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

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

Monday 1:30 PM
June 16, 2025
Room: Platinum Ballroom 2
Location: Anaheim Marriott

Session Chair: Thomas Avey, Naval Surface Warfare Center Carderock; Sven Gustafson, Cornell High Energy Synchrotron Source

1:30 PM  Invited
Advances in Scanning 3DXRD: Resolving Intra-Grain Deformation in 3D: Nils Axel Henningsson¹; ¹DTU
    Modern synchrotron facilities provide monochromatic X-rays with high energy and flux. The 3D X-ray Diffraction Microscope (3DXRD) has utilized these capabilities for over two decades, becoming a reliable tool for 3D characterization of polycrystalline materials. In the past eight years, a derivative technique, the scanning 3DXRD microscope, has emerged. It uses a narrow X-ray beam combined with raster scanning to capture spatial details at the sub-grain level in 3D. In scanning 3DXRD, the diffraction signal from different sub-domains within crystals is highly sensitive to the lattice deformation field. I pioneered several regression frameworks to reconstruct the intra-grain strain tensor and rotation fields from such data. In this talk, I will survey the history of scanning 3DXRD, present the state-of-the-art capabilities of the microscope, showcase its benefits and limitations, and discuss future developments in scanning 3DXRD.

2:00 PM
Observation of Thermal Fatigue-Induced Grain Rotation in Pb-Free Solder Joints by XSOL: Jaemyung Kim¹; Yujiro Hayashi¹; Hiroaki Tatsumi²; Hiroshi Nishikawa²; Makina Yabashi¹; ¹RIKEN; ²Osaka University
     It is believed that the failure mechanism of Pb-free solder joints under thermal cycling is correlated with the rotation of β-Sn grains. However, destructive measurement methods have prevented understanding the original orientation of β-Sn grains before thermal cycling. While conventional X-ray-based orientation microscopies exist, they are limited to small cylindrical samples and are unsuitable for plate-like structures such as solder joints. As a result, no direct evidence of grain rotation has been available until now.To overcome this limitation, we recently developed X-ray Scanning Orientation Laminography (XSOL), which enables orientation mapping of extended plate-like specimens. We applied XSOL to conduct nondestructive analysis of a 930-μm-thick plate containing solder joints. We observed that the β-Sn grains in the as-soldered joints exhibited random orientations, while the c-axis of the grains tended to align parallel to the Cu substrate after thermal cycling, providing direct evidence that grain rotation occurs due to thermal fatigue.

2:20 PM
Laboratory 3D X-Ray Micro-Beam Diffraction: Yubin Zhang¹; Jette Oddershede²; Anthony Seret¹; Azat Slyamov²; Florian Bachmann²; Jan Kehres¹; Carsten Gundlach¹; Ulrik Olsen¹; Jacob Bowen²; Henning Poulsen¹; Erik Lauridsen²; Dorte Juul Jensen¹; ¹Technical University of Denmark; ²Xnovo Tech
    The development of 3D non-destructive X-ray characterization techniques in home laboratories is essential for establishing 3D characterization as a new standard for materials research. Accessible instruments in universities and industry will enable many more researchers to conduct 3D characterization daily, overcoming the limitations of competitive access to synchrotron facilities. Recent efforts have focused on techniques like laboratory diffraction contrast tomography (LabDCT), which allows 3D characterization of fully recrystallized materials with grain size larger than 15 µm, offering a spatial resolution of 5 µm using commercial X-ray CT systems. To enhance the capabilities of these laboratory instruments, we have developed a new 3D laboratory X-ray micro-beam diffraction (LabµXRD) setup, utilizing newly developed Pt-coated twin paraboloidal capillary X-ray optics. The principles and proof-of-concept for LabµXRD will be detailed, along with its potential for integration with LabDCT and micro-CT for multiscale and multimodal 4D characterization of conventionally and additively manufactured materials.

2:40 PM
Deep Learning Enabled Rapid 3D X-Ray Tomography for In Situ Mechanical Characterization: Nathan Johnson¹; Hrishikesh Bale¹; Steve Kelly¹; Newell Moser²; Orion Kafka²; Kaushik Yanamandra³; ¹Carl Zeiss Research Microscopy Solutions; ²National Institute of Standards and Technology; ³Carl Zeiss Microscopy
    Laboratory X-ray characterization techniques often face limitations due to lower flux and brightness compared to synchrotron sources, leading to extended counting times for acquiring high-quality images. This issue is particularly acute for in situ experiments that require multiple datasets, sometimes stretching data collection to several days per sample. In this study, we introduce a deep learning-based reconstruction method tailored for sparse X-ray microscopy datasets. During an in situ tensile test on additively manufactured Inconel 718 dogbone specimens, we collected 1,000 two-dimensional projections over the course of an hour. Utilizing a commercial deep learning model (Zeiss DeepRecon) we achieved high-resolution 3D reconstructions using 100 projections, reducing acquisition time by 10X. The model captured up to 80% of pores and preserved the morphology of the largest pores. This reduction—from one hour to six minutes — notably enhances the efficiency of in situ experiments.

3:00 PM Break

3:30 PM
Pushing Boundaries in 3D Microstructure Mapping: The New DFXM Beamline at ESRF ID03: Can Yildirim¹; Helena Isern¹; Thomas Dufrane¹; Marilyn Sarkis¹; Yaozhu Li¹; Abderrahmane Benhadjira¹; Raquel Rodriguez-Lamas¹; Ricardo Hino¹; Philipp Brumund¹; Emmanuel Papillon¹; Thierry Brochard¹; Damien Scortani¹; Carsten Detlefs¹; ¹European Synchrotron Radiation Facility
    The ESRF’s Dark Field X-ray Microscopy (DFXM) beamline at ID03 heralds a new era for 3D mapping of crystalline orientation and strain, advancing multi-scale imaging capabilities within embedded microstructures. Emerging from ESRF’s EBSL2 Upgrade Project, ID03 offers unprecedented opportunities in high-resolution, non-destructive mapping. Relocated and upgraded from ID06-HXM, the beamline now features state-of-the-art X-ray optics for pink and monochromatic x-rays, a new goniometer, and a detection system tailored to capture subtle microstructural phenomena. Since opening to users in April 2024, the beamline’s unique setup supports complex studies, from metal strain mapping to functional material assessments in semiconductors, biominerals, and energy systems. By expanding access to multi-modal, in-situ exploration, ID03 is positioned to drive innovation across materials science disciplines, meeting the needs of next-generation research in structure-property relationships.

3:50 PM  Cancelled
Reconciling Conflicting Hydrogen Embrittlement Models Using Dark-Field X-Ray Microscopy: Dayeeta Pal¹; Can Yildirim²; Leora Dresselhaus-Marais¹; ¹Stanford University; ²European Synchrotron Radiation Facility
     Despite 150 years of research, the fundamental mechanisms of hydrogen (H) embrittlement are poorly understood. H atoms form a solid solution of interstitial defects in metals, altering dislocation behavior. While dislocations are essential to understand metal plasticity, it is unclear whether H enhances dislocation mobility (Hydrogen Enhanced Localized Plasticity-HELP) or reduces it (Solute Drag Theory-SDT), with no technique being able to image subsurface dislocations. Time-resolved and 3D dark-field X-ray microscopy (DFXM) has been developed to study interactions of large populations of subsurface dislocations. Since hydrogen shielding effect (HSE) is the key mechanism that explains the increased dislocation mobility in the presence of H, our work uses DFXM to generate 3D maps of dislocations, illustrating which dislocations obey the HSE mechanisms in uncharged and H-pre-charged single crystal FCC-austenitic stainless steel. We support these results with DFXM simulations and HSE models, offering the first direct measurements to reconcile conflicting H-altered mobility models.

4:10 PM
Lab-HEDM: A Laboratory-Scale Breakthrough Technique for 3D Characterization of Polycrystalline Materials: Seunghee Oh¹; Yuefeng Jin¹; Sangwon Lee¹; Wenxi Li¹; Ashley Bucsek¹; ¹University of Michigan
    High-energy diffraction microscopy (HEDM) is a 3D x-ray diffraction technique used to characterize the volume, position, orientation, and strain of thousands of grains concurrently, making it a powerful tool for studying the micromechanical behavior of bulk polycrystalline materials. However, HEDM remains accessible only at a few synchrotron facilities. Here, we introduce an innovative laboratory-scale version (Lab-HEDM) that employs a liquid-metal jet x-ray source. As a validation study, we benchmark the capabilities of Lab-HEDM against synchrotron-based HEDM and laboratory diffraction contrast tomography (Lab-DCT). Over 96% of grains detected by Lab-3DXRD were cross-validated with Lab-DCT and/or synchrotron-3DXRD, especially for coarse grains (> ~64 μm). Results also suggest that finer grains could be resolved by employing high-efficiency detectors (e.g., photon-counting detectors). Additionally, we demonstrate how the sensitivity of Lab-3DXRD to fine grains can be improved by modifying the HEDM reconstruction procedure.

4:30 PM
New Capabilities From the APS-Upgrade at the New 3D Micro/Nano Diffraction Station: Jon Tischler¹; ¹Argonne National Laboratory
    The recently completed upgrade of the Advanced Photon Source (APS) increases the brightness of the undulator sources by a factor of ~100. For micro-focusing/diffraction this provides a factor of 100 increase in the brightness of the focused spot. The improved instrument at the 3DMN station should thus have both more power and a smaller spot size of ~150 nm. In addition, using the newly developed technique to obtain depth resolution using a 1D coded aperture we expect data collection times to drop by and additional factor of ~5 with improved signal/noise. The combination of the coded aperture with the increased brightness should reduce collection times by more than a factor of 20 with an improved transverse resolution more than 2 times smaller. This talk will present examples of the first measurements and an appraisal of the improvements, as well as other improvements.