• M K Naskar

      Articles written in Bulletin of Materials Science

    • Rheological properties of boehmite sols during ageing at room temperature (30 ± 1°C) under closed condition

      M K Naskar M Chatterjee D Ganguli

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      Boehmite sols were obtained by peptizing boehmite precipitates with glacial acetic acid. The sols were aged at room temperature (30 ± 1°C) under closed condition. Rheological properties of the sols were studied at different ageing times. The sol characteristics were interpreted by measuring their viscosity, areas of hysteresis of the flow curves and yield stress (𝜏y). Viscosity and the area of hysteresis of the flow curves increased with increasing ageing time of the sols. A sharp change of yield stress was observed during the ageing period from 15 to 36 days. The change in viscous to elastic nature and the appearance of gel point of the sol was observed by studying their oscillatory flow behaviour, i.e. by measuring loss modulus (𝐺''), elastic modulus (𝐺'), and loss tangent (tan 𝛿) of the sols. Gel point of boehmite sol was found at 36 days of ageing under closed condition at room temperature (30 ± 1°C).

    • Role of some rare earth (RE) ions (RE = La, Pr, Nd, Sm, Gd and Dy) in crystal and mechanical behaviours of sol–gel derived ZrO2–2 mol% RE2O3 spun fibres calcined at 1300°C

      M K Naskar M Chatterjee D Ganguli

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      Crystal behaviours such as crystallization temperature (amorphous to tetragonal (𝑡) zirconia), tendency of phase transformation (tetragonal to monoclinic (𝑚) zirconia) and lattice strain were studied with mechanical property e.g. tensile strength of sol–gel derived ZrO2–2 mol% RE2O3 (RE = La, Pr, Nd, Sm, Gd and Dy) spun fibres. Rare earth cations of varying sizes played a significant role in changing the above mentioned properties of ZrO2–2 mol% RE2O3 fibres. It was found that with decreasing the ionic size difference between the zirconium and RE ions, crystallization temperature (amorphous $\rightarrow \ t$-ZrO2) decreased, the probability of phase transformation ($t \rightarrow m$) decreased, lattice strain which is related to lattice distortion decreased and tensile strength increased.

    • A novel technique for fabrication of near-net-shape CMCs

      A Dey M Chatterjee M K Naskar S Dalui K Basu

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      A sol–gel vacuum infiltration technique has been developed for the fabrication of near-net-shape ceramic matrix composites (CMCs) using discontinuous mullite fibre preform with 15 vol.% of fibre content and ZrO2.10 wt.% Y2O3 sol as the infiltrant. Effect of sol viscosity, number of infiltration and calcination temperature on physico-mechanical properties of fabricated CMCs were examined. Characterization of the fibre preform, matrix material (in the form of ceramic specimen without fibre) and the developed CMCs were performed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD indicated the presence of cubic (𝑐) and tetragonal (𝑡) zirconia in both the CMCs and the ceramic specimens calcined even at 1400°C. Flexural strength of the CMCs and the ceramic specimens (calcined at 1400°C), determined by the three-point bending test, was found to be about 14 mPa and 1.40 mPa, respectively. SEM indicated multiple fracture of the matrix which gave rise to pseudo elasticity. This is also evident from the load-displacement curve of the three-point bend test. SEM studies also indicated fibre pull-out in the fracture surface of the CMCs.

    • Silicalite-1 zeolite membranes on unmodified and modified surfaces of ceramic supports: A comparative study

      M K Naskar D Kundu M Chatterjee

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      Silicalite-1 zeolite membranes were prepared hydrothermally on the porous ceramic supports, both unmodified and modified with 3-aminopropyl triethoxysilane (APTES) as a coupling agent following ex situ (secondary) crystal growth process. The microstructure of the membranes was examined by scanning electron microscopy (SEM). The permeation study with a single gas, nitrogen (N2) was performed through the membranes. For the surface modified support, a more surface coverage of the seed crystals on the porous support was observed resulting in a relatively higher dense packing of the crystals during secondary crystal growth process compared to that obtained from the unmodified support. The membrane developed on surface modified support rendered lower permeance value i.e. 9 × 10-7 mol m-2 s-1 Pa-1 of N2 compared to that formed on the unmodified support which gave permeance value of 20 × 10-7 mol m-2 s-1 Pa-1 of N2.

    • Emulsion-based synthesis of NaA zeolite nanocrystals and its integration towards NaA membranes

      M K Naskar A Das D Kundu M Chatterjee

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      NaA zeolite nanoparticles (seed crystals) of size 50–65 nm were synthesized using water-in-oil (w/o) type emulsions at a considerably low temperature of 65 ± 1°C in a short duration of 2 h. The emulsions were stabilized using non-ionic surfactants e.g. sorbitan monooleate (Span 80), sorbitan monolaurate (Span 20), polyoxyethylene(5)nonylphenylether with ethoxy numbers of 5 (Igepal CO-520) and polyoxyethylene sorbitan monooleate (Tween 80) of hydrophilic-lipophilic balance (HLB) values of 4.3, 8.6, 10 and 15 respectively. Among the surfactants, the intermediate HLB values of 8.6 (Span 20) and 10 (Igepal CO-520) were effective in synthesizing highly dispersible NaA nanoparticles of size 50–65 nm. The membrane prepared hydrothermally in multi-steps at 65 ± 1°C, using the Span 20-derived seed crystals deposited on porous support, showed the formation of high quality interlocked NaA coating. Single gas nitrogen (N2) permeation of the membrane exhibited a permeance value of 1.01 × 10-8 mol m-2 s-1 Pa-1 at ambient temperature (30°C).

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