Faculty Publications
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Item Investigation of sintering kinetics and morphological evolution of silver films from nano-dispersion(Springer Verlag service@springer.de, 2018) Pujar, P.; Anusha, P.; Gupta, D.; Mandal, S.The present study aimed at investigating the sintering kinetics and the mechanism of achieving uniform film morphology from silver nano-dispersion through evaporation of the solvent. A tuned time elapse between drop casting of silver dispersion and the annealing (dwell-time) acted as the decision maker in engineering the morphology: ring stain (infinite dwell-time), uniform deposit (variable dwell-time) and dot formation (zero dwell-time). Three distinct dwell-times (10, 20 and 30 min) are chosen for the study at different temperatures (120 to 250 °C) and the conclusion is derived based on the profile of the deposit. The frozen morphology that resulted from the evaporation goes through the debonding of surfactant with simultaneous sintering to minimize the surface energy. A linear isothermal sintering model comprising initial grain size, grain growth parameter, annealing time and fractional porosity helps to predict the grain size post-annealing. Theoretical predictions of grain sizes are well matched with experimental ones. The grain growth parameter which shows an upward trend with the annealing temperature is mainly due to a reduction in the porosity and the increase in the fraction of solid–solid interface which shows betterment in the percolation paths available for the movement of carriers. © 2018, Springer-Verlag GmbH Germany, part of Springer Nature.Item Faster Biomineralization and Tailored Mechanical Properties of Marine-Resource-Derived Hydroxyapatite Scaffolds with Tunable Interconnected Porous Architecture(American Chemical Society service@acs.org, 2019) Hadagalli, K.; Panda, A.K.; Mandal, S.; Basu, B.Although hydroxyapatite (HA)-based porous scaffolds have been widely researched in the last three decades, the development of naturally derived biomimetic HA with a tunable elastic modulus and strength together with faster biomineralization properties has not yet been achieved. To address this specific issue, we report here a scalable biogenic synthesis approach to obtain submicron HA powders from cuttlefish bone. The marine-resource-derived HA together with different pore formers can be conventionally sintered to produce physiologically relevant scaffolds with porous architecture. Depending on pore formers, the scaffolds with a range of porosity of up to 51% with a larger range of pore sizes up to 50 ?m were fabricated. An empirical relationship between the compression strength and the elastic modulus with fractional porosity was established. A combination of moderate compressive strength (12-15 MPa) with an elastic modulus up to 1.6 GPa was obtained from cuttlefish-bone-derived HA with wheat flour as the pore former. Most importantly, the specific HA scaffold supports the faster nucleation and growth of the biomineralized apatite layer with full coverage within 3 days of incubation in simulated body fluid. More importantly, the marine-species-derived HA supported better adhesion and proliferation of murine osteoblast cells than HA sintered using powders from nonbiogenic resources. The spectrum of physical and biomineralization properties makes cuttlefish-bone-derived porous HA a new generation of implantable biomaterial for potential application in cancellous bone regeneration. © 2019 American Chemical Society.Item Combustion aided in situ consolidation of high strength porous ceramic structures with a minimum thermal budget(Elsevier B.V., 2020) Pujar, P.; Pal, A.; Mandal, S.The exothermic reaction between a pair of combustible pore formers (urea-ammonium nitrate) is the driving force in realizing low-temperature consolidation of hydroxyapatite (HA) particles. The particles are allowed to sinter in the proximity to the combustible pore formers. The exothermic (?H°rea = -898 kJ/mol) redox reaction between combustible pore formers is successfully utilized in deriving high compressive strength (~24 MPa) of HA at 300 °C. The evolution of gaseous products of combustion results in an interconnected porous network of HA. The estimated compressive strength of sintered HA at 300 °C is comparable with high temperature (1100 °C) conventionally sintered HA, at a fixed open porosity (~40%); which depicts nearly ~82% achievement with a reduction of sintering temperature by ~72%. Also, the pellets sintered at 600 °C have shown ~90% achievement in compressive strength of sintered HA. Further, the saturated pore area of 15% requires a sintering time of 9.58 h at a sintering temperature of 600 °C. Thus, combustion-assisted sintering is an alternative technique proves its potentiality in achieving remarkable compressive strength and paves the way for low-cost porous ceramics. © 2020 Elsevier B.V.Item Improved Fracture Toughness and Crack Arrest Ability of Graphene–Alumina Nanocomposite(Springer, 2021) Akhil Raj, V.R.; Hadagalli, K.; Jana, P.; Mandal, S.In this work, high fracture toughness graphene–alumina composite was developed through a novel chemical method using boehmite and graphene, which is followed by extrusion and consolidation. The mixed precursors were consolidated by sintering at 1550 °C in a nitrogen atmosphere. The plate-like structures of boehmite form ?-alumina; meanwhile, graphene particles at the grain boundaries hinder the growth of alumina grains. The graphene reinforcement was bonded to ?-alumina matrix by van der Waals forces. The XRD pattern reveals the presence of graphene with a plane (002) along with ?-alumina. Properties such as fracture toughness (5.6 ± 0.01 MPa m0.5), Vickers hardness (1872 ± 25 kgf/mm2) and true density (3.8 g/cm3) were achieved in 0.5 wt.% graphene–alumina composite when compared to ?-alumina with fracture toughness (5.3 ± 0.1 MPa m0.5), Vickers hardness (1984 ± 28 kgf/mm2) and true density (3.91 g/cm3). The bridging and deviation of cracks in 0.5 wt.% graphene–alumina composite are attributed to the anchoring and dissipation of energy during crack growth, which enhances the fracture toughness, whereas ?-alumina exhibits failure caused by linear crack propagation. Meanwhile, the slight decrease in Vickers hardness and true density of 0.5 wt.% graphene–alumina composite is due to the tribological and low-density properties of graphene. The obtained properties of composite could be suitable in high-temperature, wear-resistant applications such as crucibles, bearings, etc. © 2021, ASM International.Item Preparation and structural characteristics of biphasic calcium phosphates from prawn shell bio-waste(Taylor and Francis Ltd., 2023) Satish, P.; Salian, A.; Hadagalli, K.; Mandal, S.The major objective of the work is to explore the mechanical properties of biphasic calcium phosphates (BCP), a biomaterial derived from marine resources like prawn (Fenneropenaeus Indicus) shell biowaste through wet chemical treatment of CaO. We report the BCP, a mixture of hydroxyapatite and octa calcium phosphate from prawn shell biowaste using wet chemical synthesis at 80°C under pH 10. XRD of BCP revealed the coexistence of secondary phases like β-TCP and α-TCP along with HA upon sintering at different temperatures. Furthermore, the SEM and EDS opened well-sintered uniaxial grains and the presence of trace elements like Fe, Mg, Si, and Na. The specimens sintered at 1100°C showed the highest compression strength of 56.8 MPa due to MgO at the grain boundaries, which plays an important role in grain boundary diffusion. Therefore, the prawn shell biowaste-derived BCP has good mechanical properties, making them suitable materials for high-strength bone substitutes. © 2023 Institute of Materials, Minerals and Mining. Published by Taylor & Francis on behalf of the Institute.Item Effect of Temperature on Solid-State Reaction of Prawn Shell-Derived Phase-Pure β-Tricalcium Phosphate(Springer, 2024) Satish, P.; Praveen, L.L.; Gautam, V.; Hadagalli, K.; Mandal, S.Over the past three decades, bioresorbable ceramics such as beta-tricalcium phosphate (β-TCP)-based porous scaffolds have been extensively studied. β-TCP-based scaffolds or cements for bone tissue applications have proved to be an outstanding alternative to repair and regenerate bone tissue defects caused by trauma or injury. In this study, an investigation on submicron β-TCP powders derived from prawn shell (Fenneropenaeus indicus, a source of marine biowaste) via solid-state reaction approach was carried out, which has calcite (CaCO3) in its exoskeleton (nonedible). The prawn shell-derived β-TCP can be prepared conventionally with dicalcium phosphate (CaHPO4) at different temperatures 900, 1000, 1100, and 1200 °C. The EDX spectra detect the Ca:P ratio of 1.5 confirming the formation of pure β-TCP at 1100 °C, which is in complete agreement with theoretical ratio. X-ray diffraction pattern revealed the phase-pure crystalline rhombohedral crystal structure of β-TCP with an average crystallite size of ~ 25.8 nm, prepared at 1100 °C. The field emission scanning electron microscopy images showed a homogeneous distribution of β-TCP powders with an average grain size of 3.07 µm at 1100 °C. Furthermore, Raman spectroscopy and Fourier transform infrared spectroscopy confirm the characteristics peaks of β-TCP. Differential scanning calorimetry and thermogravimetric analysis are performed to study the thermal behavior of the initial precursors mixture to synthesize β-TCP. β-TCP scaffolds sintered at 1100 °C exhibited compressive strength of ~ 6.2 MPa, for which Ca/P ratio is 1.51. Biodegradation study conducted on β-TCP scaffolds sintered at 1100 °C has shown slow degradation rate up to 5 days. Therefore, the prawn shell-derived β-TCP has physical and morphological properties which projects it as a promising implantable biomaterial for synthetic bone graft substitutes. © ASM International 2024.Item Enhancing Strength Properties of Hydroxyapatite Composites with Bentonite Clay(Taylor and Francis Ltd., 2025) Satish, P.; Hadagalli, K.; Nowl, M.S.; Siddeswara, R.; Kalikeri, S.; Mandal, S.The main inorganic component of human hard tissues is hydroxyapatite (HA, Ca10(PO4)6(OH)2) and the mechanical and biological performance of HA can be improved by incorporating clay minerals to create HA-clay composite scaffolds. This study demonstrates a high-strength biocomposite of HA and bentonite with a significant reduction of open porosity, considering bentonite clay for its biocompatibility. Prawn shells (Fenneropenaeus indicus - marine resource) were utilized as a sustainable source of calcium to synthesize high-purity HA through a wet-chemical process, offering an innovative approach to valorize bio-waste. HA-bentonite clay composites were made by compacting 10-40 wt% of bentonite clay with HA using uniaxial pressing, followed by sintering at 1100°C for 2 h. Characterization techniques like X-ray diffraction, Raman, Fourier transform infrared spectroscopy and field emission scanning electron microscopy verified the phases, structures, vibrational bonds and morphology of the synthesized materials. Energy dispersive X-ray spectroscopy and inductively coupled plasma mass spectrometry analysis were performed for elemental composition and heavy metal detection, respectively. The HA-bentonite (30 wt%) composite achieved an exceptional compressive strength of 155 MPa and an open porosity of 7%, surpassing bare HA. Adding 30% bentonite increased compressive strength six fold and decreased open porosity by 51% compared to bare HA. This novel approach to HA-bentonite scaffolds promises enhanced wear resistance and cellular proliferation in bone tissue engineering. © 2025 Indian Ceramic Society.