Session Sheet - The 7th International Congress on 3D Materials Science (3DMS 2025): Emerging 3D Characterization Techniques and Instrumentation III

The 7th International Congress on 3D Materials Science (3DMS 2025): Emerging 3D Characterization Techniques and Instrumentation III
Program Organizers: Henry Proudhon, Mines Paris Centre Des Materiaux; Can Yildirim, European Synchrotron Radiation Facility

Thursday 8:00 AM
June 19, 2025
Room: Platinum Ballroom 2
Location: Anaheim Marriott

Session Chair: Chris Le, Naval Surface Warfare Center Carderock Division

8:00 AM  Invited
Diffraction Microstructure Imaging at the Materials Science Beamline, ID11, at the ESRF: Jon Wright¹; Haixing Fang¹; Wolfgang Ludwig¹; James Ball¹; ¹European Synchrotron Radiation Facility
    Synchrotron instrumentation has not stopped improving. New sources are coming online so that the X-ray flux and beam properties are better than ever before. Fast photon counting detectors are widely available and these offer a range of novel diffraction-tomographic methods for imaging microstructures in 3D. At beamline ID11 at the ESRF, there is now a suite of complementary methods that combines imaging detectors for tomographic imaging and DCT grain mapping together with far-field detectors for 3DXRD and scanning tomography. We have optimized the instrument at ID11 for beam sizes down to about 150 nm and high-energy X-rays (40-70 keV). The largest samples are typically a few millimeters in diameter. This contribution will discuss the latest developments at the beamline and the different ways that these are being exploited to address a range of different scientific questions, in a wide range of disciplines, from metallurgy to earth sciences.

8:30 AM
Colour X-Ray Imaging: 5D Non-Destructive Elemental Mapping of Materials: Tim Burnett¹; Nicola Wadeson¹; Amin Garbout¹; Matthieu Boone²; Jan Aelterman²; ¹University of Manchester; ²Ghent University
    The next dimension of X-ray imaging is here! Five dimensional Colour X-ray Imaging enables non-destructive 3D and 4D images to be complemented by a fifth chemistry dimension. Whilst the fundamental technology has been demonstrated it is, at present, inaccessible to most researchers due to the difficulty of acquisition and the processing of the vast multidimensional datasets it generates. We have recently built a new lab-based Colour X-ray CT scanner utilising a large detector array and a commercial cabinet-based system and are embarking on refining many of the data processing workflows. A 640 x 160 pixel hyperspectral HEXITEC detector with CdTe crystal has been integrated into a Nikon XTH 225 scanner. We have already demonstrated the capability of the detector for large-field-of-view bright-field imaging using absorption edge detection and are now moving to superresolution imaging using detector shifting. Initial applications include minerals, stained biomaterial, electronic waste and rare earth magnets.

8:50 AM
Interrogating 3D Grain Morphology and Crystallographic Texture via Automated Polarized Light Microscopy: Paul Chao¹; Rhianna Oakley¹; Andrew Polonsky¹; ¹Sandia National Laboratories
    Polycrystalline materials exhibit properties that are directly influenced by the morphology and crystallographic orientation of their constituent grains. In this work, we interrogate the 3D grain morphology and texture of polycrystalline materials (such as alpha titanium) via polarized light microscopy (PLM) within a commercially available automated serial-sectioning system platform. PLM leverages optical birefringence in anisotropic/uniaxial crystalline materials to assess crystal inclination relative to the incident polarized light beam, resulting in image contrast that reveals grain orientation. The serial-sectioning process automates conventional metallographic preparation, and we implement automated control routines to collect large image montages at various polarization states by rotating the sample to discrete angular intervals. We introduce data reconstruction techniques to rapidly determine the grain morphology and crystallographic texture in centimeter-scale volumes. Details of novel approaches to analysis will be presented. Applications to macroscale texture quantification and understanding mechanical properties in lower-symmetry and multi-phase systems will also be discussed.

9:10 AM
Accelerating 3D Data Collection in TriBeam Microscopes: McLean Echlin¹; James Lamb¹; Andrew Polonsky²; Nicolò Maria della Ventura¹; Kalani Moore³; Jorge Filevich⁴; Will Lenthe⁵; Steven Randolph⁶; Remco Geurts⁴; Chris Torbet¹; Daniel Gianola¹; Marc De Graef⁷; Tresa Pollock¹; ¹University of California Santa Barbara; ²Sandia National Laboratory; ³Direct Electron; ⁴Thermo Fisher Scientific; ⁵EDAX-Gatan; ⁶Oak Ridge National Laboratory; ⁷Carnegie Mellon University
    The latest generation of TriBeam microscope’s high current PFIBs and multi-wavelength femtosecond laser sources enable faster material sectioning than previous generation systems. By combining these material removal modalities, procedures for limiting subsurface damage across ever widening classes of materials is possible. For instance, 3D datasets from polymer composites, biological samples, and battery materials have been collected at various institutions with this new instrument. However, improvements to the process of building TriBeam experiment workflows would vastly increase data collection and make these instruments accessible more broadly to researchers. Furthermore, the collection of information from a wider range of modalities, such as newly developed EBSD detectors that directly detect electrons, will require control software that can flexibly incorporate new hardware APIs. These new developments in instrumentation, data modalities, and opportunities for future iterations will be discussed.

9:30 AM Break

9:50 AM
3D Intragranular Orientation Mapping in Cold-Rolled Ferrite at Industrially Relevant Deformation Levels: Aditya Shukla¹; Mads Carlsen²; N. Mavrikakis³; Virginia Sanna¹; Marilyn Sarkis¹; Carsten Detlefs¹; Yaozhu Li¹; Can Yildirim¹; ¹European Synchrotron Radiation Facility - ESRF; ²Paul Scherer Institut; ³OCAS
    Thermomechanical processing of metals introduces high dislocation densities, altering material properties through mechanisms such as work hardening. Non-destructive 3D mapping of deformation microstructures remains a challenge due to limitations in characterization tools. This study combines Dark-Field X-ray Microscopy (DFXM) and texture tomography (TT) to investigate deformation structures in 50% and 65% cold-rolled ferrite. DFXM enables non-destructive 3D mapping of intragranular deformation structures, resolving dislocation cells with elevated densities and misorientation values up to 5°, at a resolution of 100 nm. TT complements this by providing 3D grain orientation data, aligning grains relative to the rolling direction and bridging the effects of neighboring grains on deformation. These data are also validated with complementary Electron backscatter diffraction (EBSD) measurements. The combined approach reveals the evolution of intragranular deformation structures, cell size distributions, and strain hotspots as a function of deformation, advancing our understanding of plasticity and the interplay between local and global deformation behaviors. This framework offers critical insights into deformation mechanisms and recrystallization in metals.

10:10 AM
Enhancement of Multi-Modal Mechanical Polishing Serial Sectioning Technology: Michael Uchic¹; Michael Scott²; Gregory Sparks³; Michael Chapman²; ¹Air Force Research Laboratory; ²BlueHalo LLC; ³University of Dayton Research Institute
    Automated mechanical polishing serial sectioning (MPSS) experiments have been matured over the past two decades to provide accurate volumetric reconstructions of microscale feature ensembles within centimeter-scale and larger samples. However, the availability of MPSS data − especially multimodal data − is still somewhat limited. The vast majority of automated MPSS systems operate on only one sample at a time, and often with limited feedback or analysis during the experiment. This presentation will discuss the development of a novel multimodal MPSS system as an alternative to the current state-of-the-art. The system is comprised of multiple preparation systems, microscopes, and a mobile sample transfer robot, which can be used for MPSS workflows that accommodate numerous samples concurrently, including use of minimal surface damage methods such as vibratory polishing. Additionally, we discuss the implementation of “on-the-fly” analysis to further improve MPSS data uniformity and quality, and present experimental data to demonstrate these improvements.

10:30 AM
Automated Mechanical Serial Sectioning: A Robust Data-Driven Approach as Applied to a RoboMet.3D: Rhianna Oakley¹; Paul Chao¹; Andrew Polonsky¹; ¹Sandia National Laboratories
    The RoboMet.3D, a semi-automated mechanical serial sectioning (MSS) tool, enables the acquisition of microstructural data across macroscopic length scales by layer-wise material removal and imaging, generating a 3D structure representation of complex multi-material components. This process unveils features and failure mechanisms hidden from traditional 2D and non-destructive methods. However, achieving uniform material removal is hindered by system inconsistencies, often demanding manual adjustments by skilled operators, thus extending data collection and necessitating extensive post-processing. We introduce a novel one-step model predictive control (MPC) framework integrated with a run-to-run (R2R) controller, designed to automate parameter adjustments, enhancing material removal precision through iterative feedback and disturbance management. This data-driven R2R-MPC controller ensures consistent removal rates, adapting seamlessly to varying material properties. Its superiority is validated against traditional methods through both simulations and empirical results, showcasing significant advancements in efficiency and reliability for 3D microstructural analysis.

10:50 AM
3D Mapping of Intragranular Strain and Microstructure in Recrystallized Iron Using Dark-Field X-Ray Microscopy: Virginia Sanna¹; Yubin Zhang²; Wolfgang Ludwig¹; James Ball¹; Abderrahmane Benhadjira¹; Marilyn Sarkis¹; Carsten Detlefs¹; Can Yildirim¹; ¹ESRF; ²DTU
    This study examines intragranular residual strain and orientation distributions in fully recrystallized pure iron grains, using Dark-Field X-ray Microscopy (DFXM) for high-resolution, non-destructive imaging at the submicron level. Our findings reveal uneven strain distributions within grains, with localized values up to 3 × 10⁻⁴, and visualize individual dislocations, highlighting microstructural complexity even after full recrystallization. Simulations of DFXM dislocation contrast offers insights into Burgers vectors. Complementary 3D X-ray Diffraction (3DXRD) analysis using a box beam adds context on overall texture and grain size distribution, enhancing our grasp of grain-level heterogeneity. By combining the two techniques, we relate DFXM strain and orientation data to 3D grain structures, providing a clear view of residual strain landscapes. This combined approach underscores the role of residual strain effects in recrystallized grains and advances our understanding of microstructural evolution in polycrystalline materials.