The 7th International Congress on 3D Materials Science (3DMS 2025): Time Resolved 3D Characterization I
Program Organizers: Henry Proudhon, Mines Paris Centre Des Materiaux; Can Yildirim, European Synchrotron Radiation Facility
Tuesday 9:00 AM
June 17, 2025
Room: Platinum Ballroom 2
Location: Anaheim Marriott
Session Chair: Aly Badran, GE Aerospace Research
9:00 AM Invited
Capturing Grain Boundary Migration in Polycrystals: Amanda Krause1; 1Carnegie Mellon University
Curvature is considered the common local driving force for grain boundary motion in all polycrystals. However, models and simulations derived from curvature-based motion cannot predict irregular, albeit commonly observed, grain growth behavior. This talk will highlight how 3D x-ray diffraction microscopy methods provide new insights for enabling microstructural design. 3D x-ray diffraction microscopy methods are non-destructive and map the full microstructure, providing an opportunity to observe grain growth in real 3D polycrystals. In this talk, experimental observations of growth in strontium titanate, alumina, and nickel will be compared to Monte Carlo Potts simulations to interrogate the role of curvature and grain boundary energy in microstructure evolution. Then, potential descriptors for abnormal grain growth, in which a few grains maintain a growth advantage, in recrystallized pure nickel will be evaluated. The outstanding challenges and opportunities for using 3D x-ray diffraction microscopy to elucidate microstructural evolution will be discussed.
9:30 AM
On the Thermal Aging of the Nanoporous Structure of Sintered Ag on a Cu Substrate: Xavier Milhet1; Jerome Colin2; Kokouvi Happy N'Touaglo1; Adine Nait Ali1; Loic Signor2; 1Pprime Institute Cnrs Ensma; 2Institut Pprime Cnrs Université de Poitiers
As power modules are a complex assembly of different materials, all of them having different coefficients of thermal expansion, a fine evaluation of the evolution of the materials and interfaces is necessary. In this work, time resolved evolution (4D) of the nanoporous microstructure of sintered Ag (s-Ag) and sintered Ag on Cu (s-Ag/Cu) during thermal aging was monitored at high temperature using in-situ X-ray nanotomography. For both types of specimen, the density of S-Ag remains constant, the evolution is driven by the bigger pores and the pore growth follows the Ostwald ripening mechanism. Faster kinetics of growth is observed for s-Ag/Cu before deviating from Ostwald ripening after a critical time. Furthermore, complex evolutions in small pores clusters can be observed in both type of specimens. Those behaviors are discussed based on diffusion mechanisms in relation with a competition between local stresses relaxation and surface energy during diffusion.
9:50 AM
Polycrystalline Effects on Early Strain Heterogeneity Leading to Fracture for an Aluminium Alloy Under Plane Strain Tension: 3D Correlative X-Ray Tomography and Crystal Plasticity Simulations: Maryse Gille1; Thilo Morgeneyer1; Jette Oddershede2; Romain Quey3; Henry Proudhon1; 1Mines Paris-PSL; 2Xnovo Technology ApS; 3Mines Saint-Etienne
The internal strain heterogeneity leading to fracture is studied in an aluminium alloy under plane strain tension, which is a common failure state in stamping processes. The polycrystalline effects are investigated using multimodal X-ray lab tomography 3D data acquired on a miniaturized plane strain tensile specimen. The real microstructure in the center of the undeformed specimen is obtained non-destructively using lab-based diffraction contrast tomography. Crystal plasticity finite element (CP-FE) simulations are performed on the meshed microstructure. Besides, digital image correlation is performed in the material bulk using intermetallic particles visible in absorption contrast tomography data acquired during an in situ tensile test performed in 12 increments up to fracture. Strong correlations are found between the CP-FE predictions based on the meshed real grain structure and the measured strain fields. The early strain heterogeneity in form of spatially stable slanted bands as precursor of final fracture is attributed to polycrystalline effects.
10:10 AM
Tracking the Dynamics of Strain-Energy-Driven Grain Growth in 3D: Marcel Chlupsa1; Zach Croft1; Katsuyo Thornton1; Ashwin Shahani1; 1University of Michigan
Understanding microstructural dynamics under non-isothermal annealing is crucial for the manufacture of shape memory alloys (SMAs). This study examines how stored strain energy influences grain growth in a model CuAlMn SMA. Using synchrotron high-energy X-ray diffraction microscopy (HEDM), we map grains and precipitates in 3D over time, analyzing strain, grain boundary curvatures, and the relation between the two. We quenched the sample at three time-points in the heat treatment to acquire data. To complement these experiments, corresponding phase-field simulations address spatiotemporal gaps in the HEDM data. Departures from experimental observations, e.g., more compact grains, serve to highlight unique features associated with strain-energy-driven growth. Our combined experiments and simulations reveal significant variations in grain sizes, shapes, strains, and boundary curvatures over the course of the non-isothermal anneal. This work underscores the complexities of microstructural dynamics driven by stored strain energy, which are not fully captured by conventional theories or metallographic analysis.
10:30 AM Break
10:50 AM
Intragranular Evolution of Slip System Strength and Activity in Titanium Using Point-Focused High-Energy Diffraction Microscopy: Wenxi Li1; Hemant Sharma2; Peter Kenesei2; Jun-Sang Park2; Sidharth Ravi3; Orcun Koray Celebi3; Daegun You3; Tolga Berkay Celebi3; Huseyin Sehitoglu3; Ashley Bucsek1; 1University of Michigan; 2Argonne National Laboratory; 3University of Illinois at Urbana-Champaign
In-situ point-focused high-energy diffraction microscopy is used to non-destructively capture the deformation behavior of a millimeter-scale grain network in bulk commercially pure titanium with subgrain-scale spatial resolution. The intragranular crystallographic orientation, elastic strain, and slip system activity are tracked as the material is loaded in tension beyond the macroscopic yield point. The results are used to measure intragranular critical resolved shear stress values for prismatic and basal slip systems, which closely align with room-temperature values predicted by density functional theory. The local elastic strain and plastic shear strain maps are also used to investigate the heterogeneous nature of local plastic deformation. Analysis of the principal stress directions reveal that grain boundaries act as barriers to slip, leading to localized stress concentrations and driving stress redistribution. This study provides new insights into intragranular stress states, slip system activity, and grain–grain interactions, advancing the understanding of crystal plasticity in polycrystalline materials.
11:10 AM
Quantifying Ductile Fracture Mechanisms in AA2198-T851 Through Void Tracking of In-Situ Laminography Experiments: Thomas Tancogne-Dejean1; Christian Roth1; Thilo Morgeneyer2; Dirk Mohr1; 1ETH Zurich; 2MINES ParisTech, PSL University, Centre des Matériaux
Synchrotron laminography has proven to be an effective method for examining the nucleation, growth, and coalescence of voids at the material level. Here, monotonic experiments are conducted on AA2198-T8 using a laminography stage on a synchrotron X-ray line. The specimens tested include a “smiley” shear geometry, tensile specimens with notch and circular cut-outs, as well as a compact tension geometry, effectively spanning stress states from low (η=0) to high (η>>1) triaxialities. Multiple scans of the entire gage section with resolution of approximately 1µm³ allow capturing the meso-structural evolution within the material in 3D up to fracture. Additional macroscopic experiments are used to identify parameters for a non-quadratic plasticity model with isotropic hardening. A novel two-step void tracking algorithm, leveraging finite element displacement fields and heuristics, is introduced to provide deeper insight into void nucleation, growth, and coalescence. It allows for the first time a quantitative analysis of respective void populations.
11:30 AM
Micromechanical Behavior of Fe-36Ni Invar Alloy at Cryogenic Conditions Characterized Using High Energy X-Ray Diffraction Microscopy: Raghul Asok Kumar1; Dhruv Anjaria2; Kenneth Peterson1; Reilly Knox1; Katherine Shanks3; Jean-Charles Stinville2; Darren Pagan1; 1Penn State University; 2University of Illinois Urbana-Champaign; 3Cornell High Energy Synchrotron Source
Fe-36Ni Invar alloy is known to have enhanced ductility and tensile strength at cryogenic conditions and hence the alloy finds potential energy storage applications. However, in cryogenic conditions, the crystal-scale origins of these mechanical properties have not been probed for the want of appropriate characterization tools. Recent advancements in synchrotron testing capabilities enable the characterization of microstructure along with the mechanical behavior of individual crystals in polycrystalline metallic materials at low temperatures resembling service conditions. With the help of these advancements, here we track the evolution of grain-averaged lattice orientations and stress during in-situ mechanical loading of Fe-36Ni Invar alloy at 80K. These results are then compared with the material’s micromechanical response at room temperature.
11:50 AM
Interpreting Through Depth Imaging of Acoustic Phonons via Dark-Field X-Ray Microscopy With Kinematic Diffraction: Darshan Chalise1; Yifan Wang1; Mariano Trigo2; Leora Dresselhaus-Marais1; 1Stanford University; 2SLAC National Laboratory
Dark Field X-ray Microscopy (DFXM) is a full-field x-ray imaging technique with excellent resolution in real and reciprocal space. DFXM at x-ray free electron lasers can visualize the dynamics of strain wave evolution from ultrafast laser excitation via the change in Bragg condition. Meanwhile, x-ray diffuse scattering enables reconstructing phonon band structures. In this talk, we will discuss a formalism to interpret DFXM signal via both change in the Bragg condition and phonon-induced diffuse scattering. We will discuss how measurements in coherent acoustic phonons can provide frequency resolved measurement of acoustic dissipation and how thermal diffuse scattering can be used for thermometry and thermal transport measurements. For both coherent phonon imaging and diffuse scattering, we will compare the tradeoffs and the limits of real and reciprocal space resolutions. Finally, we will discuss how the resolution provided by DFXM enables extending our understanding of phonon transport.