Copper is present in brake pads in the form of fibres, tough its suppression from pads\' formulations is already a trend compared to the suppression of asbestos in the 1980\'s. As a contribution to this challenging scenario, this work investigated the behaviour of mixture additions containing copper, zirconia, graphite and magnetite in dry sliding tribotests. Pin-on-disc tribotests with interfacial media addition were performed in order to contribute on the mission of understanding how Cu, graphite and ZrO2 particles act on the oxide transfer layer formation on dry sliding conditions. Thus describing some of the tribological properties that a possible replacement for copper in brake pads should mimic. Tests were performed at 23°C in air, 400°C in air and 400°C in N2. Nanoparticulate Cu, ZrO2 and micron-sized graphite were mixed in a Fe3O4 basedmatrix. The ZrO2 particles were incorporated to the mixtures by two mixing methods: manual mixing and high-energy ball milling. This study sought to explain the coefficient of friction (CoF) behaviour of these additions individually, as well as together, by correlating the CoF with comprehensive characterization of the oxide transfer layer. The transfer layer was characterized by means of scanning electron microscopy (SEM), Focused Ion Beam (FIB) and Transmission electron microscopy. Graphite containing mixtures displayed low average CoF values (0.23 to 0.31) due to selective transfer of graphite films to the first bodies\' tribosurfaces. Copper formed agglomerates and patches within the oxide transfer layer that were responsible for raising the CoF values at 23°C and acted as soft copper films at 400°C. The nanoparticulate addition of ZrO2 in the manual mixtures prevented the formation of Cu patches and larger agglomerates, promoting the formation of a smooth and compact oxide tribolayer, though graphite\'s selective transfer was still observed. / O cobre está presente em pastilhas de freio na forma de fibras e sua eliminação das formulações de pastilhas já é comparável aos esforços para a eliminação do amianto dos freios nos anos 1980\'s. Para contribuir nessa missão, esse trabalho investigou o comportamento, em ensaios tribológicos sem lubrificação com adição de misturas de cobre, zircônia, grafite e magnetita. Foram realizados ensaios pino x disco com adição de meio interfacial com o objetivo de contribuir na descrição da atuação do Cu, grafite e partículas de ZrO2 na formação de uma camada de óxido compacta em condições sem lubrificação. De forma a descrever propriedades tribológicas relevantes que um possível substituto do cobre deve mimetizar nas pastilhas de freio. Os ensaios foram realizados a 23°C em ar, 400°C em ar e 400°C em N2. Nanopartículas de Cu, ZrO2 (50 nm) e grafite micrométrico (20 µm) foram misturados em uma base de Fe3O4 nanoparticulado. As partículas de ZrO2 foram incorporadas às misturas, por dois métodos distintos, mistura manual, e moagem de bolas de alta energia. Este estudo procurou explicar os resultados de coeficiente de atrito (CoF) dessas adições, individualmente bem como em conjunto, correlacionando os resultados de coeficiente de atrito à extensa caracterização da camada de transferência. Esta última foi caracterizada por meio de microscopia eletrônica de varredura (SEM), feixe de íons focalizado (FIB) e microscopia eletrônica de transmissão (TEM). As misturas contendo grafite apresentaram os menores valores médios de CoF (0.23 to 0.31) devido à presença de filmes contínuos de grafite na camada de transferência. A adição de cobre formou aglomerados e placas na camada de transferência, que foram responsáveis tanto pelo aumento do CoF a 23°C, e agiram como filmes moles de cobre a 400°C. A adição de ZrO2 em misturas manuais preveniu a formação de aglomerados de Cu, auxiliando na formação de uma camada mais compacta, no entanto, não foi suficiente para prevenir a formação de filmes de grafite.

Carbon fibre reinforced ceramic composites (Cf/C-SiC) have been explored as lightweight and durable disc in a friction brake. This composite was manufactured through infiltration of liquid silicon into a Cf/C perform. It has heterogeneous microstructure, composed of three key phases, silicon carbide, Cf/C, and un-reacted residual silicon. The development of the transfer layer on the friction surface of Cf/C-SiC was studied through microstructural image registration of the surface after a range of braking stops on a laboratory-scale dynamometer test rig. When an organic pad was used as the counter face brake pad, it was found that a steady transfer layer was developed in silicon regions right after initial stops; in carbon-fibre/carbon (Cf/C) regions and most of the silicon carbide region, the friction surfaces were unsteady and any possible friction transfer layers were hardly built up. Large voids and cracks/crevices likely became pools to quickly and efficiently collect the transferred materials generated by the friction, but the compacts formed inside the pools were susceptible to be stripped off by further braking operation. Three types of friction surfaces were generalized: type I, the friction transfer layer had a steady relationship with the matrix and respectable longevity; type II, the transfer layer had an unstable relationship with the matrix and poor durability; type III, the friction transfer layer had a steady relationship with the matrix but short lifetime. After testing against organic pads under the laboratory scale dynamometer testing condition, the friction surface of each key phase in Cf/C-SiC composites disc was studied by transmission electron microscopy (TEM). It was found that the transfer layer developed on Si consists of fine particles of metal silicides, silicates and minerals. The substrate damage of Si was not observed, while the precipitates having high oxygen content were found in the substrate. Formation of an interfacial bonding between transfer layer and silicon substrate is believed to be the key factor for the formation of a stable transfer layer on Si. However, the interfacial bonding between transferred materials and SiC was not detected. Kinks are common features developed on the friction surface of SiC. The interface between carbon fibre and carbon matrix was experienced mechanical damage, in form of microcracks, and the transferred material was developed in the interface. Instead of transfer layer, a thin amorphous film, produced by friction induced amorphisation of carbon fibre, was developed on top of carbon fibre.