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At least 415 records · Page 23

Multiscale porosity characterization in additively manufactured polymer nanocomposites using micro-computed tomography

Extrusion-based additive manufacturing (AM) of polymer composites exhibits complex thermally driven phenomena that introduce severe discontinuities in the internal structure across length scales, especially voids or porosity. This study utilizes a high-throughput porosity characterization technique to analyze large datasets from numerous micro-computed tomography (mu CT) scans to capture the influence of AM print parameters on the size, shape, and location of porosity across multiple print layers (up to a few cm) on fused granular fabrication (FGF) printers. The materials investigated include nanocomposite formulations based on commercially relevant nylon-12 and polyether ketone ketone (PEKK) materials comprising nano- or micro- sized fillers. The estimated global porosity follows an inverse linear correlation against the bulk density of the printed samples. Increasing the extrusion multiplier (EM) and the nozzle temperature while decreasing the print speeds reduces the global porosity. Outlier analyses (local porosity morphology) show that faster print speeds and higher extrusion rates result in long, slender inter-layer voids, while lower nozzle temperatures lead to large, symmetrical, inter-bead voids (at the bead junction). Lack of active chamber temperature increases inter-layer and intra-bead voids with a two-fold increase in global porosity. Overall, the micro filler-reinforced composites exhibit higher global porosity than nanofiller-reinforced composites, which is attributed to the increased mismatch in the thermal expansion coefficient between the filler and the polymers used in the study.

36 MATERIALS SCIENCE↗

Phase-field modeling of stored-energy-driven grain growth with intra-granular variation in dislocation density

Abstract We present a phase-field (PF) model to simulate the microstructure evolution occurring in polycrystalline materials with a variation in the intra-granular dislocation density. The model accounts for two mechanisms that lead to the grain boundary migration: the driving force due to capillarity and that due to the stored energy arising from a spatially varying dislocation density. In addition to the order parameters that distinguish regions occupied by different grains, we introduce dislocation density fields that describe spatial variation of the dislocation density. We assume that the dislocation density decays as a function of the distance the grain boundary has migrated. To demonstrate and parameterize the model, we simulate microstructure evolution in two dimensions, for which the initial microstructure is based on real-time experimental data. Additionally, we applied the model to study the effect of a cyclic heat treatment (CHT) on the microstructure evolution. Specifically, we simulated stored-energy-driven grain growth during three thermal cycles, as well as grain growth without stored energy that serves as a baseline for comparison. We showed that the microstructure evolution proceeded much faster when the stored energy was considered. A non-self-similar evolution was observed in this case, while a nearly self-similar evolution was found when the microstructure evolution is driven solely by capillarity. These results suggest a possible mechanism for the initiation of abnormal grain growth during CHT. Finally, we demonstrate an integrated experimental-computational workflow that utilizes the experimental measurements to inform the PF model and its parameterization, which provides a foundation for the development of future simulation tools capable of quantitative prediction of microstructure evolution during non-isothermal heat treatment.

Materials Science↗

Viscoplastic Model Development to Account for Strength Differential: Application to Aged Inconel 718 at Elevated Temperature

The magnitude of yield and flow stresses in aged Inconel 718 are observed to be different in tension and compression. This phenomenon, called the Strength differential (SD), contradicts the metal plasticity axiom that the second deviatoric stress invariant alone is sufficient for representing yield and flow. Apparently, at least one of the other two stress invariants is also significant. A unified viscoplastic model was developed that is able to account for the SD effect in aged Inconel 718. Building this model involved both theory and experiments. First, a general threshold function was proposed that depends on all three stress invariants and then the flow and evolution laws were developed using a potential-based thermodynamic framework. Judiciously chosen shear and axial tests were conducted to characterize the material. Shear tests involved monotonic loading, relaxation, and creep tests with different loading rates and load levels. The axial tests were tension and compression tests that resulted in sufficiently large inelastic strains. All tests were performed at 650 C. The viscoplastic material parameters were determined by optimizing the fit to the shear tests, during which the first and the third stress invariants remained zero. The threshold surface parameters were then fit to the tension and compression test data. An experimental procedure was established to quantify the effect of each stress invariant on inelastic deformation. This requires conducting tests with nonproportional three-dimensional load paths. Validation of the model was done using biaxial tests on tubular specimens of aged Inconel 718 using proportional and nonproportional axial-torsion loading. These biaxial tests also helped to determine the most appropriate form of the threshold function; that is, how to combine the stress invariants. Of the set of trial threshold functions, the ones that incorporated the third stress invariant give the best predictions. However, inclusion of the first stress invariant does not significantly improve the model predictions. The model shows excellent predictive capability for nonproportional load paths. Additionally, it reduces to the well-known models of Mises Drucker and Drucker-Prager. The requisite experiments involve reasonably simple load paths in the axial-shear stress plane and hence can be performed on a variety of different materials: be they metallic, geological. polymeric, ceramic or granular. The general form of the threshold function allows representation of inelastic deformation in a range of materials.

Iyer, Saiganesh↗

AC electrical transport detection of magnetic properties of small, granular, and heterogeneous samples

Experimental constraints and sample limitations can preclude ideal measurements of electrical transport properties of materials. In such situations, AC electrical transport methods are often employed due to a significant increase in signal-to-noise ratio they can provide. However, dynamic effects that are not often accounted for may be present that may modify the signals in these measurements. In particular, dynamic filtering effects are prominent in small, granular, and heterogeneous materials. We demonstrate that a lock-in amplifier based circuit can distinguish between these DC transport and AC filtering effects. Here, we further demonstrate that this filtering can reveal distinct signatures of magnetic transitions while providing a measure of sample quality.

47 OTHER INSTRUMENTATION↗

Computer enhancement of radiographs

Examination of three relevant noise processes and the image degradation associated with Marshall Space Flight Center's (MSFC) X-ray/scanning system was conducted for application to computer enhancement of radiographs using MSFC's digital filtering techniques. Graininess of type M, R single coat and R double coat X-ray films was quantified as a function of density level using root-mean-square (RMS) granularity. Quantum mottle (including film grain) was quantified as a function of the above film types, exposure level, specimen material and thickness, and film density using RMS granularity and power spectral density (PSD). For various neutral-density levels the scanning device used in digital conversion of radiographs was examined for noise characteristics which were quantified by RMS granularity and PSD. Image degradation of the entire pre-enhancement system (MG-150 X-ray device; film; and optronics scanner) was measured using edge targets to generate modulation transfer functions (MTF). The four parameters were examined as a function of scanning aperture sizes of approximately 12.5 25 and 50 microns.

Dekaney, A.↗

Recrystallization, cracking, and erosion of dispersoid-strengthened tungsten materials during exposure to divertor plasmas

In this study, we investigated the effects of combined intense particle and heat flux exposure on advanced tungsten plasma-facing materials within the DIII-D fusion facility. Our test matrix included two types of dispersoid-strengthened tungsten (containing either 100 nm diameter TiO 2 or Ni particles), along with high-purity polycrystalline tungsten as a reference. This experiment relied on a sample geometry angled at 15° relative to the divertor surface, thereby allowing the surfaces to intercept steady-state perpendicular heat fluxes (q ⟂ ) ranging from 10.1 to 19.6 MW/m 2 . During each shot, the samples were exposed to 42 Hz edge-localized modes (ELMs), allowing us to test the material response to transient heating. We correlated the exposure conditions with extensive post-test surface composition analysis and microscopy to determine how the plasma modified each surface. The angled specimens closest to the strike point received the highest combined heat and particle flux and melted midway through the experiment. EBSD analysis revealed they were completely recrystallized throughout, with an average grain size >100 µm. On the other hand, the specimens that received a lower steady state heat flux survived with more superficial surface damage. Whereas the high-purity polycrystalline tungsten exhibited a higher surface roughness, the dispersoid-strengthened material exhibited more extensive shallow inter-granular cracking. In addition, the surface was depleted of dispersoids following plasma exposure, possibly because of evaporation and/or sputtering. The results described here provide insights into the performance of these materials in a fusion environment which can guide further optimization for use in long-pulse devices.

Kolasinski, Robert D. [Sandia National Laboratorie↗

Leveraging staggered tessellation for enhanced spatial resolution in high-granularity calorimeters

Here we advance the concept of high-granularity calorimeters with staggered tessellations, underscoring the effectiveness of a design incorporating multifold staggering cycles based on hexagonal cells to enhance position resolution. Moreover, we introduce HEXPLIT, a sub-cell re-weighting algorithm tailored to harness staggered designs, resulting in additional performance improvements. By combining our proposed staggered design with HEXPLIT, we achieve an approximately twofold enhancement in position resolution for neutrons across a wide energy range, as compared to unstaggered designs. These findings hold the potential to elevate particle-flow performance across various forthcoming facilities.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Methods and apparatus for additively manufacturing structures using in situ formed additive manufacturing materials

A method of additively manufacturing a structure comprises nuclear reactor comprises disposing a feed material on a surface of a substrate in a reaction vessel, disposing at least one material formulated and configured to react with the feed material in the reaction vessel, and exposing the feed material and the at least one material to energy from an energy source to react the feed material and the at least one material to form an additive manufacturing material and reaction by-products. The additive manufacturing material is separated from the reaction by-products and exposed to energy from the energy source to form inter-granular bonds between particles of the additive manufacturing material and form a layer of a structure comprising the additive manufacturing material. Related apparatuses and methods are disclosed.

van Rooyen, Isabella J.↗

Low Temperature Regolith Bricks for In-Situ Structural Material

Current technology for producing in-situ structural materials on future missions to Mars or the moon relies heavily on energy-intensive sintering processes to produce solid bricks from regolith. This process requires heating the material up to temperatures in excess of 1000 C and results in solid regolith pieces with compressive strengths in the range of 14000 to 28000 psi, but are heavily dependent on the porosity of the final material and are brittle. This method is currently preferred over a low temperature cementation process to prevent consumption of precious water and other non-renewable materials. A high strength structural material with low energy requirements is still needed for future colonization of other planets. To fulfill these requirements, a nano-functionalization process has been developed to produce structural bricks from regolith simulant and shows promising mechanical strength results. Functionalization of granular silicate particles into alkoxides using a simple low temperature chemical process produces a high surface area zeolite particles that are held together via inter-particle oxygen bonding. Addition of water in the resulting zeolite particles produces a sol-gel reaction called "inorganic polymerization" which gives a strong solid material after a curing process at 60 C. The aqueous solution by-product of the reaction is currently being investigated for its reusability; an essential component of any ISRU technology. For this study, two batches of regolith bricks are synthesized from JSC-1A; the first batch from fresh solvents and chemicals, the second batch made from the water solution by-product of the first batch. This is done to determine the feasibility of recycling necessary components of the synthesis process, mainly water. Characterization including BET surface area, SEM, and EDS has been done on the regolith bricks as well as the constituent particles,. The specific surface area of 17.53 sq m/g (average) of the granular regolith material was obtained from nitrogen adsorption isotherm measurement. The size, shape and textures of regolith from SEM shows that the particles are 25-50 micrometers in size and mostly irregular in shape (Figure 1a). The elemental composition of regolith was identified from EDS analysis showed the presence of Si, Al, Fe, Na, Mg, Ca, Ti, O and C (see figure 1b). Each set of cylindrical brick samples were prepared by low energy process, and cured for 21 and 28 days, respectively to compare their compressive strength. Figure 1c, and d shows the JSC-1A brick and the compressive strength measurements. The results from the 21 day cured bricks (2 bricks) have been done and yielded an aver-age strength of 3050 psi, considerably higher than Portland cement mortars (Type IV and V). This promising technology provides the benefits of construction material similar to concrete, with a low complexity, low energy synthesis process and the likelihood of complete reusability of precious resources. Compressive strength using this method can be improved by increasing the surface area of the particles, using bi-modal particle size distribution, and adding certain additives to increase inter-particle forces.

ISRU↗

A hybrid calibration approach to Hertz-type contact parameters for discrete element models

This study aims at providing a hybrid calibration framework to estimate Hertz-type contact parameters (particle-scale shear modulus and Poisson ratio) for both two-dimensional and three-dimensional discrete element modelling (DEM). On the basis of statistically isotropic granular packings, a set of analytical formulae between macroscopic material parameters (Young modulus and Poisson ratio) and particle-scale Hertz-type contact parameters for granular systems are derived under small-strain isotropic stress conditions. However, the derived analytical solutions are only estimated values for general models. By viewing each DEM modelling as an implicit mathematical function taking the particle-level parameters as independent variables and employing the derived analytical solutions as the initial input parameters, an automatic iterative scheme is proposed to obtain the calibrated parameters with higher accuracies. Considering highly nonlinear features and discontinuities of the macro-micro relationship in Hertz-based discrete element models, the adaptive moment estimation algorithm is adopted in this study because of its capacity of dealing with noise gradients of cost functions. Here, the proposed method is validated with several numerical cases including randomly distributed monodisperse and polydisperse packings. Noticeable improvements in terms of calibration efficiency and accuracy have been made.

Constitutive law↗

Selective Pb 2+ removal and electrochemical regeneration of fresh and recycled FeOOH

Heavy metal pollution is a key environmental problem. Selectively extracting heavy metals could accomplish water purification and resource recycling simultaneously. Adsorption is a promising approach with a facile process, adaptability for the broad concentration of feed water, and high selectivity. However, the adsorption method faces challenges in synthesizing high-performance sorbents and regenerating adsorbents effectively. FeOOH is an environmentally friendly sorbent with low-cost production on a large scale. Nevertheless, the selectivity behavior and regeneration of FeOOH are seldom studied. Therefore, we investigated the selectivity of FeOOH in a mixed solution of Co 2+ , Ni 2+ , and Pb 2+ and proposed to enhance the capacity of FeOOH and regenerate it by using external charges. Without charge, the FeOOH electrode shows a Pb 2+ uptake capacity of 20 mg/g. After applying a voltage of –0.2/+0.8 V, the uptake capacity increases to a maximum of 42 mg/g and the desorption ratio is 70%–80%. In 35 cycles, FeOOH shows a superior selectivity towards Pb 2+ compared with Co 2+ and Ni 2+ , with a purity of 97% ± 3% in the extracts. The high selectivity is attributed to the lower activation energy for Pb 2+ sorption. The capacity retentions at the 5 th and the 35 th cycles are ca. 80% and ca. 50%, respectively, comparable to the chemical regeneration method. With industrially exhausted granular ferric hydroxide as the electrode material, the system exhibits a Pb 2+ uptake capacity of 37.4 mg/g with high selectivity. Our work demonstrates the feasibility of regenerating FeOOH by charge and provides a new approach for recycling and upcycling FeOOH sorbent.

36 MATERIALS SCIENCE↗

Lateral restoring force on a magnet levitated above a superconductor

The lateral restoring force on a magnet levitated above a superconductor is calculated as a function of displacement from its original position at rest using Bean's critical-state model to describe flux pinning. The force is linear for small displacements and saturates at large displacements. In the absence of edge effects the force always attracts the magnet to its original position. Thus it is a restoring force that contributes to the stability of the levitated magnet. In the case of a thick superconductor slab, the origin of the force is a magnetic dipole layer consisting of positive and negative supercurrents induced on the trailing side of the magnet. The qualitative behavior is consistent with experiments reported to date. Effects due to the finite thickness of the superconductor slab and the granular nature of high-Tc materials are also considered.

Davis, L. C.↗

Methods of forming fuel rods comprising porous fuel materials

A method of forming a fuel rod for a nuclear reactor comprises disposing a powder comprising particles of a fuel material on a substrate, exposing the powder to energy from an energy source to form a first layer of a nuclear fuel, the first layer comprising inter-granular bonds between the particles of the fuel material, disposing additional powder comprising particles of the fuel material over the first layer of the nuclear fuel, and exposing the additional powder to energy from the energy source to form a second layer of the nuclear fuel and to form the nuclear fuel to have a void fraction greater than about 0.20, the second layer comprising inter-granular bonds between the additional powder and the first layer of the nuclear fuel. Related nuclear fuels comprising a porous structure, fuel rods, nuclear reactors, and methods are disclosed.

O'Brien, Robert C.↗

Emerging contact force heterogeneity in ordered soft granular media

Under external perturbations, inter-particle forces in disordered granular media are well known to form a heterogeneous distribution with filamentary patterns. Better understanding these forces and the distribution is important for predicting the collective behavior of granular media, the media second only to water as the most manipulated material in global industry. However, studies in this regard so far have been largely confined to granular media exhibiting only geometric heterogeneity, leaving the dimension of mechanical heterogeneity a rather uncharted area. In this work, through a FEM contact mechanics model, we show that a heterogeneous inter-particle force distribution can also emerge from the dimension of mechanical heterogeneity alone. Specifically, we numerically study inter-particle forces in packing of mechanically heterogeneous disks arranged over either a square or a hexagonal lattice and under quasi-static isotropic compression. Our results show that, at the system scale, a hexagonal packing exhibit a more heterogeneous inter-particle force distribution than a square packing does; At the particle scale, for both packing lattices, preliminary analysis shows the consistent coexistence of outliers (i.e., softer disks sustaining larger forces while stiffer disks sustaining smaller forces) in comparison to their homogeneous counterparts, which implies the existence of nonlocal effect. Further analysis on the portion of outliers and on spatial contact force correlations suggest that the hexagonal packing shows more pronounced nonlocal effect over the square packing under small mechanical heterogeneity. However, such trend is reversed when assemblies becomes more mechanically heterogeneous. Lastly, we confirm that, in the absence of particle reorganization events, contact friction merely plays the role of packing stabilization while its variation has little effect on inter-particle forces and their distribution.

36 MATERIALS SCIENCE↗

Exascale granular microstructure reconstruction in 3D volumes of arbitrary geometries with generative learning

Reconstructing 3D granular microstructures within volumes of arbitrary geometries from limited 2D image data is crucial for predicting the material properties, as well as performances of structural components accounting for material microstructural effects. We present a novel generative learning framework that enables exascale reconstruction of granular microstructures within complex 3D geometric volumes. Building upon existing transfer learning techniques using pre-trained convolutional neural networks (CNN), we introduce several key innovations to overcome the difficulties inherent in arbitrary geometries. Our framework incorporates periodic boundary conditions using circular padding techniques, ensuring continuity and representativeness of the reconstructed microstructures. We also introduce a novel seamless transition reconstruction (STR) method that creates statistically equivalent transition zones to integrate multiple pre-existing 3D microstructure volumes. Based on STR, we propose a cost-effective strategy for reconstructing microstructures within complex geometric volumes, minimizing computational waste. Validation through numerical experiments using kinetic Monte Carlo simulations demonstrates accurate reproduction of grain statistics, including grain size distributions and morphology. A case study involving the reconstruction of a 4-blade propeller microstructure illustrates the method’s capability to efficiently handle complex geometries. In conclusion, the proposed framework significantly reduces computational demands while maintaining high reconstruction quality, paving the way for scalable microstructure reconstruction in materials design and analysis.

36 MATERIALS SCIENCE↗

The Strata-l Experiment on Microgravity Regolith Segregation

The Strata-1 experiment studies the segregation of small-body regolith through long-duration exposure of simulant materials to the microgravity environment on the International Space Station (ISS). Many asteroids feature low bulk densities, which implies high values of porosity and a mechanical structure composed of loosely bound particles, (i.e. the "rubble pile" model), a prime example of a granular medium. Even the higher-density, mechanically coherent asteroids feature a significant surface layer of loose regolith. These bodies will evolve in response to very small perturbations such as micrometeoroid impacts, planetary flybys, and the YORP effect. A detailed understanding of asteroid mechanical evolution is needed in order to predict the surface characteristics of as-of-yet unvisited bodies, to understand the larger context of samples from sample return missions, and to mitigate risks for both manned and unmanned missions to asteroidal bodies. Due to observation of rocky regions on asteorids such as Eros and Itokawa, it has been hypothesized that grain size distribution with depth on an asteroid may be inhomogeneous: specifically, that large boulders have been mobilized to the surface. In terrestrial environments, this size-dependent sorting to the surface of the sample is called the Brazil Nut Effect. The microgravity and acceleration environment on the ISS is similar that of a small asteroid. Thus, Strata-1 investigates size segregation of regolith in an environment analogous to that of small bodies. Strata-1 consists of four regolith simulants in evacuated tubes, as shown in Figure 1 (Top and Middle). The simulants are (1) a crushed and sieved ordinary chondrite meteorite to simulate an asteroidal surface, (2) a carbonaceous chondrite simulant with a mixture of fine and course particles, and two simplified silicate glass simulants; (3) one with angular and (4) another with spherical particles. These materials were chosen to span a range of granular complexity. The materials were sorted into three size species pre-launch, and maintained during launch and return by a device called the Entrapulator. The hypothesis under test is that the particles that constitute a granular medium in a micro-gravity environment, subjected to a known vibration environemnt, will segregate in accordance to modeled predictions. Strata-1 is currently operating on ISS, with cameras capturing images of simulant motion throughout the one year mission. Vibration data is recorded and downlinked, and the simulants will be analyzed after return to Earth.

Fries, M.↗

Nondestructive activation analysis of sample of lunar surface material returned by Luna 16 automatic station

The composition of a sample of lunar surface material returned by the Luna 16 automatic station from the Sea of Fertility was studied, using nondestructive activation analysis. The structure of the returned surface material is inhomogeneous; the surficial material is thin, quite homogeneous, and the granularity increases with depth. Based on grain size, the sample was separated into five zones. The activation analysis was conducted on a sample taken from the friable surficial layer, zone A. The content of Al, Mn, Na, Cr, Co, Fe, and Sc was determined by nondestructive activation analysis of the sample. In determining Cr, Co, Fe, and Sc, the sample was irradiated for 24 hours and cooled for 10 days. Gamma spectra of the samples were recorded with a semiconductor Ge(Li)-detector and a multichannel analyzer, and measurement data were processed with an electronic computer.

Chayko, M.↗

Demonstration of Fluid Dynamics for Plant Growing Systems in Varied Gravity Environments Through Scaled Capillary Models

The development of reliable and bioregenerative crop growth production systems is vital for human exploration into deep space. As humans prepare for space travel beyond LEO, scientists need to find a way to provide reliable and adequate water delivery for all stages of the plant's life cycle. Past production systems struggled with this and often led to overwatering in the system. To better understand this issue, NASA's Plant Water Management (PWM) experiments were able to model fluid flow through granular substrates, specifically a clay-based material arcilite, in 0-G. The PWM study can help researchers to predict fluid flow through the systems, however their model only works for an arcilite based system and was unable to account for different stages of plant growth. For future missions, payload requirements to support crop production system will need to be limited, leading to the use of in situ resources. This project aims to validate the PWM experiments as well as incorporate various materials into the design for growth systems. To meet these objectives, a series of terrestrial experiments will be deployed to mimic all gravities. By modifying the material, fluid, and size of the test subjects, the effect of Earth's gravity can be minimized. This project will aid researchers in the design of future crop production systems for surface missions by creating a refined model that can be used at all stages of plant growth and utilize in situ resources.

Plant Biology↗