Lucile Joly-Pottuz

Accurate characterization of pure silicon-substituted hydroxyapatite powders synthesized by a new precipitation route

This paper presents a new aqueous precipitation method to prepare silicon-substituted hydroxyapatites Ca10(PO4)6-y(SiO4)y(OH)2-y(VOH)y (SiHAs) and details the characterization of powders with varying Si content up to y=1.25molmolSiHA(-1). X-ray diffraction, transmission electron microscopy, solid-state nuclear magnetic resonance and Fourier transform infrared spectroscopy were used to accurately characterize samples calcined at 400°C for 2h and 1000°C for 15h. This method allows the synthesis of monophasic SiHAs with controlled stoichiometry. The theoretical maximum limit of incorporation of Si into the hexagonal apatitic structure is y<1.5. This limit depends on the OH content in the channel, which is a function of the Si content, temperature and atmosphere of calcination. These results, particularly those from infrared spectroscopy, raise serious reservations about the phase purity of previously prepared and biologically evaluated SiHA powders, pellets and scaffolds in the literature.

Superlow friction of ta-C lubricated by glycerol: An electron energy loss spectroscopy study

Energy-filtering transmission electron microscopy (EFTEM) analysis coupled with the technique of samples preparation, focused ion beam, was used to study physical, chemical, and mechanical properties of diamond-like carbon coatings (DLCs). Two different coatings (ta-C and a-C:H) were investigated, presenting different tribological behaviors in a boundary lubrication regime with glycerol. Electron energy loss spectroscopy appears to be a very powerful technique to characterize such DLC coatings. Special attention was paid to the maximum energy of the plasmon peak, which was used to evaluate some physical and mechanical properties of DLC coatings (density, sp3∕sp2 ratio, hardness). For ta-C superlubric coating, EFTEM results show a rearrangement of the DLC bulk structure under the friction process. Typically, the transformation of sp3 carbon into sp2 carbon was clearly observed and permits a self-adaptation of the coating, allowing it to support shearing without any delamination in spite of important compre...

Improvements for imaging ceramics sintering in situ in ESEM

Sintering of green samples of alumina produced by ice‐templating was followed in situ in an environmental scanning electron microscope (ESEM) up to temperatures as high as 1375°C. These alumina samples with well‐defined architectures are of great interest in the field of materials science due to their high specific strength (especially in compression), low density and adaptable porosity. For the present study, they also have the advantage to exhibit an important topography, inducing interesting contrast when imaged in an ESEM. Improvements of the imaging conditions in the ESEM were essential to really follow the sintering process involving formation of necks between grains or shift of the centre of grains. This paper describes the improvements made and the results observed on the sintering process of alumina green samples processed by ice‐templating.

The Future of Boundary Lubrication by Carbon Coatings and Environmentally Friendly Additives

This paper presents a tiibological system that produces superlubricity under boundary lubrication conditions with extremely little wear. This system is a thin coaling of Diamond-Like-Carbon in a DLC friction pair lubricated with OH-containing additives. The DLC material is hydrogen-free tetrahedrally amorphous DLC (denoted as ta-C).

A global investigation into in situ nanoindentation experiments on zirconia: from the sample geometry optimization to the stress nanolocalization using convergent beam electron diffraction

Nanoindentation experiments inside a transmission electron microscope are of much interest to characterize specific phenomena occuring in materials, like for instance dislocation movements or phase transformations. The key points of these experiments are (i) the sample preparation and the optimization of its geometry to obtain reliable results and (ii) the choice of the transmission electron microscope observation mode, which will condition the type of information which can be deduced from the experiment. In this paper, we will focus on these two key points in the case of nanoindentation of zirconia, which is a ceramic material well known to be sensitive to stress because it can undergo a phase transformation. In this case, the information sought is the stress localization at the nanometre scale and in real time. As far as the sample preparation is concerned, one major drawback of nanoindentation inside a transmission electron microscope is indeed a possible bending of the sample occurring during compression, which is detrimental to the experiment interpretation (the stress is not uniaxial anymore). In this paper, several sample preparation techniques have been used and compared to optimize the geometry of the sample to avoid bending. The results obtained on sample preparation can be useful for the preparation of ceramics samples but can also give interesting clues and experimental approaches to optimize the preparation of other kinds of materials.

Superlubricity of Steel Surfaces in Presence of Polyhydric Alcohols

Anomalous low friction of hydrogen-free tetrahedral hybridized carbon (ta-C) coated surfaces lubricated by pure glycerol was observed at 80°C. In the presence of glycerol, the friction coefficient is below 0.01 at steady state, corresponding to so-called superlubricity regime. This new mechanism of superlow friction is attributed to easy glide on tribo-formed OH-terminated surfaces. In addition to the formation of OH-terminated surfaces but at a lower temperature, we show here some evidence that superlow friction of polyhydric alcohols could also be associated with tribo-induced degradation of glycerol, producing a nanometer-thick film containing organic acids and water. Second, we show novel outstanding superlubricity of steel surfaces directly lubricated by a solution of myo-inositol in glycerol at ambient temperature (25°C). For the first time, under boundary lubrication at high contact pressure, friction of steel is below 0.01 in the absence of any long chain polar molecules. Mechanism is still unknown but could be associated with friction-induced dissociation of glycerol and interaction with steel surface.Copyright