6th International Congress on 3D Materials Science (3DMS 2022): Poster Session
Program Organizers: Dorte Juul Jensen, Technical University of Denmark; Marie Charpagne, University of Illinois; Keith Knipling, Naval Research Laboratory; Klaus-Dieter Liss, University of Wollongong; Matthew Miller, Cornell University; David Rowenhorst, Naval Research Laboratory
Monday 4:15 PM
June 27, 2022
Room: Columbia Foyer
Location: Hyatt Regency Washington on Capitol Hill
Calcium Oxalate Cluster Crystals Investigation of Ginseng Using Quantitative X-ray Micro-tomography: Yanling Xue1; Guohao Du1; Tiqiao Xiao1; 1Shanghai Synchrotron Radiation Facility/Zhangjiang Laboratory, Shanghai Advanced Research Institute, Chinese Academy of Sciences
Calcium oxalate cluster crystal (COCC) is an important characteristic of ginseng. By measuring the shape, size, content and distribution of COCCs, the authenticity and quality identification can be realized. Conventional methods for determination of calcium oxalate are destructive and only two-dimensional. In this presentation, quantitative X-ray micro-tomography method was used to investigate the microstructures of ginsengs. Four different ginseng samples were collected and investigated. The size and position distribution, the volume and amount of the COCCs are obtained accordingly. This study is the first to provide evidence of the distribution characteristics of COCCs to identify different ginsengs, concerning the species authentication and age identification. The results showed that this method provides a feasible comprehensive evaluation of the distribution of COCCs accumulation in ginseng in situ. This method is also expected to reveal important relationships between COCCs and the occurrence of the effective medicinal components of ginseng.
Full-field X-ray Nanoimaging Beamline at SSRF: Biao Deng1; Fen Tao1; Ling Zhang1; Guohao Du1; Tiqiao Xiao1; 1SSRF
Full-field X-ray nano-scope is one of the most powerful tools for in-situ, non-destructive observation of the inner structure of objects with high resolution. A dedicated full field X-ray nano-imaging beamline based on bending magnet is under construction in the SSRF phase-II project. The beamline aims at the 3D imaging of the nano-scale inner structures. The photon energy range is of 5-14keV. The design goals with the FOV of 20 microns and a spatial resolution of 20nm are proposed at 8 keV.And a full-field X-ray nano-CT system based Equally Sloped Tomography(EST) was developed at X-ray imaging beamline(BL13W1). 3D imaging of tantalum particles reconstructed by EST with 128 projections was reported[3]. The nano-scope is ready to be opened to users.
Sub-Second Three Dimensional Dynamic Imaging in Materials Application is Possible After the Relocation of X-ray Imaging Beamline at SSRF: Guohao Du1; Han Guo1; Bian Deng1; Honglan Xie1; Tiqiao Xiao1; 1Shanghai Advanced Research Institute,CAS
Due to building super long beamline in second phase of Shanghai Synchrotron Radiation Facility, the X-ray imaging beamline(BL13W) needs to give way to the long straight beamline, and needs to be relocated to BL13SB at end of 2020. Super B will be used as the light source. BL13SB will provide white beam and monochromatic beam(double multilayer monochromator). White beam mode is used for microsecond dynamic imaging and sub-second dynamic micro-CT; monochromatic beam is used for quantitative X-ray imaging. Microsecond imaging of BL13SB can be used to observe the evolution of materials after impact loading. The sub-second level three-dimensional dynamic imaging can be used to observe the change of the internal three-dimensional shape of the material under the condition of fatigue and other loading conditions, or the internal evolution of the material in some fast processes. BL13SB can provide a powerful experimental for the study of materials science.
3D Characterization of Inhalation Drug Formulations Using X-ray Microscopy
: Hrishi Bale1; Parmesh Gajjar2; Benjamin Tordoff1; Philip Withers3; Darragh Murnane4; 1Carl Zeiss Microscopy Inc.; 2The University of Manchester; 3Henry Royce Institute for Advanced Materials; 4University of Hertfordshire
Drug delivery to the lungs is a highly desirable but extremely challenging field in pharmaceutical sciences. The challenge is to engineer a drug formulation that can reach the deep lungs and can be easily aerosolized and administered when required. Understanding the microstructure of powder formulations is crucial, yet current characterization methods give incomplete information. Conventional techniques like Laser-Diffraction(LD) and Optical-Microscopy(OM) are limited due to the assumption of sphericity and can give variable results depending on particle orientation and dispersion. Furthermore, the challenges of characterizing the formulations are immensely elevated when applied to blends of active pharmaceutical ingredients(API’s) and carrier particles due to their similar density and particle sizes. We present results from a new powder analytical technique using 3D X-ray microscopy applied to characterize pure a-Lactose monohydrate powders with different characteristics. We will also demonstrate results from a new 3D particle classification workflow that accurately classifies particles in a blend.
3D Strength Prediction of a Two-phase Material Using Two-point Statistics: Mostafa Mahdavi1; Eric Hoar2; Steven Liang2; Hamid Garmestani2; 1Georgia Institute of Technology ; 2Georgia Institute of Technology
The strength of materials is depended on the direction of the tensile/compression test. The morphological features in different directions result in different strength values that originate from the apparent anisotropy. Statistical continuum mechanics theory is a fast and efficient method compared to finite element methods that is capable to use the morphological information in a microstructure and calculate the strength. In this study, two-point statistics used to extract the morphological information for a two-phase material. Then, layered fast spherical harmonics formulation was used to represent the 3D map of two-point statistics. Finally, two-point statistics were implemented into statistical continuum mechanics formulations to represent the strength. Two-phase microstructures of Ti-6Al-4V alloy were used in the current study for calibration and validation of the model. This approach is fast and efficient due to using spherical harmonics, furthermore, the model can output strength in all directions simultaneously rather than a single direction.
Reliable Semiconductor Die Attach Process with Ag/Sn/Ag Sandwich Structure: Jinseok Choi1; Sung Jin An1; 1Kumoh National Institute of Technology
A low-cost and eco-friendly die attach process for high temperatures should be developed owing to the expansion of the field of high-temperature applications, such as high-power and high-frequency semiconductors. Backside metallization process is typically used to attach a chip to a lead frame for semiconductor packaging because it has excellent bond-line and good electrical and thermal conduction. In particular, the backside metal with the Ag/Sn/Ag sandwich structure has a low-temperature bonding process (235 °C) and a high remelting temperature (above 400 °C) because the interfacial structure composed of intermetallic compounds with higher melting temperature than pure metal layers after die attach process. Here, we introduce a die attach process with a Ag/Sn/Ag sandwich structure to apply commercial semiconductor packages. After the die attachment, we evaluated mechanical and electrical characteristics of the Ag/Sn/Ag sandwich structure and compared to those of a commercial backside metal (Au-12Ge).
Corrosion of Nb-1% Zr-0.1% C Alloy in Lead-Bismuth Eutectic: Santosh Gupta1; Sanjib Jaypuria1; 1IIT Kharagpur
Lead-Bismuth Eutectic (LBE) are used in systems as coolant to convert energy as it possesses desired properties like large difference between melting and boiling point, low neutron absorptivity and non-reactive with water. Niobium alloy is used as coolant channels in Compact High Temperature Reactors (CHTR). The corrosion of parent material and welded sample is carried out in LBE in static condition at the temperature of 1035 °C in the open air to study the combined effect of corrosion by oxygen and LBE. The corrosion test is followed by measurement of weight loss, dimensional change, X-ray diffraction and SEM/EDS analysis. It is observed that the change in weight and dimension can be attributed to the formation of unstable oxides of niobium. The present study is useful in finding the feasibility of niobium alloy as structural material for coolant channels used in CHTR.
Cancelled
Generation of Synthetic Material Microstructures for Advanced Manufacturing Process Development: Donna Guillen1; Tristan Ashton1; William Harris2; 1Idaho National Laboratory; 2Massachusetts of Institute of Technology
The layer-by-layer deposition of material in additive manufacturing processes creates complex processing conditions and can produce defect-laden microstructures that affect mechanical properties and corrosion performance. Different print and post-processing parameters can result in materials with significantly different microstructures, defect populations and distributions, and internal stresses. A rapid, flexible, and nondestructive, yet statistically comprehensive, reconstruction algorithm, was created for the purpose of digitally synthesizing material microstructures for the screening of salient features. Hierarchical Algorithm for the Reconstruction of Exemplars (HARE) has been developed to reconstruct 3D features in a microstructure from up to three orthogonal 2D exemplars using nearest neighbor matching to reproduce feature qualities, such as shape, size, and distribution. HARE is a convenient and robust base from which to generate statistically representative synthetic microstructures for use in multi-scale modeling or machine learning applications to support advanced manufacturing process development.
Residual Distortion Prediction through Fast Data Driven Model Approach in Additive Manufactured Components: Anahita Imanian1; 1Technical Data Analysis
A critical element for the design, characterization, and certification of components produced by additive manufacturing (AM) processes is the ability to accurately and efficiently model the associated materials and processes. This is necessary for tailoring these processes to endow the final products with proper geometrical and functional features. Capturing these features in AM material requires to solve a multi-scale, transient, heat and thermoplastic structural problem. To minimize the computational burden associated with solving these models, a data-driven modeling approach that does not require solving the thermo-mechanical problem, but is trained to it, is proposed. The framework has been applied to efficiently predict distortions due to residual stresses through the entire AM component.
Impact Mechanics Simulation of Laser Deposited High Entropy Alloys for Aerospace Applications: Modupeola Dada1; Patricia Popoola1; Ntombizodwa Mathe2; Samson Adeosun3; Olufemi Aramide1; Smith Salifu1; 1Tshwane University of Technology; 2Council for Scientific and Industrial Research; 3University of Lagos, Akoka
Advanced materials used for aerospace structural applications must not only be lightweight for the reduction of fuel consumption but also be strong to undergo plastic deformation and prevent basic failures primarily caused by a fracture. Crack formation and propagation arise when the stresses at the temperature below the melting point of the high entropy alloy material cause the body of the operational part to separate during service. Hence, it is important to understand the damage and impact mechanisms of laser deposited high entropy alloys. In this study, the low and high-velocity impact responses of high entropy alloys were simulated using Abaqus CAE/2019 to enable the practical design of lightweight high entropy alloys with enhanced survivability for aerospace structural applications.
Study the Initiation of Hot Cracking Phenomenon During the Processes of Laser Welding: Guannan Tang1; Anthony Rollett1; 1Carnegie Mellon University
This work seeks to understand the initiation of hot cracking during laser welding process. In this work, we are presenting an analysis relating the initiation of hot cracking to micro-defects formed at grain boundaries during solidification. A new index of hot cracking susceptibility was derived out of this and was used to evaluate the susceptibility rank of 12 alloys. The ranking result agrees well with experimental measurements from the literature. Moreover, a hot cracking model was established based upon this analysis to predict local micro-defects coalescence tendency and quantify it as the local susceptibility of hot cracking initiation. This approach used a combined Thermal Lattice Boltzmann-cellular automaton (TLB-CA) code to simulate thermal distribution and microstructure evolution. The associated thermal micromechanical fields were analyzed with a spectral code called Micromechanical Analysis of Stress-Strain Inhomogeneities with Fourier transforms (MASSIF). Validation of the results was made through Dynamic X-ray Radiography (DXR) data.
Virtual Indentation: Schematic Representation, Elementary Meshing, Material Models, Simulation Results: Andrey Musienko1; 1NRC «Kurchatov Institute» - CRISM «Prometey»
Indentation is known way of studying of material, its superficial properties. Modern computer simulation allows to reproduce interesting numerical schemes in computer aided framework, arrange suitable finite element meshing, connect elasto-plastic constitutive equations and sets of parameters to model material properties in order to receive interesting results of fields in mechanical stress and deformations near indenter tip. Results of simulations for the scheme with conic indenter were obtained. Specificity of calculated fields taking into account the influence of crystallographic anisotropy were considered.
Multimodal Investigation of Particle Stimulated Nucleation in Cold Rolled AA5182 Aluminum Alloy: Elisabeth Knipschildt1; Xiuchuan Lei2; Yubin Zhang1; Søren Fæster1; Wenjun Liu3; Robert Sanders2; Dorte Juul Jensen1; 1Technical University of Denmark - DTU; 2Chongqing University; 3Argonne National Laboratory
Recrystallization governs the final microstructure of thermal processed metals and is thereby of high interest in both industry and research. However, most recrystallization experiments are carried out in 2D not fully describing the bulk 3D materials. In this study, the efficiency of particle stimulated nucleation (PSN) by large second phase particles in 75 % cold rolled AA5182 aluminum alloy is investigated by two different non-destructive high-resolution 3D techniques. Conventional absorption contrast tomography is used to reveal second phase particles, while the high resolution of Laue micro-diffraction is exploited to reveal recrystallized nuclei. Data registration between the two 3D volumes is performed by relating areas in Laue patterns with increased occurrence of un-indexed peaks with second phase particle positions in the tomography data. This registration methodology is discussed and the importance of PSN for the recrystallization of this aluminum alloy is quantified.
3D Non-destructive Characterization of Electrical Steels for Quantitative Texture Analysis with Lab-based X-ray Diffraction Contrast Tomography (DCT).: Jun Sun1; Jette Oddershede1; Ivan Petryshynets2; Li Meng3; Ning Zhang3; Yang Li4; Florian Bachmann1; Erik Lauridsen1; 1Xnovo Technology ApS; 2Slovak Academy of Sciences; 3Central Iron and Steel Research Institute; 4University of Science and Technology Beijing
Electrical steels are core materials for electrical appliances and equipment. The magnetic properties determine the material efficiency in service and strongly depend on the grain structure – in particular on texture. Knowing which texture components are present and where they are located spatially is key to understanding the mechanisms of texture evolution during processing. Recent developments of lab-based DCT include advanced acquisition strategies, allowing users to seamlessly collect and reconstruct diffraction data covering large representative volumes while accommodating a variety of sample geometries, including plate-like specimens.With case studies of both non-oriented and grain-oriented electrical steels, lab-based DCT demonstrates its potential for advanced characterization of the grain structure and texture of electrical steels. Compared with commonly used techniques such as light optical microscopy, X-ray diffraction and electron backscattered diffraction, lab-based DCT complements the characterization needs for electrical steels with its 3D capability as well as large representative volume imaging.
Dissimilar Material Welding of CFRP-AA6061 using Vaporizing Foil Actuator Welding: YuHyeong Jeong1; Wonju Lee1; Hyung-gyu Kim1; Jonghun Yoon1; 1Hanyang University
Vaporizing foil actuator welding(VFAW) performs the joining by colliding the two dissimilar materials using high pressure, which generated by vaporizing aluminum foil. To vaporize the aluminum foil, a high-rate transmission of current pulse is applied to the foil and the high vaporization pressure is formed as a result. This pressure pushes the flyer sheet and it collides to the target sheet.Al6061-T4 and carbon fiber plate were used for target and flyer sheet to attach both materials. First, a hole was drilled on the carbon fiber and aluminum sheets were located at the top and bottom side of carbon fiber. When the VFAW process was conducted in this setting, the flyer aluminum sheet was collided with other aluminum sheet, by passing through the hole of carbon fiber. As a result, both aluminum sheets were welded, and carbon fiber was bonded with them tightly.
Synergistic Nanoscale Precipitation in Austenitic Steels as Revealed by Atom-Probe Tomography: Colin Stewart1; Richard Fonda1; Keith Knipling1; Patrick Callaham1; Paul Lambert2; 1US Naval Research Laboratory; 2US Naval Surface Warfare Center, Carderock Division
A new family of precipitation-strengthened FCC Austenitic steels has been developed via an integrated computational materials engineering (ICME) approach, achieving impressive hardness values over 500 HV, for an estimated yield strength of ~180 ksi. An Austenitic Fe–17.7Mn–10.0Ni–5.0Al–4.7Cr–4.0Cu–0.48C (wt.%) alloy produces three nano-scale phases upon ageing, without prior rolling steps: (i) insoluble Cu (FCC) particles; (ii) ordered intermetallic β-NiAl (B2) precipitates; and (iii) carbides. In this series of alloys, the formation of β-NiAl particles is only observed with Cu additions, suggesting a precipitation synergy between these particles. 3D data from atom-probe tomography is used to investigate the mechanisms of particle formation and synergy. The evolution of precipitate microstructures are evaluated at various ageing time steps to assess particle size and distribution, chemical segregation, and particle co-location. The insight gained from this analysis will help inform future ICME development of other precipitation strengthened alloys.
In Operando Multimodal and Multiscale Study of Degradation and Sodium Storage Process in Sodium-ion Batteries.: Domenico Battaglia1; Anna Fedrigo2; Daniel Sørensen3; Salvatore De Angelis1; Nikolaj Zangenberg4; Søren Schmidt5; Luise Kuhn1; 1Technical University of Denmark; 2ISIS neutron and muon source; 3Max IV Laboratory; 4Danish Technological Institute; 5European Spallation Source
Neutron imaging is a great tool for battery analysis as Bragg edge imaging and tomography can investigate reversible and irreversible processes happening in sodium-ion batteries (SIBs). By measuring wavelength/time-resolved transmitted neutron intensity, Bragg edge imaging allows us to obtain wide crystallographic information on the investigated material. Neutron tomography can provide essential information on morphological properties of the electrodes, such as particles’ shape, size distribution, and interface areas. With these techniques, we will investigate SIBs, in operando, to study the ionic transport and storage mechanisms, and other phenomena such as degradation upon cycling, and the dendrite growth process. Throughout the project, we will investigate Prussian blue derivatives and hard carbon, as promising electrode materials for SIBs. This multiscale and multimodal project will rely on synchrotron techniques at large-scale facilities, to complement the neutron data and benefit from the higher resolution and fast acquisition times of such instruments.
Determination of Ligament Quality Factors in Additively Manufactured Lattice Structures Using In-situ Compression Testing Micro-CT: Vincent DiNova1; Holly Flynn1; Aaron Guckenberger1; 1Savannah River National Laboratory
In response to the need for an automated, commercial method to qualify additively manufactured lattice components, an experiment was conducted to evaluate the effects of defective lattice ligaments on compression yield strength. Lattice samples with known defective or missing ligaments were compressed using a DebenCT5000 and imaged using Micro-CT. The force and CT results were compared to defect free standards. Local and global information about each ligament in the lattice are extracted using LatticeJ, a proprietary software package developed at SRNL, and fed into COMSOL to perform finite element analysis and determine quality factors. The verification of the local and global effects of defective struts are used to train machine learning algorithms to assign each ligament with a quality factor and identify the number of defective ligaments in the lattice. The results of destructive testing will be used to qualify future parts using X-ray CT.
Machine-learning Model to Identify and Classify Dislocations in Aluminum via 3D Dark Field X-ray Microscopy: Pin-Hua Huang1; 1Stanford University
The mechanical properties of metals strongly depend on their structure dislocation composition at the level of the crystal lattice. Methods like annealing alter mechanical properties through interactions of dislocations to form 3D hierarchical structures. Dark Field X-ray Microscopy (DFXM) is a unique new method that was recently demonstrated as being able to resolve subsurface deformations. 3D DFXM was recently shown by our group to be able to construct 4D scans of space and rocking curves into spatially 3D deformation maps of the crystal, to provide direct maps of dislocations. We can now resolve detailed 3D structures of dislocation networks that span 150x300x300-μm3 volumes with 150-nm spatial resolution in post-annealed single crystalline aluminum. My work applies machine learning methods to identify and sort individual dislocations in these 3D datasets. Our approach demonstrates a progress towards full microstructural characterization over length scales now accessible with the new capabilities afforded by DFXM.
Analysis of Fibers, Pores, and Mechanical Properties in µCT-scan of a Long Fiber-reinforced Thermoplastic: Andreas Grießer1; Aaron Widera1; Martina Hümbert1; 1Math2Market GmbH
Long fiber-reinforced thermoplastics are highly popular as they combine comparably low material cost, efficient production processes, e.g. injection molding, and good mechanical properties. In this study, we analyze the µCT-scan of a glass fiber-reinforced polypropylene with a complex microstructure of fibers, polymer, and pores. The manufacturing process, leading to three layers with different fiber orientations, further increases the complexity of the microstructure. The sample is analyzed digitally to thoroughly understand this intricate microstructure.First, the fibers in the scan are identified using Artificial Intelligence. Among other analyses, the fiber orientation is examined also through the thickness of the scan. This shows the typical three-layer structure of injection molded materials. Then, the pores are identified using a watershed-based algorithm and their shape, diameter, and location are analyzed. We find that the voids are mainly located in the inner region, where the fibers do not align with the flow direction.
Buried Within: Targeted 3D Multiscale Imaging and Analysis in Bulk Samples: Stephen Kelly1; Robin White1; Hrishikesh Bale1; Sam Kalirai2; William Fadgen1; William Harris1; Tobias Volkenandt1; 1Carl Zeiss RMS; 2Carl Zeiss X-ray Microscopy
Multiscale, multimodal, correlative imaging presents a powerful opportunity for materials research, especially when extended beyond 2D surface imaging and into the 3D realm where true microstructures and important properties of complex, functional materials can be characterized. Traditional approaches to targeted multiscale 3D characterization have relied on near-surface regions in a quasi-3D or 2.5D approach, or complex disconnected bulk sectioning to reveal deeply buried features. The advent of the femtosecond laser and its subsequent integration into modern FIB-SEM instruments has opened the door for a radically different approach to this type of work where 3D non-destructive X-ray microscopy images can be used to guide active exposure and analysis of targeted, deeply buried regions of interest in bulk samples. Beyond analysis in the FIB-SEM instrument, samples can be prepared for analysis with other techniques. We demonstrate the utility of this workflow on samples ranging from advanced electronic packaging to battery electrodes.
Combining Tomography and Scanning 3DXRD to Study Voids During Ductile Failure: Bjarke Østergaard1; Mustafan Kutsal1; Kim Nielsen1; Henning Poulsen1; Grethe Winther1; 1Technical University Of Denmark
Ductile failure of metals proceeds by nucleation, expansion and coalescence of voids in the microstructure. The evolution of voids is monitored by tomography. At the same time precipitates in the metal are visualized. The initial microstructure of the polycrystalline metal (AA1050) has been characterized by 3DXRD but due to spot overlap this is not possible in the deformed microstructure at the strain level where voids appear. Instead tracking of the precipitates across deformation steps is utilized to follow the morphology of the grain structure. To obtain the local crystallography around voids, scanning-3DXRD is employed. The experimental data will serve as input to crystal plasticity simulations.
Novel tools to visualize 4D information at a glance: Flippoint Detection: Wesley De Boever1; Jan Dewanckele1; Frederik Coppens1; 1Tescan
Dynamic computed tomography (CT) approaches or uninterrupted acquisitions of deforming materials have rapidly emerged as an essential technique to understand material evolution, facilitating in situ investigations ranging from mechanical deformation to fluid flow in porous materials and beyond.Dynamic acquisitions however, generate vast amounts of raw projection data, which need to be reconstructed, further post processed and eventually quantified. It is therefore essential to devise workflow strategies to quickly identify the interesting moments prior to reconstruction to optimize the amount of data that is generated. In a next step, the data needs to be visualized. This can be done by loading a series of volumes, but typically there is too much information to be visually processed at the same time. To extract meaningful information in a fast and user friendly way, a smart ‘flippoint’ approach was implemented, directly incorporating the time dimension within the 3D analysis flow.