Osman El-Atwani

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.

Material ejection and surface morphology changes during transient heat loading of tungsten as plasma-facing component in fusion devices

We investigated the effect of edge-localized mode like transient heat events on pristine samples for two different grades of deformed tungsten with ultrafine and nanocrystalline grains as potential candidates for plasma-facing components. Pulses from a laser beam with durations ?1?ms and operating in the near infrared wavelength were used for simulating transient heat loading in fusion devices. We specifically focused on investigating and analysis of different mechanisms for material removal from the sample surface under repetitive transient heat loads. Several techniques were applied for analysing different mechanisms leading to material removal from the W surface under repetitive transient heat loads which include witness plates for collected ejected material, and subsequent analysis using x-ray photoelectron spectroscopy and scanning electron microscopy, visible imaging using fast-gated camera, and evaluating thermal emission from the particles using optical emission spectroscopy. Our results show a significantly improved performance of polycrystalline cold-rolled tungsten compared to tungsten produced using an orthogonal machining process under repetitive transient loads for a wide range of the power densities.

Experimental simulation of materials degradation of plasma-facing components using lasers

The damage and erosion of plasma-facing components (PFCs) due to extremely high heat loads and particle bombardment is a key issue for the nuclear fusion community. Currently high current ion and electron beams are used in laboratories for simulating the behaviour of PFC materials under ITER-like conditions. Our results indicate that high-power nanosecond lasers can be used for laboratory simulation of high heat flux PFC material degradation. We exposed tungsten (W) surfaces with repetitive laser pulses from a nanosecond laser with a power density ~ a few GW cm−2. Emission spectroscopic analysis showed that plasma features at early times followed by intense particle emission at later times. Analysis of laser-exposed W surface demonstrated cracks and grain structures. Our results indicate that the typical particle emission features from laser-irradiated tungsten are consistent with high-power particle beam simulation results.

The significance of in situ conditions in the characterization of GaSb nanopatterned surfaces via ion beam sputtering

A systematic study is conducted in order to elucidate the underlying mechanism(s) for nanopatterning with low-energy irradiation of GaSb (100) under normal incidence. Ion energies between 50 and 1000 eV of Ar+ and ion fluences of up to 1018 cm−2 were employed. Characterization of the shallow (e.g., 1 to 6 nm) amorphous phase region induced by irradiation and the sub-surface crystalline phase region is accomplished with low-energy ion scattering spectroscopy and x-ray photoelectron spectroscopy, respectively. In situ studies are conducted due to the strong chemical affinity for oxygen of GaSb. The studies conclude that at energies below 200 eV, the native oxide layer hampers nanopatterning until it becomes removed at a fluence of approximately 5 × 1016 cm−2. At this energy and threshold fluence, the surface is enriched with Ga atoms during irradiation. At energies above 200 eV, the native oxide layer is efficiently removed in the early irradiation stages, and thus the detrimental effects from the oxide on ...

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.

Determining the morphology of polystyrene-block-poly(2-vinylpyridine) micellar reactors for ZnO nanoparticle synthesis

We report the use of reverse PS-b-P2VP diblock copolymer micelles as true nanoscale-sized reactor vessels to synthesize ZnO nanoparticles. The reverse micelles were formed in toluene and then sequentially loaded with zinc acetate dihydrate and tetramethylammonium hydroxide reactants. Moreover, high spatial resolution Z-contrast imaging and EDX spectroscopy techniques were used to confirm the segregation of the Zn cation to the core of the loaded micelles. Determining the chemical distribution with high nanoscale spatial resolution is shown to complement the less direct characterization by AFM, DLS and FTIR, thus demonstrating broader implications for the characterization of hybrid nanocomposite systems.

Nanoscale composition mapping of segregation in micelles with tapping mode atomic force microscopy

Under energy-dissipative cantilevered tip-sample interaction, phase imaging using tapping-mode atomic force microscopy enables compositional mapping of composites containing a harder inorganic phase at the nanometer scale, embedded in a polymer matrix. The contrast in the phase images is shown to be dependent on the variation in the elastic properties of the diblock copolymer reverse micelles loaded with zinc acetate. Tapping conditions are also shown to determine whether the contrast is positive or negative for the harder core of the loaded micelles, based on the competition between attractive and repulsive tip-sample interaction forces. The broader implications are significant for scanning probe microscopy of other soft materials systems containing the segregation of a harder phase.

Formation of silicon nanodots via ion beam sputtering of ultrathin gold thin film coatings on Si

Ion beam sputtering of ultrathin film Au coatings used as a physical catalyst for self-organization of Si nanostructures has been achieved by tuning the incident particle energy. This approach holds promise as a scalable nanomanufacturing parallel processing alternative to candidate nanolithography techniques. Structures of 11- to 14-nm Si nanodots are formed with normal incidence low-energy Ar ions of 200 eV and fluences above 2 × 1017 cm-2. In situ surface characterization during ion irradiation elucidates early stage ion mixing migration mechanism for nanodot self-organization. In particular, the evolution from gold film islands to the formation of ion-induced metastable gold silicide followed by pure Si nanodots formed with no need for impurity seeding.

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.