The increasing interest in the emission from the disc brake system poses new challenges for the characterization approaches used to investigate the particles emitted from the wearing out of the relevant tribological systems. This interest stems from different factors. In the first place, a thorough characterization of brake wear particles is important for a complete understanding of the active tribological mechanisms, under different testing and servicing conditions. This information is an important prerequisite not only for the general improvement of brake systems, but also to guide the development of new materials for discs and brake pads, responding better to the specific requirements, including not only performance, but also the emission behavior. In this review paper, the main material characterization protocols used for the analyses of the brake wear products, with particular regard for the airborne fraction, are presented. Reliable results require investigating the fine and ultrafine particles as concerns their composition together with their structural and microstructural aspects. For this reason, in general, multi-analytical protocols are very much recommended.

Encapsulation is a valuable strategy to protect and deliver anthocyanins (ACNs), phenolic compounds with outstanding antioxidant capacity but limited stability. In this study, coacervation was used to encapsulate an ACN-rich red cabbage extract (RCE). Two agri-food by-product polymers, whey protein isolate (WPI) and apple high-methoxyl pectin (HMP), were blended at pH 4.0 in a specific ratio to induce the formation of nanoparticles (NPs). The process optimisation yielded a monodispersed population (PDI < 0.200) of negatively charged (−17 mV) NPs with an average diameter of 380 nm. RCE concentration influenced size, charge, and antioxidant capacity in a dose-dependent manner. NPs were also sensitive to pH increases from 4 to 7, showing a progressive breakdown. The encapsulation efficiency was 30%, with the retention of ACNs within the polymeric matrix being influenced by their chemical structure: diacylated and/or C3-triglucoside forms were more efficiently encapsulated than monoacylated C3-diglucosides. In conclusion, we report a promising, simple, and sustainable method to produce monodispersed NPs for ACN encapsulation and delivery. Evidence of differential binding of ACNs to NPs, dependent on specific acylation/glycosylation patterns, indicates that care must be taken in the choice of the appropriate NP formulation for the encapsulation of phenolic compounds.

Transmission electron microscopy is a powerful experimental tool, very effective for the complete characterization of nanocrystalline materials by employing a combination of imaging, spectroscopy and diffraction techniques. Electron powder diffraction (EPD) pattern fingerprinting in association with chemical information from spectroscopy can be used to deduce the identity of the crystalline phases. Furthermore, EPD has similar potential to X-ray powder diffraction (XRPD) for extracting additional information regarding material specimens, such as microstructural features and defect structures. The aim of this paper is to extend a full-pattern fitting procedure, broadly used for analysing XRPD patterns, to EPD. The interest of this approach is twofold: in the first place, the relatively short times involved with data acquisition allow one to speed up the characterization procedures. This is a particularly interesting aspect in the case of metastable structures or kinetics studies. Moreover, the reduced sampling volumes involved with electron diffraction analyses can better reveal surface alteration layers in the analysed specimen which might be completely overlooked by conventional bulk techniques. The first step forward to have an effective application of the proposed methodology concerns establishing a reliable calibration protocol to take into correct account the instrumental effects and thus separate them from those determined by the structure, microstructure and texture of the analysed samples. In this paper, the methodology for determining the instrumental broadening of the diffraction lines is demonstrated through a full quantitative analysis based on the Rietveld refinement of the EPD. In this regard, a CeO₂ nanopowder reference specimen has been used. The results provide indications also on the specific features that a good calibration standard should have.

Press hardening steel standardly relies on titanium microalloying for protecting boron from being tied up by residual nitrogen. This practice safeguards the hardenability effect of boron during die quenching. More recently, additional microalloying elements were added to press hardening steel to further improve properties and service performance. Niobium was found to induce microstructural refinement, leading to better toughness, bendability, and hydrogen embrittlement resistance. In that respect, niobium also extends the operating window of the press hardening process. Vanadium microalloying has been proposed to provide hydrogen trapping by its carbide precipitates. A recently developed press hardening steel employs all three microalloying elements in an attempt to further enhance performance. The current study analyses the microstructure of such multiple microalloyed press hardening steel, and compares it to the standard grade. Particularly, the effect of various heat treatments is investigated, indicating that the multiple microalloyed steel is more resistant against grain coarsening. TEM analysis is used to identify the various particle species formed in the steels, to track their formation, and to determine their size distributions. Nanosized microalloy carbide particles typically comprise a mixed composition involving niobium, titanium, and vanadium. Furthermore, these precipitates are incoherent to the matrix. Regarding tensile properties, it is found that the multiple microalloyed press hardening steel is superior to the standard grade.

Refractory high entropy alloys have shown potential to be developed as structural materials for elevated temperature applications. In the present research, the multielement alloy Fe2TiVZrW0.5 was produced by high-energy ball milling of elemental powders in the air to promote the formation of reinforcing oxide and nitride particles followed by spark plasma sintering consolidation. The sintering temperature was optimized to achieve a full-density material that was characterized from the microstructural and mechanical points of view. Hardness and KIC were measured in the as-sintered condition as well as after thermal treatment at 1100 °C. TEM observations showed the presence of a fine distribution of ZrO₂ and Ti(V)-N in the microstructure mainly constituted by the bcc Fe-V and Fe-V-W phases. The fine distribution of ceramic particles in a metallic multielement matrix is responsible for the consistent hardness and thermal stability of this alloy.

In powder metallurgy (PM), the compaction step is fundamental to determining the final properties of the sintered components. The deformation and defectiveness introduced in the powder material during uniaxial die compaction can be correlated to the activation and enhancement of the dislocation pipe diffusion, a lattice diffusion mechanism during the sintering process. Its coefficient depends on the dislocation density. The powder particles are mostly deformed along the direction of the compaction (longitudinal direction) rather than along the compaction plane; consequently, the contact areas perpendicular to the direction of the compaction present a higher density of dislocations and lattice defects. This high density intensifies the shrinkage along the direction of compaction. To demonstrate the influence of uniaxial cold compaction on the material’s stress state the powder particles and their contacts were modeled using spheres made of pure copper. These spheres are compacted in a die at different pressures to better analyze the system’s response at the grade of deformation and the consequent influence on the material’s behavior during the sintering. In the different zones of the sphere, the micro-hardness was measured and correlated to the concentration of dislocations using the model for indentation size effect (ISE). After the compaction, the spheres were more deformed along the longitudinal than the transversal direction. The results obtained using hardness indentation show differences in the dislocation density between the undeformed and deformed spheres and, in the case of the compacted sphere, between the contact area along the longitudinal and the transversal direction.