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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 Thermal and optical properties of BaO-CaF2-P2O5 glasses(Elsevier B.V., 2015) Narayanan, M.K.; Shashikala, H.D.Thermal and optical properties of ternary phosphate glasses prepared by conventional melt-quenching technique, belonging to the series (50 - X)BaO-XCaF2-50P2O5 (X = 0 to 10 mol%) were investigated with increase in CaF2 content. Thermal stability and glass forming ability studied using differential thermal analysis (DTA) were found to increase with the increase in CaF2 content. Powder X-ray diffraction (XRD) analysis of heat treated samples also revealed that CaF2 addition improves the thermal stability against crystallization. Increase in both glass transition temperature and onset crystallization temperature with the increase in CaF2 content can be attributed to the partial substitution of Ba2 + ion with Ca2 + ion, which is having larger field strength. The observed decrease in the melting temperature of glass batch with the increase in CaF2 content indicates that CaF2 acts as a flux and reduces the viscosity of the glass melt. The decrease in refractive index of the glasses with the increase in CaF2 content can be attributed to replacement of lower field strength Ba2 + by Ca2 + or the partial substitution of more polarizable oxygen ion by fluorine. Optical band gap energy slightly increased and Urbach energy marginally reduced with the increase in CaF2 content. Increase in optical band gap energy was further confirmed by calculating theoretical optical basicity of glasses. Average anion polarizability (?O/F) of (50 - X)BaO-XCaF2-50P2O5 glasses calculated from refractivity data using Lorentz-Lorentz relation was correlated with its theoretical optical basicity (?th) using the previously established correlation for oxyfluoro phosphate glasses. © 2015 Elsevier B.V. All rights reserved.Item Effect of alkali earth oxides on hydroxy-carbonated apatite nano layer formation for sio2 –bao–cao–na2 o–p2o5 glass system(Springer Science and Business Media Deutschland GmbH, 2017) Kiran, P.; Ramakrishna, V.; Shashikala, H.D.; Udayashankar, N.K.Barium soda lime phosphosilicate [(58SiO2– (32-x)BaO–xCao–6Na2 O–4P2O5 (where x = 15, 20, 25 and 30 mol%)] samples were synthesised using conventional sol–gel method at 700 °C sintering temperature. Thermal, structural properties were studied using thermo gravimetric analysis and differential thermal analysis, X-ray diffraction, scanning electron microscopy, fourier transform infrared and Raman spectroscopy. Using Raman spectra non-bridging oxygen concentrations were estimated. The hydroxy-carbonated apatite (HCA) layer formation on samples was analysed for 7 days using simulated body fluid (SBF) soaked samples. The growth of HCA layers self-assembled on the sample surface was discussed as a function of NBO/BO ratio. Results indicated that the number of Ca2? ions released into SBF solution in dissolution process and weight loss of SB-treated samples vary with NBO/BO ratio. The changes in NBO/BO ratios were observed to be proportional to HCA forming ability of barium soda lime phosphosilicate glasses. © Springer. All rights reserved.Item Dissolution and in vitro bioactive properties of BaO added Na2O-CaO-P2O5 glasses(Society of Glass Technology christine@glass.demon.co.uk, 2018) Edathazhe, A.B.; Shashikala, H.D.Na2O-CaO-P2O5 glasses with different additions of BaO were subjected to dissolution tests in deionised water and in vitro bioactivity tests in phosphate buffer saline (PBS) as well as Hank's balanced salt (HBS) solution. Phosphate glasses of composition (26-x)Na2O-xBaO-29CaO-45P2O5 (x=0, 5, 10, 15 mol%) were prepared by melt-quenching. The dissolution characteristics of these glasses were studied in deionised water under static conditions based on BaO composition. The dissolution rate of the glasses in deionised water decreased with BaO content. The in vitro bioactivity tests were carried out in PBS and HBSS for 28 days under static conditions. The bioactivity of the samples was verified by XRD, SEM/EDS and FTIR techniques. Hydroxyapatite phases were formed on all the glass samples within seven days of immersion in HBSS and the bioactivity was found to improve with BaO content. The glasses without BaO and with 15 mol% BaO showed the hydroxyapatite phases within the immersion of 14 days in PBS whereas the glasses with 5 and 10 mol% BaO showed formation of amorphous hydroxyapatite phases. © 2018 Society of Glass Technology. All rights reserved.Item Corrosion resistance and in-vitro bioactivity of BaO containing Na2O-CaO-P2O5 phosphate glass-ceramic coating prepared on 316 L, duplex stainless steel 2205 and Ti6Al4V(Institute of Physics Publishing helen.craven@iop.org, 2018) Edathazhe, A.B.; Shashikala, H.D.The phosphate glass with composition 11Na2O-15BaO-29CaO-45P2O5 was coated on biomedical implant materials such as stainless steel 316 L, duplex stainless steel (DSS) 2205 and Ti6Al4V alloy by thermal enamelling method. The structural properties and composition of glass coated substrates were studied by x-ray diffraction (XRD), Scanning electron microscopy (SEM) and Energy dispersive x-ray spectroscopy (EDS) analysis. The coatings were partially crystalline in nature with porous structure and pore size varied from micro to nanometer range. The polarization curve was obtained for uncoated and coated substrates from electrochemical corrosion test which was conducted at 37 °C in Hank's balanced salt solution (HBSS). The corrosion resistance of 316 L substrate increased after coating, whereas it decreased in case of DSS 2205 and Ti6Al4V. The XRD and SEM/EDS studies indicated the bioactive hydroxyapatite (HAp) layer formation on all the coated surfaces after electrochemical corrosion test, which improved the corrosion resistance. The observed electrochemical corrosion behavior can be explained based on protective HAp layer formation, composition and diffusion of ions on glass coated surfaces. The in-vitro bioactivity test was carried out at 37 °C in HBS solution for 14 days under static conditions for uncoated and coated substrates. pH and ion release rate measurements from the coated samples were conducted to substantiate the electrochemical corrosion test. The lower ion release rates of Na+ and Ca2+ from coated 316 L supported its higher electrochemical corrosion resistance among coated samples. Among the uncoated substrates, DSS showed higher electrochemical corrosion resistance. Amorphous calcium-phosphate (ACP) layer formation on all the coated substrates after in-vitro bioactivity test was confirmed by XRD, SEM/EDS and ion release measurements. The present work is a comparative study of corrosion resistance and bioactivity of glass coated and uncoated biomedical implants such as 316 L, DSS and Ti6Al4V. © 2018 IOP Publishing Ltd.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.Item Effect of BaO on thermal and mechanical properties of alkaline earth borosilicate glasses with and without Al2O3(Elsevier B.V., 2019) 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 suitability for various electrochemical applications. Two glass systems, one being 50 mol%[SiO2-B2O3]-xBaO-(45-x)CaO-5Al2O3 with x = 0, 10, 20, 25, 30, 35 and 40 mol%, represented as BCBSA and another without Al2O3 termed as BCBS, synthesized using melt quenching technique are considered here. The authors focus on the thermal and mechanical properties of these glasses. Reducing BaO concentrations improve the coefficient of thermal expansion (CTE/?) and other characteristic temperatures of glasses. Compacted glass pellets made of the water quenched frits show maximum shrinkage at 700 °C. Dilatometric analysis were conducted on compacts showing maximum shrinkage. CTE of these pellets are more than the bulk glasses. Glasses with low BaO concentrations exhibit high hardness and Young's modulus. Glasses bearing 20 mol% BaO, or even lesser, meet the thermal and mechanical properties required for high temperature sealants. © 2019 Elsevier B.V.Item Optimization and analysis of process parameters of melt quenching technique for multiple performances of rare earth doped barium borate glass synthesis using Taguchi's design and grey relational approach(Elsevier B.V., 2023) Ingle, A.I.; Shashikala, H.D.; Narayanan, M.K.; Dubeto, M.T.; Gupta, S.Glass materials with strong physical, structural, and optical properties are in high demand in today's social and industrial sectors. Researchers have recently established the extensive uses of these widely utilized glassy materials in optoelectronic devices, aerospace, nuclear industries, etc. Optimization usually plays a significant role in the synthesis of material. Hence, this article uses the statistical optimization of multiple process parameters of the melt quenching technique for rare earth doped barium borate glass 60B2O3-(40-X)BaO-XMO (MO-Er2O3/CeO2 and X = 0.5,1.0,1.5 mol percentage)by Taguchi's Design of Experiment. The multiple performance characteristics were studied using Grey relational analysis. An experimental format for preparing the Barium Borate glass was utilized with a standard L9 orthogonal array designed by Taguchi. Grey relational analysis was used to analyze the effects of processing parameters, including melting temperature, the composition of rare-earth oxide, and melting time of glasses on density, refractive index, and indirect bandgap. Analysis of variance (ANOVA) showed the influence of process parameters on the multiple response parameters as directed by the S/N ratio of the response parameter. The prediction of optimal conditions for contributing process parameters to the multiple response parameters was estimated efficiently. Additionally, as compared to the initial conditions, the optimal confirmatory experiment exhibited a considerable improvement in the response parameters (refractive index, density, and indirect bandgap). Grey relational grade and analysis of variance (ANOVA) revealed that melting temperature to be sole factor significantly affecting multiple responses with a 95% confidence level. The objective of the work is to optimize the melt quenching process parameters and their influence on the physical and optical properties of glass for photonic applications. Using this optimization method, melt quenching was found to be the most influential parameter contributing about 73–74% in tuning the desired response parameters. The findings also revealed a very less deviation between the statistically predicted and experimental data of response parameter, with deviation ranging from 0.37 to 2.14%. This good agreement between experimental and predicted values of response parameters indicated the suitability of Taguchi method of optimization for melt quenching technique. © 2022 The AuthorsItem Influence of V2O5 addition as a dopant and dispersed content in barium borophosphate glass on structural and optical properties(Elsevier Ltd, 2024) Rashmi, I.; Ingle, A.; Raghuvanshi, V.; Shashikala, H.D.; Nagaraja, H.S.The Barium Borophosphate glass system with molar compositions 40P2O5– 25B2O3-(35-x) BaO-xV2O5 and 40P2O5–25B2O3–35BaO-xV2O5 (x = 0,1,3,5 mol%) was synthesized using melt-quenching method. A comprehensive investigation of the structural and optical properties was conducted to compare the effects of V2O5 as a dopant and as an addition to the glass matrix. The physical parameters were assessed through the measurement of density. The influence of V2O5 introduction on vibrational modes was studied through Fourier-transform infrared (FTIR) and Raman spectroscopy. The UV–visible absorbance analysis unveiled the existence of multiple valence states of vanadium (V3+, V4+ and V5+). The reduction in bandgap was determined through the utilization of a Tauc plot, while the measurement of the refractive index allowed for the assessment of its variation with the composition of V2O5. Photoluminescence spectroscopy (PL) was employed to explore the presence of intrinsic defects within the glass matrix and the impact of V2O5 on the emission spectra. Furthermore, CIE chromaticity coordinates of synthesized samples were observed in both the white and blue regions, suggesting their potential application in display devices. Significantly, V2O5 glass doped with 1 mol% displayed chromaticity, characterized by CIE coordinates x = 0.288 and y = 0.386, closely matching the white region as well as the bandpass filter. The introduction of transition metal oxide dopants into borophosphate glass yielded exceptional emission properties. The ability to modify optical properties makes it more promising for these glass materials, particularly for applications like optical filters and displays. © 2024 Elsevier Ltd and Techna Group S.r.l.Item Synergistic enhancement of optical properties in erbium-doped borate glasses through copper nanoparticle incorporation(Elsevier Ltd, 2024) Ingle, A.; Shashikala, H.D.; Udayashankar, N.K.The present study investigated the impact of incorporating copper nanoparticles (CuNPs) on the optical properties of erbium-doped borate glasses. Through melt-quenching and heat treatment techniques, glasses with varying Cu2O concentrations (x = 0–5 mol%) were synthesized. Physical and structural analyses revealed that Cu ions serve as effective network modifiers. They foster the formation of a greater proportion of BO4 tetrahedra and thus enhancing glass homogeneity. Optical absorption spectra demonstrate a distinct modulation of Er3+ absorption bands with Cu2O embedding, indicating the formation of CuNPs, as validated by the emergence of surface plasmon resonance bands. This structural evolution results in a noticeable reduction in the bandgap energy, signifying improved semiconducting behavior. Judd-Ofelt analysis highlighted the profound influence of CuNPs on hypersensitive transitions, thereby affecting oscillator strength. Photoluminescence measurements revealed amplified emission in the visible red and near infrared (NIR) region, attributed to the synergistic effects of CuNPs and Er3+ ions, with 5 mol % Cu2O exhibiting the highest emission intensity. Analysis of the radiative properties validates the enhancement of the emission cross-section, gain bandwidth, optical gain and radiative transitions. These enhancements contribute to a notable increase in the branching ratio from 0.91 % to 5.41 % accompanied by an increase in the quantum efficiency from ∼79 % to ∼90 %. Moreover, decay analysis revealed a notable enhancement in lifetime from 3.03 ms to 15.74 ms, which is indicative of enhanced radiative transitions. Overall, the incorporation of CuNPs into erbium-doped borate glasses facilitates significant enhancements in physical, structural, and optical properties. This positions them as promising materials for a wide array of optoelectronic applications. This comprehensive study sheds light on the complex interplay between CuNPs and erbium-barium borate glasses, offering valuable insights for the development of advanced optoelectronic materials with enhanced performance and functionality. © 2024 Elsevier Ltd and Techna Group S.r.l.
