Felix Hofmann

3D lattice distortions and defect structures in ion-implanted nano-crystals

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 revolutionised sample preparation across the life, earth and materials sciences. Despite its widespread usage, detailed understanding of the FIB-induced structural damage, intrinsic to the technique, remains elusive. Here we examine the defects caused by FIB in initially pristine objects. Using Bragg Coherent X-ray Diffraction Imaging (BCDI), we are able to spatially-resolve the full lattice strain tensor in FIB-milled gold nano-crystals. We find that every use of FIB causes large lattice distortions. Even very low ion doses, typical of FIB imaging and previously thought negligible, have a dramatic effect. Our results are consistent with a damage microstructure dominated by vacancies, highlighting the importance of free-surfaces in determining which defects are retained. At larger ion fluences, used during FIB-milling, we observe an extended dislocation network that causes stresses far beyond the bulk tensile strength of gold. These observations provide new fundamental insight into the nature of the damage created and the defects that lead to a surprisingly inhomogeneous morphology.

X-ray micro-beam characterization of lattice rotations and distortions due to an individual dislocation

Understanding and controlling the behaviour of dislocations is crucial for a wide range of applications, from nano-electronics and solar cells to structural engineering alloys. Quantitative X-ray diffraction measurements of the strain fields due to individual dislocations, particularly in the bulk, however, have thus far remained elusive. Here we report the first characterization of a single dislocation in a freestanding GaAs/In0.2Ga0.8As/GaAs membrane by synchrotron X-ray micro-beam Laue diffraction. Our experimental X-ray data agrees closely with textbook anisotropic elasticity solutions for dislocations, providing one of few experimental validations of this fundamental theory. On the basis of the experimental uncertainty in our measurements, we predict the X-ray beam size required for three-dimensional measurements of lattice strains and rotations due to individual dislocations in the material bulk. These findings have important implications for the in situ study of dislocation structure formation, self-organization and evolution in the bulk.

Non-Contact Measurement of Thermal Diffusivity in Ion-Implanted Nuclear Materials

Knowledge of mechanical and physical property evolution due to irradiation damage is essential for the development of future fission and fusion reactors. Ion-irradiation provides an excellent proxy for studying irradiation damage, allowing high damage doses without sample activation. Limited ion-penetration-depth means that only few-micron-thick damaged layers are produced. Substantial effort has been devoted to probing the mechanical properties of these thin implanted layers. Yet, whilst key to reactor design, their thermal transport properties remain largely unexplored due to a lack of suitable measurement techniques. Here we demonstrate non-contact thermal diffusivity measurements in ion-implanted tungsten for nuclear fusion armour. Alloying with transmutation elements and the interaction of retained gas with implantation-induced defects both lead to dramatic reductions in thermal diffusivity. These changes are well captured by our modelling approaches. Our observations have important implications for the design of future fusion power plants.

Imaging of grain-level orientation and strain in thicker metallic polycrystals by high energy transmission micro-beam Laue (HETL) diffraction techniques

Abstract For high performance, safety-critical applications, such as aerospace components, in-depth understanding of the materials response to complex loading conditions is essential. Moreover, it is vital to know how the material behaviour may be modified as a consequence of fatigue loading and how its eventual failure occurs. Unlike bulk properties, such as stiffness, yield stress, etc. that depend on the average response of the grains in a polycrystal, material failure is determined by “weakest link” type mechanisms. These depend strongly on grain-level deformation behaviour and grain-to-grain interactions. Micro-beam Laue diffraction is a powerful tool to probe these phenomena. However, the classical setup is limited to the study of sample surface regions or thin sections, due to the limited penetration into the sample at photon energies of 5 – 25 keV. A much more useful tool for the material scientist and engineer would allow the probing of grain-level orientation and stress in thicker sections of engineering components. To this end, we have developed the high energy transmission Laue (HETL) technique, an extension of the micro-beam Laue technique to significantly higher photon energies (50 – 150 keV). For the imaging of lattice orientation and elastic strain in three dimensions, we propose two alternative approaches: Laue orientation tomography (LOT) and high energy differential aperture X-ray microscopy (HEDAXM). In this paper an overview of the recent progress in HETL, LOT and HEDAXM measurements will be given and some first results illustrating the potential of these techniques presented.

Lifetime of sub-THz coherent acoustic phonons in a GaAs-AlAs superlattice

We measure the lifetime of the zone-center 340 GHz longitudinal phonon mode in a GaAs-AlAs superlattice excited and probed with femtosecond laser pulses. By comparing measurements conducted at room temperature and liquid nitrogen temperature we separate the intrinsic (phonon-phonon scattering) and extrinsic contributions to phonon relaxation. The estimated room temperature intrinsic lifetime of 0.95 ns is compared to available calculations and experimental data for bulk GaAs. We conclude that ~0.3 THz phonons are in the transition zone between Akhiezer and Landau-Rumer regimes of phonon-phonon relaxation at room temperature.

Dislocation-based plasticity model and micro-beam Laue diffraction analysis of polycrystalline Ni foil: A forward prediction

A physically-based, rate and length-scale dependent strain gradient crystal plasticity framework was employed to simulate the polycrystalline plastic deformation at the microscopic level in a large-grained, commercially pure Ni sample. The latter was characterised in terms of the grain morphology and orientation (in the bulk) by micro-beam Laue diffraction experiments carried out on beamline B16 at Diamond Light Source. The corresponding finite element model was developed using a grain-based mesh with the specific grain orientation assignment appropriate for the sample considered. Sample stretching to 2% plastic strain was simulated, and a post-processor was developed to extract the information about the local lattice misorientation (curvature), enabling forward-prediction of the Laue diffraction patterns. The ‘streaking’ phenomenon of the Laue spots (anisotropic broadening of two-dimensional (2D) diffraction peaks observed on the 2D detector) was correctly captured by the simulation, as constructed by direct superposition of reflections from different integration points within the diffraction gauge volume. Good agreement was found between the images collected from experiments and simulation patterns at various positions in the sample.

Laue-DIC: a new method for improved stress field measurements at the micrometer scale

The increment of elastic strain distribution, with a micrometer spatial resolution, is obtained by the correlation of successive Laue images. Application to a bent Si crystal allows evaluation of the accuracy of this new Laue-DIC method, which is about 10−5.

Triaxial residual strains in a railway rail measured by neutron diffraction

Accumulation of residual stresses in rails during service can contribute to crack initiation and fracture and may result in serious accidents. It is therefore necessary and important to quantify the residual stresses that evolve under repeated rolling contact between wheel and rail. In the present study, triaxial residual strain measurements were performed in a worn British railway rail using neutron diffraction. Localized stress is observed close to the region of contact, showing the asymmetry and complexity of distributions that arise from the non-uniform plastic deformation. Contact-induced plasticity is revealed by the broadening (increase in the full width at half-maximum (FWHM)) of the diffraction peaks.

INTRAGRANULAR LATTICE MISORIENTATION MAPPING BY SYNCHROTRON X-RAY MICRO-BEAMS: LAUE VS ENERGY-RESOLVED LAUE VS MONOCHROMATIC RECIPROCAL SPACE ANALYSIS

Laue diffraction, energy scanning and reciprocal space mapping are three micro-beam synchrotron X-ray diffraction techniques allowing the investigation of local misorientation induced by the dislocation substructure. In this paper a comparison between the three methods is presented, based on the mapping of a single 311 reflection from a grain within a Ni polycrystal specimen deformed to a tensile plastic strain of ~9%. Qualitatively it is observed that the maps obtained by different techniques all share the same features, although some deviations exist due to experimental limitations associated with each of the measurement techniques.

Residual stress characterization in 12%-Cr steel friction stir welds by neutron diffraction

In the present paper we report the results of a study into friction stir welds made in 12.7 mm-thick 12%-Cr steel plates. Residual stress measurements were performed using angle-dispersive neutron diffraction. Complete characterization of the three-dimensional residual stress state in friction stir weld samples was obtained by analysing diffracted peaks; peak broadening for identifying the regions of severe plastic deformation and the associated residual strain (eigenstrain) acting as the source of residual stress and peak shifting for evaluating residual elastic strains in the welded component. Three different methods were used to address the key issue of determining the d0 variation across the weld. The comb (or matchstick) method was compared with two other approaches: the balance method, and the zero traction method. It was found that a combination of the comb and the zero traction methods allows reliable residual strain/stress distributions.