The synergies between displacement damage creation and hydrogen presence: the effect of D ion energy and flux

In this work the synergism between displacement damage creation and presence of hydrogen isotopes was studied. Tungsten samples were irradiated by 10.8 MeV W ions with or without the presence of D ions with two different energies of 300 eV/D and 1000 eV/D and different temperatures. In order to compare the results obtained with different exposure parameters the samples were afterwards additionally exposed to D ions at 450 K to populate the created defects. By increasing the W irradiation time, ion flux and energy, the increase of D concentration and D retention was observed as measured by nuclear reaction analysis and thermal desorption spectroscopy. By fitting the D depth profiles and D desorption spectra by the rate equation code MHIMS-R we could see that additional fill-levels were populated with higher flux and ion energy which ends up in higher final D concentration and retention as compared to experiments with lower D flux and energy.

Reduced defect recovery in self-ion damaged W due to simultaneous deuterium exposure during annealing

Deuterium (D) plasma exposure during annealing of self-ion damaged tungsten (W) is shown to exhibit reduced defect recovery when compared to annealing without D plasma exposure. In these experiments, samples were first damaged with 20 MeV W ions. Next, samples were annealed either with or without simultaneous D2 plasma exposure. The simultaneous annealed samples were first decorated by D2 plasma at 383 K prior to ramping up to an annealing temperature of 473, 573, 673, or 773 K and held for 1 hour with concurrent plasma exposure. The vacuum annealed samples each had a corresponding temperature history but without D$_2$ plasma treatment. Finally, all samples were exposed to D2 plasma at 383 K to decorate any remaining defects. Nuclear reaction analysis (NRA) and thermal desorption spectroscopy (TDS) shows that the simultaneous plasma-exposed and annealed samples exhibited virtually no defect recovery at annealing temperatures of up to 673 K, and had higher D retention than found in the vacuum annealed samples. TDS results indicate that only the lowest detrapping energy defects recover at an 773~K anneal for the simultaneous plasma annealed samples, while the vacuum annealed samples showed defect recovery at all anneal temperatures. This experiment clearly demonstrates that D occupied defects can significantly reduce or eliminate defect annealing in W, and is consistent with the existence of synergistic plasma exposure/displacement damage effects in fusion-energy relevant plasma facing materials.

Measuring in situ CO2 and H2O in apatite via ATR-FTIR

We present a new approach to determine in situ CO2 and H2O concentrations in apatite via attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). Absolute carbon and hydrogen measurements by nuclear reaction analysis (NRA) and elastic recoil detection (ERD) are used to calibrate ATR-FTIR spectra of CO2 and H2O in apatite. We show that CO2 and H2O contents in apatite can be determined via linear equations (r2 > 0.99) using the integrated area of CO2 and H2O IR absorption bands. The main benefits of this new approach are that ATR-FTIR analyses are non-destructive and can be conducted on polished sample material surfaces with a spatial resolution of ~ 35 μm. Furthermore, the wavenumber of the phosphate IR absorption band can be used to determine the crystallographic orientation of apatite, which allows for accurate quantification of CO2 and H2O in randomly orientated apatite grains. The limit of quantification of H2O in apatite is ~ 400 ppm and ~ 100 ppm for CO2. Via two examples, one from a carbonatite and one from a metasedimentary rock, we show that this new technique opens up new possibilities for determining volatile concentrations and behavior in a wide range of hydrothermal, igneous, and metamorphic systems.

Analysis of Hydrogen in Inorganic Materials and Coatings: A Critical Review

The currently used bulk analysis and depth profiling methods for hydrogen in inorganic materials and inorganic coatings are reviewed. Bulk analysis of hydrogen is based on fusion of macroscopic samples in an inert gas and the detection of the thereby released gaseous H2 using inert gas fusion (IGF) and thermal desorption spectroscopy (TDS). They offer excellent accuracy and sensitivity. Depth profiling methods involve glow discharge optical emission spectroscopy and mass spectrometry (GDOES and GDMS), laser-induced breakdown spectroscopy (LIBS), secondary ion mass spectrometry (SIMS), nuclear reaction analysis (NRA), and elastic recoil detection analysis (ERDA). The principles of all these methods are explained in terms of the methodology, calibration procedures, analytical performance, and major application areas. The synergies and the complementarity of various methods of hydrogen analysis are described. The existing literature about these methods is critically evaluated, and major papers concerning each method are listed.

Chromatic Change in Copper Oxide Layers Irradiated with Low Energy Ions

The color of a thin copper oxide layer formed on a copper plate was transformed from reddish-brown into dark blue-purple by irradiation with 5 keV Ar+ ions to a fluence as low as 1 × 1015 Ar+ cm−2. In the unirradiated copper oxide layer, the copper valence state of Cu2+ and Cu+ and/or Cu0 was included as indicated by the presence of a shake-up satellite line in a photoemission spectrum. While for the irradiated one, the satellite line decreased in intensity, indicating that irradiation resulted in the reduction from Cu2+ to Cu+ and/or Cu0. Furthermore, nuclear reaction analysis using a 16O(d, p)17O reaction with 0.85 MeV deuterons revealed a significant loss of oxygen (5 × 1015 O atoms cm−2) in the irradiated layer. Thus, the chromatic change observed in the present work originated in the irradiation-induced reduction of a copper oxide.

A New High-Throughput Focused MeV Ion-Beam Analysis Setup

The analysis of material composition by ion-beam analysis (IBA) is becoming a standard method, similar to electron microscopy. A pool of IBA methods exists, from which the combination of particle-induced-X-ray emission (PIXE), particle induced gamma-ray analysis (PIGE), nuclear-reaction-analysis (NRA), and Rutherford-backscattering-spectrometry (RBS) provides the most complete analysis over the whole periodic table in a single measurement. Yet, for a highly resolved and accurate IBA analysis, a sophisticated technical setup is required integrating the detectors, beam optics, and sample arrangement. A new end-station developed and installed in Forschungszentrum Jülich provides these capabilities in combination with high sample throughput and result accuracy. Mechanical tolerances limit the device accuracy to 3% for RBS. Continuous pumping enables 5*10−8 mbar base pressure with vibration amplitudes < 0.1 µm. The beam optics achieves a demagnification of 24–34, suitable for µ-beam analysis. An in-vacuum manipulator enables scanning 50 × 50 mm² sample areas with 10 nm accuracy. The setup features the above-mentioned IBA detectors, enabling a broad range of analysis applications such as the operando analysis of batteries or the post-mortem analysis of plasma-exposed samples with up to 3000 discrete points per day. Custom apertures and energy resolutions down to 11 keV enable separation of Fe and Cr in RBS. This work presents the technical solutions together with the quantification of these challenges and their success in the form of a technical reference.