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.

A quick, easy and green water-based synthesis protocol involving coprecipitation of oxalates combined with hydrothermal treatment resulted in the crystallisation of nanostructured manganites at a relatively low temperature (180 °C). The subcritical hydrothermal approach was shown to play a key role in stabilising phases which are generally achieved at much higher temperatures and under harsher conditions, thus disclosing an exciting alternative for their synthesis. Through this mild wet chemistry approach, the compounds CuMnO₂, ZnMn₂O₄ and ZnMnO₃ were synthesised as nanocrystalline powders. Noticeably, the optimised route proved to be effective in stabilising the exotic polymorph cubic spinel ZnMnO₃ in pure form. This is particularly notable, as very few records concerning this compound are available in the literature. The compounds were fully characterised from compositional, structural, morphological and magnetic points of view.

In this study, graphitic carbon nitride (g-C₃N₄, labelled as gCN) was tested in the formulation of copper-free (Cu-free) friction mixtures, which are potentially interesting for brake pad manufacturing. Three formulations of friction composites were prepared starting from a common Cu-free master batch: (i) without graphite, (ii) with graphite and (iii) with gCN. The mixtures were pressed in the form of pins by hot-press moulding. The friction-wear performance of the prepared pins was investigated using a pin-on-disc (PoD) test at room temperature (RT), high temperature (HT) (400 °C) and, again, at room temperature (H-RT). The values of the friction coefficient (µ) for the composites with gCN (or graphite) were as follows: (i) RT test, µ_RT = 0.52 (0.47); (ii) HT test, µ_HT = 0.37 (0.37); (iii) RT after the HT tests, µ_H-RT = 0.49 (0.39). With respect to wear resistance, the samples with graphite performed better than the samples without this solid lubricant. To the best of our knowledge, this is the first report regarding the evaluation of the role of gCN in friction composites designed for automotive brake lining applications. The results indicate the main role of gCN as a soft abrasive.

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.