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Register a new userGlancing-Incidence Focussed Ion Beam Milling: A Coherent X-ray Diffraction Study of 3D Nano-scale Lattice Strains and Crystal Defects
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This study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defects than normal incidence milling at the same energy. However the resulting residual lattice strains have similar magnitude and extend up to ~50 nm into the sample. At the edges of the milled surface, where the ion-beam tails impact the sample at near-normal incidence, large dislocation loops with a range of burgers vectors are formed. Further glancing incidence FIB polishing with 5 keV ion energy removes these dislocation loops and reduces the lattice strains caused by higher energy FIB milling. However, even at the lower ion energy, damage-induced lattice strains are present within a ~20 nm thick surface layer. These results highlight the need for careful consideration and management of FIB damage. They also show that low-energy FIB-milling is an effective tool for removing FIB-milling induced lattice strains. This is important for the preparation of micro-mechanical test specimens and strain microscopy samples.
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Focussed Ion Beam (FIB) milling is a mainstay of nano-scale machining. By manipulating a tightly focussed beam of energetic ions, often gallium (Ga+), FIB can sculpt nanostructures via localised sputtering. This ability to cut solid matter on the nano-scale has revolutionised sample preparation across the life-, earth- and materials sciences. For example FIB is central to microchip prototyping, 3D material analysis, targeted electron microscopy sample extraction and the nanotechnology behind size-dependent material properties. Despite its widespread usage, detailed understanding of the functional consequences of FIB-induced structural damage, intrinsic to the technique, remains elusive. Here, we present nano-scale measurements of three-dimensional, FIB-induced lattice strains, probed using Bragg Coherent X-ray Diffraction Imaging (BCDI). We observe that even low gallium ion doses, typical of FIB imaging, cause substantial lattice distortions. At higher doses, extended self-organised defect structures appear, giving rise to stresses far in excess of the bulk yield limit. Combined with detailed numerical calculations, these observations provide fundamental insight into the nature of the damage created and the structural instabilities that lead to a surprisingly inhomogeneous morphology.
Tungsten is the main candidate material for plasma-facing armour components in future fusion reactors. Bombardment with energetic fusion neutrons causes collision cascade damage and defect formation. Interaction of defects with helium, produced by transmutation and injected from the plasma, modifies defect retention and behaviour. Here we investigate the residual lattice strains caused by different doses of helium-ion-implantation into tungsten and tungsten-rhenium alloys. Energy and depth-resolved synchrotron X-ray micro-diffraction uniquely permits the measurement of lattice strain with sub-micron 3D spatial resolution and ~10-4 strain sensitivity. Increase of helium dose from 300 appm to 3000 appm increases volumetric strain by only ~2.4 times, indicating that defect retention per injected helium atom is ~3 times higher at low helium doses. This suggests that defect retention is not a simple function of implanted helium dose, but strongly depends on material composition and presence of impurities. Conversely, analysis of W-1wt% Re alloy samples and of different crystal orientations shows that both the presence of rhenium, and crystal orientation, have comparatively small effect on defect retention. These insights are key for the design of armour components in future reactors where it will be essential to account for irradiation-induced dimensional change when predicting component lifetime and performance.
Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain, however these protocols need to be evaluated for their effectiveness. Here we use non-destructive Bragg coherent X-ray diffraction imaging to study the in situ annealing of FIB-milled gold microcrystals. We simultaneously measure two non-collinear reflections for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared to thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, we analyse each reflection by considering facet area evolution, cross-correlation maps of displacement field and binarised morphology, and average strain plots. The crystals strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ~280{deg}C and the self-diffusion of gold above ~280{deg}C. The majority of FIB-induced strains are removed by 380-410degree C, depending on which reflection is being considered. Our observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.
Nanoprobe X-ray diffraction (nXRD) using focused synchrotron radiation is a powerful technique to study the structural properties of individual semiconductor nanowires. However, when performing the experiment under ambient conditions, the required high X-ray dose and prolonged exposure times can lead to radiation damage. To unveil the origin of radiation damage, we compare nXRD experiments carried out on individual semiconductor nanowires in their as grown geometry both under ambient conditions and under He atmosphere at the microfocus station of the P08 beamline at the 3rd generation source PETRA III. Using an incident X-ray beam energy of 9 keV and photon flux of 10$^{10}$s$^{-1}$, the axial lattice parameter and tilt of individual GaAs/In$_{0.2}$Ga$_{0.8}$As/GaAs core-shell nanowires were monitored by continuously recording reciprocal space maps of the 111 Bragg reflection at a fixed spatial position over several hours. In addition, the emission properties of the (In,Ga)As quantum well, the atomic composition of the exposed nanowires and the nanowire morphology are studied by cathodoluminescence spectroscopy, energy dispersive X-ray spectroscopy and scanning electron microscopy, respectively, both prior to and after nXRD exposure. Nanowires exposed under ambient conditions show severe optical and morphological damage, which was reduced for nanowires exposed under He atmosphere. The observed damage can be largely attributed to an oxidation process from X-ray induced ozone reactions in air. Due to the lower heat transfer coefficient compared to GaAs, this oxide shell limits the heat transfer through the nanowire side facets, which is considered as the main channel of heat dissipation for nanowires in the as-grown geometry.
A coherent x-ray diffraction experiment was performed on an isolated colloidal crystal grain at the coherence beamline P10 at PETRA III. Using azimuthal rotation scans the three-dimensional (3D) scattered intensity in reciprocal space from the sample was measured. It includes several Bragg peaks as well as the coherent interference around these peaks. The analysis of the scattered intensity reveals the presence of a plane defect in a single grain of the colloidal sample. We confirm these findings by model simulations. In these simulations we also analyze the experimental conditions to phase 3D diffraction pattern from a single colloidal grain. This approach has the potential to produce a high resolution image of the sample revealing its inner structure, with possible structural defects.
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