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.

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.

Dry sliding wear tests and corresponding particulate matter (PM) analysis were conducted on a newly developed SiC-graphite-based composite friction material, paired with two types of HVOF counterface/discs: WC-CoCr and WC-FeCrAlY coatings, with a conventional martensitic stainless steel counterface as a reference. The trials were conducted on a pin-on-disc testing equipment at room temperature and a constant sliding velocity and contact pressure of 7 m/s and 0.5 MPa, respectively. The coefficient of friction (CoF) curves with the uncoated disc exhibited considerable fluctuations. On the other hand, the coated discs featured an increase in the CoF at the beginning of the tests, followed by either a continuous reduction until the end of the testing duration or the attainment of a steady state regime. The pin wear and emissions with both coatings were appreciably lower when compared to the trials with the uncoated disc. The evaluation of the friction layer observed a significant contribution of the counterface for all the pairings. The PM analysis was conducted on the particles that were lying in the range of 10 μm and 2.5 μm on a scanning electron microscope (SEM), and particles from 2.5 μm and 1 μm on transmission electron microscope (TEM), with an emphasis on the particles that were detached from the pin surface and friction layer to explain the wear mechanisms for each pairing. Through this, the need for the proper selection of both friction material and counterface to avoid the emission of harmful compounds in the environment was highlighted.

Nanocrystalline (NC) materials have widespread industrial usage. X-ray and neutron diffraction techniques are primary tools for studying the structural and microstructural features of NC materials. Selected area electron diffraction (SAED) patterns collected using a transmission electron microscope (TEM) on polycrystalline nanostructured materials, featuring nested rings, that are analogous to Debye–Scherrer patterns, possess similar potentials to aid materials characterisation. The utility of SAED patterns is further enhanced by the possibility of applying crystallographic approaches, like full pattern fitting procedures, based on Rietveld refinement algorithms, enabling the evaluation of material features, such as crystallite size, lattice distortions, defect structures, and the presence of secondary phases even from very small volume scale. In this paper, we have discussed the possibilities afforded by a Rietveld code applied to SAED patterns of NC materials, including the mathematical implementation of the two-beam dynamical correction model in MAUD software (version 2.9995), and a critical discussion of the results obtained on different NC materials.