Faculty Publications
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Item Facile hydrothermal synthesis of vanadium disulfide nanomaterial for supercapacitor application(SPIE, 2023) Mandal, A.; Pandey, N.; Pandey, S.K.; Yadav, A.K.; Chakrabarti, S.Vanadium disulfide (VS2) is a prominent metallic member of transition metal dichalcogenides (TMDs) family and has already demonstrated its flair in energy storage device applications such as supercapacitors and batteries. In this work, we have synthesized hexagonal shape VS2 nanomaterial using a facile one step hydrothermal route and investigated the phase, morphology and structural properties of the material. The formation of phase has been confirmed from the X-ray diffraction (XRD) plot by correlating with the database of Joint Committee on Powder Diffraction Standards (JCPDS) 00-036-1139 of 1T VS2. Further, the crystalline behavior of VS2 nanomaterial can be seen from the high resolution transmission electron microscopy (HRTEM) measurement. Moreover, the morphology of the synthesized material is obtained from the field emission gun-scanning electron microscopy (FEG-SEM). Also, the characteristic Raman peaks of 1T VS2 at 140.3 cm-1 and 192.3 cm-1 have been observed from the Raman spectrum indicating the metallic behavior of synthesized material. The peak at 281.8 cm-1 is attributed to the in-plane vibrational mode (E2g1) while the peak at 404.5 cm-1 represents the out-of-plane vibrational mode (A1g) of V-S bond. The Fourier transform infrared (FTIR) spectrum shows the V-S-V and V=S vibrational modes around 534 cm-1 and 982 cm-1 respectively. The study introduces a low cost, large scale, highly crystalline, and metallic VS2 nanomaterial with potential application for next generation supercapacitors and other energy storage devices. © 2023 SPIE.Item An insight into microscopy and analytical techniques for morphological, structural, chemical, and thermal characterization of cellulose(John Wiley and Sons Inc, 2022) Chakraborty, I.; Rongpipi, S.; Govindaraju, I.; Rakesh, B.; Mal, S.S.; Gomez, E.W.; Gomez, E.D.; Kalita, R.D.; Nath, Y.; Mazumder, N.Cellulose obtained from plants is a bio-polysaccharide and the most abundant organic polymer on earth that has immense household and industrial applications. Hence, the characterization of cellulose is important for determining its appropriate applications. In this article, we review the characterization of cellulose morphology, surface topography using microscopic techniques including optical microscopy, transmission electron microscopy, scanning electron microscopy, and atomic force microscopy. Other physicochemical characteristics like crystallinity, chemical composition, and thermal properties are studied using techniques including X-ray diffraction, Fourier transform infrared, Raman spectroscopy, nuclear magnetic resonance, differential scanning calorimetry, and thermogravimetric analysis. This review may contribute to the development of using cellulose as a low-cost raw material with anticipated physicochemical properties. Highlights: Morphology and surface topography of cellulose structure is characterized using microscopy techniques including optical microscopy, transmission electron microscopy, scanning electron microscopy, and atomic force microscopy. Analytical techniques used for physicochemical characterization of cellulose include X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. © 2022 Wiley Periodicals LLC.Item Molybdenum based mixed oxide containing Mo0.65V 0.25W0.10 was investigated for the partial oxidation of methanol. The structural property and catalytic activity of the mixed oxide catalyst was studied by surface area (BET), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infra-red spectroscopy (FTIR) and X-ray diffraction (XRD). The thermal activation of the catalyst resulted increase in the conversion of methanol and the selectivity to formaldehyde. The thermal activation of the MoVW mixed oxide in nitrogen atmospheres induces partial crystallization of a Mo5O14-type oxide at 813 K. The SEM images of the thermally activated catalyst show needle like particles. These particles were agglomerates of platelet-like crystallites of a few hundreds of nanometers in size. SEM and EDX techniques show that the mixed oxide is characterized by an inhomogeneous elemental distribution on the length scale of a few microns. XRD of the thermally activated catalyst showed a nanocrystalline material identified as a mixture of Mo5O 14, MoO3 and MoO2-type MoVW oxides. The catalytic activity of the MoVW mixed oxide show a good conversion of methanol and selectivity to formaldehyde. © 2005 Springer Science+Business Media, Inc.(Partial oxidation of methanol to formaldehyde on molybdenum based mixed oxide catalyst) Badekai Ramachandra, B.; Choi, J.-S.; Choo, K.-Y.; Sung, J.-S.; Song, S.-D.; Kim, T.-H.2005Item Microwave-assisted synthesis and magnetic studies of cobalt oxide nanoparticles(2011) Bhatt, A.S.; Bhat, D.K.; Tai, C.-W.; Santosh, M.S.An efficient microwave-assisted route has been used to synthesize nanoparticles of cobalt oxide. The particles were well characterized by transmission electron microscopy (TEM) which showed that the average diameter of the particles is around 6 nm. X-ray diffraction (XRD) studies further confirmed the formation of the spinel Co3O4. Purity of the products was detected by Fourier transform infrared spectroscopy (FTIR) combined with thermal gravimetric analysis (TG/DTG). The magnetic measurements revealed a small hysteresis loop at room temperature indicating a weak ferromagnetic nature of the synthesized Co3O4 nanoparticles. The magnetic moment of the particles was measured to be 4.27 ?eff. © 2010 Elsevier B.V. All rights reserved.Item Characterization of poly(ethylene-co-vinyl acetate-co-carbon monoxide)/layered silicate clay hybrids obtained by melt mixing(2011) Anandhan, S.; Patil, H.G.; Babu, R.R.In recent times, polymer-layered silicate nanocomposites have drawn a great deal of attention because they often exhibit tremendous improvements in material properties compared with virgin polymers or conventional microor macro-composites. In the present study, nanocomposites were developed from organically modified clay and poly(ethylene-co-vinyl acetate-co-carbon monoxide) by melt mixing. FTIR spectroscopy reveals that the interaction between the organoclay and EVACO is thermodynamically favored. High resolution wide angle X-ray diffraction and transmission electron microscopy were used to study the morphology of the nanocomposites. Elemental mapping by scanning electron microscopy indicates good dispersion and distribution of the nanoclay in EVACO matrix. The mechanical properties of the nanocomposites are optimum at a clay loading of 3%. © Springer Science+Business Media, LLC 2011.Item Adsorption of benzene vapor onto activated biomass from cashew nut shell: Batch and column study(Bentham Science Publishers, 2012) Suresh, S.; Vijayalakshmi, G.; Rajmohan, B.; Subbaramaiah, V.The preparation of chemically modified activated cashew nut shell (ACNSB) of different impregnation ratios and their effects in adsorption of benzene vapor were studied. Effects of chemical pre-impregnation using phosphoric acid at different ratios (1:1 and 2:1) were investigated in order to patent. Physico-chemical characterization including surface area, scanning electron microscopy, energy dispersive X-ray spectroscopy, High-resolution Transmission Electron Microscopy and Fourier transform infrared spectroscopy of the ACNSB before and after benzene adsorption have been done to understand the adsorption mechanism. Optimum conditions for benzene removal were found to be, adsorbent dose m=10 g/l of solution and time (t) 120 min for the C0 range of 300-500 mg/l. Adsorption of benzene followed pseudosecond-order kinetics. Langmuir and R-P isotherms were found to best represented data for benzene adsorption onto ACSNB. In ACNSB column experiments, it can be concluded that concentration of benzene increases with the longer breakthrough time and hence higher adsorption capacity. ACSNB are many advantages includes simple and fast, organic solvent recovery, economical, energy savings, environmentally safe aspect and minimize the waste management problem. © 2012 Bentham Science Publishers.Item Synthesis of copper nanofluids using ascorbic acid reduction method via one step solution phase approach(ASTM International, 2012) Shenoy, S.U.; Nityananda Shetty, A.N.A simple one step solution phase approach to synthesize copper nanofluids has been developed, involving simultaneous in situ synthesis of nanoparticles and their dispersion in the base fluid. Copper nitrate has been reduced using ascorbic acid in ethylene glycol under thermal as well as microwave conditions. Sodium lauryl sulfate has been used to control the size of the particle as well as to act as a stabilizing agent. The effect of ratio of the reactants, pH, power of microwave, reaction time, and dilution on the size of the particles has been studied using X-ray diffraction, transmission electron microscopy, and field-emission scanning electron microscopy. The characterization of the fluids has also been done using Fourier transform infrared spectrometry, ultraviolet-visible spectroscopy, selected area electron diffraction, and energy dispersive X-ray analysis. The thermal conductivity and viscosity of the fluid were also measured at various particle concentrations. The copper particles in the fluid were found to have size less than 50nm and were well dispersed in the fluid. Thus this method was found to preserve the advantages of the polyol process and aqueous chemical reduction method as well. The fluid was stable up to 5 weeks under stationary conditions at room temperature. This method employs fast, inexpensive, extendible process for the synthesis of copper nanofluids and also overcomes the drawbacks of two step process. Copyright © 2012 by ASTM International.Item Synthesis of copper nanofluids using ascorbic acid reduction method via one step solution phase approach(2012) Shenoy, S.U.; Nityananda Shetty, A.N.A simple one step solution phase approach to synthesize copper nanofluids has been developed, involving simultaneous in situ synthesis of nanoparticles and their dispersion in the base fluid. Copper nitrate has been reduced using ascorbic acid in ethylene glycol under thermal as well as microwave conditions. Sodium lauryl sulfate has been used to control the size of the particle as well as to act as a stabilizing agent. The effect of ratio of the reactants, pH, power of microwave, reaction time, and dilution on the size of the particles has been studied using X-ray diffraction, transmission electron microscopy, and field-emission scanning electron microscopy. The characterization of the fluids has also been done using Fourier transform infrared spectrometry, ultraviolet-visible spectroscopy, selected area electron diffraction, and energy dispersive X-ray analysis. The thermal conductivity and viscosity of the fluid were also measured at various particle concentrations. The copper particles in the fluid were found to have size less than 50nm and were well dispersed in the fluid. Thus this method was found to preserve the advantages of the polyol process and aqueous chemical reduction method as well. The fluid was stable up to 5 weeks under stationary conditions at room temperature. This method employs fast, inexpensive, extendible process for the synthesis of copper nanofluids and also overcomes the drawbacks of two step process. Copyright © 2012 by ASTM International.Item Parametric study of manufacturing ultrafine polybenzimidazole fibers by electrospinning(Springer, 2012) Anandhan, S.; Ponprapakaran, K.; Senthil, T.; George, G.Polybenzimidazole (PBI), a high performance polymer, was synthesized from 3,3?-diaminobenzidine (DAB) and isophthalic acid (IPA) through polycondensation. The chemical structure of PBI was confirmed by Fourier transform infrared spectroscopy. Thermal characterization of PBI was done by thermogravimetry and differential scanning calorimetry. PBI nanofibers were fabricated by electrospinning of N, N-dimethyl acetamide solutions of PBI of different solution concentrations, at different voltages. The effects of solution and process parameters (namely, solution concentration and DC voltage) on morphology and average diameter of electrospun PBI fibers were investigated. The electrospun ultrafine fibers' diameter and morphology were characterized by using scanning electron microscopy. Nanofibers were obtained only from PBI solutions of concentrations 12 and 14 % (w/v). At concentrations of 8, 10, and 16 %, fibers could not be obtained. The process parameters were optimized by using the statistical tool, factorial or two-way ANOVA (analysis of variance), DOE (design of experiments) and the results indicate that the applied voltage and the interaction of voltage and solution concentration are influential in determining the diameter and morphology of the electrospun ultrathin PBI fibers. Electrospun PBI fibers, as small as 56 nm, could be successfully produced by using the right combination of solution concentration and spinning voltage. © 2012 Central Institute of Plastics Engineering & Technology.Item Structural characterization of nano-crystalline Co3O4 ultra-fine fibers obtained by sol-gel electrospinning(2013) George, G.; Anandhan, S.In this paper, we report the obtention of ultrafine fibers of cobalt oxide (Co3O4) by combining electrospinning method with high-temperature calcinations from the precursor sol of poly(2-ethyl-2- oxazoline) (PEtOx)/cobalt acetate tetrahydrate [Co(CH3COO) 2·4H2O] in water. The optimum electrospinning conditions for obtaining precursor composite nanofibers from PEtOx/Co(CH 3COO)2·4H2O solution in water, to produce ceramic nanofibers, were studied. The average fiber diameter of the precursor composite fibers measured by scanning electron microscopy (SEM) was approximately 200 nm. Thermogravimetric analysis of PEtOx was performed to estimate the suitable calcination temperature of the precursor fibers. SEM images of the ceramic fibers obtained after calcination revealed the shrinkage in diameter due to complete degradation of the polymer and Co(CH 3COO)2·4H2O. Fourier transform infrared spectroscopy was used to ensure the complete pyrolysis of polymer during calcinations of the composite fibers. Crystalline properties of the ceramic fibers were studied by X-ray diffraction and high resolution transmission electron microscopy. The ceramic fibers are polycrystalline with an average grain size of ?40 nm obtained at a calcination temperature of 773 K. It was observed that the grain sizes increased as the calcination temperature was increased, due to self assembly mechanism. © 2013 Springer Science+Business Media New York.