Multiwavelength Raman spectroscopy analysis of a large sampling of disordered carbons extracted from the Tore Supra tokamak

Disordered carbon often exhibit a complex Raman spectrum, with four to six components. Here, a large variety of disordered carbons, forming a collection of samples with a great variety of structures, are analysed using multi-wavelength Raman microscopy (325.0, 514.5, 785.0 nm). They allow us to extend Raman behaviour known for nano-crystalline graphite to amorphous carbons, (dependence with the excitation wavelength) and other known for amorphous carbons to nano-crystalline graphite, (differentiation of the smallest cluster size probed using different excitation wavelengths). Experimental spectra were compared to simulated spectra, built using known laws, to evidence a new source of broadening

Thermal stability and long term hydrogen/deuterium release from soft to hard amorphous carbon layers analyzed using in-situ Raman spectroscopy. Comparison with Tore Supra deposits

The thermal stability of 200 nm thick plasma enhanced chemical vapor deposited a-C:H and a-C:D layers ranging from soft to hard layers has been studied and compared to that of deposits collected on the Tore Supra tokamak plasma facing components by means of in-situ Raman spectroscopy. Linear ramp heating and long term isotherms (from several minutes to 21 days) have been performed and correlations between spectrometric parameters have been found. The information obtained on the sp 2 clustering has been investigated by comparing the G band shift and the 514 nm photon absorption evolution due to the thermal treatment of the layer. The effects of isotopic substitution have also been investigated.Comment: appears in Thin Solid Films, Elsevier, 201

Identification of BeO and BeOxDy in melted zones of the JET Be limiter tiles: Raman study using comparison with laboratory samples

Beryllium oxide (BeO) and deuteroxide (BeOxDy) have been found on the melted zone of a beryllium tile extracted from the upper dump plate of JET-ILW (2011-2012 campaign). Results have been obtained using Raman microscopy, which is sensitive to both the chemical bond and crystal structure, with a micrometric lateral resolution. BeO is found with a wurtzite crystal structure. BeOxDy is found as three different types which are not the beta-phase but behaves as molecular species like Be(OD)(2), O(Be-D)(2) and DBeOD. The presence of a small amount of trapped D2O is also suspected. Our results therefore strongly suggest that D trapping occurs after melting through the formation of deuteroxides. The temperature increase favors the formation of crystal BeO which favors deuterium trapping through OD bonding.EURATOM 63305

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)

The effect of beryllium oxide on retention in JET ITER-like wall tiles

Preliminary results investigating the microstructure, bonding and effect of beryllium oxide formation on retention in the JET ITER-like wall beryllium tiles, are presented. The tiles have been investigated by several techniques: Scanning Electron Microscopy (SEM) equipped with Energy Dispersive X-ray (EDX), Transmission Electron microscopy (TEM) equipped with EDX and Electron Energy Loss Spectroscopy (EELS), Raman Spectroscopy and Thermal Desorption Spectroscopy (TDS). This paper focuses on results from melted materials of the dump plate tiles in JET. From our results and the literature, it is concluded, beryllium can form micron deep oxide islands contrary to the nanometric oxides predicted under vacuum conditions. The deepest oxides analyzed were up to 2-micron thicknesses. The beryllium Deuteroxide (BeOxDy) bond was found with Raman Spectroscopy. Application of EELS confirmed the oxide presence and stoichiometry. Literature suggests these oxides form at temperatures greater than 700 °C where self-diffusion of beryllium ions through the surface oxide layer can occur. Further oxidation is made possible between oxygen plasma impurities and the beryllium ions now present at the wall surface. Under Ultra High Vacuum (UHV) nanometric Beryllium oxide layers are formed and passivate at room temperature. After continual cyclic heating (to the point of melt formation) in the presence of oxygen impurities from the plasma, oxide growth to the levels seen experimentally (approximately two microns) is proposed. This retention mechanism is not considered to contribute dramatically to overall retention in JET, due to low levels of melt formation. However, this mechanism, thought the result of operation environment and melt formation, could be of wider concern to ITER, dependent on wall temperatures.EUROfusion 63305

Raman micro-spectroscopy as a tool to measure the absorption coefficient and the erosion rate of hydrogenated amorphous carbon films heat-treated under hydrogen bombardment

We present a fast and simple way to determine the erosion rate and absorption coefficient of hydrogenated amorphous carbon films exposed to a hydrogen atomic source based on ex-situ Raman micro-spectroscopy. Results are compared to ellipsometry measurement. The method is applied to films eroded at different temperatures. A maximum of the erosion rate is found at ~ 450 {\degree}C in agreement with previous results. This technique is suitable for future quantitative studies on the erosion of thin carbonaceous films, especially of interest for plasma wall interactions occurring in thermonuclear fusion devices

Long Term H-Release from Amorphous Carbon Evidenced by in Situ Raman Microscopy under Isothermal Heating

We study the kinetics of the H release from plasma-deposited hydrogenated amorphous carbon films under isothermal heating at 450, 500 and 600 {\degree}C for long times up to several days using in situ Raman microscopy. Four Raman parameters are analyzed. They allow the identification of different processes such as the carbon network reorganization and the H release from sp3 or sp2 carbon atoms and the corresponding timescales. Carbon reorganization with aromatization and loss of sp3 hybridization occurs first in 100 minutes at 500 {\degree}C. The final organization is similar at all investigated temperatures. Full H release from sp3 carbon occurs on a longer timescale of about 10 hours while H release from sp2 carbon atoms is only partial, even after several days. All these processes occur more rapidly with higher initial H content, in agreement with what is known about the stability of these types of films. A quantitative analysis of these kinetics studies gives valuable information about the microscopic processes at the origin of the H release through the determination of activation energies

Raman study of CFC tiles extracted from the toroidal pump limiter of Tore Supra

International audienceThe structure of six tiles extracted from the erosion and deposition zones (thin and thick deposition) of the Tore Supra toroidal pump limiter (TPL) have been analysed in the framework of the DITS campaign using micro-Raman spectroscopy. This post-mortem analysis gives information on both carbon structure and D content. We have found that the carbon structure is most often similar to that of plasma-deposited hard amorphous carbon layers. The role of the surface temperature during the discharge in the D content is investigated: in all locations where the temperature does not reach more than 500°C the D content seems to be roughly uniform with D/D+C ≈ 20%

Raman microscopy to characterize plasma-wall interaction materials: from carbon era to metallic walls

Plasma-wall interaction in magnetic fusion devices is responsible for wall changes and plasma pollution with major safety issues. It is investigated both in situ and ex situ, especially by realizing large scale dedicated post-mortem campaigns. Selected parts of the walls are extracted and characterized by several techniques. It is important to extract hydrogen isotopes, oxygen or other element content. This is classically done by ion beam analysis and thermal desorption spectroscopy. Raman microscopy is an alternative and complementary technique. The aim of this work is to demonstrate that Raman microscopy is a very sensitive tool. Moreover, if coupled to other techniques and tested on well-controlled reference samples, Raman microscopy can be used efficiently for characterization of wall samples. Present work reviews long experience gained on carbon-based materials demonstrating how Raman microscopy can be related to structural disorder and hydrogen retention, as it is a direct probe of chemical bonds and atomic structure. In particular, we highlight the fact that Raman microscopy can be used to estimate the hydrogen content and bonds to other elements as well as how it evolves under heating. We also present state-of-the-art Raman analyses of beryllium- and tungsten-based materials, and finally, we draw some perspectives regarding boron-based deposits.</p