Synthesis, Physical, Optical and Structural Studies of B2O3-CdO-Al2O3-PbF2 Glasses Modified with MoO3 Ions

doi:10.21203/rs.3.rs-1495935/v1

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Synthesis, Physical, Optical and Structural Studies of B₂O₃-CdO-Al₂O₃-PbF₂ Glasses Modified with MoO₃ Ions

https://doi.org/10.21203/rs.3.rs-1495935/v1

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This manuscript deals with the preparation and detailed physical and structural study of B₂O₃-CdO-Al₂O₃-PbF₂ glasses reinforced with MoO₃ ions. With the addition of MoO₃, the density and band gap values decreased while the refractive index increased, confirming the transformation of Mo⁶⁺ ions to Mo⁵⁺ ions and resulting in the generation of NBO's in these glasses. The FTIR spectra revealed the presence of different borate and aluminate units. The FTIR spectra also indicated the conversion of Mo⁶⁺ ions to Mo⁵⁺ ions. The effect of MoO₃ ions on Raman spectra was clearly visible and indicated the conversion of BO₄ to BO₃ units, increasing NBO’s which helped to explain the density variation.

The extreme importance of glasses has been increasing in day to day regular needs and in most of the areas, which in turn impelled researchers to magnify their view in various chemical compositions with borate, silicate, phosphate, etc for its large area of applications [1, 2]. Because of its low melting point, transparency, thermal stability, and solubility, borate is being considered mostly as a glass forming material [3, 4]. Physical, chemical, and optical characteristics all change significantly when Al₂O₃ is incorporated to the borate matrix. Depending on the proportion of Al₂O₃, it can be detected in the glass network as AlO₄ or AlO₆ units. An increase in Al₂O₃ concentration can greatly improve mechanical strength, chemical durability, and moisture resistance capacity. Alumino borate glasses can also mix with other metal oxides and transition metal ions (TMI) [5–7].

CdO is amongst the most prominent metal oxides being used glass compositions to increase density, and it is widely known that CdO is employed as control rods in nuclear reactors. Fluorides are added to borate glasses to give them a larger transmission window, solubility, and fluorescence lifespan, including other properties[7–9]. PbF₂when added with borate glasses improves specific optical characteristics and IR transparency, which are employed in communication and laser engineering systems[10].

On the other hand, it was discovered that molybdenum ions exhibit exceptional activity and selectivity in a range of oxidation activities in various oxide glasses, making them suitable candidates for studying catalytic characteristics. Molybdenum ions may exist in a variety of valence states (+ 3, + 4, + 5, and + 6), which may help the glasses to improve their optical, electrical, and electrochromic characteristics. Owing to electron hopping around molybdenum ions, the occurrence of molybdenum ions in multivalence states increases the electronic contribution to conduction[11–13].

Ali et al [14] studied the influence of MoO₃ on PbO–Sb₂O₃–As₂O₃–MoO₃ glasses and concluded that the former and modifier role of MoO3 in these glasses based on its mol%. Alrowaili et al [15] prepared the P₂O₅–B₂O₃–Li₂O–MoO₃ glasses and observed that the density, refractive index, metallization criteria and shielding ability were enhanced while the Urbach energy lowered with the MoO₃ concentration. Various other researchers, Shaaban et al[16], Rada et al[17], Manisha et al[18], etc prepared glasses with various compositions containing the MoO₃ and confirmed that the glasses when incorporated with MoO₃ found better applications related to optical and shielding features. As a result, the union of borate with MoO₃ can result in the formation of glasses. Furthermore, recent research has shown that even a minute amount of TMI injected to glasses causes major alterations in the glass network. Moreover, when borate doped cadmium alumina matrix with variable mole percentages of metal fluoride and transition metal ion unveils the finest properties apart from the best optical possessions, electronic, optoelectronic and electro chromic applications.

The glass samples were prepared with unique composition 60B₂O₃-20CdO-5Al₂O₃-(15-x)PbF₂-xMoO₃ (where x = 0, 0.5, 1, 1.5, and 2mol%). The method employed in preparation of glass samples was melt quenching. All the required chemicals were annular grade, which are weighed with required mole percentages for five sets of glass compositions. The dissimilar mole percentages of chemicals being measured using an electronic monopan balance and then physically mixed in an agate mortar until the chemicals were uniformly blended. This mixer of chemicals was taken in porcelain crucible and kept in an electronic furnace, which is under normal atmospheric conditions, maintained at 1000^⁰C temperature for 1 hour to melt congruently. Further melts are stirred to gain homogeneity. The obtained melt was quenched on steel plate, which is at 200^⁰C for couple of hours to release the internal stresses and finally the glass samples are ready for further characterization.

On a Philips Xpert Pro X-Ray diffractometer, X-Ray diffraction (XRD) spectra being measured in the range of 10^o – 80^o for 2θ to know the nature of the specimens. The Archimedes principle is then used to evaluate density where Xylene is being used as the dipping liquid. For density measurements, three experimental pieces from each glass were collected, and the aggregate density of the three sample pieces was used to get the final density. The accuracy of the computation is 0.005 g/cc. Fourier transform infrared (FTIR) spectra were recorded using a Bruker FTIR spectrometer with a resolution of 0.5cm^− 1 and a precision of 0.01 cm^− 1. On a J. Y. H. LABRAM-HR Raman spectrometer, Raman spectra of BCAPM glasses were scanned in the wavenumber range of 200 cm^− 1 to 1800 cm^− 1. On a Shimadzu UV-1800 Spectrometer in absorption mode, the UV-Visible spectra of BCAPM glasses were scanned across a wavelength range of 200nm to 1000nm. At room temperature, EPR spectra were scanned between 2500 and 4000G using a Bruker EPR spectrometer.

3.1. X-Ray Diffraction (XRD)

Figure 1 shows the XRD patterns of the BCAPM glasses. The figure clearly displays wide humps between 2θ ≈ 20⁰ to 30⁰. Furthermore, there are no sharp peaks, implying that BCAPM samples are amorphous.

3.2. Physical and optical properties

The density is indeed a significant physical characteristic which shares insights about solids; such evidence will be more beneficial if the structure is properly understood [19, 20]. The volume of structural units contained in the glass may be determined using the density data of the samples. The density values in the current BCAPM glass system were dropped nonlinearly from 4.072g/cc (BCAPM0) to 4.009g/cc (BCAPM4). The molar volume (V_m) was calculated using the measured density and molecular weight (M) data (Table 2). In Fig. 2, the fluctuation of ⍴ and V_m with MoO₃ is displayed.

Table 1

Sample code and the glass compositions
Sample Code	Composition in mole %
	B₂O₃	CdO	Al₂O₃	PbF₂	MoO₃
BCAPM0	60	20	5	15	0
BCAPM1	60	20	5	14.5	0.5
BCAPM2	60	20	5	14	1
BCAPM3	60	20	5	13.5	1.5
BCAPM4	60	20	5	13	2

Table 2

Physical and optical parameters of BCAPM glasses
Physical & Optical parameters	Sample Code
Physical & Optical parameters	BCAPM0	BCAPM1	BCAPM2	BCAPM3	BCAPM4
Average molecular weight	141.754	141.248	140.742	140.235	139.729
Density (ᵨ) gm/cc	4.072	4.057	4.041	4.025	4.009
Molar Volume (V_m) cc/mol	34.80	34.81	34.82	34.83	34.84
Optical band gap (E_opt) eV	3.063	3.049	3.013	3.002	2.951
Refractive index (n)	2.379	2.383	2.393	2.396	2.410
Dielectric constantnt (ε)	5.660	5.682	5.728	5.743	5.809
Molar refractivity (Rm) cm^− 3	21.17	21.21	21.30	21.34	21.45
Electronic polarizability (αm) 10^− 21 cm^− 3	8.38	8.40	8.44	8.45	8.50
Urbach energy (ΔE) eV	0.257	0.191	0.213	0.216	0.223

The density of the BCAPM glasses drops non - linearly as the mole percentage of MoO₃ grows, as seen by the respective crystal densities of MoO₃ (4.70gm/cc) and PbF₂ (8.44gm/cc). Fractional substitution of PbF₂ (245.2 g/mol) by MoO₃ (143.94 g/mol) might potentially explain the reduction in density. The fall in density values might potentially be due to the conversion of [BO₄] units to [BO₃] units where [BO₄] is denser than [BO₃], according to the literature[21, 22].

Absorption spectra of BCAPM glasses are presented in Fig. 3. The analysis of the valence and conduction band transitions using the primitive absorption edge in the UV-Visible zone is a fascinating method. The prime aspect of the absorption edge in non-crystalline solids is the absorption coefficient α(ν) with smaller values as a function of the photon energy hν [23].

$$\alpha \left(\vartheta \right)= Cexp\left(\frac{h\vartheta }{\varDelta E}\right)$$

where ΔE is Urbach energy and C is a constant. The α (ν) can be obtained from the absorbance A by using the equation below;

$$\alpha \left(\vartheta \right)=2.303\frac{A}{d}$$

where ‘d’ is the thickness. Davis et al [24] and Tauc et al [25] suggested relation:

(${\alpha }\text{h}\upsilon$) =${B}^{2}{(\text{h}\upsilon -{E}_{g})}^{2}$ (3)

Figure 4 shows the Tauc plot of BCAPM glasses. The optical band gap (E_g) values (see Table 2) are acquired by extrapolating the linear region of the curve. With the enhancement of MoO₃ from x = 0 to 2 mole% in the current BCAPM glasses, E_g declines from 3.063 eV (BCAPM0) to 2.951 eV (BCAPM4). With the insertion of MoO₃, the bandgap drops, indicating that localised states for electrons near the conduction band are established. The bandgap can indeed be reduced by associating these localised states with the conduction band. Conversion of Mo⁶⁺ ions to Mo⁵⁺ ions may have caused the reduction in band gap. Increases in Mo⁵⁺ ions, which occupy octahedral positions and function as modifiers in the glass network, can lead to an increase in non-bridging oxygens and a drop in bandgap[11, 26].

The inverse slope of the linear section of the Urbach plot, as illustrated in Fig. 5, is used to calculate Urbach energy. The magnitude of disorder present in the glass network can be accessed by the Urbach energy. These values were found to be much lower for the BCAPM glass system, indicating that the glass structure had less disorder [27].

The other parameters such as refractive index (n), molar electronic polarizability (α_m), and molar refraction (R_m) are evaluated using the following relations [28–30].

$$\frac{{n}^{2}-1}{{n}^{2}+2}=1-\sqrt{\frac{{E}_{g}}{20}}$$

$${\text{R}}_{\text{m}}=\frac{{\text{n}}^{2}-1}{{\text{n}}^{2}+2}\text{*}{\text{V}}_{\text{m}}$$

$${{\alpha }}_{\text{m}}=\left(\frac{3}{4\text{П}{\text{N}}_{\text{A}}}\right)\text{*}{\text{R}}_{\text{m}}$$

With an excess of MoO₃ in BCAPM glasses, the n values were elevated from 2.379 (BCAPM0) to 2.410 (BCAPM4). As both R_m and ${{\alpha }}_{\text{m}}$are related to molar volume, they show a raising trend with composition.

3.3. FTIR spectroscopy:

FTIR spectroscopy is the measurement for acquiring infrared absorption or transmission spectra in order to detect the presence of various functional groups in materials. The influence of MoO₃ on the structural characteristics of BCAPM glasses containing lead fluoride may be studied using FTIR spectra. The infrared absorption spectra of BCAPM glasses are shown in Fig. 6 in the wave number range of 400 to 1600 cm^− 1. The various IR bands observed from FTIR spectra are 423, 461, 517, 579, 673, 724, 901, 995, 1061, 1116, 1168, 1279, 1376, 1466, and 1549 cm^− 1. In general, the IR examination reveals two distinct frequency zones. The stretching vibrations BO₃ and BO₄ borate units are attributed to the ranges from 1200 to 1600 cm^− 1 and 800 to 1200 cm^− 1, respectively[31–33]. Significant differences in the infrared spectra during analysis revealed the emergence of three primary broad bands at around 670, 1050, and 1380 cm^− 1. The widths of the bands become wider as the MoO₃ concentration increased, although the spectra indicated no change in the centre of the bands. Relying on their valence states, molybdenum ions can join the glass network as network modifiers or network formers, with Mo⁵⁺ ions claiming the modifying sites and Mo⁶⁺ ions claiming the former sites. By converting the hexavalent molybdenum ions to the pentavalent ions, the addition of MoO₃ at the expense of PbF₂ in BCAPM glasses increases Mo⁵⁺ ions (which function as modifiers).

The bands between 423–517 cm^− 1 in BCAPM glass system are attributed to Pb²⁺and Cd²⁺ vibrations and vibrations of AlO₆ octahedral[5, 6, 34]. The peak near 579 cm^− 1 might be attributed to the Mo-O bond vibrations in distorted MoO₄[13, 35]. IR band positions observed 673 cm^− 1 in BCAPM glasses indicates the elongations of B–O–B bonds in BO₃ units groups[36]. The peak at around 724 cm^− 1 is assigned to the bending vibrations of B–O linkages. The structure's Mo–O–Mo bridging bonds are responsible for the band at 900 cm^− 1. [13]. B-O stretching vibrations of tetrahedral BO₄ units, cause the bands between 995 and 1060 cm^− 1[37, 38]. Stretching vibrations of tetragonal BO₃ units from different borate groups cause the bands between 1116 and 1279 cm^− 1. The stretching elongations of the B–O of trigonal (BO₃)³⁻ units are assigned to the band at approximately 1376 cm^− 1. Anti-symmetrical elongations B–O–B groups are responsible for the IR band at 1476–1549 cm^− 1 [39–41].

3.4 Raman spectroscopy:

Vibrational spectroscopy is amongst the best means for understanding the structure of glasses. Glasses comprise structural units that are equivalent to crystalline examples and may be positioned freely in a 3D network while being amorphous. Among the most powerful vibrational spectroscopy approaches for exploring glass structure is Raman spectroscopy. Raman spectra of BCAPM glasses is shown in Fig. 7 and deconvolution spectra for BCAPM1 sample is depicted in Fig. 8 to locate exact Raman band positions. The various Raman bands observed from Raman spectra are 344cm^− 1, 498cm^− 1, 674cm^− 1, 789cm^− 1, (983cm^− 1 shift 925 cm^− 1), 1079cm^− 1, 1229cm^− 1, (1347cm^− 1 shift 1337cm^− 1), 1437cm^− 1, and 1738cm^− 1. The Raman band rising sharply at 344cm^− 1 is ascribed to corner-shared MoO₆ octahedra[42, 43]. Another band existing at 498cm^− 1 is due to isolated diborate groups[44]. Anti-symmetric elongations of O-Mo-O linkages were observed in BCAPM glasses due to the presence of the Raman band at 674cm^− 1[45]. Another Raman band present at 789cm^− 1 is attributed to stretching vibrations of Mo-O-Mo linkages and the formation of AlO4 tetrahedra[5, 42]. An important band increasing sharply in BCAPM glasses is observed at ~ 950cm^− 1 and is ascribed to the vibrations of Mo-O and Mo = O bonds in single and paired MoO₆ units [46, 42]. The two Raman peaks, one at 344cm^− 1 and the other at 950cm^− 1, are clearly rising sharply with increasing MoO₃ in the current BCAPM glass system, as seen by Raman spectra. Furthermore, the Raman band at 950cm^− 1 is migrating from 983cm^− 1 to 925cm^− 1, and the intensity of this Raman band is growing with the concentrations of MoO₃. This might be due to the replacing of PbF₂ with MoO₃, which has a low molecular weight. The change of [BO₄] units to [BO₃] with MoO₃ concentration might be responsible for the shifting behavior towards lower frequencies and increased intensity in BCAPM glasses. This finding backs up the fact that increasing MoO₃ doping concentration reduces density variation in BCAPM glasses. The Raman band at 1079 cm^− 1 is due to the existence of diborate groups. When the PbF₂ is replaced with MoO₃ in BCAPM glasses, the intensity of the Raman bands at 789 cm^− 1 and 1229 cm^− 1 were observed to be diminished from BCAPM0 to BCAPM4 glass samples and finally merged with the neighborhood Raman bands. An intense Raman band in BCAPM glasses at 1340 cm^− 1 is assigned to pyroborate groups and elongated B-O bands coupled to the borate groups[49, 48]. The bands near 1437cm^− 1 in this glass system are ascribed to B–O⁻ vibrations of the BO₃ units and the band at 1738cm^− 1 is due to chain and ring type metaborate units[49–51].

The glasses with the formula 60B₂O₃-20CdO-5Al₂O₃-(15-x)PbF₂-xMoO₃ (where x = 0, 0.5, 1, 1.5, and 2mol%) is been prepared using conventional melt quenching method. These samples were analyzed using physical, optical, FTIR and Raman spectroscopic techniques to investigate the impact of MoO₃ on the structural changes occur in the samples. Drop in the density of the samples with MoO₃ is attributed to the molecular weights of PbF₂/MoO₃ and the transformation of BO₄ to BO₃ units. Decline in the optical band gap values was observed, which were evaluated from UV-Visible spectra. This decline is due to transformation of Mo⁶⁺ to Mo⁵⁺ ions as MoO₃ content is increased at the expense of PbF₂. FTIR and Raman spectra confirmed the presence of different borate and aluminate groups. These spectra also supports the transformation of Mo⁶⁺ to Mo⁵⁺ ions and confirmed that the MoO₃ act as modifier in these glasses.

The authors whose names are listed immediately below the title of the manuscript certify that they have NO affiliations with or involvement in any organization or entity with any financial interest (such as honoraria; educational grants; participation in speakers' bureaus; membership, employment, consultancies, stock ownership, or other equity interest; and expert testimony or patent-licensing arrangements), or non-financial interest (such as personal or professional relationships, affiliations, knowledge or beliefs) in the subject matter or materials discussed in this manuscript.

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10 May, 2022
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29 Mar, 2022
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Synthesis, Physical, Optical and Structural Studies of B₂O₃-CdO-Al₂O₃-PbF₂ Glasses Modified with MoO₃ Ions

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Abstract

Figures

1. Introduction:

2. Experimental:

3. Results And Discussions:

3.1. X-Ray Diffraction (XRD)

3.2. Physical and optical properties

3.3. FTIR spectroscopy:

3.4 Raman spectroscopy:

4. Conclusions:

Declarations:

References:

Status:

Version 1