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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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The basis for graphite in nuclear core components. Why graphite, what makes it tick, what is it's behavior, and some speculation on graphite behavior. How does graphite fit into the discussion for different types of reactors and what types of reactors are considering graphite. The importance of graphite for future reactor designs and what work needs to be conducted in characterizing nuclear graphite.
Oxidation kinetics and scale formation were examined in 21–2N Stainless Steel alloys in a CO 2 environment at 700 °C. Several characterization techniques were used to identify the morphology, crystallographic structure, and chemical composition of the oxide scale formation during exposures up to 1925 h. High manganese content played an important role in homogenous oxide scale formation of Mn 3 O 4 and MnCr 2 O 4 at the scale/gas and scale/alloy interfaces and as an FCC stabilizer in the alloy. Depletion of Mn resulted in an FCC to BCC phase transformation at the scale/alloy interface. No carburization was observed, indicating that the oxide layer is preventing carbon uptake.
The Whole Powder Pattern Modelling (WPPM) approach of diffraction line profile analysis (LPA) was applied for the first time on PuO 2 in order to understand the evolution of the microstructural properties as a function of process conditions. Crystallite size distributions and defect concentrations were determined by WPPM on three different PuO 2 samples - including one with a bimodal distribution and compared to the result of more common LPA analyses used in PuO 2 literature studies (e.g. Scherrer equation, double Voigt method). The conclusion was that a lognormal distribution of spherical crystallites with dislocations most closely represent the microstructure of PuO 2 produced by heating Pu 2 (C 2 O 4 ) 3 (H 2 O) 6 •3H 2 O between 650°C and 850°C. The volume-weighted mean column length (Lvol) parameter obtained from the double Voigt method for the monomodal samples were the same as the Lvol obtained from the WPPM within uncertainty. The two LPA methods did not agree on the Lvol parameters of the bimodal distribution sample with only the WPPM getting values that were consistent with the individual components. The WPPM can potentially provide more insight into future studies of the influences on the microstructure properties of PuO 2 .
Chemical disordering is one feature of damage that occurs in irradiation environments and is common in ceramic compounds. This paper reviews irradiation-induced chemical disordering in SiC-based materials at elevated temperatures. Here the results were obtained using advanced analytical tools to characterize atomistic defects and to evaluate the chemistry of defect clusters and homonuclear bond structures. Finally, this paper demonstrates that chemical disordering is crucial to understanding microstructural stability and establishing a mechanistic modeling of microstructural evolution of irradiated SiC.
The SiC-based materials, particularly SiC-fiber-reinforced SiC matrix (SiC/SiC) composites, show strong potential for structural and functional applications in future fusion power plants because they can operate at high temperatures with a range of coolants and breeders, thereby enabling higher energy conversion efficiency. Here, this paper presents recent advancements in the development of SiC-based materials, focusing on processing techniques and material performance and resistance under fusion-relevant environments. The processing activities have emphasized near-net-shape fabrication and the joining of SiC subcomponents, with processing methods and material compositions informed by previous irradiation experiments on various grades of SiC. Research on irradiation effects has remained focused on degradation mechanisms and the microstructural optimization of SiC/SiC composites irradiated to high neutron damage levels. Analysis of irradiation defects in SiC has advanced via the application of cutting-edge characterization methods, among which Raman spectroscopy is becoming a common tool to assess atomic-scale chemical disorder. Fusion–fission crosscutting irradiation research has explored combined effects in SiC/SiC composites with application-relevant geometries, including bowing of SiC/SiC composite channels under neutron flux gradients, stress evolution in SiC/SiC composite tubes under through-thickness temperature gradients, and irradiation-enhanced corrosion in SiC. Finally, research opportunities for component testing and assessment under fusion-relevant conditions, in support of emerging concepts from the private fusion sector, are discussed.
To explore the feasibility of using laser powder bed fusion systems to print bulk amorphous Al alloys, a single autogenous weld produced by laser remelting on a cast Al-5La-9Ni (at.%) alloy was studied for its microstructure and mechanical behavior. The solidification rates experienced by material within the welds were high enough to produce entirely amorphous regions within the welds. Welds were characterized using SEM, STEM, and APT and were found to contain Ni-rich amorphous clusters. Micropillar compression tests were used to assess mechanical properties of the welds and found that all of the amorphous regions exhibited yield strengths around 1 GPa. In conclusion, these results are discussed in the context of diffusivity of Ni and rare earth elements in liquid, glass forming ability, thermodynamic driving force for phase formation during solidification, free volume concentrations in bulk metallic glasses, and cluster-related softening.
Stereo-defects present in stereo-regular polymers often diminish thermal and mechanical properties, and hence suppressing or eliminating them is a major aspirational goal for achieving polymers with optimal or enhanced properties. Here, we accomplish the opposite by introducing controlled stereo-defects to semicrystalline biodegradable poly(3-hydroxybutyrate) (P3HB), which offers an attractive biodegradable alternative to semicrystalline isotactic polypropylene but is brittle and opaque. We enhance the specific properties and mechanical performance of P3HB by drastically toughening it and also rendering it with the desired optical clarity while maintaining its biodegradability and crystallinity. This toughening strategy of stereo-microstructural engineering without changing the chemical compositions also departs from the conventional approach of toughening P3HB through copolymerization that increases chemical complexity, suppresses crystal-lization in the resulting copolymers, and is thus undesirable in the context of polymer recycling and performance. More specifically, syndio-rich P3HB (sr-P3HB), readily synthesized from the eight-membered meso-dimethyl diolide, has a unique set of stereo-microstructures comprising enriched syndiotactic [rr] and no isotactic [mm] triads but abundant stereo-defects randomly distributed along the chain. This sr-P3HB material is characterized by high toughness (UT = 96 MJ/m 3 ) as a result of its high elongation at break (>400%) and tensile strength (34 MPa), crystallinity (T m = 114 degrees C), optical clarity (due to its submicron spherulites), and good barrier properties, while it still biodegrades in freshwater and soil.
This report describes the outcomes of the third and final year of a project to research the feasibility of tagging uranium materials, especially nuclear fuels. The experimental focus remained on metallic uranium forms under prospective surface and bulk tagging scenarios. Overall, the results showed that the tags could be successfully imparted and characterized in both as-built and degraded conditions. This was in line with expectations coming into this project, indicating promise for both surface and bulk tagging of metallic forms of uranium. Multiple surface tagging techniques and detection strategies were explored in FY21, with an emphasis on improving tag quality, readability, and detection in the field. Non-radioactive materials were used as a testbed. Selective deposition via laser beam was determined to be successful in imparting a readable titanium deposit on a stainless steel base plate, and can be read with high resolution characterization techniques (e.g., scanning electron microscopy) and field capable tools (e.g., eddy current testing). Other deposition techniques, such as selective deposition via electron beam and photoluminescent tags, were explored in FY21, and while success for these techniques would be dependent on additional work, these techniques showed potential for surface tagging applications. To survey bulk taggant elements for bulk uranium metal, 16 tagging elements were spread among 18 depleted uranium castings (4 baseline, 3 mix, 1 dilution, and 10 recycle). Most of these were made and characterized in FY21. Taggant acceptability was based upon manufacturability, detectability, and persistence from the standpoint of two detection options: bulk chemical analysis (for “chemical taggants”) and microstructural analysis (for “second phase taggants”). Taggant detection in both up-front manufacturing and in the face of “degradations” such as dilution, mixing, and recycling was generally good. Two independent laboratories carried out chemical analysis on most of the castings, and often at several locations within a casting, and the results are discussed. Scanning electron microscopy+EDS microanalysis revealed the second phases mostly contained the expected tagging elements. The shapes and 2 spatial distributions of these micron-sized carbides, oxides, and intermetallic particles offers opportunities for further science-based investigation and tagging optimization. Overall, V and Co currently appear as the best choices for chemical taggants while Al, Ti, Mn, Co, Pd, and Tb all look good as second phase taggants. The other elements considered here – Sc, Ni, Ge, Nb, Ce, Ta, W, Ir, and Au – while not being ruled out, require more study to become viable options. It is of special note that in the recycling study only one of the 12 elements fell out of detection even after 10 meltings, demonstrating their persistence. An Appendix tabulates all chemical analysis results to enable more quantitative and statistical studies of detection opportunities and limitations, as a part of a related project.
Principal advantage of angular-power-spectrum scanning (APSS) is that, unlike x-radiography and prior ultrasonic techniques, it reveals subtle distributions of microstructural features; e.g., variations in densities of micropores or regions in which fibers and matrices are poorly bonded to each other. Potential applications include development and characterization of composite-material components of large structures, such as buildings and bridges; determination of quality and detection of damage in fiberglass hulls, surfboards, ladders, and scaffolds; and development of porous prosthetic skins and complicated "smart" materials. Superposed diffraction patterns give clues to internal structural features of ceramic composites.
The present investigation examines the effects of manufacturing process on the total axial strain controlled low cycle fatigue behavior of polycrystalline NiAl at 1000 K, a temperature above the monotonic Brittle-to-Ductile Transition Temperature (BDTT). The nickel aluminide samples were produced by three different processing routes: hot isostatic pressing of pre- alloyed powders, extrusion of prealloyed powders, and extrusion of vacuum induction melted ingots. The LCF behavior of the cast plus extruded material was also determined at room temperature (below the BD77) for comparison to the high temperature data. The cyclic stress response, cyclic stress-strain behavior, and strain-life relationships were influenced by the alloy preparation technique and the testing temperature. Detailed characterization of the LCF tested samples was conducted by optical and electron microscopy to determine the variations in fracture and deformation modes and to determine any microstructural changes that occurred during LCF testing. The dependence of LCF properties on processing route was rationalized on the basis of starting microstructure, brittle-to-ductile transition temperature, deformation induced changes in the basic microstructure, deformation substructure, and synergistic interaction between the damage modes.
On the Moon, the energetics of smaller impactors and the physical/chemical characteristics of the granular regolith target combine to form a key product of lunar space weathering: chemically reduced shock melts containing optically-active nanophase Fe metal grains (npFe0) [1]. In addition to forming the optically dark glassy matrix phase in lunar agglutinitic soil particles [1], these shock melts are becoming increasingly recognized for their contribution to optically active patina coatings on a wide range of exposed rock and grain surfaces in the lunar regolith [2]. In applying the lessons of lunar space weathering to asteroids, the potential similarities and differences in regolith-hosted shock melts on the Moon compared to those on asteroids has become a topic of increasing interest [3,4]. In a series of impact experiments performed at velocities applicable to the asteroid belt [5], Horz et al. [6] and See and Horz [7] have previously shown that repeated impacts into a gabbroic regolith analog target can produce melt-welded grain aggregates morphologically very similar to lunar agglutinates [6,7]. Although these agglutinate-like particles were extensively analyzed by electron microprobe and scanning electron microscopy (SEM) as part of the original study [7], a microstructural and compositional comparison of these aggregates to lunar soil agglutinates at sub-micron scales has yet to be made. To close this gap, we characterized a representative set of these aggregates using a JEOL 7600 field-emission scanning electron microscope (FE-SEM), and JEOL 2500SE field-emission scanning transmission electron microscope (FE-STEM) both optimized for energy dispersive X-ray spectroscopy (EDX) compositional spectrum imaging at respective analytical spatial resolutions of 0.5 to 1 micron, and 2 to 4 nm.
The multiscale structure of biomaterials enables their exceptional mechanical robustness, yet the impact of each constituent at their relevant length scale remains elusive. Here, we used SAXD analysis to expose the intact chitin-fiber architecture within the exoskeleton on a scorpion's claw, revealing varying orientations, including Bouligand and unidirectional regions different from other arthropod species. We uncovered the contribution of individual components’ constituent behavior to its mechanical properties from the micro- to the nanoscale. At the microscale, in-situ micromechanical experiments were used to determine site-specific stiffness, strength, and failure of the biocomposite due to fiber orientation, while metal-crosslinking of proteins is characterized via fluorescence maps. At the constituent level, combined with FEA simulations, we uncovered the behavior of fiber-matrix deformation with fiber diameter <53.7 nm and protein modulus in the range 1.4–11 MPa. The unveiled microstructure-mechanics relationship sheds light on the evolved structural functionalities and constituents' interactions within the scorpion cuticle.
Directed energy deposition (DED) with a coaxial wire-laser configuration has gained significant attention in recent years for the production of large-scale metallic components because of its low directional dependence, fast deposition rate, high feedstock efficiency, and low manufacturing costs. This work studies the coaxial wire-laser DED process of Inconel 718 alloy under a stable deposition condition with a relatively low input volumetric energy density (55.5J/mm 3 ). Post characterization reveals a cluster of refined grains at the center-bottom region of the as-printed track. Operando high-energy synchrotron X-ray experiments and multi-physics modeling are applied innovatively to study the fundamental mechanism responsible for the formation of this microstructure. The X-ray diffraction experiment provides direct evidence, which is supported by the simulation, that the feeding wire can reach the melt pool bottom and release solid particles (primarily carbides) near the mushy zone owing to insufficient melting. Consequently, these sub-micron sized particles suppress the growth of large columnar grains and cause the formation of unique microstructural heterogeneity. In conclusion, this discovery offers new opportunities for tailoring the solidification microstructure by controlling the melting state of the feedstock wire in DED process, in addition to commonly known factors such as the thermal gradient and solidification velocity.
Additive manufacturing of functional materials is limited by control of microstructure and assembly at the nanoscale. In this work, we integrate nonequilibrium self-assembly with direct-write three-dimensional (3D) printing to prepare bottlebrush block copolymer (BBCP) photonic crystals (PCs) with tunable structure color. After varying deposition conditions during printing of a single ink solution, peak reflected wavelength for BBCP PCs span a range of 403 to 626 nm (blue to red), corresponding to an estimated change in d-spacing of >70 nm (Bragg- Snell equation). Physical characterization confirms that these vivid optical effects are underpinned by tuning of lamellar domain spacing, which we attribute to modulation of polymer conformation. Using in situ optical microscopy and solvent-vapor annealing, we identify kinetic trapping of metastable microstructures during printing as the mechanism for domain size control. More generally, we present a robust processing scheme with potential for on-the-fly property tuning of a variety of functional materials.
Physical imaging is a foundational characterization method in areas from condensed matter physics and chemistry to astronomy and spans length scales from atomic to universe. Images encapsulate crucial data regarding atomic bonding, materials microstructures, and dynamic phenomena such as microstructural evolution and turbulence, among other phenomena. The challenge lies in effectively extracting and interpreting this information. Variational Autoencoders (VAEs) have emerged as powerful tools for identifying the underlying factors of variation in image data, providing a systematic approach to distilling meaningful patterns from complex data sets. However, a significant hurdle in their application is the definition and selection of appropriate descriptors reflecting local structures. Here, we introduce the scale-invariant VAE approach (SI-VAE) based on the progressive training of the VAE with the descriptors sampled at different length scales. The SI-VAE allows the discovery of the length scale-dependent factors of variation in the system. Here, we illustrate this approach using the ferroelectric domain images and generalize it to the movies of the electron-beam induced phenomena in graphene and topography evolution across combinatorial libraries. This approach can further be used to initialize the decision making in automated experiments including structure–property discovery and can be applied across a broad range of imaging methods. This approach is universal and can be applied to any spatially resolved data including both experimental imaging studies and simulations, and can be particularly useful for exploration of phenomena such as turbulence and scale-invariant transformation fronts.
Two of the most common plessite structures, duplex and black plessite, in the taenite region of the Windmanstatten pattern of two iron meteorites (Grant and Carlton) are characterized using high-resolution electron microscopy and microanalysis techniques. Two types of gamma precipitates, found in the duplex plessite and black plessite regions, respectively, are identified, and their morphologies are described. The formation of the plessite structure is discussed using the information obtained in this study and results of a parallel investigation of decomposed martensitic Fe-Ni laboratory alloys.
This paper discusses the fabrication aspects of a sensor device that is based on a sputter deposited multilayer giant magnetoresistive (GMR) sensor. The device consists of a micromachined microstructure (membrane), GMR sensor, and a sputtered hard magnetic thin film element on to microstructure.
In metal additive manufacturing (AM), understanding the process-structure-performance relationships requires a combination of multi-scale characterization techniques that allows for the measurement of the melt pool shape and boundary and classifying various defects and flaws in the AM parts. Such approaches can be destructive, only 2D in nature, or have a small field of view and can be complex to co-register and analyze. Here, in this work, we present a non-destructive 3D inspection technique that employs dual-energy X-ray computed tomography (XCT) along with a model-based iterative reconstruction (MBIR) and a new segmentation algorithm. The proposed approach and algorithm are not only capable of classifying and quantifying flaws such as pores, cracks, and inclusions, but they also allow for the extraction of microstructural features such as melt pool boundaries (MPB) and melt pool regions (MPR), that can help understand process-structure-performance relationships for alloys under study. As an exemplar application, we employed the method for characterization of an additively manufactured aluminum alloy crept under tensile stress at 300 °C for 1064 h. Our results demonstrate high quality segmentation and classification of various flaws and MPB and MPR, for the first time, using 3D X-ray CT inspection. The delineated MPB and MPR in the crept samples reveal the preferential growth paths of cracks that formed during creep deformation. The technique was used for successfully quantifying the characteristics (number of defects, their density, volume fraction, etc.) of the manufacturing-induced pores and creep-induced cracks, which is necessary to better understand the creep failure mechanisms of the material.