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At least 397 records · Page 22

A Novel Approach to Simulate Realistic Concrete Microstructures under Irradiation

The concrete biological shield of light water reactors is exposed to high neutron and gamma irradiation doses in the long term. Irradiation deteriorates the physical and mechanical properties of concrete. Such effects need to be investigated to predict the concrete’s performance in the event of a lifetime extension of a nuclear power plant. This work combines high-resolution characterization techniques with fast-Fourier transform (FFT)-based 2-D simulations to evaluate the radiation-induced volumetric expansion (RIVE) and damage in concrete microstructures under neutron irradiation. Two concrete microstructures from samples provided by the Japan Concrete Aging Management Program (JCAMP) were characterized using micro x-ray fluorescence (mXRF) to obtain elemental intensity maps, and energy-dispersive x-ray spectroscopy to complement mXRF with local elemental information for Na. Minerals and cement paste are then identified based on the elemental composition to produce high-resolution phase maps, resulting in a more accurate representation of the microstructures compared to previous work. Simulations of radiation-induced volumetric expansion (RIVE), creep, and damage in JCAMP concrete use the fast Fourier transform (FFT)-based code Microstructure Oriented Scientific Analysis of Irradiated Concrete (MOSAIC) combined with the irradiated minerals, aggregates, and concrete (IMAC) database, which contains mineral-specific RIVE models. Overall, the simulation results are in fair agreement with experimental data.

Cheniour, Amani↗

Microstructure and Mechanical Properties of Additively Manufactured Haynes 282: A Comparative Analysis between L-PBF and LP-DED Technologies

This study compares the microstructure and tensile properties of Haynes 282 fabricated using laser powder bed fusion and laser powder directed energy deposition. Both sets underwent stress-relieving, followed by hot isostatic pressing, and the standard double aging heat treatment. Tensile testing was conducted at room temperature on specimens fabricated with both technologies to evaluate and compare their tensile behaviors. Results show that the ultimate tensile and yield strengths of laser powder bed fused specimens were 18% and 57% higher, respectively than those of laser powder directed energy deposited ones, whereas the elongation to failure was similar in both. The difference in strengths is attributed to the differences in the size of ɣ' precipitates and grains, i.e., those in the LP-DED specimens being larger, whereas similar elongation to failure is attributed to the carbide debonding dominating the fracture mechanism in both batches.

Additive manufacturing↗

Surface and subsurface characterization of laser-interference structured Ti6Al4V

Ti6Al4V specimens were exposed to high-energy laser pulses of 1.24 J/cm 2 fluences per pulse using a two-beam optical configuration to attain laser-interference. In addition to the formation of periodic surface textures by laser-interference, scanning electron microscope (SEM) images demonstrated several microstructural changes on the surface processed. Moreover, the surface and subsurface of Ti6Al4V specimens were characterized for the as-received and laser-interference processed conditions using x-ray photoelectron spectroscopy (XPS) and electron energy dispersive spectroscopy (EDS). The XPS data showed that this laser technique is effective at removal of surface contaminants for Ti6Al4V. The XPS analysis also revealed the formation of an oxy-nitride layer on the laser treated material. Finally, the microstructure analysis indicates that grain refinement, dendrite and twin structures were found near the surface due to laser processing.

36 MATERIALS SCIENCE↗

Determination Of Grain-Size Distributions

Images of microstructures analyzed by transform methods. Report discusses determination of distributions of grain sizes by analysis of images of microstructures.

Generazio, Edward R.↗

Microstructure Scale Lithium-Ion Battery Modeling, Part IV: The Representativity of Microstructure Parameters and Electrochemical Response

Lithium-ion battery electrochemical models require an accurate description of the electrodes microstructures to be predictive, that can be achieved through nanoscale imaging. Such observations are however limited by their field of view (FOV), as they provide only a subset of the whole electrode volume that does not necessarily represent the whole electrode microstructure heterogeneity, and therefore can bias the analysis. A representativity analysis has been performed on the microstructure parameters and, in a novel way, on the full cell electrochemical response to evaluate the predictions representativeness, and thus relevance, of a microstructure scale electrochemical model. The microstructure parameter deviation propagations to the electrochemical response have been quantified for different charge rates. This defines a threshold for the microstructure parameters FOV for a desired maximum deviation of the electrochemical response. Electrochemical model shows cell representative section areas are increasing with C-rate, due to higher in-plane heterogeneities, indicating larger FOVs are required specifically for fast charge modeling. Representativity analysis determines a cell FOV of 144.4 × 154.4 μm 2 is large enough to establish a convergence on the representative section areas for low-intermediate C-rate (≤2.5 C), therefore positively concludes on the model representativeness for these rates, but is not large enough to conclude for higher rates.

25 ENERGY STORAGE↗

Machine learning insights into microstructural origins of transport and mechanical properties in porous microstructures

Multifunctional porous materials are increasingly needed across various fields, but their complex microstructures create significant challenges due to the intricate microstructure-property relationships. This complexity, combined with limitations of traditional analysis methods, hinders efforts to understand and optimize microstructure–property relationships. Here, to address this, we integrate physics-based mesoscale modeling with interpretable machine learning (ML) to uncover how microstructural features govern effective diffusivity and elastic modulus. At constant porosity, we show diffusivity varies by over 150 × and modulus by ∼50 ×, highlighting the power of microstructure engineering. Statistical analysis reveals bimodal behavior in diffusivity and unimodal in modulus. ML identifies connectivity as the dominant factor, while modulus is also sensitive to domain size and feature interactions. Controlled simulations further highlight domain shape as a critical feature for modulus. This framework enables efficient exploration of microstructure-property correlations, offering new insights to guide the design of advanced porous materials.

Bicontinuous microstructure↗

Volumetric analysis and mesh generation of real and artificial microstructural geometries

Producing a viable finite element mesh of realistic microstructural structural geometry is a critical step in analyzing the thermo-mechanical behavior of complex multi-material composites. Advancements in imaging technology such as micro computed tomography have allowed modelers to access high resolution mesoscale geometries for direct numerical simulation. However, converting from voxel based 3D images to usable finite element meshes has been challenging. A robust method including algorithms and software scripts for generating finite element meshes from 3D imaged microstructures is presented in this paper. It includes a routine for inserting cohesive elements around material interfaces to enable modeling of interface properties including delamination and damage. The algorithms and procedures presented in this method leverage currently available software packages for processing surface based geometry into volume based meshes. In addition to converting real geometry from physical imaging systems, algorithms for producing numerically generated and statistically equivalent microstructural geometry are also included. These artificial microstructures can be a valuable resource for modelers when physical specimens do not exist or are limited in quantity: Method establishes a workflow from voxel data to viable finite element mesh including interface information, and Includes a method for synthetic geometry generation based on metrics from real microstructures.

36 MATERIALS SCIENCE↗

Coordinated Microstructural and Isotopic Characterization of Diamond Inclusions within the Kenna Ureilite

Introduction: The origin of diamonds in ureilitic meteorites, a major family of ultramafic achondrites, has long been debated, with various formation mechanisms inferred, including: 1) shock conversion of preexisting graphite due to a hypervelocity impact on the ureilite parent body [e.g., 1]; 2) vapor deposition during condensation of the solar nebula [e.g., 2]; or 3) static transformation in the mantle of a large planetesimal (>1000 km in diameter) [e.g., 3]. The Kenna ureilite is a 10.9 kg stone that was found in Kansas in 1972 and is dominantly composed of olivine and pigeonite (68% and 22% modal abundance, respectively), together with minor metal and carbon-rich regions. Within the carbon-rich domains researchers have identified microdiamonds up to ~10 µm in size [4]. Methods: Due to the proximity of the extremely hard microdiamonds with soft graphite and moderately hard silicates, achieving an appropriately flat surface for electron backscatter diffraction (EBSD) analysis has proven challenging. We have, therefore, employed a Hitachi ArBlade 5000 broad beam Ar ion milling system to prepare a sample with an adequately uniform surface flatness across the various minerals. The ion milling dramatically im-proved indexing of the EBSD patterns and facilitated high-resolution microstructural analysis of the carbon-rich domains. After microstructural EBSD analyses using an Oxford Symmetry detector we collected coordinated hy-perspectral cathodoluminescence (CL) analyses using a Gatan Monarc system mounted on a JEOL 7900F field emission (FE) scanning electron microscope at NASA Johnson Space Center. A focused ion beam (FIB) foil was extracted from a region of interest and analyzed using a JEOL 2500 FE scanning transmission electron microscope (STEM). In situ carbon and nitrogen isotopic analyses were collected from diamond-bearing domains using a Cameca NanoSIMS 50L at NASA JSC. Results: The carbon rich regions occur as tabular domains between polygonal olivine and pigeonite, and are composed of aggregates of micrometer-scale diamond with intermediate graphite, oxides and metal grains. Within the microdiamonds, {111} twins are abundant, many of which form ragged lamellae consistent with mechanical twinning. The microdiamond assemblages appear to pseudomorph tabular graphite habits, which together with the abundant deformation twins, support a shock transformation mechanism for microdiamond formation within the Kenna meteorite. Further supporting this observation, the diamond laths show close alignment of <111> and <110> between domains, consistent with a solid-state transformation from graphite along <0001> and <1-210>, respec-tively [5]. A FIB foil was extracted from a region with mechanical twins, and high resolution STEM analyses reveal cross-cutting veins of graphite and oriented kamacite crystals together with additional sets of {111} nano-twins formed in at least three orientations. Isotopic analyses of C and N reveal sector zoning patterns [cf. 3] that are unre-lated to the diamond substructure identified by EBSD yet consistent with hyperspectral CL images. Conclusions: These data provide new constraints on microdiamond formation within ureilites. The microdia-monds exhibit orientation variants defined by aligned <111> and <110> axes consistent with inherited crystallo-graphic orientations from transformation of a single hexagonal graphite parent crystal [5]. Crosscutting the micro-diamonds are veins of graphite and kamacite, together with additional {111} nanotwins. Taken together these data suggest that microdiamonds from ureilites formed from a solid state, diffusionless transformation from graphite, likely associated with a major shock event, which was subject to subsequent reversion either during decompression or a later deformation event. The N and C isotopic sector zoning is unrelated to diamond microstructures and likely reflects inheritance from the parent graphite crystal.

Ureilite↗

Modeling of Damage Initiation and Progression in a SiC/SiC Woven Ceramic Matrix Composite

The goal of an ongoing project at NASA Glenn is to investigate the effects of the complex microstructure of a woven ceramic matrix composite and its variability on the effective properties and the durability of the material. Detailed analysis of these complex microstructures may provide clues for the material scientists who `design the material? or to structural analysts and designers who `design with the material? regarding damage initiation and damage propagation. A model material system, specifically a five-harness satin weave architecture CVI SiC/SiC composite composed of Sylramic-iBN fibers and a SiC matrix, has been analyzed. Specimens of the material were serially sectioned and polished to capture the detailed images of fiber tows, matrix and porosity. Open source analysis tools were used to isolate various constituents and finite elements models were then generated from simplified models of those images. Detailed finite element analyses were performed that examine how the variability in the local microstructure affected the macroscopic behavior as well as the local damage initiation and progression. Results indicate that the locations where damage initiated and propagated is linked to specific microstructural features.

Mital, Subodh K.↗

Microstructure reconstruction of battery polymer separators by fusing 2D and 3D image data for transport property analysis

A new approach to generate high-fidelity 3D microstructure reconstructions by leveraging resolution and sample volume characteristics from 2D and 3D microscopy methods is presented here. This approach is employed to model the microstructure of a highly orthotropic polypropylene separator used in lithium-ion batteries, which have challenging multi-scale features of fibrils (<100 nm) and lamellae (>100 nm) to resolve in 3D. Phase contrast nano X-ray computed tomographic data are used to reconstruct the lamellae phase, while 2D scanning electron microscopy data are used to characterize sub-100 nm microstructure features such as the thin fibrils that are beyond the effective resolution of X-ray computed tomography. Fibril geometries are reconstructed stochastically based on the 2D higher resolution data, and integrated with the lamellae geometries in 3D space. Transport property analyses are performed to investigate the bias of microstructure models without considering the fibrils. A sensitivity study is also conducted to facilitate understanding of the relationship between microstructure characteristics and transport properties.

25 ENERGY STORAGE↗

Simulation-guided analysis of resonant soft X-ray scattering for determining the microstructure of triblock copolymers

Resonant soft X-ray scattering (RSoXS) probes structure with chemical sensitivity that is useful for determining the morphology of multiblock copolymers. However, the hyperspectral scattering data produced by this technique can be challenging to interpret. Here, in this study, we use computational scattering simulations to extract the microstructure of a model triblock copolymer from the energy-dependent scattering from RSoXS. An ABC triblock terpolymer formed from poly(4-methylcaprolactone) (P4MCL), poly(2,2,2-trifluoroethylacrylate) (PTFEA), and poly (dodecylacrylate) (PDDA), P4MCL-block-PTFEA-block-PDDA, was synthesized as the model triblock system. Through quantitative evaluation of simulated scattering data from a physics-informed set of candidate structure models against experimental RSoXS data, we find the best agreement with hexagonally packed core–shell cylinders. This result is also consistent with electron-density reconstruction from hard X-ray scattering data evaluated against electron-density maps generated with the same model set. These results demonstrate the utility of simulation-guided scattering analysis to study complex microstructures that are challenging to image by microscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of powder layer thickness on the microstructural development of additively manufactured SS316

By Increasing the powder layer thickness we could increase material deposition rates and reduce build times during laser powder bed fusion (LPBF). However, increasing the powder layer thickness could also negatively affect the local melting and subsequent microstructure of the printed material. This study systematically investigated, for the first time, the defect evolution and microstructural changes of LPBF stainless steel 316 (SS316) processed by using various powder layer thicknesses of 40, 80, and 120 μm while also varying the laser dwell time for the pulsed laser. Through image analysis, the pore density was found to increase with increasing powder layer thickness, particularly when the dwell time was too high or too low. The maximum achievable density (>99%) was found over a wide processing window when using the smallest powder layer thickness of 40 μm between dwell times of 60 and 100 μs. Increasing the powder layer thicknesses to 80 and 120 μm resulted in maximum densities of 98.7 and 96.8%, respectively, but the window for acceptable laser dwell times that could achieve these densities narrowed considerably. A microstructural analysis of the melt pools was performed to measure the melt pool depths and widths, both of which increased with increasing dwell time. However, increasing the powder layer thickness did not affect the melt pool depth and only minorly affected the width. A sub-grain cellular structure distinguished the melt pool boundaries. The cell size increased with increasing dwell time and decreasing powder layer thickness. Moreover, the cell size was used to calculate a cooling rate that had a magnitude of 10 7 K/s and increased with increasing powder layer thickness.

36 MATERIALS SCIENCE↗

Microstructural Constraints on the Formation of Diamond in Ureilites, the Case from the Kenna Meteorite

The origin of diamonds in ureilitic meteorites, a major family of ultramafic achondrites, has long been debated, with various formation mechanisms inferred, including: 1) shock conversion of preexisting graphite due to a hypervelocity impact on the ureilite parent body; 2) vapor deposition during condensation of the solar nebula; or 3) static transformation in the mantle of a large planetesimal (>1000 km in diameter). The Kenna ureilite is a 10.9 kg stone that was found in Kansas in 1972 and is dominantly composed of olivine and pigeonite (68% and 22% modal abundance, respectively), together with minor metal and carbon-rich regions. Within the carbon-rich domains researchers have identified microdiamonds up to ~10 µm in size. Due to the proximity of the extremely hard microdiamonds with soft graphite and moderately hard silicates, achieving an appropriately flat surface for electron backscatter diffraction (EBSD) analysis has proved challenging. We have, therefore, employed a Hitachi ArBlade 5000 broad beam Ar ion milling system to prepare a sample with an adequate surface uniformity. The ion milling dramatically improved indexing of the EBSD patterns and facilitated high-resolution microstructural analysis of the carbon-rich domains. The carbon-bearing regions occur as tabular domains between polygonal olivine and pigeonite, and are composed of aggregates of micrometer-scale diamond with intermediate graphite, oxides and metal grains. Within the microdiamonds, {111} twins are abundant, many of which form ragged lamellae consistent with mechanical twinning. The microdiamond assemblages appear to pseudomorph tabular graphite habits, which together with the abundant deformation twins, supports a shock transformation mechanism for microdiamond formation within the Kenna meteorite. To compliment the EBSD microstructural analyses, coordinated laser Raman, focused ion beam/transmission electron microscopy imaging and diffraction data, and NanoSIMS N and C tomographic isotopic imaging will be collected. These data will provide further constraints on the formation of diamonds within ureilites.

Timmons M Erickson↗

Influence of geometry on columnar to equiaxed transition during electron beam powder bed fusion of IN718

Correlation between spot-melt scan parameters (linear spot-density aka areal energy density), build geometry, and solidification microstructure evolution (columnar vs equiaxed) in a powder bed fusion technology is investigated. It is shown that to maintain the equiaxed solidification microstructure evolution in electron beam powder bed additive manufacturing (AM), the areal energy density per layer needs to be scaled with respect to the 2D cross-sectional area of the layer being melted. Samples with two different cross-sectional areas (40 × 40 mm and 20 × 20 mm) have been fabricated with varying areal energy densities. For a given square cross-section (20 × 20 mm), increasing the areal energy density (4.8 MJ/sq.m to 14.7 MJ/sq.m) transitioned the solidification microstructure from columnar to equiaxed. The observed microstructure data (Electron Back Scattered Diffraction - EBSD) is quantified by calculating the principal component (PC) score using a spatial statistics methodology. The sample with equiaxed grains is found to have a low PC score while the sample with columnar grain had a high PC score. A semi-analytical model is used to simulate the heat transfer and the local solidification conditions as a function of processing parameters (linear spot-density). The result from the heat transfer model is correlated with previously quantified microstructure data. Space-Time analysis of the melt pattern is done and correlated with the observed microstructure. In addition, from the findings, appropriate parameters have been used to additively manufacture a turbine blade with site-specific or hybrid solidification microstructure (traditional fabrication possible via a patented method of localized cold working and heat treatment).

36 MATERIALS SCIENCE↗

Characterization of Al-Cu-Mg-Ag Alloy RX226-T8 Plate

Aluminum-copper-magnesium-silver (Al-Cu-Mg-Ag) alloys that were developed for thermal stability also offer attractive ambient temperature strength-toughness combinations, and therefore, can be considered for a broad range of airframe structural applications. The current study evaluated Al-Cu-Mg-Ag alloy RX226-T8 in plate gages and compared performance with sheet gage alloys of similar composition. Uniaxial tensile properties, plane strain initiation fracture toughness, and plane stress tearing resistance of RX226-T8 were examined at ambient temperature as a function of orientation and thickness location in the plate. Properties were measured near the surface and at the mid-plane of the plate. Tensile strengths were essentially isotropic, with variations in yield and ultimate tensile strengths of less than 2% as a function of orientation and through-thickness location. However, ductility varied by more than 15% with orientation. Fracture toughness was generally higher at the mid-plane and greater for the L-T orientation, although the differences were small near the surface of the plate. Metallurgical analysis indicated that the microstructure was primarily recrystallized with weak texture and was uniform through the plate with the exception of a fine-grained layer near the surface of the plate. Scanning electron microscope analysis revealed Al-Cu-Mg second phase particles which varied in composition and were primarily located on grain boundaries parallel to the rolling direction. Fractography of toughness specimens for both plate locations and orientations revealed that fracture occurred predominantly by transgranular microvoid coalescence. Introduction High-strength, low-density Al-Cu-Mg-Ag alloys were initially developed to replace conventional 2000 (Al-Cu-Mg) and 7000 (Al-Zn-Cu-Mg) series aluminum alloys for aircraft structural applications [1]. During the High Speed Civil Transport (HSCT) program, improvements in thermal stability were demonstrated for candidate aircraft wing and fuselage skin materials through the addition of silver to Al-Cu-Mg alloys based on Al 2519 chemistry [2]. Thermal stability of the resulting Al-Cu-Mg-Ag alloys, C415-T8 and C416-T8, was due to co-precipitation of the thermally stable . (AlCu) and ' (Al2Cu) strengthening phases [1-4]. The strength and toughness behavior was investigated for these alloys produced as 0.090-inch thick rolled sheet in the T8 condition and after various thermal exposures. The mechanical properties were shown to be competitive with conventional aircraft alloys, 2519-T8 and 2618-T8 [2]. During the Integral Airframe Structure (IAS) program, advanced aluminum alloys were examined for use in an integrally stiffened airframe structure where the skin and stiffeners would be machined from plate and extruded frames would be mechanically attached (see Figure 1) [5]. Advantages of integrally stiffened structure include reduced part count, and reduced assembly times compared to conventional built-up airframe structure. The near-surface properties of a thick plate are of significance for a machined integrally stiffened airframe structure since this represents the skin location. Properties measured at the mid-plane of the plate are more representative of the stiffener web. RX226 was developed to exploit strength-toughness improvements and thermal stability benefits of Al-Cu-Mg-Ag alloys in plate gages. This study evaluated the microstructure and properties of three gages of plate produced in the T8 condition.

Lach, Cynthia L.↗

Boundary characterization using 3D mapping of geometrically necessary dislocations in AM Ta microstructure

Additive manufacturing (AM) of high strength metallic materials produces microstructures and defects that deviate substantially from those created through conventional manufacturing methods. It has recently been demonstrated that with application of extreme energy densities, a high-temperature refractory metal, tantalum (Ta), can be printed to a fully dense state with exceptionally low porosity. Here we employ a combination of three-dimensional electron backscattered diffraction (EBSD) TriBeam technology and crystallographic geometrically necessary dislocation (GND) theory to characterize the microstructure and defect boundaries of this unusual AM product. Two-dimensional (2D) EBSD and these three-dimensional (3D) measurements indicate that the microstructure of AM Ta is highly oriented <111> along the build direction, yet at the same time contains large crystallographic orientation gradients that span mm’s across the build. Crystallographic GND density analysis of the 3D microstructure reveals that highly misoriented subboundaries exist within this strongly textured microstructure that have large dislocation densities of 1×10 16 m –2 , just as large as those comprising the high-angle grain boundaries (HAGBs) in the same material. The 3D crystallographic GND density mapping reveals these subboundaries are part of a complex, finely spaced network that extends throughout the entire microstructure. Here, the orientation of these boundaries can be related to the scan strategy used during printing. TEM measurements corroborate an extremely high dislocation density at the microscale and indicate a cell-like dislocation network structure existing in the AM Ta at the sub-μm scale.

36 MATERIALS SCIENCE↗

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Ceramics↗

X-ray computed tomography-based porosity analysis: Algorithms and application for porous woody biomass

The properties of lignocellulosic biomass, such as bulk physical, thermal, and mechanical properties, as well as the mobility of enzymes or catalysts, are largely affected by porosity, pore structures, and pore size distribution. While X-ray computed tomography (CT) has been introduced to effectively produce 3D volumetric images of material microstructure, a quantitative porosity analysis from the 3D images has never been done. This work introduces a first-of-its-kind X-ray CT-based quantitative porosity analysis method and applies the developed toolkit to characterize the internal porosity distribution of loblolly pine. A sample loblolly pine chip was scanned by a nano-resolution X-ray CT system and digitally reconstructed after a sequence of image processing operations. Here, a comprehensive porosity analysis was then performed to quantify the envelope porosity, the spatial distribution of local porosity, and the directional porosity. Solutions to the various challenges in image processing, porosity calculation, and large data handling are provided.

42 ENGINEERING↗