Results in Physics 7 (2017) 119–125

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Results in Physics
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Optical study of gamma irradiated sodium metaphosphate glasses

containing divalent metal oxide MO (ZnO or CdO)
E. Nabhan a, W.M. Abd-Allah b,⇑, F.M. Ezz-El-Din b
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

a r t i c l e i n f o a b s t r a c t

Article history: Sodium metaphosphate glasses containing divalent metal oxide, ZnO or CdO with composition 50 P2O5 –
Received 25 October 2016 (50
x) Na2O – x MO (ZnO, or CdO) where x = 0, 10, 20 (mol%) were prepared by conventional melt
Received in revised form 1 December 2016 method. UV/visible spectroscopy and FTIR spectroscopy are measured before and after exposing to suc-
Accepted 1 December 2016
cessive gamma irradiation doses (5–80 kGy). The optical absorption spectra results of the samples before
Available online 5 December 2016
irradiation reveal a strong UV absorption band at (230 nm) which is related to unavoided iron impuri-
ties. The effects of gamma irradiation on the optical spectral properties of the various glasses have been
Keywords:
compared. From the optical absorption spectral data, the optical band gap is evaluated. The main struc-
Sodium metaphosphate glass
UV–visible spectra
tural groups and the influence of both divalent metal oxide and gamma irradiation effect on the structural
IR spectra vibrational groups are realized through IR spectroscopy. The FTIR spectra of c-irradiated samples are
Deconvolution characterized by the stability of the number and position for the main characteristic band of phosphate
Optical band gap groups. To better understood the structural changes during c-irradiation, a deconvolution of FTIR spectra
Gamma ray 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.
Ó 2016 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Introduction thermal expansion coefficient and high refractive indices, low melt-
ing temperature, low glass transition temperature, low thermo-
The short range structure of glassy P2O5 consists of a network of optical coefficient and large emission. Thus, they are suitable for
Q3 tetrahedral units where three of the oxygens are bridging (P-O- many applications such as glass to metal seals [2–4], biomedical
P) and one non-bridging (P@O),with the addition of alkali oxide engineering. However, their relatively poor chemical durability
(Na2O) to P2O5, the conversion of is P-O-P bridging to P-O-M+, makes them unsuitable for practical applications. The addition of
non-bridging oxygens takes place, which indicate the formation of one or more of divalent oxides like ZnO or CdO leads to improvement
Q2 tetrahedral with two non-bridging oxygen atoms. Thus the addi- in the chemical durability, mechanical properties, and thermal
tion of alkali oxide to vitreous P2O5 results in the creation of non- expansion by increasing the strength of bonds and the compaction
bridging oxygens at the expense of bridging oxygens. As alkali oxide of the phosphate glass system, these cations can enter the glass net-
is added to P2O5, the phosphate structural groups pass from Q3 to Q2 work either network former or network modifier [5]. It is important
to Q1 to Q0 as the molar ratio of alkali oxide to P2O5, R = M2O/P2O5, to study the interaction of gamma ray with a glass system as it may
passes from 0 to 1 to 2 and finally to 3. These modifications are sim- be lead to various changes in the structural, optical and electrical
ilar to those taking place in a silicate network upon the addition of properties of the glasses [6]. The radiation interaction with the host
alkali earth oxides, such as Na2O to P2O5, results in the conversion glass may cause the displacement of lattice atoms or electronic
of the three dimensional network, to linear phosphate chains. This defects which involve changes in the valence state of the lattice or
linear chain structure due to the cleavage of P–O–P linkages and impurity atoms. Also, it may involve ionization and charge trapping
the creation of NBOs in the glass [1]. Recently, Phosphate glasses and/or radiolysis or photochemical reactions as high energy radia-
are technologically important because they generally have a high tions 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
⇑ Corresponding author at: National Center for Radiation Research and
Technology, Nasr-City, Cairo, Egypt.
kinds of defect centers generated as a result of creation and capture
E-mail address: [email protected] (W.M. Abd-Allah). of electron and hole pair during the irradiation process [7,8].

http://dx.doi.org/10.1016/j.rinp.2016.12.001
2211-3797/Ó 2016 The Authors. Published by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
120 E. Nabhan et al. / Results in Physics 7 (2017) 119–125

Table 1 samples were placed in a manner that each glass sample was sub-
Chemical composition of investigated glass (mol%). jected to the same irradiation dose.
Glass sample Composition
P2O5 Na2O ZnO CdO Results and discussion
G1 50 50 – –
G2 50 40 10 – Absorption spectra before irradiation
G3 50 40 10
G4 50 30 20
Fig. 1 Illustrate the UV–visible absorption spectrum of samples
(G1–G3) before irradiation. The spectra were recorded from (200-
The main objective of this work is to evaluate the effects of ZnO 800 nm), reveal a strong UV absorption band centered at
or CdO on optical study and also study the effect of gamma irradi- (230 nm), and no visible absorption is observed. The observed UV
ation on the measured spectral properties and justify the induced absorption band (230 nm) can be assumed to originate from the
defects generated, so as to explore its use for nuclear industry. presence of trace unavoidable iron impurity species (Fe3+ and
Fe2+) in the raw materials used to prepare the studied glasses
Experimental [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
Preparation of the glasses charge transfer bands with different absorption coefficients, being
more than one order of magnitude higher for Fe3+ than for Fe2+ [6].
Sodium metaphosphate glasses prepared from P2O5 was Also, The broadness of the extending band (200 ? 300 nm) in the
introduced in the form of pure ammonium hydrogen phosphate present study is attributed to the possible presence of more than
(NH4H2PO4), sodium oxide was introduced in the form of its one site of both iron species Fe2+ and Fe3+ ion [12]. Thus we can
respective anhydrous sodium carbonate Na2CO3 (Analar quality) assert the intense charge-transfer absorption near 230 nm in glass
and MO was added in the form of its respective pure oxide. The is related to Fe3+ ions. This result is supported by recent investiga-
composition (50
x) Na2O – 50 P2O5 – x MO (ZnO, or CdO), where tions done by several publications [13,14]. They have concluded
x = 0, 10, 20 mol%. The composition of the studied glasses as shown that these glasses exhibit characteristic charge transfer ultraviolet
in Table 1. The batches were melted in silica crucibles from 900 to absorption bands because of the presence of transition metal ions
1100 °C ± 20 °C (depending on composition) for two hours in the (e.g. Fe3+, Cr6+, etc.) even if present in the ppm level. With careful
electrically heated furnace and each melt was stirred by rotating examination of UV/visible spectra, there is an obvious difference
the crucible several times every 30 min. The homogeneous melts between G2 and G3 is observed in UV–visible spectra of the
were cast into preheated stainless steel molds. Then the prepared glasses. Thus, the observed increase in the intensity of G2 than
samples were immediately transferred to an annealing furnace G3 at (250 nm) may be assumed to the function of G2 which
regulated at 220 °C. The muffle after one hour was left to cool to increase the absorption trace iron impurities than the G3 which
room temperature at rate of 25 °C/h. causes retardation of the absorption of iron ions leading to the
observed decrease in the intensity retarded the effect of iron impu-
rities so, its intensity decrease.
UV–visible absorption measurements

The optical absorption of highly polished samples measured Effect of gamma irradiation on absorption spectra of base sodium
against air at room temperature 25 °C. Optical absorption mea- metaphosphate glass
surements before and after successive gamma irradiation were car-
ried out with a recording double-beam spectrophotometer (type Fig. 2a Shows the UV–visible spectrum of base sodium
Unicam spectrometer made in England), covering the range from metaphosphate glass (G1) after gamma irradiation. The spectrum
190 to 1000 nm. before irradiation reveals a prominent band at 230 nm in UV region
and, no absorption bands is observed in visible region. On

Infrared absorption spectra measurements

The FTIR absorption spectra were registered at room tempera-

tures 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 Fig. 1. Optical absorption spectra of the sodium metaphosphate glass containing
gamma-rays cell (2000 Ci) with a dose rate 4.26 kGy/h. The divalent metal oxide.
 E. Nabhan et al. / Results in Physics 7 (2017) 119–125 121

Fig. 2. Optical absorption spectra of sodium metaphosphate glasses and sodium metaphosphate containing divalent metal oxide after gamma irradiation.

4.5 Effect of gamma irradiation on absorption spectra of divalent metal

oxide doped sodium metaphosphate glasses
4.0
G1
Fig. 2(b, c) Illustrate the optical absorption spectra of G2, G3
G2
G3 glasses respectively after gamma irradiation. The optical spectra
3.5
reveal the following spectral features:
The UV–visible spectra of (G2, G3) on subjecting these glasses to
hν (eV)

3.0 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
2.5
the effect of gamma irradiation on the host phosphate glass itself
and the formation of phosphorus oxygen hole center (POHC) and
2.0 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
1.5
to increase in the number of phosphorus non-bridging oxygen hole
0 20 40 60 80 center (NBOHC) as suggested by various authors [16,17] .On the
other hand the minor change in G3 may be due to many reasons:
Dose(kGy)
The UV induced defects of G3 doped glass reveal very low inten-
Fig. 3. The relation between energy gap and doses of gamma irradiation for G1, G2, sity bands indicating the possible retardation effect of Cd2+ions. It
G3. 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
subjecting this glass G1 to three successful doses 30, 50 and obvious resolution of induced visible band which seem to be due to
80 kGy, visible band is induced at (500 nm) and increase in the combined effect of induced defect obtained from both Cd ions and
intensity with increase the irradiation dose. Möncke and Ehrt phosphate network. The very weak bands due to Cd2+ are mainly
[11] have reached to the identification of this band (500 nm) by located in the UV region and interfere with ultraviolet iron impu-
the deconvolution method induced bands in phosphate glasses. rities bands [18], this effect may be explained by assuming that
There are three bands that observed in the visible region, which Cd2+ ions compete with iron impurities for capturing electrons
are assigned to a phosphate-bonded oxygen hole centers (POHCs), and this seems to cause the obvious retardation [19].
and other three bands are related to oxygen hole centers (OHCs),
and further three bands within the UV region, which are related Optical energy gap
to electron centers (PECs). Experimental optical results indicate
that the induced bands in the G1 after irradiation extend in both The study of optical absorption is a useful method for the
the UV and visible regions. It seems that the induced bands in investigation of optically induced transition and for the
the UV region are correlated mainly with defects generated provision of information about the picture of the band structure
through photochemical reactions with trace iron impurities while and energy gap of non-crystalline materials, the optical transition
the induced visible bands 500 nm are due to the effect of gamma is preferred to be indirect transition due to lack of translation sym-
irradiation on the host phosphate glass itself and causing the for- metry where the wave vector (momentum) is not defined. Energy
mation of positive hole centers of POHCs and OHCs as mentioned gab can be calculated by the following (1) equation is given by
by F.H. ElBatal et al. [15]. Davis and Mott [20].
122 E. Nabhan et al. / Results in Physics 7 (2017) 119–125

G3
1/2
(α hν) [Cm eV]
-1
1/2

before
30kGy
50kKy
80kGy

3 4 5 6 7

hν(eV)
Fig. 6. Example of the deconvolution of IR spectra of G2 before irradiation.
Fig. 4. Indirect optical band gap determination for G3.

1=2
ðahmÞ ¼ Bðhm
Eg Þ ð1Þ region of the curve to the hm axis where (ahm)1/2 = 0 and the values
were calculated for all samples before and after irradiation. Fig. 3 as
Where hm is the incident photon energy, B is the band tailing shown the relation between the optical energy gap and doses of
parameter constant, Eg is the optical band gap energy, and a is gamma irradiation for G1,G2 and G3. It can be observed from
the absorption coefficient determined by the formula results, that most values of Eg decrease under the influence of
(a = 2.303  Absorbance/glass thickness) in units of cm
1. The opti- replacement of Na2O with M (ZnO or CdO) for the glass samples
cal band gap value can be determined from extrapolating the linear in indirect transition, Although the replacement of Na2O with the

Fig. 5. Infrared absorption spectra of sodium metaphosphate undoped and doped after gamma irradiation.
 E. Nabhan et al. / Results in Physics 7 (2017) 119–125 123

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. 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. in the energy level positions and broadening of the band. In addi-
tion, the measured spectrum usually consists of one or more broad
bands due to different color centers, and the bands often overlap.
divalent metal oxides CdO or ZnO decrease the non-bridging oxygen However, the observed slight increase in Eg of G3 glass after irradi-
NBOs, which form defects levels higher than the valance band and ation, may be referred to the larger radius of Cd2+(0.91 Å) than Zn2+
so Eg increase. In other hand as NBOs decrease lead to the crosslink (0.70 Å),which This mean the probability of saturation of some
density increase and causes compaction. This compaction will cause induced defects which are formed during irradiation is higher in
the energy levels to be closely spaced and so the energy gap will glass containing Zn2+ions than in the glass containing Cd2+ ions
decrease. However, there is significant decrease in the band gap [21].
after 30, 50 and 80 kGy in all samples comparison to unirradiated
glass composition for G1, G2 and G3 respectively. As shown previ- Infrared absorption spectra
ously in Fig 3 and also in Fig. 4 represented G3 for example. This
can be understood and take into consideration that radiation causes Effect of gamma irradiation on the IR spectra
the following effects: The FT-IR spectra of the sodium meta phosphate glasses
(i) Increase in degree of disorder of the amorphous phase after undoped and doped with the divalent metal oxides have been
irradiation. studied in a previous work without studied the effect of gamma
(ii) The defect centers formed by charge trapping of the radi- irradiation [22]. Fig. 5 Shows the IR spectra of G1,G2,G3 and G4
olytic, the valence and conduction bands. before and after gamma irradiation with different doses (30, 50,
(iii) Induce transitions between the valence band and the defect and 80 kGy). The FT-IR results can be realized and interpreted from
levels or from the defect levels to exited states or the con- Fig. 5 based on the concept of the free independent vibration of
duction band. various structural groups the following assignments are introduce
for sodium metaphosphate glasses.
In principle, the optical band of defect center could be extre-
mely narrow and well defined, but site-to-site variation arising a) The two bands at about 1280 and 1180 cm
1 are related to
from the random nature of the glass invariably causes a distortion O-P-O groups asymmetric and symmetric respectively [22].
124 E. Nabhan et al. / Results in Physics 7 (2017) 119–125

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 irra-
diation [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 irradia-
tion 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 num-
bers 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 replace-
ment of Na2O with 20 mol% ZnO before and after irradiated with dif-
ferent 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 resis-
tant to the irradiation and the sample containing CdO is more resis-
Fig. 9. The dose effect of gamma irradiation on the structural group O- P-O- sy and tant than that containing ZnO.
O-P-O asy for the studied glass samples.
A typical deconvolution in Gaussian bands of IR spectrum of the
sodium metaphosphate glasses before and after gamma irradiation
b) The two bands at about 1100 and 1000 cm
1 are related to To ascertain that the addition of ZnO or CdO to sodium
P-O- groups, non bridging oxygen portion of PO4 in Q1 metaphosphate glasses the glass become more resistant to the irra-
tetrahedra, P-O
asy and P-O
sym respectively in PO4 diation a quantitative analysis was carried out by a deconvolution
tetrahedra in the chain structure [1,23]. of the infrared absorption spectra using the (peak fit) program as
c) The band at 880 cm
1 is attributed to different metaphos- shown in Fig. 6. A typical deconvolution in Gaussian bands of IR
phate groups [2]. spectrum of the phosphate glasses to determine the relative area
d) The characteristic absorption bands of cyclic phosphates in of the phosphate groups (P-O-P) sy, (P-O-P) asy, P-O-sy, P-O-asy,
the region 720–780 cm
1 centered at about 750 cm
1 PO2sy and PO2asy. It is stated that the relative area of each band
symmetric stretching vibrations of P-O-P rings [24]. is considered proportional to the concentration of phosphate struc-
e) The bands in the range 500–400 cm
1 assigned to the bend- tural groups which produces particular band [Moustafa et al. 1998]
ing vibration of O–P–O units, d(PO2) modes of (PO2)n chain [1]. From Figs. 7–9,it is stated that the changes in the concentration
groups, and the band at about 500 cm
1 is related as a of different structural groups with radiation is small to be consid-
fundamental frequency of (PO4)3
[25]. ered 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
In Fig. 5 after sample G1 is exposed to first dose 30 kGy, its the addition of ZnO or CdO to the studied glass affected on the glass
spectra and its peak seem to remain in the same position except to be more resistant to irradiation but the deconvolution data
the intensity of the absorption peak slightly decreases in all explain that the samples containing CdO is more resistant than
frequency range (400–1600) cm
1 . However, at 50 and 80 kGy, the that containing ZnO.
 E. Nabhan et al. / Results in Physics 7 (2017) 119–125 125

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