S. Gonderman

In-situ TEM observation of the response of ultrafine- and nanocrystalline-grained tungsten to extreme irradiation environments

The accumulation of defects, and in particular He bubbles, can have significant implications for the performance of materials exposed to the plasma in magnetic-confinement nuclear fusion reactors. Some of the most promising candidates for deployment into such environments are nanocrystalline materials as the engineering of grain boundary density offers the possibility of tailoring their radiation resistance properties. In order to investigate the microstructural evolution of ultrafine- and nanocrystalline-grained tungsten under conditions similar to those in a reactor, a transmission electron microscopy study with in situ 2 keV He+ ion irradiation at 950°C has been completed. A dynamic and complex evolution in the microstructure was observed including the formation of defect clusters, dislocations and bubbles. Nanocrystalline grains with dimensions less than around 60 nm demonstrated lower bubble density and greater bubble size than larger nanocrystalline (60–100 nm) and ultrafine (100–500 nm) grains. In grains over 100 nm, uniform distributions of bubbles and defects were formed. At higher fluences, large faceted bubbles were observed on the grain boundaries, especially on those of nanocrystalline grains, indicating the important role grain boundaries can play in trapping He and thus in giving rise to the enhanced radiation tolerance of nanocrystalline materials.

Ultrafine tungsten as a plasma-facing component in fusion devices: effect of high flux, high fluence low energy helium irradiation

This work discusses the response of ultrafine-grained tungsten materials to high-flux, high-fluence, low energy pure He irradiation. Ultrafine-grained tungsten samples were exposed in the Pilot-PSI (Westerhout et al 2007 Phys. Scr. T128 18) linear plasma device at the Dutch Institute for Fundamental Energy Research (DIFFER) in Nieuwegein, the Netherlands. The He flux on the tungsten samples ranged from 1.0 × 1023–2.0 × 1024 ions m−2 s−1, the sample bias ranged from a negative (20–65) V, and the sample temperatures ranged from 600–1500 °C. SEM analysis of the exposed samples clearly shows that ultrafine-grained tungsten materials have a greater fluence threshold to the formation of fuzz by an order or magnitude or more, supporting the conjecture that grain boundaries play a major role in the mechanisms of radiation damage. Pre-fuzz damage analysis is addressed, as in the role of grain orientation on structure formation. Grains of (1 1 0) and (1 1 1) orientation showed only pore formation, while (0 0 1) oriented grains showed ripples (higher structures) decorated with pores. Blistering at the grain boundaries is also observed in this case. In situ TEM analysis during irradiation revealed facetted bubble formation at the grain boundaries likely responsible for blistering at this location. The results could have significant implications for future plasma-burning fusion devices given the He-induced damage could lead to macroscopic dust emission into the fusion plasma.

Materials analysis and particle probe: a compact diagnostic system for in situ analysis of plasma-facing components (invited).

The objective of the materials analysis particle probe (MAPP) in NSTX is to enable prompt and direct analysis of plasma-facing components exposed to plasma discharges. MAPP allows multiple samples to be introduced to the level of the plasma-facing surface without breaking vacuum and analyzed using X-ray photoelectron spectroscopy (XPS), ion-scattering and direct recoil spectroscopy, and thermal desorption spectroscopy (TDS) immediately following the plasma discharge. MAPP is designed to operate as a diagnostic within the ∼12 min NSTX minimum between-shot time window to reveal fundamental plasma-surface interactions. Initial calibration demonstrates MAPPs XPS and TDS capabilities.

Nanopatterning of metal-coated silicon surfaces via ion beam irradiation: Real time x-ray studies reveal the effect of silicide bonding

We investigated the effect of silicide formation on ion-induced nanopatterning of silicon with various ultrathin metal coatings. Silicon substrates coated with 10 nm Ni, Fe, and Cu were irradiated with 200 eV argon ions at normal incidence. Real time grazing incidence small angle x-ray scattering (GISAXS) and x-ray fluorescence (XRF) were performed during the irradiation process and real time measurements revealed threshold conditions for nanopatterning of silicon at normal incidence irradiation. Three main stages of the nanopatterning process were identified. The real time GISAXS intensity of the correlated peaks in conjunction with XRF revealed that the nanostructures remain for a time period after the removal of the all the metal atoms from the sample depending on the binding energy of the metal silicides formed. Ex-situ XPS confirmed the removal of all metal impurities. In-situ XPS during the irradiation of Ni, Fe, and Cu coated silicon substrates at normal incidence demonstrated phase separation and the formation of different silicide phases that occur upon metal-silicon mixing. Silicide formation leads to nanostructure formation due the preferential erosion of the non-silicide regions and the weakening of the ion induced mass redistribution.

Ion beam nanopatterning of III-V semiconductors: Consistency of experimental and simulation trends within a chemistry-driven theory

Several proposed mechanisms and theoretical models exist concerning nanostructure evolution on III-V semiconductors (particularly GaSb) via ion beam irradiation. However, making quantitative contact between experiment on the one hand and model-parameter dependent predictions from different theories on the other is usually difficult. In this study, we take a different approach and provide an experimental investigation with a range of targets (GaSb, GaAs, GaP) and ion species (Ne, Ar, Kr, Xe) to determine new parametric trends regarding nanostructure evolution. Concurrently, atomistic simulations using binary collision approximation over the same ion/target combinations were performed to determine parametric trends on several quantities related to existing model. A comparison of experimental and numerical trends reveals that the two are broadly consistent under the assumption that instabilities are driven by chemical instability based on phase separation. Furthermore, the atomistic simulations and a survey of material thermodynamic properties suggest that a plausible microscopic mechanism for this process is an ion-enhanced mobility associated with energy deposition by collision cascades.

Real time x-ray studies during nanostructure formation on silicon via low energy ion beam irradiation using ultrathin iron films

Real time grazing incidence small angle x-ray scattering and x-ray fluorescence (XRF) are used to elucidate nanodot formation on silicon surfaces during low energy ion beam irradiation of ultrathin iron-coated silicon substrates. Four surface modification stages were identified: (1) surface roughening due to film erosion, (2) surface smoothing and silicon-iron mixing, (3) structure formation, and (4) structure smoothing. The results conclude that 2.5 × 1015 iron atoms in a 50 nm depth triggers surface nanopatterning with a correlated nanodots distance of 25 nm. Moreover, there is a wide window in time where the surface can have correlated nanostructures even after the removal of all the iron atoms from the sample as confirmed by XRF and ex-situ x-ray photoelectron spectroscopy (XPS). In addition, in-situ XPS results indicated silicide formation, which plays a role in the structure formation mechanism.

Near sputter-threshold GaSb nanopatterning

Nanopatterning at sputter-threshold energies with Ar irradiation of GaSb (100) surfaces is presented. Comparison with high-energy irradiations up to 1000 eV is conducted measuring in-situ the composition evolution over irradiation time at early stages (e.g., <1017 cm−2) and up to nanostructure saturation (e.g., ∼1018 cm−2). Low-energy irradiation is conducted for energies between 15–100 eV and a low-aspect ratio nanostructured dot formation is found. Furthermore, the role of oxide on GaSb is found to delay nanostructure formation and this is predominant at energies below 100 eV. In-situ quartz crystal microbalance measurements collect sputtered particles yielding the sputter rate at threshold energies indicating a correlation between erosion and surface composition consistent with recent theoretical models. Ion-induced segregation is also found and indicated by both compositional measurements of both the surface and the sputtered plume.

The Materials Analysis Particle Probe (MAPP) Diagnostic System in NSTX

Lithium conditioning of plasma-facing surfaces has been implemented in National Spherical Torus Experiment (NSTX) leading to improvements in plasma performance such as reduced D recycling and a reduction in edge localized modes. Analysis of postmortem tiles and offline experiments along with atomistic modeling has identified interactions between Li-O-D and Li-C-D as chemical channels for deuterium retention in ATJ graphite. However, previous surface chemistry analysis of NSTX tiles were conducted postmortem (i.e., after a completed annual campaign), and it was not possible to correlate the performance of particular discharges with the state of the material surface at the time. Materials Analysis Particle Probe (MAPP) is the first in-vacuo surface analysis diagnostic directly integrated into a tokamak and capable of chemical surface analysis of plasma facing samples retrieved from the vessel in between discharges. It uses X-ray photoelectron spectroscopy, direct recoil spectroscopy, low energy ion surface spectroscopy, and thermal desorption spectroscopy to investigate the chemical functionalities between D and lithiated graphite at both the near surface (5-10 nm) and top surface layer (0.3-0.6 nm), respectively. MAPP will correlate plasma facing component surface chemistry with plasma performance and lead the way to improved understanding of plasma-surface interactions and their effect on global plasma performance. Remote operation and data acquisition, integrated into NSTX diagnostic and interlocks, make MAPP an advanced PMI diagnostic with stringent engineering constraints.

The Materials Analysis patticle Probe (MAPP) diagnostic system in NSTX

Lithium conditioning of plasma-facing surfaces (PFS) has been implemented in NSTX leading to improvements in plasma performance such as reduced D recycling and a reduction in edge localized modes (ELMS). Analysis of post-mortem tiles and offline experiments has identified interactions between Li-O-D and Li-C-D as chemical channels for deuterium retention in ATJ graphite. MAPP is the first in-vacuo surface analysis diagnostic directly integrated into a tokamak and capable of shot-to-shot chemical surface analysis of plasma material interactions (PMI). X-ray photoelectron spectroscopy (XPS) and low energy ion surface spectroscopy (LEISS) can show the chemical functionalities between D and lithiated graphite at both the near surface (5–10 nm) and top surface layer (0.3–0.6 nm) for XPS and LEISS respectively. MAPP will correlate plasma facing component (PFC) surface chemistry with plasma performance to lead the way to improved understanding of plasma-surface interactions and their effect on global plasma performance. Remote operation and data acquisition, integrated into NSTX diagnostic and interlocks, make MAPP an advanced PMI diagnostic with stringent engineering constraints.