Use of a nanoindentation fatigue test to characterize the ductile-brittle transition

When considering grinding of minerals, scaling effect induces competition between plastic deformation and fracture in brittle solids. The competition can be sketched by a critical size of the material, which characterizes the ductile-brittle transition. A first approach using Vickers indentation gives a good approximation of the critical size through an extrapolation from the macroscopic to the microscopic scales. Nanoindentation tests confirm this experimental value. According to the grain size compared to the indent size, it can reasonably be said that the mode of damage is deformation-induced intragranular microfracture. This technique also enables to perform cyclic indentations to examine calcite fatigue resistance. Repeated loadings with a nanoindenter on CaCO3 polycrystalline samples produce cumulative mechanical damage. It is also shown that the transition between ductile and brittle behaviour depends on the number of indentation cycles. The ductile domain can be reduced when the material is exposed to a fatigue process.Comment: Journal of European Ceramic Society accept\'e pour publication (2008) sous-press

Adhesion forces due to nano-triboelectrification between similar materials

Contact electrification and triboelectrification are well-known in the case of dissimilar materials, however the case of charge exchange during friction between nominally identical insulating materials is less documented. We experimentally investigated the triboelectrification between two smooth monocrystalline α-Al 2O 3 (sapphire) antagonists by surface force measurements with a Surface Force Apparatus (SFA). The force between a sphere and a plane, both in sapphire, was measured as a function of the sphere-plane distance D, before and after nano-friction tests, under dry argon atmosphere. Respective contributions of van der Waals, water meniscus and electrostatic forces were determined. The estimated Hamaker constant was in good agreement with the Lifshitz theory, and the dominant meniscus attraction at low separation could be overcome with small radius sphere. We demonstrated that electrostatic forces were generated by the nano-friction test and we quantified the adhesion that results from this contact-electrification. In the first stage of the unloading process, the short range electrostatic force was found to vary both with time and distance D. Experimental results were correlated with surface densities of mobile charges on the two surfaces, and the time-dependence was related to classical surface transport phenomena on alumina surfaces

Effets de la génération, de l'injection et du piégeage des charges électriques sur les propriétés des isolants

The results presented in this report are first mainly related to the study of the generation, the injection, the transport, and the trapping of electrical charges in insulators. The aim of this work is to understand the mechanisms of creation (or injection), propagation and storage of the electrical charges thanks to the "Mirror" (SEMM) and Induced Current (ICM) Methods performed in a Scanning Electron Microscope. Secondly the influence of these electrical charges on various properties such as the friction, the adhesion, or the breakdown strength of the insulating samples has been put in evidence. The methods of charging characterization have been coupled with other experimental set-ups such as Surface Force Apparatus, and the appropriate models and simulations have been developed to interpret the experimental results.Les travaux de recherche exposés dans ce mémoire concernent principalement l'étude des phénomènes de génération, de transport et de piégeage des charges électriques dans les isolants, ainsi que leur influence sur les propriétés (frottement, adhésion, tenue au claquage...) de ces matériaux. Le but est d'accéder à la compréhension des mécanismes d'apparition, de propagation, de stockage et de déstockage des charges dans des matériaux divers, par l'intermédiaire d'une méthode de caractérisation originale, "la méthode miroir", par son couplage avec d'autres appareillages (machine à force de surface...) et en développant les modèles ou outils de simulations approprié

Carbon nanotube-based composites and production and applications thereof

Title composite material is composed of 0.01-99 wt.% carbon nanotubes, 0-99.9 wt.% polymer (P1) selected from poly(alkyl acrylate), polystyrene, polyvinyl chloride, chlorinated polyvinyl chloride, polyvinylidene fluoride, PMMA, polycarbonates, polyamides, polyesters, polylactones, polyepoxides, polyimines, polyphosphazenes, polyolefins, polybutadienes, polyvinyl acetate, polyvinyl alc., polyketone, and polyurethanes, and a block copolymer having ≥1 block bearing ionic or ionizable functions and a block that is compatible with P1. The compatibilizer prepd. by controlled radical polymn. can control and optimize the interfacial interactions and thus to obtain a stable composite material that can be used in paints, coatings, antistatic materials, thermosets, and thermoplastics. Thus, carbon nanotubes and acrylic acid were dispersed in 1,4-dioxane and polymd. using alkoxyamine as initiator, followed by introducing a second monomer, Me acrylate, to provide a block copolymer

Electrical charges and tribology of insulating materials.

International audienceElectrical charges generation occurring during contact and friction of insulating materials has been identified for a long time. However the contribution of these electrical charges to the friction behaviour is usually neglected in the energetical balances. Based on published results and on our own experimental results on the ability of the dielectric materials to trap charges, we show in this study that the interaction energy during friction depends markedly on these trapped charges. Eventually, we propose the complementary use of the "mirror " method and of surface forces measurements to obtain a quantitative evaluation of this contribution. dielectric behaviour / friction / triboelectrification / interfacial interactions / surface free energy / space charge / surface force

Alumina based ceramics for high-voltage insulation

International audienceDielectric breakdown constitutes an important limitation in the use of insulating materials under high-voltage since it can lead to the local fusion and sublimation of the insulator. The role of electrical charge transport and trapping in alumina ceramics on their resistance to this catastrophic phenomenon is studied in this work. In polycrystalline materials, the interfaces between the various phases play a main role because they constitute potential sites for the trapping of electrical charges. The density and the nature of these interfaces can be controlled by the way of the microstructure parameters. So, the aim of the present paper is to highlight the influence of average grain size and intergranular phase crystallization rate on the ability of polycrystalline alumina materials to resist to dielectric breakdown. Thus, it is shown that the control of the process conditions (sintering aids content, powder grain size and thermal cycle) makes it possible to change not only the density (by the average grain size) but also the nature (by the crystallization or not of anorthite) of the grain boundaries. On one hand, at room temperature a high density of interfaces, due to low grain size and highly crystallized intergranular phase, leads to a high dielectric strength. On the other hand, at higher temperature (250 degrees C), the presence of vitreous intergranular phase makes it possible to delay breakdown. That behaviour is explained thanks to charge transport and trapping characterizations

Adhesion forces due to nano-triboelectrification between similar materials

International audienceContact electrification and triboelectrification are well-known in the case of dissimilar materials, however the case of charge exchange during friction between nominally identical insulating materials is less documented. We experimentally investigated the triboelectrification between two smooth monocrystalline α-Al 2O 3 (sapphire) antagonists by surface force measurements with a Surface Force Apparatus (SFA). The force between a sphere and a plane, both in sapphire, was measured as a function of the sphere-plane distance D, before and after nano-friction tests, under dry argon atmosphere. Respective contributions of van der Waals, water meniscus and electrostatic forces were determined. The estimated Hamaker constant was in good agreement with the Lifshitz theory, and the dominant meniscus attraction at low separation could be overcome with small radius sphere. We demonstrated that electrostatic forces were generated by the nano-friction test and we quantified the adhesion that results from this contact-electrification. In the first stage of the unloading process, the short range electrostatic force was found to vary both with time and distance D. Experimental results were correlated with surface densities of mobile charges on the two surfaces, and the time-dependence was related to classical surface transport phenomena on alumina surfaces

Relationships between dielectric breakdown resistance and charge transport in alumina materials—Effects of the microstructure

International audienceDielectric breakdown is the main cause of insulator degradation. Breakdown strength strongly depends on materials microstructure (grain size, grain boundaries nature,...) [Liebault, J., Vallayer, J., Goeuriot, D., Tréheux D., Thévenot, F., How the trapping of charges can explain the dielectrics breakdown performance of alumina ceramics, J. Eur. Ceram. Soc., 2001, 21, 389–397; Si Ahmed, A., Kansy, J., Zarbout, K., Moya, G., Liebault, J., Goeuriot, D., Microstructural origin of the dielectric breakdown strength in alumina: a study by positron lifetime spectroscopy, J. Eur. Ceram. Soc., 2005, 25, 2813–2816]. The experimental study of these materials behaviour towards charge injection was performed by the scanning electron microscopy mirror effect (SEMME) method. It allows to measure the amount of injected charges finally trapped in the insulator. In order to explain the experimental results, we developed an iterative computer simulation of the self-consistent charge transport in bulk alumina samples during electron beam irradiation, based on a new flight-drift model (FDM). Ballistic and drift electron and hole transport as well as their recombination, trapping and detrapping (due to temperature and electric field) are taken into account. As a main result the time dependent secondary electron emission rate and the spatial distributions of currents, charges, field and potential are obtained. The analysis of these two kinds of results allowed us to identify the effect of the microstructure on the behaviour of the injected charges in the insulator and then to propose some mechanisms depending on the temperature leading to a good dielectric breakdown resistance. Indeed, at room temperature a huge localisation of charges limits further injection into the sample that permits to delay breakdown. On the other hand, when the temperature increases, the efficiency of the charge spreading behaviour is improved, leading to a higher dielectric breakdown strength

Selfconsistent electrical charging in insulators

Publié suite au congrès : 9th Electroceramics Congress Cherbourg, FRANCE, MAY 31-JUN 06, 2004International audienceA Monte Carlo program based on acoustic and optical phonon scattering as well as on impact ionisation of valence band electrons has advantages in description of very low energy electron scattering (in eV and meV regions) and is aimed especially to wide gap dielectrics and insulators. Thus, the rapid relaxation and the ballistic transport of excited electrons within the conduction band of a wide gap insulator occurs over femtoseconds. The field-dependent transport and trapping parameters allow us to model the selfconsistent charge transport and charging-up of SiO2 thin layers as well as bulk Al2O3 samples during electron bombardment. The resulting distributions of currents, charges and electric fields within these samples explain, e.g. the phenomena of field-enhanced and field-blocked secondary electron emission. In order to prove the accessible quantity of the surface charging-up potential we have chosen the X-ray bremsstrahlung (BS) spectra, i.e. the shift of the short wavelength threshold due to the negative surface potential V0 and respective retarding of the incident electron beam. This effect is demonstrated for a 3 mm bulk Al2O3 sample and E0 = 30 keV electron beam irradiation resulting in a huge negative surface potential of V0exp = -17 kV