G. Giacometti

Raman spectroscopy investigation of the H content of heated hard amorphous carbon layers

We revisit here how Raman spectroscopy can be used to estimate the H content in hard hydrogenated amorphous carbon layers. The H content was varied from 2 at.% to 30 at.%, using heat treatments of a a-C:H, from room temperature to 1300 K and was determined independently using ion beam analysis. We examine the correlation of various Raman parameters and the consistency of their thermal evolution with thermo-desorption results. We identify a weak band at 860 cm-1 attributed to H bonded to C(sp2). We show that the HD/HG parameter (Height ratio between the D and G bands) is quasi-linear in the full range of H content and can thus be used to estimate the H content. Conversely, we show that the m/HG parameter (ratio between the photoluminescence background, m, and the height of the G band), often used to estimate the H content, should be used with care, first because it is sensitive to various photoluminescence quenching processes and second because it is not sensitive to H bonded to C(sp2).

Modelling of the micrometric erosion pattern observed on the Tore Supra limiter tiles

Recently, the surface of carbon fibre composite tiles of the toroidal pump limiter of Tore Supra has been analysed by scanning electron and atomic force microscopies. In regions where fibres are perpendicular to the surface, a specific erosion pattern has been observed. It is constituted of a striation oriented with an angle oblique with respect to the magnetic field. The characteristic wavelength of this structure is micrometric, and similar to the fibre size. Modelling has been undertaken to reproduce this micrometric pattern. It is shown to originate from the carbon composite structure, for which it has been found by measurement using laboratory plasma that the erosion rate of the fibres is different from that of the surrounding matrix. Modelling emphasizes the effect of the impinging flux angle distributions of deuterium ions and carbon impurities that are preliminarily determined from computation of the magnetic sheath. In the case of deuterium the sheath is shown to have little effect on the particle trajectories for the simulation parameters considered here, although when impurities are included the sheath deflection is significant. Furthermore this study shows how the fibre organization in the composite influences the striation direction and points out the importance of the angular dependence of the sputtering yield.

Structural analysis of eroded carbon fiber composite tiles of Tore Supra: insights on ion transport and erosion parameters

As part of the deuterium inventory in the Tore Supra project, a detailed structural analysis of the eroded tiles (carbon fiber composite tiles) of the main plasma-facing component of Tore Supra, the toroidal pump limiter, has been performed. It combines scanning electron microscopy, atomic force microscopy and Raman microscopy. A tile cross-section has been scanned, showing the eroded profile of the tile and allowing the net erosion rate to be determined. Ripples are observed on the surface of the eroded tiles and this pattern gives a clear indication of the ion flux direction. The height profile along the valleys indicates that the fibers are eroded faster than the matrix, the difference in the erosion rates probably originating from differences in microstructure.

Formation of thin tungsten oxide layers: characterization and exposure to deuterium

Thin tungsten oxide layers with thicknesses up to 250 nm have been formed on W surfaces by thermal oxidation following a parabolic growth rate. The reflectance of the layers in the IR range 2.5-16 mu m has been measured showing a decrease with the layer thickness especially at low wavelengths. Raman microscopy and x-ray diffraction show a nanocrystalline WO3 monoclinic structure. Low energy deuterium plasma exposure (11 eV/D+) has been performed inducing a phase transition, a change in the sample colour and the formation of tungsten bronze (DxWO3). Implantation modifies the whole layer suggesting a deep diffusion of deuterium inside the oxide. After exposure, a deuterium release due to the oxidation of DxWO3 under ambient conditions has been evidenced showing a reversible deuterium retention.

Raman microscopy investigation of beryllium materials

We report for the first time on the ability of Raman microscopy to give information on the structure and composition of Be related samples mimicking plasma facing materials that will be found in ITER. For that purpose, we investigate two types of material. First: Be, W, Be1W9, and Be5W5 deposits containing a few percents of D or N, and second: a Mo mirror exposed to plasma in the main JET chamber (in the framework of the first mirror test in JET with ITER-like wall). We performed atomic quantifications using ion beam analysis for the first samples. We also did atomic force microscopy. We found defect induced Raman bands in Be, Be1W9, and Be5W5 deposits. Molybdenum oxide has been identified showing an enhancement due to a resonance effect in the UV domain.

Multi-technique coupling for analysis of deuterium retention in carbon fiber composite NB31

This paper presents an extensive set of measurements from complementary surface analysis techniques performed for characterizing deuterium retention in carbon fiber composite Sepcarb®NB31 subsequently to a deuterium beam exposition: adsorption isotherm measurements and Hg porosimetry to characterize the porous network, coupled deuterium beam exposure and in situ µ-NRA analysis to follow the dynamics of the penetration of the retained deuterium in the material, TEM and Raman microscopy to investigate the change in the material structure induced by ion irradiation, and finally TPD to estimate the respective proportion of deuterium retained in the surface layer and in the bulk material. The parameters extracted from this set of characterizations are introduced in a 2D Monte Carlo model which couples the propagation of deuterium and eroded carbon atoms in a network of rectilinear pores and plasma–surface interaction parameters from the SRIM code. The simulations reproduce satisfactorily the main features of the measured deuterium concentration profile and behavior of the retained deuterium amount with incident fluence, validating the physical picture of deuterium retention in CFC as due to the simultaneous implantation of the incident ions in the few 10-nm-depth layer the closest to the surface and penetration of atoms deeper in the material (several tens of microns) through the pore network.