in some of the intensities but the main structural bands remain unchanged in their number or position [15]. From the IR spectra it can be concluded that with the addition of ZnO or CdO to sodium

metaphosphate glasses the glass become more resistant to the irradiation and the sample containing CdO is more resistant than that containing ZnO.

A typical deconvolution in Gaussian bands of IR spectrum of the sodium metaphosphate glasses before and after gamma irradiation
To ascertain that the addai (addition)tion of ZnO or CdO to sodium metaphosphate glasses the glass become more resistant to the irradiation a quantitative analysis was carried out by a deconvolution of the infrared absorption

spectra using the (peak fit) program as shown in Fig. 6. A typical deconvolution in Gaussian bands of IR spectrum of the phosphate glasses to determine the relative area of the phosphate groups (P-O-P) sy, (P-O-P) asy, P-O-sy, P-O-asy,

PO2sy and PO2asy. It is stated that the relative area of each band is considered proportional to the concent (concentration)eration of phosphate structural groups which produces particular band [Moustafa et al. 1998] [1]. From Figs. 7–9,it

is stated that the changes in the concentration of different structural groups with radiation is small to be considered for the glass contain ZnO and too small to be considered for CdO in agreement with Moustafa et al. [1]. So it can
concluded that the addition of ZnO or CdO to the studied glass affected on the glass to be more resistant to irradiation but the deconvolution data explain that the samples containing CdO is more resistant than that containing ZnO.

Fig. 6 Example of the deconvolution of IR spectra of G2 before irradiation.

Fig. 7 The dose effect of gamma irradiation on the structural group P-O-P sy and P-O-P asy for the studied glass samples.
Fig. 8 The dose effect of gamma irradiation on the structural group P-O- sy and P-O- asy for the studied glass samples.
Fig. 9 The dose effect of gamma irradiation on the structural group O- P-O- sy and O-P-O asy for the studied glass samples.

Conclusion
Comparative combined optical and FTIR spectral measurements of some prepared sodium metaphosphate glasses with one of the divalent metal oxides (ZnO or CdO) before and after gamma irradiation have
been studied. Optical spectra of all the studied glasses reveal strong UV absorption due to the presence of unavoidable trace iron impurities contaminated within the raw materials used for the preparation of these
glasses. Glasses containing ZnO reveal induced defects upon irradiation in the visible region are due to the effect of gamma irradiation on the host phosphate glass itself and the formation of positive hole centers of
POHCs and OHCs. The indirect optical band gaps are found to decrease with increasing the divalent metal oxide ratio, which can be interpreted to increase in the crosslink density by decreasing the NBOs and
strength of the P-O-P bonds which cause compaction. The same results were observed when glasses were irradiated with 30, 50 80 kGy dose of gamma irradiation and the decreases in band gap values are attributed
to the presence of induced transition between the defect levels and conduction or valence bands. Infrared absorption spectra of the parent glass exhibit the presence of several structural phosphate groups. The FTIR
data show resemblance of IR spectra obtained from zinc, sodium metaphosphate and cadmium sodium metaphosphate glasses. The effect of gamma irradiation on the IR spectra is limited and referred to the stability
of network forming units. A final conclusion of this comparative study of ZnO up to 20 mol%) sodium meta- phosphate glass was resistance to gamma irradiation while, CdO at 10 mol% sodium meta phosphate glasses
more resistance for irradiation and this is ascertained from the deconvolution data obtained from deconvolutions of IR spectra of the studies glasses.

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Queries and Answers

Query: Please check the layout of Table 1, and correct if necessary.
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