Alice Bastos da Silva Fanta

Time-of-Flight Three Dimensional Neutron Diffraction in Transmission Mode for Mapping Crystal Grain Structures

The physical properties of polycrystalline materials depend on their microstructure, which is the nano- to centimeter scale arrangement of phases and defects in their interior. Such microstructure depends on the shape, crystallographic phase and orientation, and interfacing of the grains constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND enables studies of samples that can be both larger in size and made of heavier elements. Moreover, ToF 3DND facilitates the use of complicated sample environments. The basic ToF 3DND setup, utilizing an imaging detector with high spatial and temporal resolution, can easily be implemented at a time-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure. The reconstruction algorithms have been validated by reconstructing two stacked Co-Ni-Ga single crystals, and by comparison with a grain map obtained by post-mortem electron backscatter diffraction (EBSD).

The complementary use of electron backscatter diffraction and ion channelling imaging for the characterization of nanotwins

On the example of electrodeposited nickel films, it is shown that unique information on twins with dimensions on the nanoscale can be obtained by suitable combination of ion channelling imaging and electron backscatter diffraction analysis, whereas both (routine) single techniques cannot meet the requirements for analysis of these films. High‐resolution electron backscatter diffraction is inadequate for full characterization of nanotwins, but image quality maps obtained from electron backscatter diffraction at least yield a qualitative estimation of the location and number of nanotwins. Complementing this information with ion channelling imaging provides more representative insights into the microstructure, because it supplements the quantitative investigation of the number and width of twin lamellae with additional crystallographic orientation analysis provided by EBSD. To this end, two methods for adjusting EBSD data based on ion channelling images are proposed. Thorough selection of the complementary techniques opens future perspectives for the investigation of other challenging samples with nanoscale features in the microstructure.

Columns formed by multiple twinning in nickel layers—An approach of grain boundary engineering by electrodeposition

Complementary microscopic and diffraction based methods revealed a peculiar microstructure of electrodeposited nickel. For the as-deposited layer, thus, without any additional treatment, multiple twinning yields a high population of Σ3n boundaries, which interrupts the network of normal high angle grain boundaries. A peculiar arrangement of Σ3 boundaries forming five-fold junctions is observed. The resulting microstructure meets the requirements for grain boundary engineering. Twinning induced effects on the crystallographic orientation of grains result in one major texture component being a ⟨210⟩ fiber axis and additional minor orientations originating from first and second generation twins of ⟨210⟩, i.e., ⟨542⟩ and ⟨20 2 1⟩.

Influence of Ti and Cr Adhesion Layers on Ultrathin Au Films

Efficient adhesion of gold thin films on dielectric or semiconductor substrates is essential in applications and research within plasmonics, metamaterials, 2D materials, and nanoelectronics. As a consequence of the relentless downscaling in nanoscience and technology, the thicknesses of adhesion layer and overlayer have reached tens of nanometers, and it is unclear if our current understanding is sufficient. In this report, we investigated how Cr and Ti adhesion layers influence the nanostructure of 2-20 nm thin Au films by means of high-resolution electron microscopy, complemented with atomic force microscopy and X-ray photoelectron spectroscopy. Pure Au films were compared to Ti/Au and Cr/Au bilayer systems. Both Ti and Cr had a striking impact on grain size and crystal orientation of the Au overlayer, which we interpret as the adhesion layer-enhanced wetting of Au and the formation of chemical bonds between the layers. Ti formed a uniform layer under the Au overlayer. Cr interdiffused with the Au layer forming a Cr-Au alloy. The crystal orientation of the Au layers was mainly [111] for all thin-film systems. The results showed that both adhesion layers were partially oxidized, and oxidation sources were scrutinized and found. A difference in bilayer electrical resistivity between Ti/Au and Cr/Au systems was measured and compared. On the basis of these results, a revised and more detailed adhesion layer model for both Ti/Au and Cr/Au systems was proposed. Finally, the implications of the results were analyzed, and recommendations for the selection of adhesion layers for nano-optics and nanoelectronics applications are presented.

Grain boundary mediated hydriding phase transformations in individual polycrystalline metal nanoparticles

Grain boundaries separate crystallites in solids and influence material properties, as widely documented for bulk materials. In nanomaterials, however, investigations of grain boundaries are very challenging and just beginning. Here, we report the systematic mapping of the role of grain boundaries in the hydrogenation phase transformation in individual Pd nanoparticles. Employing multichannel single-particle plasmonic nanospectroscopy, we observe large variation in particle-specific hydride-formation pressure, which is absent in hydride decomposition. Transmission Kikuchi diffraction suggests direct correlation between length and type of grain boundaries and hydride-formation pressure. This correlation is consistent with tensile lattice strain induced by hydrogen localized near grain boundaries as the dominant factor controlling the phase transition during hydrogen absorption. In contrast, such correlation is absent for hydride decomposition, suggesting a different phase-transition pathway. In a wider context, our experimental setup represents a powerful platform to unravel microstructure–function correlations at the individual-nanoparticle level.Grain boundaries are thought to significantly mediate phase transformations in nanoparticles. Here, the authors combine multichannel plasmonic nanospectroscopy and transmission Kikuchi diffraction to study the role of grain boundaries in hydriding reactions of Pd nanoparticles on a single-particle level.