4th International Congress on 3D Materials Science (3DMS) 2018: Energy Materials I
Program Organizers: Hugh Simons, Denmark Technical University; Henning Poulsen, Denmark Technical University; David Rowenhorst, Naval Research Laboratory; Peter Voorhees, Northwestern University; Satoshi Hata, Kyushu Univ; McLean Echlin, UC Santa Barbara

Monday 1:30 PM
June 11, 2018
Room: Store Scene
Location: Kulturværftet (Culture Yard) Conference Center

Session Chair: Hugh Simons, Denmark Technical University

1:30 PM  Invited
CINEMA - the allianCe for ImagiNg and Modelling of Energy Applications: Jens Andreasen1; Anders Dahl1; Henning Sørensen2; Lars Mikkelsen1; Erik Lauridsen3; Brian Vinter2; Carsten Gundlach1; Rajmund Mokso4; Henning Poulsen1; 1Technical University of Denmark; 2University of Copenhagen; 3Xnovo Technologies; 4MAX IV Laboratory
    CINEMA is a strategic research alliance that focuses on development of in situ X-ray imaging and modelling of energy materials, with 15 PhDs and 5 post docs dedicated to the effort. The scope of CINEMA will be presented and an overview of the most important results, within development of in situ equipment for 3D imaging, and in analysis tools for quantification and modelling of 3D data. The tools developed are generic to most 3D imaging modalities and are disseminated to facilities such as MAXIV, through the Centre for quantification of imaging data from MAX IV (QIM), and to other fields, including electron imaging in a new European Innovative Training Network, MUMMERING. The methodology of 3D imaging, analysis and modelling is taught at an annual summer school CINEMAX, and through an interactive e-learning course eCINEMA, that will launch in 2018. Tools learned and applied in Jupyter notebooks will be demonstrated.

2:00 PM  
High-resolution Mapping of Bismuth Ferrite-based Multiferroics by X-ray Diffraction Computed Tomography: Marta Majkut1; Hugh Simons2; Tadej Rojac3; Andreja Bencan Golob3; Jeppe Ormstrup2; John Daniels4; Jonathan Wright1; 1European Synchrotron Radiation Facility; 2Technical University of Denmark; 3Jozef Stefan Institute; 4University of New South Wales
    Bismuth ferrite-based ceramics are multiferroics with interesting properties such as an electric-field-induced phase transformation that results in large macroscopic strain, thus making these materials attractive candidates for electromechanical applications. As in many polycrystalline materials, such macroscopic responses are highly influenced by grain-scale heterogeneities and intergranular interactions, and their study benefits from grain-resolved characterisation techniques such as three-dimensional X-ray diffraction (3DXRD). While 3DXRD has successfully been applied to coarse-grained materials, fine-grained materials such as bismuth-ferrite have proven challenging due to limited spatial resolution and a ‘powder-like’ diffraction pattern in which diffraction spots cannot be resolved. The nano-focus end-station at beamline ID11 at the ESRF offers a solution with an X-ray diffraction computed tomography approach using a ~200 nm x 200 nm focussed beam. We present the high-resolution grain map of a bismuth-ferrite ceramic highlighting microstructure and grain neighbourhood properties, and the impact on studies of other sub-micron scale materials and phenomena.

2:20 PM  
Sulphur Evolution Before and After Cycling in Lithium-sulphur Batteries Revealed by High Resolution X-ray Tomography: Shaogang Wang1; Lei Zhang1; 1Institute of Metal Research, Chinese Academy of Sciences
    Li-S batteries are considered to be a promising next generation high energy electrochemical energy storage system. The specific capacity and energy density of Li-S batteries is strongly related to its sulphur loading (mg cm-2) and sulphur content (wt. %). Ingenious design of 3D electrode structures can simultaneously improve the sulphur loading and sulphur content while keep good electrochemical properties for high performance Li-S batteries. In this talk, four elaborate 3D electrode microstructures such as a 3D hybrid graphene hierarchical network macrostructure will be presented. Multi-scale in-situ and ex-situ ultra-high resolution lab-based 3D X-ray tomography techniques with the pixel size from 65 nm to 20 um were explored to reveal the 3D and 4D evolution characteristics of sulphur in these state-of-the art electrodes before and after cycling. Our results would lay insight on the design and development of high specific capacity, high specific energy density and long life Li-S batteries.

2:40 PM  
3D Characterization of Nuclear Fuels by Neutron Diffraction and Energy-resolved Neutron Imaging: Kenneth McClellan1; Anton Tremsin2; Adrian Losko1; Sven Vogel1; 1Los Alamos National Laboratory; 2University of California Berkeley
    3D characterization of nuclear fuels pre- and post-irradiation is of paramount importance to maximize the knowledge gain from expensive irradiation tests. Due to the heavy elements present in ceramic (U-O, U-Si, U-N, U-C etc.) or metallic (U-Mo, U-Pu-Zr etc.) fuels, X-ray and synchrotron characterization is limited to small volumes. At LANSCE, the unique advantages of neutrons for characterization of nuclear fuel materials are applied to accelerate the development of new nuclear fuel forms. By characterizing slices or volumes within the sample, spatially resolved measurements of phase composition, strains, and textures are possible. In parallel, energy-resolved neutron tomography is developed, not only allowing to visualize cracks, arrangement of fuel pellets in rodlets etc., but also characterization of isotope densities by means of neutron absorption resonance analysis. This novel approach allows spatial resolution below 50 micrometer. We provide an overview of characterizations for accident-tolerant fuel consisting of uranium nitride/uranium silicide composite fuels.

3:00 PM  
Sample Design and Preparation Techniques for Dynamic Microstructural Studies of High Temperature Electrochemical Cells: Jacob Bowen1; Salvatore De Angelis1; José Xavier Trujillo1; Peter S. Jørgensen1; Henning Poulsen1; Esther Tsai2; Mirko Holler2; Julie Villanova3; Philip Cook3; 1Technical University of Denmark; 2Paul Scherrer Institute; 3European Synchrotron Radiation Facility
    Understanding the dynamics of 3D microstructural change in high temperature electrochemical cells, primarily solid oxide fuel cells or electrolysers, is a pressing driving force for performing time resolved ex-situ, in-situ and in-operando nano-tomography and diffraction based experiments at synchrotron X-ray sources. These experiments must meet simultaneous challenging demands: precision beamline compatible samples that are stable at high temperature, supply of electric potential, and control of atmosphere. Correct sample design is an absolute necessity for experimental success. Here, the merits of possible sample configurations and environments are explored and evaluated against fabrication challenges and experimental feasibility. Experience with designing and performing experiments of selected configurations will be presented. Results of 3D nano-tomography of Ni-yttria stabilized zirconia (YSZ) fuel electrode microstructure evolution during Ni oxidation, reduction and annealing, and spatially resolved in-operando diffraction studies of YSZ electrolytes under at high polarization will be summarised.

3:20 PM Break