In situ production of low-modulus Ti-Nb alloys by selective laser melting and their functional assessment toward orthopedic applications.

This work aimed to manufacture Ti-28.5Nb and Ti-40.0Nb (wt%) alloys in situ via selective laser melting (SLM) from Ti and Nb elemental powders. X-ray diffraction analysis revealed complete ß-phase (cubic) in Ti-40.0Nb and a mixture of (α'' orthorhombic + ß cubic) phases in Ti-28.5Nb were formed, whereas few of the Nb particles remained only partially fused during manufacturing. The fraction of partially melted Nb particles was determined as ∼2 and ∼18% in Ti-28.5Nb and Ti-40Nb, respectively. Mechanical characterization revealed higher hardness and more strength in Ti-28.5Nb than in Ti-40.0Nb due to the presence of the α'' phase in the former. Tribocorrosion tests reveal a significantly better wear-corrosion resistance for Ti-40.0Nb, as determined from a lower total volume loss in Ti-40.0Nb (∼2 × 10-4 mm-3) than in Ti-28.5Nb (∼13 × 10-2 mm-3). The lower volume loss and better corrosion resistance behavior are attributed to the ß phase, which was dominant in Ti-40.0Nb. Cell studies reveal no toxicity for up to 7 days. Both the alloys were better at supporting cell proliferation than wrought Ti6Al4V. This study presents a route to preparing Ti-Nb alloys in situ by SLM that are promising candidates for biomedical applications.

Surface nanocrystallization enhances the biomedical performance of additively manufactured stainless steel.

Additive manufacturing enables the fabrication of patient-specific implants of complex geometries. Although selective laser melting (SLM) of 316L stainless steel (SS) is well established, post-processing is essential to preparing high-performance biomedical implants. The goal of this study was to investigate surface mechanical attrition treatment (SMAT) as a means to enhance the electrochemical, biomechanical, and biological performances of 316L SS fabricated by SLM in devices for the repair of bone tissues. The SMAT conditions were optimized to induce surface nanocrystallization on the additively manufactured samples. SMAT resulted in a thicker oxide layer, which provided corrosion resistance by forming a passive layer. The fretting wear results showed that the rate of wear decreased after SMAT owing to the formation of a harder nanostructured layer. Surface modification of the alloy by SMAT enhanced its ability to support the attachment and proliferation of pre-osteoblasts in vitro. The study of the response in vivo to the additively manufactured alloy in a critical-sized cranial defect murine model revealed enhanced interactions with the cellular components after the alloy was subjected to SMAT without inducing any adverse immune response. Taken together, the results of this work establish SMAT of additively manufactured metallic implants as an effective strategy for engineering next-generation, high-performance medical devices for orthopedics and craniomaxillofacial applications.

Wear behaviour of lithography ceramic manufactured dental zirconia.

OBJECTIVE: The study aims to evaluate the wear surface using 3D surface roughness and other material characterization of zirconia fabricated using photopolymerization based Lithography-based Ceramic Manufacturing (LCM). METHOD: LCM technology was used to fabricate zirconia specimens of size 10 × 10 × 2mm3. Scanning Electron Microscope, 3D-profilometer, X-ray Diffraction, and hardness test characterized the samples before and after wear and Coefficient of friction (COF) was monitored. RESULT: The COF was around 0.7 and did not differ much between the horizontally and vertically printed specimens. However, the surface roughness after wear for horizontally printed specimen was 0.567 ± 0.139 µm, while that for vertically printed specimen was 0.379 ± 0.080 µm. The reduced valley depth and the dale void volume were low for the vertically printed zirconia specimen, indicating lesser voids and low fluid retention. In addition, it was observed that the hardness value of the vertically printed sample was better. The scanning electron microscopic images and 3D surface profiles of the zirconia specimens depicted the surface topography and revealed the wear track. CONCLUSION: The study shows that zirconia fabricated using LCM technology possesses surface roughness of about 0.5 µm with no machining scars that are usually associated with CAD/CAM dentistry and also indicating agreement with clinically acceptable values for minimal surface roughness of dental restorations. Dental restorations using LCM fabricated zirconia redues the requirement of post-processing work flow that is part of CAD/CAM dentistry.

Biological and mechanical response of laser shock peening orthopaedic titanium alloy (Ti-6Al-7Nb).

This paper focuses on the evaluation of mechanical and biological properties of laser shock peening (LSP) orthopaedic grade Ti-6Al-7Nb alloy. LSP surface treatment was conducted at laser energy of 3 to 7 J with overlaps of 33%-67%, and with a 3 mm laser spot size. Cell viability on laser shock peened surface was evaluated through in-vitro MTT assay, using osteoblast-like MG63 cells for the first-time. Residual stresses, microhardness, microstructure, sliding wear and wetting properties were investigated. Compressive residual stresses were found at various depths due to controlling the LSP parameters, compared to the as-received surface. The laser shock peened surfaces were hardened from 365HV0.05 to 405HV0.05, while the as-received surface was 320HV0.05. The average sub-grain size was refined from 14% to 36% after LSP. The wear resistance was also controllable by altering LSP parameters. The MTT results show that the cell viability on the laser shock peened surfaces was comparatively lower than that of the untreated surface after 24 h. However, after 72 h, the cell viability on modified surfaces were significantly improved. This work indicated that laser shock peened surfaces have a strong potential to decrease the pain from orthopaedic implant failures and promote the cytocompatibility between the bone and implant.

Anisotropy of Additively Manufactured Co-28Cr-6Mo Influences Mechanical Properties and Biomedical Performance.

Additive manufacturing (AM) of biomedical alloys such as Co-Cr-Mo alloys holds immense potential for fabricating implants with complex geometry and tailored to meet patient-specific needs. However, layer-by-layer fabrication in AM processes results in undesired anisotropy due to the solidification texture and grain morphology. The present study aimed to investigate the effect of build orientation on the mechanical properties and functional performance, including tribocorrosion behavior and cytocompatibility of an orthopedic Co-28Cr-6Mo alloy manufactured by selective laser melting. Although the fabricated alloy showed weak crystallographic texture due to the rotational scanning strategy, significant anisotropy was found in the tensile properties due to the grain size and morphology. The presence of larger, elongated grains along the build direction as compared to smaller, equiaxed grains perpendicular to the build direction imparted the observed tensile anisotropy. Quantitative analysis based on current models for strengthening mechanisms is insufficient to explain the observed anisotropy, which is ascribed to the possible role of the cellular dendrites and stacking fault strengthening in Co-Cr alloys. Unlike the electrochemical behavior, which was largely independent of the build orientation, the bio-tribocorrosion studies revealed an anisotropic wear rate under fretting conditions. Osteoblast attachment and proliferation were found to be higher on the plane perpendicular to the build direction, owing to the differences in grain size. This work provides novel insights into the role of the manufacturing parameters in a selective-laser-melted Co-Cr alloy and its potential application in engineering load-bearing orthopedic implants.

Influence of Graphene Nanoplatelets on the Performance of Axial Suspension Plasma-Sprayed Hydroxyapatite Coatings.

Axial suspension plasma spraying (ASPS) is an alternative technique to atmospheric plasma spraying (APS), which uses a suspension of much finer powders (<5-micron particle size) as the feedstock. It can produce more refined microstructures than APS for biomedical implants. This paper highlights the influence of incorporated graphene nanoplatelets (GNPs) on the behavior of ASPS hydroxyapatite (HAp) coatings. The characterization of the ASPS coatings (HAp + varying GNP contents) was carried out using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), confocal Raman microscopy (CRM), white light interferometry (WLI), and contact angle measurements. The evaluation of the mechanical properties such as the hardness, roughness, adhesion strength, and porosity was carried out, along with a fretting wear performance. Additionally, the biocompatibility of the Hap + GNP coatings was evaluated using cytotoxicity testing which revealed a decrease in the cell viability from 92.7% to 85.4%, with an increase in the GNP wt.%. The visualization of the cell's components was carried out using SEM and Laser Scanning Microscopy. Furthermore, the changes in the genetic expression of the various cellular markers were assessed to analyze the epigenetic changes in human mesenchymal stem cells. The gene expression changes suggested that GNPs upregulated the proliferation marker and downregulated the pluripotent markers by a minimum of three folds.

Surface mechanical attrition treatment of low modulus Ti-Nb-Ta-O alloy for orthopedic applications.

Surface mechanical attrition treatment (SMAT) is recognized as a surface severe plastic deformation (SPD) method that is effective in improving the surface-dependent mechanical and functional properties of conventional metallic biomaterials. In this study, we aimed to systemically investigate the effect of SMAT on the physical, electrochemical, tribological and biological performances of a newly developed low modulus ß Ti-Nb-Ta-O alloy with two different microstructures, namely, single phase ß-treated and dual phase ß + α aged. The microhardness results showed considerable hardening for the ß-treated condition due to formation of deformation substructures; that was associated with increased corrosion resistance resulting from a stronger and denser passive layer on the surface, as revealed by Tafel polarization, impedance studies and Mott-Scottky plots. The wear volume loss during fretting in serum solution was found to decrease by 46% while friction coefficient decreased only marginally, due to presence of a harder and more brittle surface. In the ß + α condition of the alloy, minimal hardening was observed due to coarsening of the precipitates during SMAT. However, this also reduced the number of α-ß interfaces, which in turn minimized the tendency for galvanic corrosion resulting in lower corrosion rate after SMAT. Wear resistance was enhanced after SMAT, with 32% decrease in wear volume loss and 21% decrease in friction coefficient resulted due to improved ductility on the surface. The attachment and growth of osteoblasts on the alloys in vitro were not affected by SMAT and was comparable to that on commercially pure Ti. Taken together, these results provide new insights into the effects of surface SPD of low modulus ß- Ti alloys for orthopedic applications and underscore the importance of the initial microstructure in determining the performance of the alloy.

Role of aging induced α precipitation on the mechanical and tribocorrosive performance of a ß Ti-Nb-Ta-O orthopedic alloy.

A low modulus ß Ti-Nb-Ta-O alloy was subjected to heat treatment to investigate its phase stability upon aging. The resultant effect on the mechanical and functional properties was systematically evaluated. The aging of the ß-only microstructure, obtained by solutionizing and quenching, resulted in the formation of ultrafine α-precipitates with increasing order of size as the aging temperature increased from 400 °C to 600 °C. The variation in the size of α-precipitates effected the mechanical properties at the three different aging temperature. The highest hardening observed at 400 °C was associated with macroscopic embrittlement, whereas age softening was observed in samples aged at 600 °C due to coarsening of precipitates and softening of the ß-matrix. In contrast, aging at 500 °C resulted in about 32% increase in tensile strength from the ß-solutionized condition. As the samples aged at 500 °C showed optimum combination of mechanical properties among the aged samples, these were further characterized for their electrochemical, tribological and biological responses. The fretting wear studies showed that the wear rate of the solution-treated samples increased after aging due to the higher corrosion rate leading to a higher rate of tribocorrosive dissolution and formation of a transfer layer harder than that of solution treated sample. The Ti-Nb-Ta-O alloy supported the attachment and proliferation of osteoblasts similar to that on commercially pure Ti. Taken together, this work provides new insights into the preparation of next-generation Ti alloys for biomedical applications with high strength and low modulus through microstructural control induced by heat treatment.

Hydrothermal treatment of etched titanium: A potential surface nano-modification technique for enhanced biocompatibility.

Nanoengineering the topology of titanium (Ti) implants has the potential to enhance cytocompability and biocompatibility properties as implant surfaces play a decisive role in determining clinical success. Despite developments in various surface engineering strategies, antibacterial properties of Ti still need to be enhanced. Here a facile, cost-effective hydrothermal route was used to develop nano-patterned structures on a Ti surface. Changing hydrothermal treatment parameters such as temperature, pressure, and time, resulted in various topographies, crystal phases, and hydrophobicity. Specifically, hydrothermal treatment performed at 225 °C for 5 h, presented a novel topography with nanoflower features, exhibited no mammalian cell cytotoxicity for a time period of 14 days, and increased calcium deposition from osteoblasts. Treated samples also demonstrated antibacterial properties (without resorting to the use of antibiotics) against Staphylococcus aureus and methicillin resistant Staphylococcus aureus. In conclusion, hydrothermal oxidation on an etched Ti surface can generate surface properties that have excellent prospects for the biomedical field.

Performance of Hybrid Powder-Suspension Axial Plasma Sprayed Al2O3-YSZ Coatings in Bovine Serum Solution.

Ceramic coatings on metallic implants are a promising alternative to conventional implants due to their ability to offer superior wear resistance. The present work investigates the sliding wear behavior under bovine serum solution and indentation crack growth resistance of four coatings, namely (1) conventional powder-derived alumina coating (Ap), (2) suspension-derived alumina coating (As), (3) composite Al2O3-20wt % Yittria stabilized Zirconia (YSZ) coating (AsYs) deposited using a mixed suspension, and (4) powder Al2O3-suspension YSZ hybrid composite coating ApYs developed by axial feeding plasma spraying, respectively. The indentation crack growth resistance of the hybrid coating was superior due to the inclusion of distributed fine YSZ particles along with coarser alumina splats. Enhanced wear resistance was observed for the powder derived Ap and the hybrid ApYs coatings, whereas the suspension sprayed As and AsYs coatings significantly deteriorated due to extensive pitting.

Enhanced Tribocorrosion Resistance of Hard Ceramic Coated Ti-6Al-4V Alloy for Hip Implant Application: In-Vitro Simulation Study.

Developing coatings for various applications is an area of research of uttermost importance, to protect surfaces from severe damage by improving the wear and corrosion resistance of the materials. Recently, there has been increasing interest in ceramic coatings for biomedical applications, as the surface may become more inert in nature for the biological reactions and potentially increase the lifespan of the implants and minimize the side effects on the patients. Hence this study is focused on the tribocorrosion behavior of the ceramic coatings for the hip implant application on commonly used implant titanium alloy. The three types of the ceramic coatings are conventional monolithic micron alumina (IDA), micron alumina-40 wt % yttria-stabilized zirconia (YSZ) composite coating (IDAZ), and by-layer nanostructured alumina-13 wt % titania/YSZ (IDZAT) on Ti-6Al-4V alloy. A series of tests, under free potential and potentiostatic mode, were conducted using a hip simulator tribocorrosion setup under simulated joint fluid (bovine calf serum with protein concentration 30g/L). The tribological conditions are pin-on-ball contact with a load of 16N (approximately contact pressure of 50 MPa), the frequency of 1 Hz (walking frequency), and with an amplitude of 30°. The tribocorrosion studies clearly revealed that the coatings have better wear and corrosion resistance and the predominant damage mechanism was mechanical wear rather than corrosion. Among the coatings, the IDZAT shows enhanced tribocorrosion performance by exhibiting more positive OCP, no induced current, and a lower coefficient of friction.

Axial Suspension Plasma Spraying: An ultimate technique to tailor Ti6Al4V surface with HAp for orthopaedic applications.

Dissolution of atmospheric plasma sprayed (APS) hydroxyapatite (HAp) coatings on Ti-6Al-4 V medical implants have always been a challenge to overcome in the field of biomedical industry. In the present work, an attempt has been made to develop a HAp coating using a novel thermal spray process called axial suspension plasma spraying (SPS), which leads to thin adherent coatings. Two HAp coatings fabricated by APS (P1 and P2) and four SPS HAp coatings (S1, S2, S3 and S4) produced with varying spraying parameters were characterized in terms of (1) microstructure, porosity, hardness, adhesion strength, contact angle and phase purity; (2) corrosion resistance in 10% Fetal bovine serum (FBS); (3) in-vitro cell adherence and cell viability using human umbilical cord blood-derived mesenchymal stem cells (hMSCs). Amongst different APS and SPS coatings, P1 and S3 exhibited superior properties. S3 coating developed using SPS exhibited 1.3 times higher adhesion strength when compared to APS coating (P1) and 9.5 times higher corrosion resistance than P1. In addition, both S3 and P1 exhibited comparatively higher biocompatibility as evidenced by the presence of more than 92% viable hMSCs.

In-vitro cell adhesion and proliferation of adipose derived stem cell on hydroxyapatite composite surfaces.

The goal of this work was to enhance the mechanical strength and fracture toughness of brittle hydroxyapatite (HAP) by reinforcing it with nanocomposites such as graphene oxide (GO), carbon nanotubes (CNT) and Titania. The goal was also to evaluate the cytotoxicity and the cellular adhesion/proliferation of these composites. The composites were characterized for their crystallinity, functionality, morphology and mechanical properties. Altering the composition by adding 1wt% GO and CNT significantly altered the wettability, hardness and roughness. Further, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FITR) and X-ray photoelectron spectroscopy (XPS) results confirm the crystal structure, bulk chemical composition and surface elemental composition respectively of the composites. The bulk hardness of HAP with CNT was significantly higher than that of HAP. The wettability of HAP with GO was significantly lower than that of HAP with GO and Titania. Adipose Derived Stem Cells (ADSCs) were used for this study to evaluate cytotoxicity and viability. HAP with CNT and HAP with CNT and Titania were found to be least cytotoxic compared to other composites as evaluated by Lactate Dehydrogenase (LDH) assay and alamarBlue assay. ADSC adhesion and proliferation was investigated after 1, 4 and 7days of culture using fluorescence microscopy. All the composites nurtured ADSC adhesion and proliferation, however, distinct morphological changes were observed by using Scanning Electron Microscopy (SEM). Overall, these composites have the potential to be used as bone graft substitutes.