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At least 163 records · Page 9

Electrophoretic Porosimetry of Sol-Gels

It has been hypothesized that gravity has an effect on the formation and resulting microstructure of sol-gels. In order to more clearly resolve the effect of gravity, pores may be non-destructively analyzed in the wet gel, circumventing the shrinkage and coarsening associated with the drying procedure. We discuss the development of an electrophoretic technique, analogous to affinity chromatography, for the determination of pore size distribution and its application to silica gels. Specifically a monodisperse charged dye is monitored by an optical densitometer as it moves through the wet gel under the influence of an electric field. The transmittance data (output) represents the convolution of the dye concentration profile at the beginning of the run (input) with the pore size distribution (transfer function), i.e. linear systems theory applies. Because of the practical difficulty in producing a delta function input dye profile we prefer instead to use a step function. Average pore size is then related to the velocity of this dye front, while the pore size distribution is related to the spreading of the front. Preliminary results of this electrophoretic porosimetry and its application to ground and space-grown samples will be discussed.

Snow, L. A.↗

On Efficient Multigrid Methods for Materials Processing Flows with Small Particles

Multiscale modeling of materials requires simulations of multiple levels of structural hierarchy. The computational efficiency of numerical methods becomes a critical factor for simulating large physical systems with highly desperate length scales. Multigrid methods are known for their superior efficiency in representing/resolving different levels of physical details. The efficiency is achieved by employing interactively different discretizations on different scales (grids). To assist optimization of manufacturing conditions for materials processing with numerous particles (e.g., dispersion of particles, controlling flow viscosity and clusters), a new multigrid algorithm has been developed for a case of multiscale modeling of flows with small particles that have various length scales. The optimal efficiency of the algorithm is crucial for accurate predictions of the effect of processing conditions (e.g., pressure and velocity gradients) on the local flow fields that control the formation of various microstructures or clusters.

Thomas, James↗

Space Weathering of Olivine in Lunar Soils: A Comparison to Itokawa Regolith Samples

Regolith particles from airless bodies preserve a record of the space weathering processes that occurred during their surface exposure history. These processes have major implications for interpreting remote-sensing data from airless bodies. Solar wind irradiation effects occur in the rims of exposed grains, and impact processes result in the accumulation of vapordeposited elements and other surface-adhering materials. The grains returned from the surface of Itokawa by the Hayabusa mission allow the space weathering "style" of a chondritic, asteroidal "soil" to be compared to the lunar case. Here, we present new studies of space-weathered olivine grains from lunar soils, and compare these results to olivine grains from Itokawa. Samples and Methods: We analyzed microtome thin sections of olivine grains from the 20-45 micron fractions of three lunar soils: 71061, 71501 and 10084 (immature, submature and mature, respectively). Imaging and analytical data were obtained using a JEOL 2500SE 200kV field-emission scanning-transmission electron microscope equipped with a thin-window energy-dispersive x-ray spectrometer. Similar analyses were obtained from three Hayabusa olivine grains. Results and Discussion: We observed lunar grains showing a range of solar flare track densities (from <10(exp 9) to approx.10(exp 12)/sq cm). The lunar olivines all show disordered, highly strained, nanocrystalline rims up to 150-nm thick. The disordered rim thickness is positively correlated with solar flare track density. All of the disordered rims are overlain by a Si-rich amorphous layer, ranging up to 50-nm thick, enriched in elements that are not derived from the host olivine (e.g., Ca, Al, and Ti). The outmost layer represents impact-generated vapor deposits typically observed on other lunar soil grains. The Hayabusa olivine grains show track densities <10(exp 10)/sq cm and display disordered rims 50- to 100-nm thick. The track densities are intermediate to those observed in olivines in immature and submature lunar soils and indicate surface exposures of approx. 10(exp 5) years. The outermost few nanometers of the disordered rims on Hayabusa olivines are more Si-rich and Mg- and Fe-depleted relative to the cores of the grains and likely represent a minor accumulation of impact-generated vapors or sputter deposits. Nanophase Fe metal particles are less abundant in the Hayabusa rims compared to the rims on lunar grains. Conclusions: The Hayabusa and lunar olivine grain rims have widths and microstructures consistent with formation from atomic displacement damage from solar wind ions. The space weathering features in the Hayabusa grains are similar to those observed in olivines from immature to submature lunar soils. A major difference, however, is that the Hayabusa grains appear to lack the hypervelocity impact products (melt spherules, thick vapor deposits, and abundant nanophase Fe metal particles) that are common in lunar soil grains with a similar exposure history.

Keller, L. P.↗

Compositional and Microstructural Effects in the Protection of SiC Components in Water Vapor

Greater gas turbine engine efficiency is a major goal in aeronautics research often pursued through increased engine operating temperatures. However, it is necessary to replace the current hot-stage alloy components with more thermally robust parts, such as promising Silicon-based ceramics and composites. Unfortunately, these materials are still susceptible to the effects of oxidation, water vapor, and (Calcium-Magnesium-Alumino-Silicate) CMAS interaction, among other issues at high temperature. To mitigate these effects, environmental barrier coating (EBC) materials are employed to help control the rate of degradation to the underlying composite. Often, a thermally grown oxide (TGO) layer forms between the EBC and the composite which can act as a point of failure. The current study focuses on the combined effects of water vapor, composite composition, and microstructure in TGO formation on protected and unprotected SiC samples which have been produced under different processing conditions.

Kowalski, Benjamin↗

Predicting Melt Properties Using Atomistic Simulations With A Highly Accurate Physically Informed Neural Network Interatomic Potential

The use of a recently developed machine learning (ML) interatomic potential for molecular dynamics simulations of aluminum melt properties will be presented. Such properties are critical for process modeling in additive manufacturing, including the melt pool size, solidification, and formation of solidification microstructures. Direct first-principles modeling of these processes is computationally prohibitive whereas simulations employing ML potentials combine the high accuracy of quantum-mechanical methods with high computational speeds. The physically-informed neural network (PINN) method used herein, integrates a high-dimensional regression implemented by an artificial neural network with a physics-based bond-order interatomic potential. PINN potentials can accurately reproduce many properties of aluminum in both crystalline-solid and liquid phases. We examine the accuracy of a PINN Al potential in predicting the density, self-diffusivity, viscosity, and the tension of the liquid surface and liquid-solid interfaces. Comparison with experimental data and ab initio molecular dynamics calculations shows very good agreement for all properties tested.

molecular dynamics↗

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

Nb₃Sn has emerged as a leading alternative material due to its higher superconducting critical temperature (Tc) and superheating field (Hsh), promising a viable solution to the intrinsic performance limit currently faced by Nb superconducting radiofrequency (SRF) cavities. We sputter-coated Nb₃Sn inside Nb SRF cavity using a stoichiometric Nb₃Sn tube target in a DC cylindrical magnetron sputter coater. The target was fabricated by growing an estimated >20 μm thick Nb₃Sn layer on a Nb tube via Sn vapor diffusion using Jefferson Lab’s coating system. Approximately 150 nm thick Nb-Sn films were sputter-deposited onto flat Nb samples at positions representing the beam tubes and equator of a 2.6 GHz Nb cavity. Post-deposition annealing at 950 °C for 3 h resulted in the formation of Nb₃Sn. Microstructural analysis of the annealed films was carried out to investigate the morphology and structure of the Nb₃Sn films. Later, a 2.6 GHz Nb SRF cavity was coated with a ~1.2 μm thick sputtered Nb-Sn film using a stoichiometric Nb₃Sn target, followed by annealing. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, indicating the formation of Nb₃Sn. After a light Sn recoating treatment, the cavity achieved a quality factor (Q0) of 6.7E+08 at lower field at 2.0 K.

Accelerator Physics↗

Characterization of the radial microstructural evolution in LWR UO 2 using electron backscatter diffraction

Studies on high burnup UO 2 subjected to loss-of-coolant accident conditions have shown that restructured regions of the fuel are susceptible to pulverization and eventual dispersal. Due to a lack of pre-test characterization, the distinct microstructural features rendering the fuel prone to fragmentation remain ambiguous. Four samples of commercially irradiated light-water reactor UO 2 have been characterized utilizing electron backscatter diffraction to assess the susceptible microstructure. The microscopy focused on determining the burnup and temperature conditions responsible for the formation of the different microstructural regions where the regions were denoted as the high-burnup structure (HBS), HBS transition, mid-radial, restructured central, and central region. Previous works have outlined the specific conditions required for the restructuring of the microstructure into the HBS, but the conditions responsible for the restructuring in the central region of the fuel are not well understood. The four analyzed samples confirm a burnup threshold of 61 GWd/tU, and an unknown temperature range is needed to facilitate the formation of the restructured central region. In conclusion, additional fuel performance evaluations are needed to quantify the temperature range promoting restructuring in the central region.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Evolution and Control of 2219 Aluminum Microstructural Features Through Electron Beam Freeform Fabrication

The layer-additive nature of the electron beam freeform fabrication (EBF3) process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗

Evolution and Control of 2219 Aluminum Microstructural Features through Electron Beam Freeform Fabrication

Electron beam freeform fabrication (EBF3) is a new layer-additive process that has been developed for near-net shape fabrication of complex structures. EBF3 uses an electron beam to create a molten pool on the surface of a substrate. Wire is fed into the molten pool and the part translated with respect to the beam to build up a 3-dimensional structure one layer at a time. Unlike many other freeform fabrication processes, the energy coupling of the electron beam is extremely well suited to processing of aluminum alloys. The layer-additive nature of the EBF3 process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗

Transmission Electron Microscopy of Non-Etched Presolar Silicon Carbide

Our solar system formed from nuclei produced in earlier generations of stars. Mixing in the proto-solar nebula isotopically homogenized most of this material, but some grains, called presolar grains, retain their original isotopic composition. The isotopic properties of presolar SiC grains indicate that most of the grains formed in the outflows of carbon-rich Asymptotic Giant Branch (AGB) stars. The microstructure of these presolar grains reflects the conditions of the dust formation and subsequent alteration. Early microstructural studies of SiC grains obtained by acid dissolution from meteorites show that most isotopically anomalous SiC grains have the face-centered cubic b- SiC structure. However, Daulton et al. have shown that a small fraction of sub-micron presolar SiC grains are of the hexagonal 2H polytype (a-SiC). Although the harsh chemical treatments of these grains does not alter their crystal structure, significant alteration of the surface morphology of the grains due to the acid treatments has been observed. In addition, the acid treatments may preferentially remove cracked or fissured grains, and possible sub-grains, such as graphite. By studying SiC grains isolated by physical separation and found in situ, we attempt to obtain a more complete analysis of presolar SiC microstructures, including the surface morphology, in order to address the formation and processing history of the grains. In our prior work, we reported on one in situ SiC grain (hereafter CBIS1). Here we present results from two additional grains, one in situ, and one prepared as a physical separate.

Stroud, Rhonda M.↗

Surface Film Formation on Al-V Alloys with Far-From-Equilibrium Microstructure

Nanocrystalline supersaturated Al-V alloys produced by high-energy ball milling have been reported to exhibit enhanced corrosion resistance and mechanical properties compared to commercial Al alloys. Corrosion of passive alloys such as Al-V alloy relies on the characteristics of the surface film, which is studied using scanning/transmission electron microscopy and time-of-flight secondary ion mass spectrometry. The effect of microstructure and composition on the surface film has been investigated after different immersion periods (30 min, 2 h, and 1 day) in 0.1 M NaCl. The surface film was complex and composed of oxidized Al and V. The heterogeneous surface film was observed due to the presence of secondary phases and initiation of localized corrosion. The void formation was observed beneath the surface film that would potentially cause pitting corrosion. The generation of nano-sized voids was dependent on grain orientation. Compared to pure Al, the chloride penetration is suppressed in Al-V alloys. The effect of composition and microstructure on surface film formation and attendant corrosion behavior is discussed herein.

36 MATERIALS SCIENCE↗

The growth of metastable peritectic compounds

The influence of gravitationally driven thermosolutal convection on the directional solidification of peritectic alloys is considered as well as the relationships between the solidification processing conditions, and the microstructure, chemistry, and magnetic properties of such alloys. Analysis of directionally solidified Pb-Bi peritectic samples indicates that appreciable macrosegregation occurs due to thermosolutal convection and/or Soret diffusion. A peritectic solidification model which accounts for partial mixing in the liquid ahead of the planar solidification interface and describes macrosegregation has been developed. Two-phase dendritic and banded microstructures were grown in the Pb-Bi peritectic system, refined two-phase microstructures have were observed, and candidate formation mechanisms proposed. Material handling, containment, casting, microstructural and magnetic characterization techniques were developed for the Sm-Co system. Alloys produced with these procedures are homogeneous.

Larson, D. J., Jr.↗

Perspectives on Quenching and Tempering 4340 Steel

Steels are ubiquitous due to their affordability and the landscape of useful properties that can be generated for engineering applications. But to further expand the performance envelope, one must be able to understand and control microstructure development by alloying and processing. In this paper we use multiscale, advanced characterization to better understand the structural and chemical evolution of AISI 4340 steel after quenching and tempering (Q&T), including the role of quench rate and short-time, isothermal tempering below 573 K (300 °C), with an emphasis on carbide formation. We compare the microstructure and/or property changes produced by conventional tempering to those produced by higher temperature, short-time “rapid” tempering. We underscore that no single characterization technique can fully capture the subtle microstructure changes like carbon redistribution, transition carbide and/or cementite formation, and retained austenite decomposition that occur during Q&T. Only the use of multiple techniques begins to unravel these complexities. After controlled fast or slow quenching, η transition carbides clearly exist in the microstructure, likely associated with autotempering of this high martensite start temperature (Ms) steel. Isothermal tempering below 598 K (325 °C) results in the relief of carbon supersaturation in the martensite, primarily by the formation of η transition carbides that exhibit a range of carbon levels, seemingly without substitutional element partitioning between the carbide and matrix phases. Hägg transition carbide is present between 300 °C and 325 °C. After conventional tempering at or above 598 K (325 °C) for 2 h, cementite is predominant, but small amounts of cementite are also present in other conditions, even after quenching. Previous work has indicated that silicon (Si) and substitutional elements partition between the cementite, which initially forms under paraequilibrium conditions, and the matrix. Phosphorous (P) may also be preferentially located at cementite/matrix interfaces after high temperature tempering. Slower quench rates result in greater amounts of retained austenite compared to those after fast quenching, which we attribute to increased austenite stability resulting from “autopartitioning”. Rapid, high temperature tempering is also found to diminish tempered martensite embrittlement (TME) believed to be associated with the extent of austenite decomposition, resulting in mechanical properties not attainable by conventional tempering, which may have important implications with respect to industrial heat treatment processes like induction tempering. Controlling the amount and stability of retained austenite is not only relevant to the properties of Q&T steels, but also next-generation advanced high strength steels (AHSS) with austenite/martensite mixtures.

36 MATERIALS SCIENCE↗

Free dendritic growth

Free dendritic growth refers to the unconstrained development of crystals within a supercooled melt, which is the classical 'dendrite problem'. Great strides have been taken in recent years in both the theoretical understanding of dendritic growth and its experimental status. The development of this field will be sketched, showing that transport theory and interfacial thermodynamics (capillarity theory) were sufficient ingredients to develop a truly predictive model of dendrite formation. The convenient, but incorrect, notion of 'maximum velocity' was used for many years to estimate the behavior of dendritic transformations until supplanted by modern dynamic stability theory. The proper combinations of transport theory and morphological stability seem to able to predict the salient aspects of dendritic growth, especially in the neighborhood of the tip. The overall development of cast microstructures, such as equiaxed zone formation, rapidly solidified microstructures, etc., also seems to contain additional non-deterministic features which lie outside the current theories discussed here.

Glicksman, M. E.↗

Dolomites in hydrated fine-grained Antarctic micrometeorites: Effective tools for analyzing secondary processes

We report detailed transmission electron microscope (TEM) observations of carbonates from one hydrated fine-grained Antarctic micrometeorite (H-FgMM). These carbonates show the occurrence of complex chemical variations and microstructures that provide important evidence regarding the formation and evolution of rarely analyzed H-FgMMs. The chemical variations were identified at both micrometer and nanometer scales, indicating that these carbonates formed under localized fluid conditions that suggest a variable chemical microenvironment. Individual carbonates grew from isolated reservoirs of fluid. Moreover, these carbonates contain manganese amounts almost twice as high as those measured in CM chondrites but similar to those identified in CI chondrites. Their particular compositions indicate reducing and progressively evolving conditions in the fluid from which these carbonates precipitated, probably due to water consumption during phyllosilicates formation. In addition to the compositional variability, microstructural features are pervasive in these carbonates, similar to those described in heavily shocked meteorites indicating that these carbonates were probably modified during shock processes after their formation. Since carbonates are highly susceptible to shock metamorphism, we suggest that it is essential to investigate their structure in detail before interpreting the isotopic measurements related to the time of their formation. Additionally, associated with carbonates, ubiquitous phosphates were identified in the micrometeorite analyzed. Future studies of these mineral associations will provide us further insight into the formation and evolution of asteroids, especially since they were both identified in the surface materials of Ryugu and Bennu.

58 GEOSCIENCES↗

An analysis of fluff formation in metallic fuel via data analyzes from EBR-II experiments and BISON fuel code modeling

During the operation of EBR-II, it was found that a highly porous structure (over 40% area fraction) formed at the top of several fuel columns. Previous work has shown that this structure, designated fluff in this paper, contains a significant fraction of fuel elements (e.g., U and Pu) which could potentially impact neutronics. This work aims in analyzing the formation mechanism of this microstructure so its impact can be incorporated into future metallic fuel modeling codes and algorithms. This paper details a preliminary examination into the formation mechanisms of fluff by performing qualitative and statistical analysis of EBR-II experimental data. Additionally, the operating conditions that have the greatest impact on fluff formation were determined based on this data set. Also, BISON fuel code simulations were used to help postulate potential fluff formation mechanisms. From this analysis it was found that the largest contributors to fluff formation were fuel burnup and composition, with fluff formation exhibiting a roughly linear positive correlation with increasing burnup and a negative correlation with increasing Pu content. It was also found that higher pin operating temperatures decreased fluff formation but only for U-10Zr fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Cooling dynamics of two titanium alloys during laser powder bed fusion probed with in situ X-ray imaging and diffraction

Metal parts produced by laser powder bed fusion (LPBF) additive manufacturing exhibit characteristic microstructures comparable to those observed in laser welding. The primary cause of this characteristic microstructure is rapid, localized heating and cooling cycles, which result in extreme thermal gradients where material solidification is followed by fast cooling in the solid state. The final microstructure and mechanical performance are also influenced by pore formation caused by melt pool fluid dynamics. Here, we use high speed, in situ X-ray diffraction to probe the kinetics of cooling and solid-solid phase transitions after laser melting in two aerospace titanium alloys: Ti-6Al-4V, an α + β alloy; and Ti-5Al-5V-5Mo-3Cr, a near-β alloy. We complement these diffraction studies with in situ X-ray imaging to probe melt pool dynamics and pore formation. From these two complementary probes, we quantify pore formation during melting and the subsequent microstructural evolution as the material rapidly cools after solidification. These results are critical for understanding defect formation and residual stress development in different titanium alloys under LPBF conditions and can help inform process models to predict final part performance.

36 MATERIALS SCIENCE↗

Kink mechanism in Cu/Nb nanolaminates explored by $\mathcal{in}$ $\mathcal{situ}$ pillar compression

We report Nano metallic laminates (NMLs) exhibit different failure modes depending on the loading conditions due to their mechanical anisotropies. Kinking is a typical failure mode in many NMLs compressed along a layer-parallel direction. However, a detailed description of the microstructure evolution during kink band (KB) formation and an in-depth understanding of the formation mechanisms are lacking. In this work, the KB process is investigated in Cu/Nb NMLs by in situ micro pillar compression in the scanning electron microscope (SEM) along a layer-parallel direction. Post-mortem S/TEM and transmission Kikuchi diffraction (TKD) analyses show that kink banding leads to significant microstructure changes characterized by an accumulation of geometrically necessary dislocations (GNDs) and of tilt geometrically necessary boundaries (GNBs) near KB boundaries (KBBs). The distinct microstructure evolution implies that KB formation is facilitated by the inhomogeneous microstructures resulting in constrained deformation modes. Specifically, dislocations active on slip planes nearly parallel to the interfaces make a major contribution to kink evolution after the onset of kinking. Once layer-parallel slip systems are activated, preexisting lattice dislocations and dislocations nucleating from interfaces will accumulate as GNDs near KBBs via the stochastic storage of lattice dislocations that have certain Burgers vectors. GNDs can further transform into GNBs via cross-slip and climb driven processes near the KBB. Furthermore, GNBs near KBBs can grow by incorporating more GNDs or by coalescence to accommodate the KB evolution. We further hypothesize that microstructural perturbations and their ensuing stresses can initiate KB formation in Cu/Nb NMLs.

36 MATERIALS SCIENCE↗