Faculty Publications
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Item Optical and mechanical properties of calcium phosphate glasses(Maik Nauka Publishing / Springer SBM compmg@maik.ru, 2014) Venkateswara Rao, G.V.; Shashikala, H.D.Binary calcium phosphate glasses in the system, xCaO-(100 - x) P 2O5 with x = 30, 35, 40, 45, and 50 mol % were prepared by conventional melt quenching technique. The density, molar volume and refractive index of the glasses were found to increase with the increase in CaO content. Structural investigation by FTIR spectroscopy revealed that the substitution of P2O5 by CaO depolymerizes the phosphate glass network by systematic conversion of Q3 structural units to Q2 structural units by breaking the P-O-P links. From the optical absorption studies, the optical band gap values were found to decrease with increasing CaO content which can be due to increase in the concentration of non-bridging oxygens in the glass network. Vickers hardness increased with the calcium oxide content due to densification. The fracture toughness decreases with the increase in CaO content due to the increase in the bond density between the modifying cations and the non-bridging oxygens in the glass network. It was observed that brittleness increases with the addition of CaO content which can be mainly attributed to the decrease in the molar volume. © 2014 Pleiades Publishing, Ltd.Item Structural, optical and mechanical properties of ternary CaO-CaF2-P2O5 glasses(Tsinghua University, 2014) Venkateswara Rao, G.V.; Shashikala, H.D.The ternary phosphate glass series (50?x)CaO-xCaF2-50P2O5 (x = 0–20 mol%) were synthesized using melt quench technique. Structural, optical and mechanical properties were investigated with increase in CaF2 content. Using X-ray diffraction (XRD), synthesized glasses were confirmed to be amorphous in nature. Replacement of oxygen ions by fluorine ions increased the values of density. Decrease in refractive index due to the low polarizability of fluorine ions in the glass matrix was observed. In Fourier transform infrared (FTIR) spectra, the slight variation in ?as (PO2) band position and intensity could be attributed to replacement of fluorine ions for oxygen ions in phosphate glass structure. These data were well supported by Raman spectra. Optical band gap energy increased from 3.44 eV to 3.64 eV with increase in CaF2 content, and Urbach energy decreased suggesting that the fluorine ions reduced the tail energy states in the band gap compared to the oxygen ions. Mechanical parameters such as Vickers hardness, fracture toughness and brittleness were evaluated from the Vickers micro indentation measurements. Increase in Vickers hardness, decrease in fracture toughness and increase in brittleness were observed with increase in CaF2 content. © 2014, The Author(s).Item Optical, dielectric and mechanical properties of silver nanoparticle embedded calcium phosphate glass(Elsevier, 2014) Venkateswara Rao, G.V.; Shashikala, H.D.Silver nanoparticles have been embedded in 50 mol% CaO-50 mol% P 2O5 glass using melt quenching technique. The quenched glasses were heat treated at 550 °C for different durations between 10 and 50 h. The growth of silver nanoparticles in glass matrix appeared to be time dependent. FTIR spectra revealed that silver nanocluster formation had not affected the position of vibration bands of basic phosphate tetrahedral network. The Ag nanoparticle embedded glass matrix showed the red shift and broadening of the surface plasmon resonance (SPR) peak in the visible region with the increase in the duration of the heat treatment. Results showed the increase in size of the nanoparticles in glass matrix with heat treatment which was further confirmed using transmission electron microscopy and XRD. X-ray diffraction studies indicated the presence of Ag crystalline peaks along with amorphous structure on heat treatment at 550 °C for 50 h. The dielectric constant of these glasses increased as the duration of the heat treatment increased. Increase in both Vickers hardness and fracture toughness, and decrease in brittleness were observed which can be attributed to the increase in size of the nanoparticles in glass matrix. © 2014 Elsevier B.V.Item Statistical optimization of melt-quenching process parameters for multiple properties of ternary barium phosphate glasses(Elsevier Ltd, 2015) Narayanan, M.K.; Shashikala, H.D.; Manjaiah, M.In the present work simultaneous optimization of density, refractive index and hardness (multiple performance characteristics) of ternary barium phosphate glasses has been carried out using Taguchi based grey relational analysis. Effect of the parameters such as CaF2 content, melting temperature and melting time on the response parameters of (50 - X)BaO-XCaF2-50P2O5 (X = 0, 10, 20 mol%) glasses prepared according to the experimental layout of Taguchi's standard orthogonal array has been studied. Highest grey relational grade is the performance criteria used in this study to indicate the optimum level of process parameters needed for the best multiple performance characteristics. Analysis of variance (ANOVA) conducted on grey relational grade shows that under 95% confidence level, CaF2 content is the only parameter significantly affecting multiple performance characteristics. Experimental values of response parameters obtained by conducting the confirmatory experiment at optimum level of process parameters are closer to the optimal set of predicted values. © 2014 Elsevier B.V. All rights reserved.Item Effect of heat treatment on optical, dielectric and mechanical properties of silver nanoparticle embedded CaOCaF2P2O5 glass(Elsevier Ltd, 2015) Venkateswara Rao, G.; Shashikala, H.D.Silver nanoparticle have been embedded in CaOCaF2P2O5 glass using melt quenching technique. The quenched glasses were heat treated at 550 °C for 10, 20, 30, 40 and 50 h. The growth of silver nanoparticle in the glass matrix appeared to be time dependent. FTIR spectra show that silver nanoparticle formation has not affected the vibration bands of basic phosphate tetrahedral network. The increase in compactness of the glass structure is confirmed by increase in measured density of the glasses with increase in the duration of the heat treatment. Glass containing spherical silver nanoparticle shows the red shift and increase in the full width half maxima (FWHM) of the surface plasmon resonance (SPR) in the visible region with increase in the duration of the heat treatment. X-ray diffraction pattern indicated the presence of Ag crystalline peaks along with amorphous structure on heat treating at 550°C for 50 h. For the glass samples, the increase in dielectric constant and low dielectric loss around 0.005 were observed with increase in duration of the heat treatment. Both Vickers hardness and fracture toughness increased while the brittleness decreased which can be attributed to the increase in size of the nanoparticles in glass matrix. © 2014 Elsevier B.V. All rights reserved.Item Physical, mechanical and structural properties of BaO-CaF2-P2O5 glasses(Elsevier, 2015) Narayanan, M.K.; Shashikala, H.D.Mechanical properties and structure of melt-quenched ternary barium phosphate glasses belonging to the composition (50 - X)BaO-XCaF2-50P2O5 (X = 0 to 10 mol%) were studied using Vickers indentation and vibrational spectroscopy. Elastic moduli of prepared samples were calculated using the Makishima and Mackenzie (M-M) model. Density of glasses was measured using the Archimedes method, while molar volume and atomic packing density were calculated from measured density to study structural changes in the glass matrix. Vickers hardness and brittleness increased and fracture toughness decreased with increase in CaF2 content. This can be attributed to increase in the compactness of phosphate bonds and reduction in the molar volume of glasses with partial substitution of Ba2 + with Ca2 +. Infrared and Raman spectroscopies revealed that the glass network mainly consisted of metaphosphate units arranged in chain and ring structures together with small amounts of ultraphosphate and pyrophosphate units. © 2015 Elsevier B.V. All rights reserved.Item Investigation of mixed alkali effect on mechanical, structural and thermal properties of three-alkali borate glass system(Elsevier Ltd, 2016) Subhashini, u.; Shashikala, H.D.; Udayashankar, N.K.In the present communication, the results of investigation on mixed alkali effect (MAE) in mechanical, structural and thermal investigation of alkali zinc borate glasses with nominal composition 5Li2O-(25-x)K2O-xNa2O-60B2O3-10ZnO (x = 0, 5, 10, 15, 20 and 25 mol%) are reported. The samples were prepared using standard melt quenching technique. Fourier transform infrared (FTIR) spectroscopy, differential scanning calarometry (DSC) and Vickers indentation studies were performed to investigate the mixed alkali effect in the samples. From the DSC studies, it was observed that the thermal parameters viz., glass transition temperature (Tg), glass melting temperature (Tm), glass crystallization temperature (Tc), glass stability (S) and fragility (F) exhibit a non linear variation with respect to increase in compositional parameter (RNa). This behavior clearly indicated the presence of strong MAE in the samples. FTIR studies confirmed the presence of both [BO3] and [BO4] units, indicating the present glass networks to be made up of these two units placed in different structural groups. The non linear variation of peak positions of B-O-B bending and stretching of [BO3] and [BO4] units of each glass sample explain the role of modifier alkali elements and validates the existence of strong MAE. The microhardness and fracture toughness of the samples were measured using Vickers micro indentation technique and non linear variation of both the properties have been observed confirming the presence of MAE in these glass samples. © 2015 Elsevier B.V.Item Optical absorption, mechanical properties and FTIR studies of silver-doped barium phosphate glasses(Society of Glass Technology christine@glass.demon.co.uk, 2016) Narayanan, M.K.; Shashikala, H.D.Silver-doped barium phosphate glasses, of composition 50BaO-50P2O5-4Ag2O-4SnO, were prepared by conventional melt quenching and subsequent heat treatment. Prepared glasses were heat treated for a fixed duration of 10 h at different temperatures 400, 450 and 500°C to develop silver nanoparticles of different sizes. Formation and the size of the silver nanoparticles were evaluated using the surface plasmon resonance (SPR) band of the optical absorption spectrum, which revealed that both of them were temperature dependent. Spectral positions of the SPR peaks of the glass samples heat treated at 450 and 500°C were observed around 3.0 eV. Absence of significant size dependent shift in SPR peaks of these samples from 3.0 eV indicates the formation of spherical silver nanoparticles smaller than 20 nm inside the glass matrix, which falls in the quasi-static regime of Mie theory. The effect of heat treatment on the local network structure of the phosphate glass matrix assessed using FTIR spectra shows that formation and growth of silver nanoclusters do not affect the basic metaphosphate network structure. A slight improvement is observed in density as well as in the mechanical properties of the heat treated samples due to densification of the glass matrix by dispersed silver nanoparticles.Item Effect of BaO addition on the structural and mechanical properties of soda lime phosphate glasses(Elsevier Ltd, 2016) Edathazhe, A.; Shashikala, H.D.The phosphate glasses of composition (26-x)Na2O-xBaO-29CaO-45P2O5 (x = 0,5,10,15 mol%) are prepared by melt-quenching technique. The variations in structural and mechanical properties are studied on glasses prepared at 1000, 1100 and 1200? C. The density of glasses increases with barium content for glasses prepared at different temperatures. The molar volume is nearly constant with compositional parameter. The amorphous nature of samples is confirmed by XRD. The calculated values of mass percentage of elements in the batch composition and EDS data are in a reasonable agreement. The FTIR spectra show that the main structural units in these glasses are Q1 and Q2 phosphate units. The frequency of the P[sbnd]O[sbnd]P band remains constant with barium substitution. The microhardness is measured using Vickers indentation method by applying 0.98 N for 10 s. The hardness and fracture toughness are independent of composition. The nature of crack formations is examined by SEM. The brittleness and crack length are correlated with plastic flow in the material. © 2016 Elsevier B.V.Item Optical and structural properties of BCBS glass system with and without alumina(Elsevier B.V., 2018) Bhattacharya, S.; Shashikala, H.D.BaO–CaO–Al2O3–SiO2 (BCAS) glass and their derivatives have gained extreme importance for their high endurance to elevated temperatures and being suitable for various electrochemical applications. Two glass systems, one being 50mol% [SiO2–B2O3]-xBaO-(45-x)CaO–5Al2O3 called as BCBSA and another without Al2O3 termed as BCBS were synthesized using melt quenching technique in the present work. Addition of ZnO and MgO as flux helped in melting them at 1300 °C which is much lower than the usual melting temperature of these glasses [1–4]. Density of the quenched glasses was measured by Archimedes method and structural bond vibrations were confirmed through FTIR. UV Visible spectroscopy was used to determine band gap energy and confirm the insulating nature of the synthesized glasses. The samples were isothermally heated at 700 °C, 800 °C for 50 h and at 900 °C for 50 and 100 h duration in air to allow the devitrification process to take place. The heat treated samples were analyzed by X-ray diffraction to identify the developed phases. Five Al2O3 free samples synthesized at 1300 °C by regular melt quenching technique were found to be devoid of the monocelsian phase. This is a detrimental phase for high temperature sealant applications as it has a very low coefficient of thermal expansion (CTE). Al2O3 free BCBS glasses, properties of which are being reported for the first time and glasses with low BaO concentrations are found to meet the requirements for high temperature applications as sealants in Solid Oxide Fuel Cell (SOFC). © 2018 Elsevier B.V.