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    Surface design of Mg-Zn alloy temporary orthopaedic implants: Tailoring wettability and biodegradability using laser surface melting
    (Elsevier B.V., 2018) Manne, B.; Thiruvayapati, H.; Bontha, S.; Motagondanahalli Rangarasaiah, R.; Das, M.; Balla, V.K.
    Magnesium-based alloys have attracted significant attention for biomedical applications due to its biodegradability as well as density and elastic modulus which are close to those of human bone. However, the uncontrolled biodegradation and hydrogen evolution are of major concern. In this work, laser surface melting (LSM) has been carried out to tailor initial corrosion rates of Mg-2.2Zn alloy implants. Melt pool dimensions, microstructure and surface topography of the LSM samples were analysed. The wettability and in vitro degradation characteristics of untreated and treated alloy were compared. LSM resulted in much finer cellular microstructural features than as-cast alloy and the melted region depths between 65 and 115 ?m. Higher treatment depths helped to extend the corrosion protection time by suppressing the corrosion front movement. Polished LSM samples resulted in overall corrosion rates of 0.5–0.62 mm/year which was about 40%–50% reduction compared to the as-cast alloy. Accelerated biomineralisation of the surface via enhancements in the surface energy due to microstructural refinement as well as microstructural homogeneity and Zn enrichment in ?-Mg, favoured improvement of the overall corrosion performance of LSM-treated alloy. © 2018 Elsevier B.V.
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    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.
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    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.
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    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.
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    Tailoring surface characteristics of bioabsorbable Mg-Zn-Dy alloy using friction stir processing for improved wettability and degradation behavior
    (Elsevier Editora Ltda, 2021) Rokkala, U.; Bontha, S.; Ramesh, M.R.; Balla, V.K.; Srinivasan, A.; Kailas, S.V.
    Magnesium (Mg) and its alloys are currently under consideration for use as temporary implants. However, early degradation and maintaining mechanical integrity is a significant concern. Surface modification techniques are used to improve mechanical and corrosion properties of Mg based alloys. In the present study, friction stir processing (FSP) was used to tailor the surface characteristics of Mg-1Zn-2Dy (wt.%) alloy for temporary implant applications. The FSPed alloy was characterized using EBSD to understand the influence of FSP on crystallographic texture, grain size and grain boundaries and thereby their effect on corrosion, wettability and hardness. Results showed that the grain size of stir zone (SZ) was refined to less than 3 ?m, as a result of dynamic recrystallization (DRX) during FSP and the FSPed alloy exhibited better wettability than as-cast alloy. An increase in the hardness (11.7%) and elastic modulus (6.84%) of FSPed alloy were also observed. Electrochemical corrosion and weight loss methods were conducted in Dulbecco's Modified Eagle's Medium (DMEM) with, 10% Fetal Bovine Serum (FBS) physiological solution. The lower degradation rate (0.72 mm/yr) of FSPed alloy has been attributed to the fine grains and evenly distributed secondary phase particles. Further, the influence of grain boundary characteristics and crystallographic texture on the corrosion behavior have been investigated. © 2021 The Author(s).
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    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.
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    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.
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    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.