Refinements for Bragg coherent X-ray diffraction imaging: electron backscatter diffraction alignment and strain field computation.

Bragg coherent X-ray diffraction imaging (BCDI) allows the 3D measurement of lattice strain along the scattering vector for specific microcrystals. If at least three linearly independent reflections are measured, the 3D variation of the full lattice strain tensor within the microcrystal can be recovered. However, this requires knowledge of the crystal orientation, which is typically attained via estimates based on crystal geometry or synchrotron microbeam Laue diffraction measurements. Presented here is an alternative method to determine the crystal orientation for BCDI measurements using electron backscatter diffraction (EBSD) to align Fe-Ni and Co-Fe alloy microcrystals on three different substrates. The orientation matrix is calculated from EBSD Euler angles and compared with the orientation determined using microbeam Laue diffraction. The average angular mismatch between the orientation matrices is less than ∼6°, which is reasonable for the search for Bragg reflections. The use of an orientation matrix derived from EBSD is demonstrated to align and measure five reflections for a single Fe-Ni microcrystal via multi-reflection BCDI. Using this data set, a refined strain field computation based on the gradient of the complex exponential of the phase is developed. This approach is shown to increase accuracy, especially in the presence of dislocations. The results demonstrate the feasibility of using EBSD to pre-align BCDI samples and the application of more efficient approaches to determine the full lattice strain tensor with greater accuracy.

In situ Bragg coherent X-ray diffraction imaging of corrosion in a Co-Fe alloy microcrystal.

Corrosion is a major concern for many industries, as corrosive environments can induce structural and morphological changes that lead to material dissolution and accelerate material failure. The progression of corrosion depends on nanoscale morphology, stress, and defects present. Experimentally monitoring this complex interplay is challenging. Here we implement in situ Bragg coherent X-ray diffraction imaging (BCDI) to probe the dissolution of a Co-Fe alloy microcrystal exposed to hydrochloric acid (HCl). By measuring five Bragg reflections from a single isolated microcrystal at ambient conditions, we compare the full three-dimensional (3D) strain state before corrosion and the strain along the [111] direction throughout the corrosion process. We find that the strained surface layer of the crystal dissolves to leave a progressively less strained surface. Interestingly, the average strain closer to the centre of the crystal increases during the corrosion process. We determine the localised corrosion rate from BCDI data, revealing the preferential dissolution of facets more exposed to the acid stream, highlighting an experimental geometry effect. These results bring new perspectives to understanding the interplay between crystal strain, morphology, and corrosion; a prerequisite for the design of more corrosion-resistant materials.

High-throughput physical vapour deposition flexible thermoelectric generators.

Flexible thermoelectric generators (TEGs) can provide uninterrupted, green energy from body-heat, overcoming bulky battery configurations that limit the wearable-technologies market today. High-throughput production of flexible TEGs is currently dominated by printing techniques, limiting material choices and performance. This work investigates the compatibility of physical vapour deposition (PVD) techniques with a flexible commercial process, roll-to-roll (R2R), for thermoelectric applications. We demonstrate, on a flexible polyimide substrate, a sputtered Bi2Te3/GeTe TEG with Seebeck coefficient (S) of 140 µV/K per pair and output power (P) of 0.4 nW per pair for a 20 °C temperature difference. For the first time, thermoelectric properties of R2R sputtered Bi2Te3 films are reported and we demonstrate the ability to tune the power factor by lowering run times, lending itself to a high-speed low-cost process. To further illustrate this high-rate PVD/R2R compatibility, we fabricate a TEG using Virtual Cathode Deposition (VCD), a novel high deposition rate PVD tool, for the first time. This Bi2Te3/Bi0.5Sb1.5Te3 TEG exhibits S = 250 µV/K per pair and P = 0.2 nW per pair for a 20 °C temperature difference.