Electrokinetic behaviour of porous TiO2-coated implants.

It is known that the "race for the surface" determining the in vivo response is strictly connected to the physico-chemical properties of the material, especially at its surface. Accordingly, the study of surface roughness, charge and wettability is fundamental to predict the bio-response to the implant. In this work, streaming potential was chosen as a reliable method to quantify the solid surface charge of hydrothermally treated (HT) TiO2-anatase nano-crystalline coatings, grown on titanium substrates. The influence of metal and ionic conductance on the zeta potential values was taken into account, allowing for the correlation of the surface charge with the coating porosity, the semiconductor character of the TiO2 nano-crystals and the metallic nature of the bulk titanium.

Processability and Separability of Commercial Anti-Corrosion Coatings Produced by In Situ Hydrogen-Processing of Magnetic Scrap (HPMS) Recycling of NdFeB.

The recycling of NdFeB magnets is necessary to ensure a reliable and ethical supply of rare earth elements as critical raw materials. This has been recognized internationally, prompting the implementation of large-scale legislative measured aimed at its resolution; for example, an ambitious recycling quote has been established in the Critical Raw Materials Act Successful recycling in sufficient quantities is challenged by product designs that do not allow the extraction and recycling of these high-performance permanent magnets without excessive effort and cost. This is particularly true for smaller motors using NdFeB magnets. Therefore, methods of recycling such arrangements with little or no dismantling are being researched. They are tested for the hydrogen-processing of magnetic scrap (HPMS) method, a short-loop mechanical recycling process. As contamination of the recycled material with residues of anti-corrosion coatings, adhesives, etc., may lead to downcycling, the separability of such residues from bulk magnets and magnet powder is explored. It is found that the hydrogen permeability, expansion volume, and the chosen coating affect the viable preparation and separation methods as recyclability-relevant design features.

The Future of Permanent-Magnet-Based Electric Motors: How Will Rare Earths Affect Electrification?

In this review article, we focus on the relationship between permanent magnets and the electric motor, as this relationship has not been covered in a review paper before. With the increasing focus on battery research, other parts of the electric system have been neglected. To make electrification a smooth transition, as has been promised by governing bodies, we need to understand and improve the electric motor and its main component, the magnet. Today's review papers cover only the engineering perspective of the electric motor or the material-science perspective of the magnetic material, but not both together, which is a crucial part of understanding the needs of electric-motor design and the possibilities that a magnet can give them. We review the road that leads to today's state-of-the-art in electric motors and magnet design and give possible future roads to tackle the obstacles ahead and reach the goals of a fully electric transportation system. With new technologies now available, like additive manufacturing and artificial intelligence, electric motor designers have not yet exploited the possibilities the new freedom of design brings. New out-of-the-box designs will have to emerge to realize the full potential of the new technology. We also focus on the rare-earth crisis and how future price fluctuations can be avoided. Recycling plays a huge role in this, and developing a self-sustained circular economy will be critical, but the road to it is still very steep, as ongoing projects show.

Analytical electron microscopy of W-core ß-SiC fibers for use in an SiC-based composite material for fusion applications.

In this work, the interactions between tungsten (W) and silicon carbide (SiC) in Sigma SiC fibers at high temperatures were characterized using scanning and transmission electron microscopy. These fibers could have the potential for use in fusion-related applications owing to their high thermal conductivity compared with pure SiC-based fibers. The as-received fibers were composed of a 100-µm-thick shell of radially textured ß-SiC grains and a 15-µm-thick tungsten core, composed of a few hundreds of nm-sized elongated tungsten grains. The interfaces between the tungsten and the SiC and the SiC and the outer coatings were sharp and smooth. After heat treatment at 1,600°C for 3 h in Ar, the tungsten core reacted with SiC to form a rough interface surface. Inside the core, W5Si3, W3Si, and W2C phases were detected using energy-dispersive X-ray spectroscopy and electron-diffraction techniques. The mechanical properties of the fibers deteriorate after the heat treatment.

Limitations in the Grain Boundary Processing of the Recycled HDDR Nd-Fe-B System.

Fully dense spark plasma sintered recycled and fresh HDDR Nd-Fe-B nanocrystalline bulk magnets were processed by surface grain boundary diffusion (GBD) treatment to further augment the coercivity and investigate the underlying diffusion mechanism. The fully dense SPS processed HDDR based magnets were placed in a crucible with varying the eutectic alloys Pr68Cu32 and Dy70Cu30 at 2-20 wt. % as direct diffusion source above the ternary transition temperature for GBD processing followed by secondary annealing. The changes in mass gain was analyzed and weighted against the magnetic properties. For the recycled magnet, the coercivity (HCi) values obtained after optimal GBDP yielded ~60% higher than the starting recycled HDDR powder and 17.5% higher than the SPS-ed processed magnets. The fresh MF-15P HDDR Nd-Fe-B based magnets gained 25-36% higher coercivities with Pr-Cu GBDP. The FEG-SEM investigation provided insight on the diffusion depth and EDXS analysis indicated the changes in matrix and intergranular phase composition within the diffusion zone. The mechanism of surface to grain boundary diffusion and the limitations to thorough grain boundary diffusion in the HDDR Nd-Fe-B based bulk magnets were detailed in this study.

Coercivity Increase of the Recycled HDDR Nd-Fe-B Powders Doped with DyF3 and Processed via Spark Plasma Sintering & the Effect of Thermal Treatments.

The magnetic properties of the recycled hydrogenation disproportionation desorption recombination (HDDR) Nd-Fe-B powder, doped with a low weight fraction of DyF3 nanoparticles, were investigated. Spark plasma sintering (SPS) was used to consolidate the recycled Nd-Fe-B powder blends containing 1, 2, and 5 wt.% of DyF3 grounded powder. Different post-SPS sintering thermal treatment conditions (600, 750, and 900 °C), for a varying amount of time, were studied in view of optimizing the magnetic properties and developing characteristic core-shell microstructure in the HDDR powder. As received, recycled HDDR powder has coercivity (HCi) of 830 kA/m, and as optimally as SPS magnets reach 1160 kA/m, after the thermal treatment. With only 1-2 wt.% blended DyF3, the HCi peaked to 1407 kA/m with the thermal treatment at 750 °C for 1 h. The obtained HCi values of the blend magnet is ~69.5% higher than the starting recycled HDDR powder and 17.5% higher than the SPS processed magnet annealed at 750 °C for 1 h. Prolonging the thermal treatment time to 6 h and temperature conditions above 900 °C was detrimental to the magnetic properties. About ~2 wt.% DyF3 dopant was suitable to develop a uniform core-shell microstructure in the HDDR Nd-Fe-B powder. The Nd-rich phase in the HDDR powder has a slightly different and fluorine rich composition i.e., Nd-O-F2 than in the one reported in sintered magnets (Nd-O-F). The composition of reaction zone-phases after the thermal treatment and Dy diffusion was DyF4, which is more abundant in 5 wt.% doped samples. Further doping above 2 wt.% DyF3 is ineffective in augmenting the coercivity of the recycled HDDR powder, due to the decomposition of the shell structure and formation of non-ferromagnetic rare earth-based complex intermetallic compounds. The DyF3 doping is a very effective single step route in a controlled coercivity improvement of the recycled HDDR Nd-Fe-B powder from the end of life magnetic products.

Electron microscopy and microanalysis of the fiber-matrix interface in monolithic silicone carbide-based ceramic composite material for use in a fusion reactor application.

A composite material made from continuous monolithic silicone carbide (SiC) fibers and a SiC-based matrix (SiC(f)/SiC), was prepared using a novel technique, i.e. adapted dip coating and infiltration of SiC fibers with a water suspension containing SiC particles and a sintering additive. This kind of material could be used in the first-wall blanket of a future fusion reactor. Using magnetron sputtering, the SiC fibers were coated with various thin layers (TiC, CrN, CrC, WC, DLC-diamond-like carbon) of the interface material by physical vapor deposition (PVD). Using scanning and transmission electron microscopy and microanalysis, detailed microstructural studies of the fiber-matrix interface were performed. Both samples, with coated and uncoated fibers, were examined under a load. The microcracks introduced by the Vickers indenter continued their path through the fibers, and thus caused the failure of the composite material, in the case of the uncoated fibers or deviated from their primary direction at the fiber-matrix interface in the case of the coated fibers.

The influence of surface modification on bacterial adhesion to titanium-based substrates.

This study examines bacterial adhesion on titanium-substrates used for bone implants. Adhesion is the most critical phase of bacterial colonization on medical devices. The surface of titanium was modified by hydrothermal treatment (HT) to synthesize nanostructured TiO2-anatase coatings, which were previously proven to improve corrosion resistance, affect the plasma protein adsorption, and enhance osteogenesis. The affinity of the anatase coatings toward bacterial attachment was studied by using a green fluorescent protein-expressing Escherichia coli (gfp-E. coli) strain in connection with surface photoactivation by UV irradiation. We also analyzed the effects of surface topography, roughness, charge, and wettability. The results suggested the dominant effects of the macroscopic surface topography, as well as microasperity at the surface roughness scale, which were produced during titanium machining, HT treatment, or both. Macroscopic grooves provided a preferential site for bacteria deposit within the valleys, while the microscopic roughness of the valleys determined the actual interaction surface between bacterium and substrate, resulting in an "interlocking" effect and undesired high bacterial adhesion on nontreated titanium. In the case of TiO2-coated samples, the nanocrystals reduced the width between the microasperities and thus added nanoroughness features. These factors decreased the contact area between the bacterium and the coating, with consequent lower bacterial adhesion (up to 50% less) in comparison to the nontreated titanium. On the other hand, the pronounced hydrophilicity of one of the HT-coated discs after pre-irradiation seemed to enhance the attachment of bacteria, although the increase was not statistically significant (p > 0.05). This observation may be explained by the acquired similar degree of wetting between gfp-E. coli and the coating. No correlation was found between the bacterial adhesion and the ζ-values of the samples in PBS, so the effect of surface charge was considered negligible in this study.

Enhanced osteogenesis on titanium implants by UVB photofunctionalization of hydrothermally grown TiO2 coatings.

Even though Ti-based implants are the most used materials for hard tissue replacement, they may present lack of osseointegration on the long term, due to their inertness. Hydrothermal treatment (HT) is a useful technique for the synthesis of firmly attached, highly crystalline coatings made of anatase titanium dioxide (TiO2), providing favorable nanoroughness and higher exposed surface area, as well as greater hydrophilicity, compared to the native amorphous oxide on pristine titanium. The hydrophilicity drops even more by photofunctionalization of the nanostructured TiO2-anatase coatings under UV light. Human mesenchymal stem cells exhibited a good response to the combination of the positive surface characteristics, especially in respect to the UVB pre-irradiation. The results showed that the cells were not harmed in terms of viability; even more, they were encouraged to differentiate in osteoblasts and to become osteogenically active, as confirmed by the calcium ion uptake and the formation of well-mineralized, bone-like nodule structures. In addition, the enrichment of hydroxyl groups on the HT-surfaces by UVB photofunctionalization accelerated the cell differentiation process and greatly improved the osteogenesis in comparison with the nonirradiated samples. The optimal surface characteristics of the HT-anatase coatings as well as the high potentiality of the photo-induced hydrophilicity, which was reached during a relatively short pre-irradiation time (5 h) with UVB light, can be correlated with better osseointegration ability in vivo; among the samples, the superior biological behavior of the roughest and most hydrophilic HT coating makes it a good candidate for further studies and applications.

Photoinduced properties of nanocrystalline TiO2-anatase coating on Ti-based bone implants.

The paper reports on the photoinduced properties of hydrothermally treated (HT) titanium used for bone implants. The anatase coatings composed of 30-100nm anatase crystals exhibited high photocatalytic activity and good photo-induced wettability, reaching a superhydrophilic state, despite the larger crystal dimensions than the previously reported optimal ones. These properties are due to a suitable combination of surface texture, roughness, thickness, crystal morphology and particle size, which allowed the two independent photo-induced phenomena to occur simultaneously. The results on caffeine degradation by photocatalysis and the prolonged effect (up to two weeks) of photo-induced wettability in dark suggested a possible applicability of the HT anatase coatings as bacteria-repelling surfaces for body implants, in favor of a better osseointegration in vivo.

Improvement to the Corrosion Resistance of Ti-Based Implants Using Hydrothermally Synthesized Nanostructured Anatase Coatings.

The electrochemical behavior of polycrystalline TiO2 anatase coatings prepared by a one-step hydrothermal synthesis on commercially pure (CP) Ti grade 2 and a Ti13Nb13Zr alloy for bone implants was investigated in Hank's solution at 37.5 °C. The aim was to verify to what extent the in-situ-grown anatase improved the behavior of the substrate in comparison to the bare substrates. Tafel-plot extrapolations from the potentiodynamic curves revealed a substantial improvement in the corrosion potentials for the anatase coatings. Moreover, the coatings grown on titanium also exhibited lower corrosion-current densities, indicating a longer survival of the implant. The results were explained by considering the effects of crystal morphology, coating thickness and porosity. Evidence for the existing porosity was obtained from corrosion and nano-indentation tests. The overall results indicated that the hydrothermally prepared anatase coatings, with the appropriate morphology and surface properties, have attractive prospects for use in medical devices, since better corrosion protection of the implant can be expected.

Long-term oxidization and phase transition of InN nanotextures.

The long-term (6 months) oxidization of hcp-InN (wurtzite, InN-w) nanostructures (crystalline/amorphous) synthesized on Si [100] substrates is analyzed. The densely packed layers of InN-w nanostructures (5-40 nm) are shown to be oxidized by atmospheric oxygen via the formation of an intermediate amorphous In-Ox-Ny (indium oxynitride) phase to a final bi-phase hcp-InN/bcc-In2O3 nanotexture. High-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy, electron energy loss spectroscopy and selected area electron diffraction are used to identify amorphous In-Ox-Ny oxynitride phase. When the oxidized area exceeds the critical size of 5 nm, the amorphous In-Ox-Ny phase eventually undergoes phase transition via a slow chemical reaction of atomic oxygen with the indium atoms, forming a single bcc In2O3 phase.

Dual purpose laser ablation-inductively coupled plasma mass spectrometry for pulsed laser deposition and diagnostics of thin film fabrication: preliminary study.

PLD (pulsed laser deposition) is an attractive technique to fabricate thin films with a stoichiometry reflecting that of the target material. Conventional PLD instruments are more or less black boxes in which PLD is performed virtually "blind", i.e. without having great control on the important PLD parameters. In this preliminary study, for the first time, a 213 nm Nd-YAG commercial laser ablation-inductively coupled plasma mass spectrometer (LA-ICPMS) intended for microanalysis work was used for PLD under atmospheric pressure and in and ex situ ICPMS analysis for diagnostics of the thin film fabrication process. A PLD demonstration experiment in a He atmosphere was performed with a Sm(13.8)Fe(82.2)Ta(4.0) target-Ta-coated silicon wafer substrate (contraption with defined geometry in the laser ablation chamber) to transfer the permanent magnetic properties of the target to the film. Although this paper is not dealing with the magnetic properties of the film, elemental analysis was applied as a means of depicting the PLD process. It was shown that in situ ICPMS monitoring of the ablation plume as a function of the laser fluence, beam diameter and repetition rate may be used to ensure the absence of large particles (normally having a stoichiometry somewhat different from the target). Furthermore, ex situ microanalysis of the deposited particles on the substrate, using the LA-ICPMS as an elemental mapping tool, allowed for the investigation of PLD parameters critical in the fabrication of a thin film with appropriate density, homogeneity and stoichiometry.