In-vitro biomineralization and biocompatibility of friction stir additively manufactured AZ31B magnesium alloy-hydroxyapatite composites.

The present study aims to evaluate effect of hydroxyapatite (HA, Ca10(PO4)6OH2), a ceramic similar to natural bone, into AZ31B Mg alloy matrix on biomineralization and biocompatibility. The novel friction stir processing additive manufacturing route was employed to fabricate Mg-HA composites. Various HA contents (5, 10, 20 wt%) were incorporated into Mg matrix. Microstructural observation and chemical composition analysis revealed that refined Mg grains and dispersion of HA particles at micro/nanoscales were achieved in Mg-HA composites after the friction stir processing. The biomineralization evaluation were carried out using immersion experiments in simulated body fluid followed by mineral morphology observation and chemical composition analysis. The wettability measurements were conducted to correlate the biomineralization behavior. The results showed improvement in wettability and bone-like Ca/P ratio in apatite deposit on the composites compared to as-received Mg. In addition, the increase of blood compatibility, cell viability and spreading were found in the higher HA content composites, indicating the improved biocompatibility. Therefore, friction stir processed Mg-20 wt%HA composite exhibited the highest wettability and better cell adhesion among other composites due to the effect of increased HA content within Mg matrix.

Embedded Corrosion Sensing with ZnO-PVDF Sensor Textiles.

Corrosion in underground and submerged steel pipes is a global problem. Coatings serve as an impermeable barrier or a sacrificial element to the transport of corrosive fluids. When this barrier fails, corrosion in the metal initiates. There is a critical need for sensors at the metal/coating interface as an early alert system. Current options utilize metal sensors, leading to accelerating corrosion. In this paper, a non-conductive sensor textile as a viable solution was investigated. For this purpose, non-woven Zinc (II) Oxide-Polyvinylidene Fluoride (ZnO-PVDF) nanocomposite fiber textiles were prepared in a range of weight fractions (1%, 3%, and 5% ZnO) and placed at the coating/steel interface. The properties of ZnO-PVDF nanocomposite meshes were characterized using scanning electron microscopy (SEM), x-ray diffraction (XRD), Fourier transform infrared (FTIR) and d33 meter. Electrochemical impedance spectroscopy (EIS) testing was performed during the immersion of the coated samples to validate the effectiveness of the sensor textile. The results offer a new option for sub-surface corrosion sensing using low cost, easily fabricated sensor textiles.

Computational Assessment of Thermokinetics and Associated Microstructural Evolution in Laser Powder Bed Fusion Manufacturing of Ti6Al4V Alloy.

Although most of the near non-equilibrium microstructures of alloys produced by laser powder bed fusion (LPBF) additive manufacturing (AM) are being reported at a rapid rate, the accountable thermokinetics of the entire process have rarely been studied. In order to exploit the versatility of this AM process for the desired properties of built material, it is crucial to understand the thermokinetics associated with the process. In light of this, a three-dimensional thermokinetic model based on the finite element method was developed to correlate with the microstructure evolved in additively manufactured Ti6Al4V alloy. The computational model yielded the thermal patterns experienced at given location while building a single layer through multiple laser scans and a whole part through multiple layers above it. X-ray analysis of the resultant microstructure confirmed the presence of acicular martensitic (α') phase of (002) texture within the build-plane. Computationally predicted magnitude of the thermal gradients within the additively manufactured Ti6Al4V alloy in different directions (X, Y, and Z) facilitated the understanding about the evolution of grain morphology and orientation of acicular martensite in prior ß grains. The scanning electron microscopy observations of the alloy revealed the distinct morphology of phase precipitated within the martensitic phase, whose existence was, in turn, understood through predicted thermal history.

In-vitro bio-corrosion behavior of friction stir additively manufactured AZ31B magnesium alloy-hydroxyapatite composites.

Magnesium and its alloys have been considered for consumable bio-implant applications due to their similar mechanical properties to the natural bone and biodegradability. Nevertheless, uncontrollable corrosion rate and limited bioactivity of Mg based materials in biological environment restrain their application. In light of this, objective of the present study was to explore addition of hydroxyapatite (HA, Ca10(PO4)6OH2), a ceramic similar to bone mineral, into AZ31B Mg alloy and its effects on bio-corrosion behavior. Friction stir processing based additive manufacturing route was employed for producing AZ31B Mg-HA composites. Various HA contents (5, 10, and 20 wt%) were incorporated into Mg matrix. The microstructural observation revealed that the size of α-Mg grains reduced significantly after friction stir process. HA incorporation took place at micro/nanoscale in α-Mg matrix under the thermo-mechanical forces exerted by friction stir process. The corrosion behavior of friction stir processed Mg-HA composites was investigated using electrochemical methods in simulated body fluid. The results indicated an improvement in corrosion resistance for the composites compared to untreated AZ31B which was attributed to significant grain refinement upon friction stir process. On the other hand, incremental addition of HA had an opposing effect due to localized micro/nano-galvanic couples. As a result, friction stir process Mg-5 wt% HA composite demonstrated the highest corrosion resistance due to an optimum balance between beneficial effects of grain size refinement and limited number of local galvanic couples compared to the other friction stir process samples explored in the present work.

Thermal Assessment of Ex Vivo Laser Ablation of Cortical Bone.

As a potential osteotomy tool, laser ablation is expected to provide rapid machining of bone, while generating minimal thermal damage (carbonization) and physical attributes within the machined region conducive to healing. As these characteristics vary with laser parameters and modes of laser operation, the clinical trials and in vivo studies render it difficult to explore these aspects for optimization of the laser machining parameters. In light of this, the current work explores various thermal and microstructural aspects of laser-ablated cortical bone in ex vivo study to understand the fundamentals of laser-bone interaction using computational modeling. The study employs the Yb-fiber Nd:YAG laser (λ = 1064 nm) in the continuous wave mode to machine the femur section of bovine bone by a three-dimensional machining approach. The examination involved thermal analysis using differential scanning calorimetry and thermogravimetry, phase analysis using X-ray diffractometry, qualitative analysis using X-ray photoelectron spectroscopy, and microstructural and semiquantitative analysis using scanning electron microscopy equipped with energy-dispersive spectrometry. The mechanism of efficient bone ablation using the Nd:YAG laser was evaluated using the computational thermokinetics outcome. The use of high laser fluence (10.61 J/mm2) was observed to be efficient to reduce the residual amorphous carbon in the heat-affected zone while achieving removal of the desired volume of the bone material at a rapid rate. Minimal thermal effects were predicted through computational simulation and were validated with the experimental outcome. In addition, this work reveals the in situ formation of a scaffold-like structure in the laser-machined region which can be conducive during healing.

Optimization of biocompatibility in a laser surface treated Mg-AZ31B alloy.

Biodegradable bone implants can remove the need for subsequent bone-implant surgeries by controlled biomineralization and degradation. Although Mg-alloys generally possess biocompatible properties, they corrode rapidly, thereby preventing sufficient hydroxyapatite formation and biomineral growth. In an attempt to address these limitations, laser surface treatments were performed via the employment of a continuous wave Nd:YAG laser on the Mg-AZ31B alloy using laser fluences in the range of 1.06-4.24 J/mm2 (250-1000 W). The laser-treated samples were investigated for their wettability in simulated body fluid. In vitro analyses were performed in simulated body fluid to examine corrosion and biomineralization behavior on the laser-treated samples. Statistical optimization algorithms based on wettability data predicted an optimal laser fluence of 3.286J/mm2 (775 W) within the range of laser fluences used in the present study for achieving a balance between biodegradation and biomineralization. Confirmatory tests on optimized samples indicated an up to 84% grain size reduction in laser-treated surface regions, a several-fold increase in Mg17Al12 (ß) phase volume fraction, a reasonably abundant formation of hydroxyapatite, and increased rates of biomineralization that exceeded degradation. These findings indicate the potential of laser surface engineering to realize Mg-AZ31B alloy as a viable biodegradable bone implant material.

Microstructure and corrosion behavior of laser surface-treated AZ31B Mg bio-implant material.

Although magnesium and magnesium alloys are considered biocompatible and biodegradable, they suffer from poor corrosion performance in the human body environment. In light of this, surface modification via rapid surface melting of AZ31B Mg alloy using a continuous-wave Nd:YAG laser was conducted. Laser processing was performed with laser energy ranging from 1.06 to 3.18 J/mm2. The corrosion behavior in simulated body fluid of laser surface-treated and untreated AZ31B Mg alloy samples was evaluated using electrochemical technique. The effect of laser surface treatment on phase and microstructure evolution was evaluated using X-ray diffraction and scanning electron microscopy. Microstructure examination revealed grain refinement as well as formation and uniform distribution of Mg17Al12 phase along the grain boundary for laser surface-treated samples. Evolution of such unique microstructure during laser surface treatment indicated enhancement in the corrosion resistance of laser surface-treated samples compared to untreated alloy.

Laser surface modification of AZ31B Mg alloy for bio-wettability.

Magnesium alloys are the potential degradable materials for load-bearing implant application due to their comparable mechanical properties to human bone, excellent bioactivity, and in vivo non-toxicity. However, for a successful load-bearing implant, the surface of bio-implant must allow protein absorption and layer formation under physiological environment that can assist the cell/osteoblast growth. In this regard, surface wettability of bio-implant plays a key role to dictate the quantity of protein absorption. In light of this, the main objective of the present study was to produce favorable bio-wettability condition of AZ31B Mg alloy bio-implant surface via laser surface modification technique under various laser processing conditions. In the present efforts, the influence of laser surface modification on AZ31B Mg alloy surface on resultant bio-wettability was investigated via contact-angle measurements and the co-relationships among microstructure (grain size), surface roughness, surface energy, and surface chemical composition were established. In addition, the laser surface modification technique was simulated by computational (thermal) model to facilitate the prediction of temperature and its resultant cooling/solidification rates under various laser processing conditions for correlating with their corresponding composition and phase evolution. These predicted thermal properties were later used to correlate with the corresponding microstructure, chemical composition, and phase evolution via experimental analyses (X-ray diffractometer, scanning electron microscope, energy-dispersive spectroscopy).

Integrated experimental and theoretical approach for corrosion and wear evaluation of laser surface nitrided, Ti-6Al-4V biomaterial in physiological solution.

A laser based surface nitriding process was adopted to further enhance the osseo-integration, corrosion resistance, and tribological properties of the commonly used bioimplant alloy, Ti-6Al-4V. Earlier preliminary osteoblast, electrochemical, and corrosive wear studies of laser nitrided titanium in simulated body fluid clearly revealed improvement of cell adhesion as well as enhancement in corrosion and wear resistance but mostly lacked the in-depth fundamental understanding behind these improvements. Therefore, a novel integrated experimental and theoretical approach were implemented to understand the physical phenomena behind the improvements and establish the property-structure-processing correlation of nitrided surface. The first principle and thermodynamic calculations were employed to understand the thermodynamic, electronic, and elastic properties of TiN for enthalpy of formation, Gibbs free energy, density of states, and elastic properties of TiN were investigated. Additionally, open circuit potential and cyclic potentio-dynamic polarization tests were carried out in simulated body fluid to evaluate the corrosion resistance that in turn linked with the experimentally measured and computationally predicted surface energies of TiN. From these results, it is concluded that the enhancement in the corrosion resistance after laser nitriding is mainly attributed to the presence of covalent bonding via hybridization among Ti (p) and N (d) orbitals. Furthermore, mechanical properties, such as, Poisson׳s ratio, stiffness, Pugh׳s ductility criteria, and Vicker׳s hardness, predicted from first principle calculations were also correlated to the increase in wear resistance of TiN. All the above factors together seem to have contributed to significant improvement in both wear and corrosion performance of nitride surface compared to the bare Ti-6Al-4V in physiological environment indicating its suitability for bioimplant applications.

Laser deposited biocompatible Ca-P coatings on Ti-6Al-4V: microstructural evolution and thermal modeling.

A high intensity continuous wave diode pumped ytterbium laser source was used to deposit Ca-P coatings on a Ti-6Al-4V biocompatible alloy in order to generate a physically textured surface, enhancing osseointegration. Scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM) and energy dispersive spectroscopy (EDS) studies were coupled with X-ray and micro diffraction work to determine the structure, composition, and phases present in various zones of a sample prepared across the coating/substrate interaction zone. Three-dimensional thermal modeling was also carried out to determine the cooling rate and maximum temperature experienced by different regions of the substrate. Combining these results provide us with valuable insights regarding the thermo-physical as well as chemical interactions that take place across the coating-substrate interface.