Helium nano-bubble formation in plasma facing materials has emerged as a major concern for the next-step fusion experiment ITER, where helium plasmas will be used during the tokamak's start-up phase. Here, we demonstrate that grazing incidence small-angle x-ray scattering is a powerful technique for the analysis of helium nano-bubble formation in tungsten. We measured helium bubbles with sizes between 1.5-2.5 nm in tungsten exposed to helium plasma at 700 • C, where a smaller number of larger bubbles were also observed. Depth distributions can be estimated by taking successive measurements across a range of x-ray incidence angles. Compared with traditional approaches in the field, such as transmission electron microscopy, this technique provides information across a much larger volume with high statistical precision, whilst also being non-destructive.
To determine the effect of pre-existing defects on helium-vacancy cluster nucleation and growth, tungsten samples were self-implanted with 1 MeV tungsten ions at varying fluences to induce radiation damage, then subsequently exposed to helium plasma in the MAGPIE linear plasma device. Positron annihilation lifetime spectroscopy was performed both immediately after self-implantation, and again after plasma exposure. After self-implantation vacancies clusters were not observed near the sample surface (<30 nm). At greater depths (30-150 nm) vacancy clusters formed, and were found to increase in size with increasing W-ion fluence. After helium plasma exposure in the MAGPIE linear plasma device at ~300 K with a fluence of 10 23 Hem -2 , deep (30-150 nm) vacancy clusters showed similar positron lifetimes, while shallow (<30 nm) clusters were not observed. The intensity of positron lifetime signals fell for most samples after plasma exposure, indicating that defects were filling with helium. The absence of shallow clusters indicates that helium requires pre-existing defects in order to drive vacancy cluster growth at 300 K. Further samples that had not been pre-damaged with W-ions were also exposed to helium plasma in MAGPIE across fluences from 1x10 22 to 1.2x10 24 Hem -2. Samples exposed to fluences up to 1x10 23 Hem -2 showed no signs of damage. Fluences of 5x10 23 Hem -2 and higher showed significant helium-cluster formation within the first 30 nm, with positron lifetimes in the vicinity 0.5-0.6 ns. The sample temperature was significantly higher for these higher fluence exposures (~400 K) due to plasma heating. This higher temperature likely enhanced bubble formation by significantly increasing the rate interstitial helium clusters generate vacancies, which is we suspect is the rate-limiting step for helium-vacancy cluster/bubble nucleation in the absence of pre-existing defects.
Helium retention is measured in tungsten samples exposed to mixed H/He plasma in the Magnum-PSI linear plasma device. It is observed that there is very little He retention below helium ion impact energies of
9.0
±
1.4
eV, indicating the existence of a potential barrier which must be overcome for implantation to occur. The helium retention in samples exposed to plasma at temperatures >1000 K is strongly correlated with nano-bubble formation measured using grazing incidence small-angle x-ray scattering. The diameters of nano-bubbles were not found to increase with increasing helium concentration, indicating that additional helium must be accommodated by increasing the bubble concentration or an increase in bubble pressure. For some samples pre-irradiation with heavy ions of 2.0 MeV energy is investigated to simulate the effects of neutron damage. It is observed that nano-bubble sizes are comparable between samples pre-irradiated with heavy-ions, and those without heavy-ion pre-irradiation.
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