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Item Microstructure and corrosion behavior of laser processed NiTi alloy(Elsevier Ltd, 2015) Marattukalam, J.J.; Singh, A.K.; Datta, S.; Das, M.; Balla, V.K.; Bontha, S.; Kalpathy, S.K.Abstract Laser Engineered Net Shaping (LENS™), a commercially available additive manufacturing technology, has been used to fabricate dense equiatomic NiTi alloy components. The primary aim of this work is to study the effect of laser power and scan speed on microstructure, phase constituents, hardness and corrosion behavior of laser processed NiTi alloy. The results showed retention of large amount of high-temperature austenite phase at room temperature due to high cooling rates associated with laser processing. The high amount of austenite in these samples increased the hardness. The grain size and corrosion resistance were found to increase with laser power. The surface energy of NiTi alloy, calculated using contact angles, decreased from 61 mN/m to 56 mN/m with increase in laser energy density from 20 J/mm2 to 80 J/mm2. The decrease in surface energy shifted the corrosion potentials to nobler direction and decreased the corrosion current. Under present experimental conditions the laser power found to have strong influence on microstructure, phase constituents and corrosion resistance of NiTi alloy. © 2015 Elsevier B.V.Item Effect of heat treatment on microstructure, corrosion, and shape memory characteristics of laser deposited NiTi alloy(Elsevier Ltd, 2018) Marattukalam, J.J.; Balla, V.K.; Das, M.; Bontha, S.; Kalpathy, S.K.The aim of this work is to study the effect of heat treatment on the microstructure, phase transformations, shape memory characteristics and corrosion behaviour of laser deposited equiatomic NiTi alloy. Dense samples of NiTi alloy were fabricated using Laser Engineered Net Shaping (LENS™) with two different laser energy densities by varying the scan speed and laser power. These samples were annealed for 30 min at 500 °C and 1000 °C in flowing argon, followed by furnace-cooling to room temperature. The resulting microstructures and properties were compared with the corresponding as-deposited samples. Microstructural analysis after heat treatment showed needle-shape martensite in the samples processed at lower laser energy density of 20 J/mm2, and lenticular or plate-like martensite in the samples processed at 80 J/mm2. The XRD results revealed relatively high concentration of martensite (B19?) in heat-treated NiTi alloy compared to as-processed samples. Furthermore, the heat treatment decreased the forward and reverse transformation temperatures of NiTi alloy from 80 – 95 °C to 20–40 °C, presumably due to annihilation of thermally induced defects. Interestingly, the samples annealed at 500 °C showed a measurable increase of 1–2% in the shape memory recovery, from the net recovery of 8% exhibited by the as-processed NiTi alloy. The corrosion resistance of laser-processed NiTi alloy decreased upon annealing. © 2018 Elsevier B.V.Item Effect of zinc and rare-earth element addition on mechanical, corrosion, and biological properties of magnesium(Cambridge University Press, 2018) Kottuparambil, R.R.; Bontha, S.; Ramesh, M.R.; Arya, S.; Jana, A.; Das, M.; Balla, V.K.; Amrithalingam, S.; Prabhu, T.R.The present work aims to understand the effect of zinc and rare-earth element addition (i.e., 2 wt% Gd, 2 wt% Dy, and 2 wt% of Gd and Nd individually) on the microstructure evolution, mechanical properties, in vitro corrosion behavior, and cytotoxicity of Mg for biomedical application. The microstructure results indicate that the Mg-Zn-Gd alloy consists of the lamellar long period stacking ordered phase. The electrochemical and immersion corrosion behavior were studied in Hanks balanced salt solution. Enhanced corrosion resistance with reduced hydrogen evolution volume and magnesium (Mg2+) ion release were estimated for the Mg-Zn-Gd alloy as compared to the other two alloy systems. At the early stage of corrosion, formation of the oxide film inhibited the corrosion propagation. However, at the later stages, the breaking of the oxide film leads to shallow pitting mode of corrosion. The ultimate tensile strength of Mg-Zn-Gd-Nd is better than the other two alloys due to the uniform distribution of the Mg12Nd precipitate phase. The moderate strength in the Mg-Zn-Gd alloy is due to the low volume fraction of the secondary phase. The MTT (methylthiazoldiphenyl-tetrazolium bromide) assay study was carried out to understand the cell cytotoxicity on the alloy surfaces. Studies revealed that all three alloys had significant cellular adherence and no adverse effect on cells. © 2018 Materials Research Society.Item Laser surface modification of Mg-Zn-Gd alloy: Microstructural, wettability and in vitro degradation aspects(Institute of Physics Publishing helen.craven@iop.org, 2018) Rakesh, K.R.; Bontha, S.; Ramesh, M.R.; Arya, S.; Das, M.; Balla, V.K.; Srinivasan, A.Mg-Zn-Gd have great potential for biomedical applications owing to excellent bioactivity and non-toxicity properties. In the present study, laser surface melting (LSM) was carried out on newly developed Mg-1Zn -2Gd (wt%) alloy. Effects of laser energy on microstructural evolution, corrosion properties, surface energy, and hardness have been investigated. The surface modified sample processed at different energy densities showed fine grain structure in the melt zone compared to the untreated substrate. Grain refinement in the laser melted region improved the hardness by 60%. The surface roughness was found to be increased with increasing laser energy density. At higher energy density, removal of materials from the surface is enhanced, resulting in deeper grooves and higher surface roughness. The wettability studies indicated that the variations in surface geometry, grain size and surface roughness of LSM samples strongly influence the surface energy and hydrophilicity. Improved wetting of LSM sample was achieved owing to grain refinement and low surface roughness. The corrosion resistance determined by immersion and electrochemical methods of laser melted sample in Hank's balanced salt solution improved considerably due to grain refinement, meltpool depth and uniform distribution of secondary phases. © 2018 IOP Publishing Ltd.Item Laser surface melting of Mg-Zn-Dy alloy for better wettability and corrosion resistance for biodegradable implant applications(Elsevier B.V., 2019) K.r, R.; Bontha, S.; M.r, R.; Das, M.; Balla, V.K.In order to improve the performance of magnesium (Mg) for resorbable implant applications, Mg-1Zn-2Dy alloy was developed and the surface of the alloy has been modified by melting using lasers. Laser melted samples, at different laser energy density, were then subjected to microstructural, hardness, wettability and in-vitro degradation assessment. The microstructure of the Mg-Zn-Dy alloy mainly consisted of ?-Mg and eutectic phase (Mg 8 ZnDy). The melted region of the alloy surface evolved with fine grain microstructure at the near surface region and columnar grains near to the liquid solid substrate. The degree of grain size refinement obtained at the melted zone in the order of 1–2 ?m. The cross sectional microhardness of the modified zone was measured by Vickers microhardness tester. Due to these microstructural refinements and solid solution strengthening the surface hardness of laser treated alloy increased by two-fold. It was found that as the energy density increased the surface roughness along with the surface energy also increased. The wetting behaviour of the surface was estimated through measuring the contact angle by dropping the polar and non-polar liquid. Results showed that the surface energy is also found to change with LSM due to changes in the surface morphology, microstructure and chemical composition of the material. The detailed degradation study was carried out by immersing the samples in hanks balances salt solution (HBSS).The improvement in the degradation behaviour followed by laser surface melting is related to the microstructural refinement as a result of rapid heating and cooling of the melted zone. © 2019 Elsevier B.V.Item Comparative investigation of coating and friction stir processing on Mg-Zn-Dy alloy for improving antibacterial, bioactive and corrosion behaviour(Elsevier B.V., 2021) Rokkala, U.; Jana, A.; Bontha, S.; Ramesh, M.R.; Balla, V.K.Magnesium based alloys are well-known materials for temporary implant applications. However, failures due to early degradation and bacterial infection are limiting their applications. To overcome these problems, in the present work a Mg-Zn-Dy alloy based composite surface was prepared using coating and friction stir processing (FSP) techniques. Herein, hydroxyapatite (HA) and silver (Ag) particles were deposited on Mg-Zn-Dy alloy to obtain HA and Ag coated surface (C-HAg). Later, FSP was carried out on the C-HAg surface to develop a Mg-Zn-Dy alloy based composite surface (F-HAg). Field emission scanning electron microscope (FESEM) and energy dispersive X-ray analysis (EDS) confirm the mixing of HA and Ag particles with the Mg-Zn-Dy substrate. Antibacterial studies reveal that both C-HAg and F-HAg samples inhibit Escherichia coli and Staphylococcus aureus bacteria. In vitro cytotoxicity study indicates that the both samples are non-toxic in nature. Results of in vitro corrosion study reveal a significant reduction (72%) in corrosion rate of F-HAg sample when compared to C-HAg sample. The F-HAg samples showed simultaneous improvement in corrosion resistance and antibacterial properties with good biocompatibility. The results of this study indicate that the developed composite surface is a promising material for antibacterial and biodegradable implant applications. © 2021 Elsevier B.V.Item Influence of friction stir processing on microstructure, mechanical properties and corrosion behaviour of Mg-Zn-Dy alloy(Springer, 2023) Rokkala, U.; Bontha, S.; Ramesh, M.R.; Balla, V.K.In the present study, friction stir processing (FSP) was carried out on as-cast Mg-Zn-Dy alloy to tailor grain size and texture which alter the mechanical properties and corrosion behaviour. The grain size of the as-cast alloy was reduced from 60 ± 2 µm to 3 ± 0.1 µm after FSP due to dynamic recrystallization. The effect of grain size, crystallographic orientation and fine precipitates on mechanical properties were investigated using field emission scanning electron microscope (FESEM) and electron back scattered diffraction (EBSD). The ultimate tensile strength, yield strength, % elongation and hardness of FSPed alloy improved by 55%, 60%, 53% and 46% when compared to as-cast alloy. The FSPed Mg-Zn-Dy alloy exhibited a 79% decrease in corrosion rate when compared to as-cast alloy which can be attributed to grain refinement, uniform distribution of secondary precipitates and strong basal texture. The surface of FSPed sample after immersion corrosion exhibited calcium phosphate rich minerals which help in apatite formation on the sample surface. Cytotoxicity studies using MTT assay revealed more than 80% cell viability for both as-cast and FSPed alloy illustrating non-toxic nature of both the samples. The results of this study indicate that FSPed Mg-Zn-Dy alloy is a potential material for biodegradable implants due to its high strength, corrosion resistance and biocompatibility. Graphical Abstract: [Figure not available: see fulltext.]. © 2023, The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature.Item Multi-step fabrication of bioactive Mg–Zn–Dy–AlO3/HA composites: exploring the synergistic effects of plasma spray and friction stir processing(Springer, 2024) Rokkala, U.; Bontha, S.; Ramesh, M.R.; Balla, V.K.Magnesium (Mg) alloys are gaining more attention in recent times as biodegradable materials. However, two major problems with Mg alloy implants are bacterial infections and poor corrosion resistance. In this context, a composite surface (Mg–Zn–Dy–Al2O3/HA) is developed using surface modification techniques. First, Al2O3 + HA composite powder is coated on Mg–Zn–Dy alloy to attain coated surface (C-AHa). Next, the C-AHa surface is subjected to friction stir processing to develop composite surface (F-AHa). Microstructural characterization reveals that, the Al2O3 + HA particles were distributed evenly into the Mg–Zn–Dy substrate. Antimicrobial activities against Escherichia coli and Staphylococcus aureus reveal low adhesion of bacteria on the F-AHa sample surface due to low surface energy (37.83 ± 0.22 mN/m) and low surface roughness (0.36 ± 0.1 µm). Further, the cytotoxicity tests confirm that the F-AHa sample shows significant improvement in cell viability (98%) after 7 days and non-toxic against the mouse osteoblast cells. In Vitro corrosion study observations demonstrate that the corrosion rate for the F-AHa sample is decreased by 72% compared to the C-AHa sample. Thus, the results of this study for the fabricated composites are promising for antimicrobial, biocompatible and bioabsorbable temporary implants. © The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature 2024.Item Microstructure - corrosion performance correlation of laser directed energy deposited Inconel 625(Elsevier Ltd, 2025) Praharaj, A.K.; Bontha, S.; Balla, V.K.; Chakrapani, S.K.; Suvin, P.S.The primary objective of the current work is to understand the influence of process parameters on the corrosion performance of laser directed energy deposited Inconel 625 (IN625). In this regard, IN625 bulk samples were deposited using optimized laser power and three different scanning speeds. The as-deposited (AD) samples are named as AD-L, AD-M, and AD-H corresponding to low, medium, and high scanning speeds, respectively. Comprehensive microstructural characterization, microhardness evaluation, and electrochemical corrosion testing (medium: 3.5 wt% NaCl solution) were performed to correlate the process parameters with the microstructural features and corrosion performance. The results revealed that average grain size of the AD-H sample was lowered by 22.8 % and 19 %, respectively than the AD-L and AD-M samples, resulting in an enhancement of 8.4 % and 3.3 % in microhardness. Electrochemical corrosion tests indicated that AD-H sample possessed a higher corrosion potential (Ecorr) and a lower corrosion current density (Icorr) when compared to other samples, confirming the corrosion resistance of the samples in the order of AD-H > AD-M > AD-L. The higher scanning speed resulted in finer grains, high dislocation density, and lowered volume fraction of secondary phases, which are attributed to superior corrosion resistance of the AD-H sample. Surface analysis of the corroded samples suggested a greater susceptibility to localized corrosion over pitting corrosion. The current work provides valuable insights to the correlation between process parameters, microstructure, and corrosion performance of LDED fabricated IN625, confirming notable influence of scanning speed on the corrosion behavior. © 2025 Elsevier B.V.Item Microstructural Evolution of Mg-Zn-Gd Alloy Using Equal Channel Angular Pressing to Enhance Mechanical and Corrosion Properties(Springer, 2025) Rokkala, U.; Patil, A.; Bontha, S.; Ramesh, M.R.; Balla, V.K.; Srinivasan, A.Equal channel angular pressing (ECAP) was used on the Mg-Zn-Gd alloy in this study to improve its corrosion and mechanical properties. Microstructural and phase analysis reveal that, after ECAP, a substantial grain refinement occurred, and secondary phases were observed. The grain size of the as-cast (AC) sample is reduced from 20 ± 1 to 0.88 ± 0.6 µm, attributed to dynamic recrystallization. The mechanical properties of the ECAP sample were significantly improved when compared to the AC sample. An improvement in the microhardness (43%), ultimate tensile strength (73%), yield strength (76%), and ductility (50%) were observed for the ECAP sample. A decrease in the corrosion rate was observed for ECAP sample (9 ± 1 mm/year) compared to the AC (16 ± 2 mm/year) sample. The grain refinement and crystallographic orientation of the ECAP samples contributed to the enhancement of corrosion resistance. © ASM International 2025.