Biomedical Device Surface Treatment by Laser-Driven Hydroxyapatite Penetration-Synthesis Technique for Gapless PEEK-to-Bone Integration.

Polyetheretherketone (PEEK), a bioinert polymer known for its mechanical properties similar to bone, is capable of averting stress shielding. Due to these attributes, it finds applications in diverse fields like orthopedics, encompassing cervical disc replacement for the neck and spine, along with dentistry and plastic surgery. However, due to insufficient bonding with bone, various methods such as hydroxyapatite (HA) coating on the surface are attempted. Nonetheless, the interface between the polymer and ceramic, two different materials, tended to delaminate after transplantation, posing challenges in preventing implant escape or dislodgement. This research delves into the laser-driven hydroxyapatite penetration-synthesis technique. Differing from conventional coating methods that bond layers of dissimilar materials like HA and PEEK, this technology focuses on synthesizing and infiltrating ionized HA within the PEEK substrate resulting in an interface-free HA-PEEK surface. Conversely, HA-PEEK with this technology applied achieves complete, gap-free direct bone-implant integration.  Our research involved the analysis of various aspects. By means of these, we quantitatively assesed the enhanced bone bonding characteristics of HA-PEEK surfaces treated with this approach and offered and explanation for the mechanism responsible for direct bone integration.

Study of the effect of magnetic fields on static degradation of Fe and Fe-12Mn-1.2C in balanced salts modified Hanks' solution.

Iron and its alloys are attractive as biodegradable materials because of their low toxicity and suitable mechanical properties; however, they generally have a slow degradation rate. Given that corrosion is an electrochemical phenomenon where an exchange of electrons takes place, the application of magnetic fields from outside the body may accelerate the degradation of a ferrous temporary implant. In the present study, we have investigated the effect of alternating and direct low magnetic field (H = 6.5 kA/m) on the corrosion process of pure iron (Fe) and an iron-manganese alloy (FeMnC) in modified Hanks' solution. A 14-day static immersion test was performed on the materials. The corrosion rate was assessed by mass and cross-sectional loss measurements, scanning electron microscopy, X-ray diffractometry, Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy before and after degradation. The results show that the presence of magnetic fields significantly accelerates the degradation rate of both materials, with the corrosion rate being twice as high in the case of Fe and almost three times as high for FeMnC. In addition, a homogenous degradation layer is formed over the entire surface and the chemical composition of the degradation products is the same regardless of the presence of a magnetic field.

Electrochemical and in vitro biological behaviors of a Ti-Mo-Fe alloy specifically designed for stent applications.

There is a deep interest in developing new Ni-free Ti-based alloys to replace 316 L stainless steel and Co-Cr alloys for endovascular stent application, mainly because the release of Ni can generate toxicity and allergenicity. Interactions of Ti alloy biomaterials with bone cells and tissues have been widely investigated and reported, while interactions with vascular cells and tissues, such as endothelial cells (ECs) and smooth muscle cells (SMCs), are scarce. Therefore, this study focused on the relationship among the surface finishing features, corrosion behavior and in vitro biological performances regarding human ECs, SMCs and blood of a newly developed Ti-8Mo-2Fe (TMF) alloy, specifically designed for balloon-expandable stent applications. The alloy performances were compared to those of 316 L and pure Ti, prepared with the same surface finishing techniques, which are mechanical polishing and electropolishing. Surface properties were investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM), contact angle (CA) and x-ray photoelectron spectroscopy (XPS). The corrosion behavior was assessed with potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) tests in phosphate buffered saline (PBS) solution. No significant differences were observed regarding the corrosion rate measured with PDP analyses, which was of the order of 2 × 10-4 mm/y for all the studied materials. Moreover, similarly to pure Ti, TMF exhibited an advantage over 316 L for biomedical applications, namely remarkable resistance to pitting corrosion up to high potentials. The results evidenced a good cytocompatibility and hemocompatibility, making this group of alloy a potential candidate for cardiovascular implants. In fact, both ECs and SMCs proliferated on TMF surfaces showing a 7-day viability similar to that of pure Ti. Regarding hemocompatibility, TMF did not cause hemolysis, and blood coagulation was delayed on its surface in comparison to pure Ti. When compared to 316 L, TMF showed similar hemocompatibility.

Surface Modification of an Absorbable Bimodal Fe-Mn-Ag Alloy by Nitrogen Plasma Immersion Ion Implantation.

Recently, Fe-Mn-based alloys have been increasingly catching the attention of the scientific community, because of their tunable and outstanding mechanical properties, and suitable degradation behavior for biomedical applications. In spite of these assets, their corrosion rate (CR) is, in general, too low to satisfy the requirements that need to be met for cardiovascular device applications, such as stents. In fact, the CR is not always the same for all of the degradation stages of the material, and in addition, a finely tuned release rate, especially during the first steps of the corrosion pattern, is often demanded. In this work, a resorbable bimodal multi-phase alloy Fe-3Mn-1Ag was designed by mechanical alloying and spark plasma sintering (SPS) to accelerate the corrosion rate. The presence of several phases, for example α-Fe, α-Mn, γ-FeMn and Ag, provided the material with excellent mechanical properties (tensile strength UTS = 722 MPa, tensile strain A = 38%) and a higher corrosion rate (CR = 3.2 ± 0.2 mm/year). However, higher corrosion rates, associated with an increased release of degradation elements, could also raise toxicity concerns, especially at the beginning of the corrosion pattern. In this study, The focus of the present work was the control of the CR by surface modification, with nitrogen plasma immersion ion implantation (N-PIII) treatment that was applied to mechanically polished (MP) samples. This plasma treatment (PT) improved the corrosion resistance of the material, assessed by static degradation immersion tests (SDITs), especially during the first degradation stages. Twenty-eight days later, the degradation rate reached the same value of the MP condition. Nitrogen compounds on the surface of the substrate played an important role in the corrosion mechanism and corrosion product formation. The degradation analysis was carried out also by potentiodynamic tests in modified Hanks' balanced salt solution (MHBSS), and Dulbecco's phosphate buffered saline solution (DPBSS). The corrosion rate was higher in MHBSS for both conditions. However, there was no significant difference between the corrosion rate of the PT in DPBSS (CR = 1.9 ± 0.6 mm/year) and in MHBSS (CR = 2 ± 1.4 mm/year). The cell viability was assessed with human vein endothelial cells (HUVECs) via an indirect metabolic activity test (MTT assay). Due to the lower ion release of the PT condition, the cell viability increased significantly. Thus, nitrogen implantation can control the in vitro corrosion rate starting from the very first stage of the implantation, improving cell viability.

Characterization of a Magnesium Fluoride Conversion Coating on Mg-2Y-1Mn-1Zn Screws for Biomedical Applications.

MgF2-coated screws made of a Mg-2Y-1Mn-1Zn alloy, called NOVAMag® fixation screws (biotrics bioimplants AG), were tested in vitro for potential applications as biodegradable implants, and showed a controlled corrosion rate compared to non-coated screws. While previous studies regarding coated Mg-alloys have been carried out on flat sample surfaces, the present work focused on functional materials and final biomedical products. The substrates under study had a complex 3D geometry and a nearly cylindrical-shaped shaft. The corrosion rate of the samples was investigated using an electrochemical setup, especially adjusted to evaluate these types of samples, and thus, helped to improve an already patented coating process. A MgF2/MgO coating in the µm-range was characterized for the first time using complementary techniques. The coated screws revealed a smoother surface than the non-coated ones. Although the cross-section analysis revealed some fissures in the coating structure, the electrochemical studies using Hanks' salt solution demonstrated the effective role of MgF2 in retarding the alloy degradation during the initial stages of corrosion up to 24 h. The values of polarization resistance (Rp) of the coated samples extrapolated from the Nyquist plots were significantly higher than those of the non-coated samples, and impedance increased significantly over time. After 1200 s exposure, the Rp values were 1323 ± 144 Ω.cm2 for the coated samples and 1036 ± 198 Ω.cm2 for the non-coated samples, thus confirming a significant decrease in the degradation rate due to the MgF2 layer. The corrosion rates varied from 0.49 mm/y, at the beginning of the experiment, to 0.26 mm/y after 1200 s, and decreased further to 0.01 mm/y after 24 h. These results demonstrated the effectiveness of the applied MgF2 film in slowing down the corrosion of the bulk material, allowing the magnesium-alloy screws to be competitive as dental and orthopedic solutions for the biodegradable implants market.

Effect of silver in thermal treatments of Fe-Mn-C degradable metals: Implications for stent processing.

Twinning-induced plasticity (TWIP) steels are considered excellent materials for manufacturing products requiring extremely high mechanical properties for various applications including thin medical devices, such as biodegradable intravascular stents. It is also proven that the addition of Ag can guarantee an appropriate degradation while implanted in human body without affecting its bioactive properties. In order to develop an optimized manufacturing process for thin stents, the effect of Ag on the recrystallization behavior of TWIP steels needs to be elucidated. This is of major importance since manufacturing stents involves several intermediate recrystallization annealing treatments. In this work, the recrystallization mechanism of two Fe-Mn-C steels with and without Ag was thoroughly investigated by microstructural and mechanical analyses. It was observed that Ag promoted a finer microstructure with a different texture evolution, while the recrystallization kinetics resulted unaffected. The presence of Ag also reduced the effectiveness of the recrystallization treatment. This behavior was attributed to the presence of Ag-rich second phase particles, precipitation of carbides and to the preferential development of grains possessing a {111} orientation upon thermal treatment. The prominence of {111} grains can also give rise to premature twinning, explaining the role of Ag in reducing the ductility of TWIP steels already observed in other works. Furthermore, in vitro biological performances were unaffected by Ag. These findings could allow the design of efficient treatments for supporting the transformation of Fe-Mn-C steels alloyed with Ag into commercial products.

Improving the radiopacity of Fe-Mn biodegradable metals by magnetron-sputtered W-Fe-Mn-C coatings: Application for thinner stents.

In this exploratory work, micrometric radiopaque W-Fe-Mn-C coatings were produced by magnetron sputtering plasma deposition, for the first time, with the aim to make very thin Fe-Mn stents trackable by fluoroscopy. The power of Fe-13Mn-1.2C target was kept constant at 400 W while that of W target varied from 100 to 400 W producing three different coatings referred to as P100, P200, P400. The effect of the increased W power on coatings thickness, roughness, structure, corrosion behavior and radiopacity was investigated. The coatings showed a power-dependent thickness and W concentration, different roughness values while a similar and uniform columnar structure. An amorphous phase was detected for both P100 and P200 coatings while γ-Fe, bcc-W and W3C phases found for P400. Moreover, P200 and P400 showed a significantly higher corrosion rate (CR) compared to P100. The presence of W, W3C as well as the Fe amount variation determined two different micro-galvanic corrosion mechanisms significantly changing the CR of coatings, 0.26 ± 0.02, 59.68 ± 1.21 and 59.06 ± 1.16 µm/year for P100, P200 and P400, respectively. Sample P200 with its most uniform morphology, lowest roughness (RMS = 3.9 ± 0.4 nm) and good radiopacity (∼6%) appeared the most suitable radiopaque biodegradable coating investigated in this study.

Surface processing for iron-based degradable alloys: A preliminary study on the importance of acid pickling.

The formation of a heterogeneous oxidized layer, also called scale, on metallic surfaces is widely recognized as a rapid manufacturing event for metals and their alloys. Partial or total removal of the scale represents a mandatory integrated step for the industrial fabrication processes of medical devices. For biodegradable metals, acid pickling has already been reported as a preliminary surface preparation given further processes, such as electropolishing. Unfortunately, biodegradable medical prototypes presented discrepancies concerning acid pickling studies based on samples with less complex geometry (e.g., non-uniform scale removal and rougher surface). Indeed, this translational knowledge lacks a detailed investigation on this process, deep characterization of treated surfaces properties, as well as a comprehensive discussion of the involved mechanisms. In this study, the effects of different acidic media (HCl, HNO3, H3PO4, CH3COOH, H2SO4 and HF), maintained at different temperatures (21 and 60 °C) for various exposition time (15-240 s), on the chemical composition and surface properties of a Fe-13Mn-1.2C biodegradable alloy were investigated. Changes in mass loss, morphology and wettability evidenced the combined effect of temperature and time for all conditions. Pickling in HCl and HF solutions favor mass loss (0.03-0.1 g/cm2) and effectively remove the initial scale.

Six-Month Long In Vitro Degradation Tests of Biodegradable Twinning-Induced Plasticity Steels Alloyed with Ag for Stent Applications.

Twinning-induced plasticity (TWIP) Fe-Mn-C steels are biodegradable metals with far superior mechanical properties to any biodegradable metal, including Mg alloys, used in commercially available devices. For this reason, the use of Fe-Mn-C alloys to produce thinner and thinner implants can be exploited for overcoming the device size limitations that biodegradable stents still present. However, Fe-Mn steels are known to form a phosphate layer on their surface over long implantation times in animals, preventing device degradation in the required timeframe. The introduction of second phases in such alloys to promote galvanic coupling showed a short-term promise, and particularly the use of Ag looked especially effective. Nonetheless, the evolution of the corrosion mechanism of quaternary Fe-Mn-C-Ag alloys over time is still unknown. This study aims at understanding how corrosion changes over time for a TWIP steel alloyed with Ag using a simple static immersion setup. The presence of Ag promoted some galvanic coupling just in the first week of immersion; this effect was then suppressed by the formation of a mixed carbonate/hydroxide layer. This layer partly detached after 2 months and was replaced by a stable phosphate layer, over which a new carbonate/hydroxide formed after 4 months, effectively hindering the sample degradation. Attachment of phosphates to the surface matches 1-year outcomes from animal tests reported by other authors, but this phenomenon cannot be predicted using immersion up to 28 days. These results demonstrate that immersion tests of Fe-based degradable alloys can be related to animal tests only when they are carried out for a sufficiently long time and that galvanic coupling with Ag is not a viable strategy in the long term. Future works should focus more on surface modifications to control the interfacial behavior rather than alloying in the bulk.

Plasma-immersion ion implantation surface oxidation on a cobalt-chromium alloy for biomedical applications.

Co-Cr alloys such as L605 are widely applied for the manufacture of medical devices, including tiny cardiovascular stents. The presence of potentially toxic and allergenic release of Ni, Co, and Cr ions from these devices remains an unsolved concern. Surface modification by oxygen plasma immersion implantation (PIII) could be an excellent technique to create a dense and thin passive oxide layer on a relatively complex shape of a tiny device, such as a stent, thus reducing the potential release of metallic ions. The effect of oxygen PIII was investigated on L605 alloy specimens, from 5 to 50 mTorr gas pressures, and under pulsed bias voltages from -0.1 to -10 kV. The surface chemistry was investigated by x-ray photoelectron spectroscopy, while its morphology and surface energy were evaluated, respectively, by atomic force microscopy and scanning electron microscopy and by a sessile drop static contact angle. Electrochemical characterization was performed by potentiodynamic tests in the saline solution. Mechanical properties of the modified surface layer, specifically film adhesion and hardness (H), were assessed by scratch and nanoindentation tests. Results shown that the oxidized layers were composed of a mixture of Co and Cr oxides and hydroxides and were rich in Co. The corrosion rate was considerably reduced after O PIII, even for treatments using low bias voltage (-0.1 kV) and with consequent low oxygen implantation depth. Moreover, O PIII also improved surface hardness. The oxidized layers were found to have good adhesion and to be scratch resistant.

The addition of silver affects the deformation mechanism of a twinning-induced plasticity steel: Potential for thinner degradable stents.

While Fe-based alloys have already been reported to possess all mechanical properties required for vascular stenting, their relatively low degradation rate in vivo still constitutes their main bottleneck. The inflammatory reaction generated by a stent is inversely proportional to its mass. Therefore, the tendency in stenting is to lower the section so to reduce the inflammatory reaction. Twinning-induced plasticity steels (TWIP) possess excellent mechanical properties for envisaging the next generation of thinner degradable cardiovascular stents. To accelerate the degradation, the addition of noble elements was proposed, aimed at promoting corrosion by galvanic coupling. In this context, silver was reported to generally increase the degradation rate. However, its impact on the deformation mechanism of TWIP steels has not been reported yet. Results show that the use of Ag significantly reduces the ductility without altering the strength of the material. Furthermore, the presence of Ag was found to promote a different deformation texture, thus stimulating the formation of mechanical martensite. Since a stent works in the deformed state, understanding the microstructure and texture resulting from plastic deformation can effectively help to forecast the degradation mechanisms taking place during implantation and the expected degradation time. Moreover, knowing the deformed microstructure allows to understand the formability of very small tubes, as precursors of the next generation of thin section degradable stents. STATEMENT OF SIGNIFICANCE: Commercial degradable magnesium stents are limited from their relatively big structure size. Twinning-induced plasticity steels possess outstanding mechanical properties, but their degradation time goes beyond the timeframe expected from clinics. The inclusion of noble Ag particles, which favor galvanic coupling, is known to promote corrosion and solve this limitation. However, it is necessary to understand the impact that Ag has on the deformation microstructure and on the mechanical properties. The addition of Ag reduces the ductility of a twinning-induced plasticity steel because of a different deformation microstructure. Since a stent works in a deformed state inside an artery, understanding the microstructural evolution after plastic deformation allows to better predict the device performances during service life.

Surface modification and direct plasma amination of L605 CoCr alloys: on the optimization of the oxide layer for application in cardiovascular implants.

Stents are cardiovascular devices used to treat atherosclerosis, and are deployed into narrowed arteries and implanted by expansion to reopen the biological lumen. Nevertheless, complications after implantation are still observed in 10-14% of the implantations. Therefore, functionalizing these devices with active molecules to improve the interfacial effects with the surrounding tissue strongly impacts their success. A plasma-based procedure to directly graft biomolecules to the surface of cobalt chromium alloys, without any polymeric coating, has been recently reported. Assuring the stability of the coating during plastic deformation generated during the implantation whilst avoiding the corrosion of the surface is crucial. This study explores different surface treatments to be used as a pre-treatment for this novel procedure. The effects of (i) electropolishing, (ii) thermal treatments, and (iii) the plasma immersion ion implantation of oxygen on the chemical composition, roughness, wettability and efficiency during the plasma-amination procedure whilst avoiding cracks after deformation, thus maintaining corrosion resistant behaviour, were investigated by XPS, AFM, ToF-SIMS imaging and depth profile, and WCA. Furthermore, the hemocompatibility of the surface and cell viability assays were also performed. Results showed that all of the treatments created a different surface chemical composition: EP mainly of chromium oxide, PIII with a layer of cobalt oxide and TT with a mixture of oxides, as observed by XPS and ToF-SIMS. Moreover, EP was the process that generated a surface with the highest efficiency to amination and the most corrosion resistance among the treatments, and it appeared as the most suitable pre-treatment for stent functionalization.

Influence of cold rolling on in vitro cytotoxicity and electrochemical behaviour of an Fe-Mn-C biodegradable alloy in physiological solutions.

The properties of cold-worked Fe-13Mn-1.2C steel, as candidate material for scaffolding and stenting applications, have been investigated. The study of the electrochemical corrosion susceptibility of Fe-13Mn-1.2C alloy in protein bearing and non-protein bearing physiological solutions, revealed that there were no differences between the as-received, 10% and 20% cold worked Fe-13Mn-1.2C samples. Although protein addition reduces the overall corrosion rate in static immersion degradation tests for both the cold worked and non-cold worked alloys, there were no discernible differences in the corrosion rates of samples with different percentages of cold work deformations. Similarly, potentiodynamic testing showed no differences between the corrosion rates in solutions with and without protein addition. Atomic absorption spectroscopy (AAS) results-post static immersion-showed similar values of Fe and Mn concentrations in the electrolyte for all the investigated conditions. Cold working was found to increase Grain Average Misorientation (GAM) and deformation twins within the steel, and, consequently, this led to an increase in the elastic modulus. Hence, cold-rolling may be used to achieve smaller sections (volumes) in order to support the equivalent load of the non-cold worked counterpart, giving a larger surface area to the volume ratio, thereby increasing the corrosion rate, and, in turn, rendering the degradation process shorter. When considering cytocompatibility in vitro, the collected supernatant particulate free Fe-13Mn-1.2C steel electrolytes were seen to be equally cytocompatible with no differences being observed between the different percentage cold work conditions. The presence of solid 80 µm size particles in the seeded elutions were seen to change the results and render the Fe-13Mn-1.2C steel non-cytocompatible.

Effect of electrolyte composition and deposition current for Fe/Fe-P electroformed bilayers for biodegradable metallic medical applications.

With its proven biocompatibility and excellent mechanical properties, iron is an excellent source material for clinical cardiac and vascular applications. However, its relatively low degradation rate limits its use for the healing and remodeling of diseased blood vessels. To address these issues, a multi-purpose fabrication process to develop a bilayer alloy composed of electroformed iron (E-Fe) and iron-phosphorus (Fe-P) was employed. Bilayers of Fe/Fe-P were produced in an electrolytic bath. The effects of electrolyte chemical composition and deposition current density (idep) on layer structure and chemical composition were assessed by scanning electron microscopy, electron probe microanalysis, X-ray diffraction and X-ray photoelectron spectroscopy. The corrosion rate was determined by potentiodynamic polarization tests. The bilayers showed an increasing amount of P with increasing NaH2PO4·H2O in the electrolyte. Fe-P structure became finer for higher P amounts. Potentiodynamic polarization tests revealed that the corrosion rate was strongly influenced by deposition conditions. For a P amount of ~2 wt.%, the corrosion rate was 1.46mm/year, which confirms the potential of this material to demonstrate high mechanical properties and a suitable corrosion rate for biomedical applications.

The use of multiple pseudo-physiological solutions to simulate the degradation behavior of pure iron as a metallic resorbable implant: a surface-characterization study.

Understanding the interactions of a pure iron surface with biological elements, such as ions and proteins in an aqueous medium, is essential for an accurate in vitro assessment of corrosion patterns. In fact, the synergy of chlorides, carbonates, phosphates and complex organic molecules present in the body environment is a key factor affecting both in vivo and in vitro degradation of materials, especially iron and its alloys. The aim of this work was the assessment of degradation patterns of pure iron in 5 commercial pseudo-physiological solutions by a thorough study of degraded surface chemistry and morphology. It also provides a methodological basis to understand the short-term degradation mechanism of degradable iron depending on the surrounding physiological media. The standard static immersion corrosion test was modified to adapt the procedure to pseudo-physiological solutions. After a 14-day static immersion test, the surfaces of samples were investigated by scanning electron microscopy, stylus profilometry and atomic force microscopy techniques. The chemistry and phase composition of the degraded layers were evaluated, respectively, by X-ray photoelectron spectrometry and X-ray diffractometry. The morphology and composition of the degradation layers were found to be different for the test-solutions: for phosphate-rich solutions, the formation of an adherent passive layer was found; degradation mechanisms related to general corrosion were predominant for all the other solutions. In conclusion, the chemical composition of the used medium plays a fundamental role in the degradation pattern of pure iron, so that direct comparisons of solutions with different ion concentrations, as reported in the literature, need to be carefully assessed.

In vitro degradation behavior of Fe-20 Mn-1.2C alloy in three different pseudo-physiological solutions.

High manganese austenitic steels such as Fe-20Mn-1.2C alloys are among the most promising candidates for biodegradable stents applications due to their high strength, high ductility and their chemical composition. In the current work, 14 day static in-vitro tests were performed in controlled atmosphere to assess the degradation behavior in three common pseudo-physiological solutions, i.e. commercial Hanks' (CH), modified Hanks' (MH) and albumin-enriched Dulbecco's modified phosphate buffered saline (DPBS) solutions. The degraded samples surfaces as well as the degradation products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Degradation of material and degradation products are shown to be strongly dependent on the test medium due to the presence of different ionic species such as HCO3(-), CO3(2-), Cl(-), Ca(2+) or phosphate groups. In both MH and CH solutions, the increased content of HCO3(-) ions seems to promote MnCO3 crystal growth on sample surfaces whereas the presence of albumin and high content of phosphate ions promotes the formation of an amorphous layer rich in phosphates, iron and manganese.

Effect of grain sizes on mechanical properties and biodegradation behavior of pure iron for cardiovascular stent application.

Pure iron has been demonstrated as a potential candidate for biodegradable metal stents due to its appropriate biocompatibility, suitable mechanical properties and uniform biodegradation behavior. The competing parameters that control the safety and the performance of BMS include proper strength-ductility combination, biocompatibility along with matching rate of corrosion with healing rate of arteries. Being a micrometre-scale biomedical device, the mentioned variables have been found to be governed by the average grain size of the bulk material. Thermo-mechanical processing techniques of the cold rolling and annealing were used to grain-refine the pure iron. Pure Fe samples were unidirectionally cold rolled and then isochronally annealed at different temperatures with the intention of inducing different ranges of grain size. The effect of thermo-mechanical treatment on mechanical properties and corrosion rates of the samples were investigated, correspondingly. Mechanical properties of pure Fe samples improved significantly with decrease in grain size while the corrosion rate decreased marginally with decrease in the average grain sizes. These findings could lead to the optimization of the properties to attain an adequate biodegradation-strength-ductility balance.

Influence of cross-rolling on the micro-texture and biodegradation of pure iron as biodegradable material for medical implants.

Iron-based biodegradable metals have been shown to present high potential in cardiac, vascular, orthopaedic and dental in adults, as well as paediatric, applications. These require suitable mechanical properties, adequate biocompatibility while guaranteeing a low toxicity of degradation products. For example, in cardiac applications, stents need to be made by homogeneous and isotropic materials in order to prevent sudden failures which would impair the deployment site. Besides, the presence of precipitates and pores, chemical inhomogeneity or other anisotropic microstructural defects may trigger stress concentration phenomena responsible for the early collapse of the device. Metal manufacturing processes play a fundamental role towards the final microstructure and mechanical properties of the materials. The present work assesses the effect of mode of rolling on the micro-texture evolution, mechanical properties and biodegradation behaviour of polycrystalline pure iron. Results indicated that cross-rolled samples recrystallized with lower rates than the straight-rolled ones due to a reduction in dislocation density content and an increase in intensity of {100} crystallographic plane which stores less energy of deformation responsible for primary recrystallization. The degradation resulted to be more uniform for cross-rolled samples, while the corrosion rates of cross-rolled and straight-rolled samples did not show relevant differences in simulated body solution. Finally, this work shows that an adequate compromise between biodegradation rate, strength and ductility could be achieved by modulating the deformation mode during cold rolling.