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Compact and defect-free high melting point oxide strengthened metallic matrix configurations are promising to resolve the hydrogen permeation and brittleness issues relevant to the fusion research community. Previous studies on oxide addition to metallic matrix demonstrated a mitigation in brittleness behavior, while deposition techniques and material configurations are still to be investigated. Thus, here, we report the structural, morphological, and mechanical characterization of metal-oxides thin layers co-deposited by radio frequency (RF)and direct current (DC) magnetron sputtering. A total of six configurations were deposited such as single thin layers of oxides (Al2O3, Er2O3) and co-deposition configurations as metal-oxides (W, Be)—(Al2O3, Er2O3). The study of films roughness by atomic force microscopy (AFM) method show that for Al2O3 metallic-oxides is increased to an extent that could favor gaseous trapping, while co-depositions with Be seem to promote an increased roughness and defects formation probability compared to W co-depositions. Lower elastic modulus on metal-oxide co-depositions was observed, while the indentation hardness increased for Be and decreased for W matrix configurations. These outputs are highly relevant for choosing the proper compact and trap-free configuration that could be categorized as a permeation barrier for hydrogen and furtherly studied in laborious permeation yield campaigns.

Beryllium-tungsten 2 μm thick layers were co-deposited on molybdenum, graphite and silicon substrates in a reactive argon-deuterium/argon-deuterium-nitrogen gas mixture by means of combining multi-pulse High Power Impulse Magnetron Sputtering and Direct Current Magnetron Sputtering techniques. The elemental composition and thickness of the layers were well controlled during the deposition process. Structural and chemical investigations were undertaken by means of X-ray diffraction and Rutherford backscattering methods. The results showed a change in the samples structure with the adding of nitrogen into the sputtering gas mixture, evidenced by the appearance of W 2 N peaks in the diffraction patterns. The RBS showed in-depth uniformity of beryllium and tungsten concentrations for the deposited coatings. In order to investigate the deuterium retention mechanisms and to make an assessment of the deuterium inventory, thermal desorption spectrometry was performed. The deuterium desorption spectra for the batch of samples obtained with nitrogen showed an obvious behaviour of shifting to higher temperatures. This behaviour may be related to the nitrogen desorption.

Cleaning techniques for metallic first mirrors are needed in more than 20 optical diagnostic systems from ITER to avoid reflectivity losses. Plasma sputtering is considered as one of the most promising techniques to remove deposits coming from the main wall (mainly beryllium and tungsten). Previous plasma cleaning studies were conducted on mirrors contaminated with beryllium and tungsten where argon and/or helium were employed as process gas, demonstrating removal of contamination and recovery of optical properties. Still, both above-mentioned process gases have a non-negligible sputtering yield on mirrors. In this work, we explored the possibility to use a sputter gas having a small impact on mirrors while being efficient on Be deposits, e.g. deuterium. Two sputtering regimes were studied, on laboratory deposits as well as on mirrors exposed in JET-ILW, namely physical sputtering (220 eV ion energy) and chemically assisted physical sputtering (60 eV ion energy) using capacitively coupled plasma with radio frequency. The removal of Be and mixed Be/W contaminants, as well as the recovery of reflectivity, was achieved when deuterium was employed at 220 eV while cleaning at 60 eV was only fully efficient on laboratory beryllium deposits. On mirrors exposed in JET-ILW, the situation is more complex due to the presence of tungsten in the contaminant film, leading to the formation of a tungsten enriched surface that is not easily sputtered, especially at 60 eV.

This work is focused on the structural and morphological investigations of polyaniline and poly(o-anisidine) polymers generated in a direct current glow discharge plasma, in the vapors of the monomers, without a buffer gas, using an oblique angle-positioned substrate configuration. By atomic force microscopy and scanning electron microscopy we identified the formation of worm-like interlinked structures on the surface of the polyaniline layers, the layers being compact in the bulk. The poly(o-anisidine) layers are flat with no kind of structures on their surfaces. By Fourier transform infrared spectroscopy we identified the main IR bands characteristic of polyaniline and poly(o-anisidine), confirming that the polyaniline chemical structure is in the emeraldine form. The IR band from 1070 cm-1 was attributed to the emeraldine salt form of polyaniline as an indication of its doping with H⁺. The appearance of the IR band at 1155 cm-1 also indicates the conducting protonated of polyaniline. The X-ray diffraction revealed the formation of crystalline domains embedded in an amorphous matrix within the polyaniline layers. The interchain separation length of 3.59 A is also an indicator of the conductive character of the polymers. The X-ray diffraction pattern of poly(o-anisidine) highlights the semi-crystalline nature of the layers. The electrical conductivities of polyaniline and poly(o-anisidine) layers and their dependence with temperature are also investigated.

Reduced activation ferritic and martensitic steel like EUROFER (9Cr-1W) are considered as potential structural materials for the first wall of the future next-generation DEMOnstration Power Station (DEMO) fusion reactor and as a reference material for the International Thermonuclear Experimental Reactor (ITER) test blanket module. The primary motivation of this work is to study the re-deposition of the main constituent materials of EUROFER, namely tungsten (W), iron (Fe), and chromium (Cr), in a DEMO type reactor by producing and analyzing complex WxCryFe1&minus, x&minus, y layers. The composite layers were produced in laboratory using the thermionic vacuum arc (TVA) method, and the morphology, crystalline structure, elemental composition, and mechanical properties were studied using scanning electron microscopy (SEM), X-ray diffraction (XRD), micro-X-ray fluorescence (micro-XRF), and glow discharge optical emission spectrometry (GDOES), as well as nanoindentation and tribology measurements. The results show that the layer morphology is textured and is highly dependent on sample positioning during the deposition process. The formation of polycrystalline WxCryFe1&minus, y was observed for all samples with the exception of the sample positioned closer to Fe anode during deposition. The crystalline grain size dimension varied between 10 and 20 nm. The composition and thickness of the layers were strongly influenced by the in-situ coating position, and the elemental depth profiles show a non-uniform distribution of Fe and Cr in the layers. The highest hardness was measured for the sample positioned near the Cr anode, 6.84 GPa, and the lowest was 4.84 GPa, measured for the sample positioned near the W anode. The tribology measurements showed an abrasive sliding wear behavior for most of the samples with a reduction of the friction coefficient with the increase of the normal load.

Since the largest area of the JET first wall is composed of beryllium, it is expected that nuclear fuel is largely retained in beryllium-based co-deposits with low amounts of carbon. Co-deposited layers obtained in the laboratory, with similar stoichiometry with the ones found in JET ITER-like wall (ILW) experiments, can provide complementary information regarding the hydrogen isotopes inventory and release behaviour. We report on the analysis of the beryllium-based layers deposited by the direct current magnetron sputtering method on pure tungsten and silicon substrates. The thickness of studied layers with various amounts of deuterium, oxygen, and carbon was between 2 and 7 μm. Samples from the same batch were distributed to different laboratories and characterised by various analytical methods. Scanning electron microscopy was applied to determine the exact thickness, data from elastic backscattering spectrometry and nuclear reaction analysis to profile the depth content of light elemental species as deuterium, and thermal desorption spectroscopy to quantify the amount of deuterium and also to observe release kinetics. The main finding is that a high amount of deuterium, from 8 at.% up to 28 at.%, can be retained in the films. Deuterium release at a heating rate of 0.125 °C/s reached its maximum intensity at peaks of various widths and shape, which appeared at temperatures from 340 °C up to 660 °C, depending on the thickness, the layer stoichiometry and deposition parameters.