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573 records · Page 32
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Characterization of Alloy 709 Commercial Heats

The creep-resistant austenitic stainless steel Alloy 709 (Fe-20Cr-25Ni (wt%) based steel) is being investigated as a candidate structural material for the next generation of advanced reactors. Unlike conventional solid solution strengthened austenitic stainless steels, Alloy 709 develops a variety of precipitates during aging at different temperatures and times. In this study, precipitate evolution during short-term aging at 775°C was characterized. The effect of aging time (e.g., 10 vs. 100 hours) and cooling after aging (e.g., water quench vs. air cool) on grain size and precipitates have been investigated using light optical microscopy (OM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDS). MX (Ni,Tb)(C,N) and M23C6 (Cr,Mo)C precipitates were observed in all the statically-aged samples. The grain size distribution in the sample aged for 10 hours and water quenched (10Q) versus the one aged for 100 hours and air cooled (100A) were comparable. This indicates that grain structure was fairly stable when aging at 775°C for up to 100 hours. In contrast, the sample aged for 10 hours and air cooled (10A) showed the smallest and the most uniform grain size distribution. This phenomenon was observed in only one sample. More studies on duplicate samples are needed to confirm the results obtained. The cooling medium (e.g., water quench vs. air cool) was not observed to impact the size nor the distribution of the MX and M23C6 precipitates. Increasing the aging time resulted in the following: (1) a decrease in dislocations as well as the number density of small precipitates; (2) an increase in the ratio of free precipitates that were not pinning dislocations; (3) relatively higher N, Nb, and Ti concentration in MX precipitate; (4) some increase in length of M23C6 carbides which were located on the coherent boundaries; and (5) the introduction of Sienriched M6X precipitates. The tensile tests at room temperature showed similar properties for each of the static aging treatments, indicating that the differences observed in the microstructural analysis did not have a significant impact on the tensile properties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Formation and Restacking of Disordered Smectite Osmotic Hydrates

Clay swelling, an important phenomenon in natural systems, can dramatically affect the properties of soils and sediments. Something of particular interest in low-salinity, saturated systems are osmotic hydrates, forms of smectite in which the layer separation greatly exceeds the thickness of a single smectite layer due to the intercalation of water. In situ X-ray diffraction (XRD) studies have shown a strong link between ionic strength and average interlayer spacing in osmotic hydrates but also indicate the presence of structural disorder that has not been fully described. In the present study the structural state of expanded smectite in sodium chloride solutions was investigated by combining very low electron dose, high-resolution cryogenic-transmission electron microscopy observations with XRD experiments. Wyoming smectite (SWy-2) was embedded in vitreous ice to evaluate clay structure in aqua. Lattice-fringe images showed that smectite equilibrated in aqueous, low-ionic-strength solutions, exists as individual smectite layers, osmotic hydrates composed of parallel layers, as well as disordered layer conformations. There was no evidence found here for edge-to-sheet attractions, but significant variability in interlayer spacing was observed. Whether this variation could be explained by a dependence of the magnitude of long-range cohesive (van der Waals) forces on the number of layers in a smectite particle was investigated here. Calculations of the Hamaker constant for layer-layer interactions showed that van der Waals forces may span at least five layers plus the intervening water and confirmed that forces vary with layer number. The drying of the disordered osmotic hydrates induced re-aggregation of the smectite to form particles that exhibited coherent scattering domains. Clay disaggregation and restacking may be considered as an example of oriented attachment, with the unusual distinction that it may be cycled repeatedly by changing solution conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Enhanced Propagating Surface Plasmon Signal Detection

Overcoming the dissipative nature of propagating surface plasmons (PSPs) is pre-requisite to realizing functional plasmonic circuitry, in which large bandwidth signals can be manipulated over length scales far-below the diffraction limit of light. To this end, we report on a novel PSP enhanced signal detection technique achieved in an all-metallic substrate. We take advantage of two strategically spatio-temporally separated phase-locked femtosecond laser pulses, incident onto lithographically patterned PSP coupling structures. We follow PSP propagation with joint femtosecond temporal and nanometer spatial resolution in a time-resolved non-linear photoemission electron microscopy scheme. Initially, a PSP signal wave packet is launched from a hole etched into the silver surface from where it propagates through an open trench structure and is decoded through the use of a timed probe pulse. FDTD calculations demonstrate that PSP signal waves may traverse open trenches in excess of 10 microns in diameter, thereby allowing remote detection even through vacuum regions. This arrangement results in a 10X enhancement in photoemission relative to readout from the bare metal surface. The enhancement is attributed to an all-optical homodyne detection technique that mixes signal and reference PSP waves in a non-linear scheme. Larger readout trenches achieve higher readout levels, however reduced transmission through the trench limits the trench size to 6 microns for maximum readout levels. However, the use of an array of trenches increases the maximum enhancement to near 30X. The attainable enhancement factor may be harnessed to achieve extended coherent PSP propagation in ultrafast plasmonic circuitry.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2020

Multi-beam X-ray ptychography for high-throughput coherent diffraction imaging

X-ray ptychography is a rapidly developing coherent diffraction imaging technique that provides nanoscale resolution on extended field-of-view. However, the requirement of coherence and the scanning mechanism limit the throughput of ptychographic imaging. Herein, we propose X-ray ptychography using multiple illuminations instead of single illumination in conventional ptychography. Multiple locations of the sample are simultaneously imaged by spatially separated X-ray beams, therefore, the obtained field-of-view in one scan can be enlarged by a factor equal to the number of illuminations. We have demonstrated this technique experimentally using two X-ray beams focused by a house-made Fresnel zone plate array. Two areas of the object and corresponding double illuminations were successfully reconstructed from diffraction patterns acquired in one scan, with image quality similar with those obtained by conventional single-beam ptychography in sequence. Multi-beam ptychography approach increases the imaging speed, providing an efficient way for high-resolution imaging of large extended specimens.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations

Solid-phase epitaxy (SPE) and other three-dimensional epitaxial crystallization processes pose challenging structural and chemical characterization problems. The concentration of defects, the spatial distribution of elastic strain, and the chemical state of ions each vary with nanoscale characteristic length scales and depend sensitively on the gas environment and elastic boundary conditions during growth. The lateral or three-dimensional propagation of crystalline interfaces in SPE has nanoscale or submicrometer characteristic distances during typical crystallization times. Here, an in situ synchrotron hard x-ray instrument allows these features to be studied during deposition and crystallization using diffraction, resonant scattering, nanobeam and coherent diffraction imaging, and reflectivity. The instrument incorporates a compact deposition system allowing the use of short-working-distance x-ray focusing optics. Layers are deposited using radio-frequency magnetron sputtering and evaporation sources. The deposition system provides control of the gas atmosphere and sample temperature. The sample is positioned using a stable mechanical design to minimize vibration and drift and employs precise translation stages to enable nanobeam experiments. Results of in situ x-ray characterization of the amorphous thin film deposition process for a SrTiO 3 /BaTiO 3 multilayer illustrate implementation of this instrument.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

Interfacial design and strengthening mechanisms of AZ91 alloy reinforced with in-situ reduced graphene oxide

Highlights: • An in-situ process was developed to synthesize magnesium alloy composite reinforced by graphene. • Microstructure and phase composition of oxide films were investigated by OM, SEM, EDS and XRD analysis. • The interfacial structure of Mg composites reinforced with reduced graphene oxide was characterized. • The interfacial reaction mechanisms between GO (graphene oxide) and the Mg metal was studied. - Abstract: This work highlights to develop an in-situ process to disperse uniformly graphene possessing good interfacial bonds with the matrix of Mg alloy. A homogeneous distribution of graphene in the matrix has been successfully obtained through in-situ reduction of graphene oxide (RGO) by sintering process after the graphene oxide (GO) was uniformly dispersed in AZ91 powders. The interface product nano-sized MgO can significantly improve the interfacial bonding strength between RGO and α-Mg with analysis by transmission electron microscopy. The orientation relationships of ( 2-bar 00){sub MgO}//( 1-bar 10 2-bar ){sub α‐Mg} and [011]{sub MgO}//[2 4-bar 2 3-bar ]{sub α‐Mg} with the semi-coherent interface characteristics were clarified for the first time at the interface of MgO/α-Mg, suggesting a good lattice space matching. By employing such process, a composite containing 0.5 wt% of GO shows an 85.7% and 61.4% increase in yield strength and elongation, respectively, over unreinforced AZ91 alloy. The underlying strengthening mechanisms of in-situ reduced graphene oxide are discussed in detail.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

Electric field driven domain wall dynamics in BaTiO 3 nanoparticles

We report a detailed investigation into the response of single BaTiO 3 (BTO) nanocrystals under applied electric fields (E-field) using Bragg coherent diffraction imaging. Our study reveals pronounced domain wall migration and expansion of a sample measure under applied electric field. The changes are most prominent at the surface of the nanocrystal, where the lack of external strain allows greater domain wall mobility. The observed domain shifts are correlated to the strength and orientation of the applied E-field, following a side-by-side domain model from Suzana []. Notably, we identified a critical electric field strength of 3 MV/m, which leads to irreversible structural changes, suggesting plastic deformation. The findings highlight how surface effects and intrinsic defects contribute to the enhanced dielectric properties of BTO at the nanoscale, in contrast to bulk materials, where strain limits domain mobility. These findings deepen our understanding of nanoscale dielectric behavior and inform the design of advanced nanoelectronic devices. Published by the American Physical Society 2025

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Investigations on residual strains and the cathodoluminescence and electron beam induced current signal of grain boundaries in silicon

Cathodoluminescence (CL) and electron beam induced current (EBIC) measurements were used to investigate the optical behavior and electrical activity of grain boundaries (GBs) in coarsely grained silicon. Electron backscatter diffraction (EBSD) was applied for a comprehensive characterization of the structural properties of the high angle and low angle GBs (HAGBs and LAGBs) in the sample. It was found that not only the EBIC but also the panchromatic (pan) CL contrast of Σ3 HAGBs strongly depends on the hkl-type of the boundary plane. At room temperature coherent Σ3 GBs exhibit no significant contrast in the CL or EBIC images, whereas at low temperatures the pan-CL contrast is strong. For incoherent Σ3 GBs, a strong pan-CL and EBIC contrast was observed in the entire temperature range. Only on a LAGB (misorientation angle 4.5°) CL investigations at low temperatures revealed a line with peak position at about (0.82 ± 0.01) eV, usually related to the dislocation associated D1 transition. Cross-correlation EBSD was applied to analyze the strain fields of Σ3 HAGBs as well as of the LAGB. All the components of the local strain tensors were quantitatively determined. The relationship between the extension of the strain field at the LAGB and the spatial D1 intensity distribution is discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

AI-enabled high-resolution scanning coherent diffraction imaging

Ptychographic imaging is a powerful means of imaging beyond the resolution limits of typical x-ray optics. Capturing recovered images from raw ptychographic data, however, requires the solution of an inverse problem, namely, phase retrieval. Phase retrieval algorithms are computationally expensive, which precludes real-time imaging. In this work, we propose PtychoNN, an approach to solve the ptychography data inversion problem based on a deep convolutional neural network. We demonstrate how the proposed method can be used to predict real-space structure and phase at each scan point solely from the corresponding far-field diffraction data. Our results demonstrate the practical application of machine learning to recover high fidelity amplitude and phase contrast images of a real sample hundreds of times faster than current ptychography reconstruction packages. Furthermore, by overcoming the constraints of iterative model-based methods, we can significantly relax sampling constraints on data acquisition while still producing an excellent image of the sample. Besides drastically accelerating acquisition and analysis, this capability has profound implications for the imaging of dose sensitive, dynamic, and extremely voluminous samples.

47 OTHER INSTRUMENTATION↗
DOE OSTI2011

On the selective growth of titania polymorphs in acidic aqueous medium

Highlights: Black-Right-Pointing-Pointer Mutual influence of peptizing and anions addition of titania hydrothermal growth was studied. Black-Right-Pointing-Pointer Sulfate and chloride control TiO{sub 2} phase or particles shape depending on the order of introduction. Black-Right-Pointing-Pointer A rationale of difference between sulfate and chloride effect was provided. Black-Right-Pointing-Pointer Ground state DFT and semi-empirical calculations of Ti species support the conclusions. -- Abstract: The influence of preparation conditions on the phase composition and morphology of titania was studied for the solids synthesized by hydrothermal treatment (HT) and peptizing of hydrous TiO{sub 2} sols in acidic medium. Mutual influence of peptizing and of additive anions (SO{sub 4}{sup 2-}, Cl{sup -}) on the nature of obtained polymorphs was for the first time systematically studied and coherently explained. The solids were characterized by XRD, Raman spectroscopy, and transmission electron microscopy. It was found that peptizing step preceding HT and the presence of anions play a crucial role for the selective formation of TiO{sub 2} anatase or rutile polymorphs. Low temperature peptizing leads to acicular rutile particles, whereas HT produces highly dispersed anatase. However if the HT was preceded by peptizing step, rutile was obtained in most cases. The influence of additives strongly depends on the moment of their introduction. Sulfate and chloride species can act as phase growth controllers, or as morphology modifiers. Sulfate hindered formation of rutile and favored anatase al low temperatures, but for already formed rutile seed, sulfate acted only as a shape controller. By contrast, chloride showed a strong tendency to promote rutile growth, whatever the conditions. A qualitative model was proposed explaining the effects observed, supported by ground state DFT and semi-empirical calculations of the aqueous Ti species.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Continuous motion scan ptychography: Characterization for increased speed in coherent x-ray imaging

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object’s complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous “fly-scan” mode for ptychographic data collection in which the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.

43 PARTICLE ACCELERATORS↗
DOE OSTI2023

Antiferromagnetic real-space configuration probed by dichroism in scattered x-ray beams with orbital angular momentum

X-ray beams with orbital angular momentum (OAM) are a promising tool for x-ray characterization techniques. Beams with OAM have a helicity - an azimuthally varying phase - which leads to a gradient of the light field. New material properties can be probed by utilizing the helicity of an OAM beam. Here, we demonstrate a dichroic effect in resonant diffraction from an artificial antiferromagnet with a topological defect. We found that the scattered OAM beam has circular dichroism at the antiferromagnetic Bragg peak whose sign is coupled to its helicity, which reveals the real-space configuration of the antiferromagnetic ground state. Thermal cycling of the artificial antiferromagnet can change the ground state, as indicated by reversal of the sign of circular dichroism. This result is one of the first demonstrations of a soft x-ray spectroscopy characterization technique utilizing the OAM of x rays. In conclusion, this helicity-dependent circular dichroism exemplifies the potential to utilize OAM beams to probe matter in a way that is inaccessible using currently available x-ray techniques.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Decomposition of molybdate-hexamethylenetetramine complex: One single source route for different catalytic materials

Decomposition of ammonium heptamolybdate-hexamethylentetramine (HMTA) complex (HMTA){sub 2}(NH{sub 4}){sub 4}Mo{sub 7}O{sub 24}.2H{sub 2}O was studied as a function of treatment conditions in the range 300-1173 K. The evolution of solid products during decomposition was studied by thermal analysis and in situ EXAFS. Depending on the nature of the gas used for treatment, single phases of highly dispersed nitrides Mo{sub 2}N, carbide Mo{sub 2}C, or oxide MoO{sub 2} can be obtained. The nature of the products obtained was explained by qualitative thermodynamical considerations. Morphology of the solids considerably depends on such preparation parameters as temperature and mass velocity of the gas flow. For the nitride-based materials, catalytic activity was evaluated in the model thiophene HDS reaction. It was demonstrated that NH{sub 3}-treated samples showed better catalytic activity than N{sub 2}-treated ones due to cleaner surface and better morphology. Transmission microscopy, XRD and XPS studies showed that MoS{sub 2} is formed on the surface during HDS reaction or sulfidation with H{sub 2}S. Optimized nitride-derived catalysts showed mass activity several times higher than unsupported MoS{sub 2} or MoS{sub 2}/Al{sub 2}O{sub 3} reference catalyst. - Graphical Abstract: Depending on the conditions, decomposition of molybdate-HTMA complex yields highly dispersed molybdenum nitride, carbide or oxide. Research Highlights: > Decomposition of molybdate-HTMA complex yields highly dispersed Mo{sub 2}N, Mo{sub 2}C or MoO{sub 2}. > In situ EXAFS shows formation of common amorphous product MoC{sub x}N{sub y}O{sub z} at 673 K. > Crystalline Mo{sub 2}N with surface area near 200 m{sup 2}/g was obtained at 823 K. > High mass activity in thiophene HDS was observed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Mechanistic Insights into Defect-Mediated Crystallization Revealed by Lattice Strain Evolution

Structural defects and lattice strain are intrinsic to many crystalline materials, yet their roles in controlling chemical reaction mechanisms and directing crystallization pathways remain poorly understood. Here, in this study, we revealed the three-dimensional evolution of strain and dislocation defects at the nanoscale during the growth of heterogeneously nucleated barite (BaSO 4 ) and calcite (CaCO 3 ) crystals by using coherent X-ray scattering, electron microscopy, and molecular simulations. Unlike barite, which formed with minimal internal strain, calcite developed dislocation defects and exhibited spatially varying strain that increased during growth. During growth in Sr-rich solutions, calcite likely incorporates Sr 2+ into the defects, which further modulates the local lattice structure and increases both the compressive and tensile strain. These findings suggest that calcite crystallization was likely dominated by attachment of precursor phases, which gave rise to defect-enriched domain structures not predicted by classical growth models. By linking defect formation to ion incorporation and growth dynamics, this work provides fundamental insight into how lattice-level strain heterogeneity governs the chemical reactivity of ionic crystals.

Bragg coherent diffractive imaging↗
NASA NTRS2022

Atomic-Scale Structure and Non-Stoichiometry of Meteoritic Hibonite: A Transmission Electron Microscope Study

Hibonite (CaAl_12O_19) is a common refractory mineral in Ca-Al-rich inclusions (CAIs) in primitive meteorites. Transmission electron microscope (TEM) studies have identified enigmatic planar defects in different occurrences of hibonite in the Allende meteorite that give rise to strong streaking along c* in electron diffraction patterns. Atomic resolution high-angle annular dark-field (HAADF) imaging and energy-dispersive X-ray (EDX) analyses were used to determine the nature and origin of these planar features. HAADF images of hibonite grains reveal lamellar intergrowths of common 1.6 nm spacing, and less commonly 2.0 and 2.5 nm spacings, interspersed in stoichiometric hibonite showing 1.1 nm (002) spacing. Stoichiometric hibonite consists of alternating Ca-containing (“R”) and spinel-structured (“S”) blocks stacked in a sequence RS. In contrast, the 1.6 nm layers result from a doubled S block such that the stacking sequence is RSS, while in the widest defect observed, the stacking sequence is RSSSS. These intergrowths are epitaxial and have coherent, low-strain boundaries with the host hibonite Meteoritic hibonite shows common Ti and Mg substitution for Al in its structure. Atomic-resolution EDX maps of hibonite grains in the Allende CAI confirm the preferred site occupancy of Mg on tetragonal M3 sites in S blocks and of Ti on trigonal bipyramidal M2 and octahedral M4 sites in R blocks. Mg is highly concentrated, but Ti is absent in the planar defects where wider S blocks show Al-rich compositions compared to stoichiometric MgAl_2O_4 spinel. Therefore, Mg likely played the major role in the formation and metastability of planar defects in hibonite. Electron energy loss spectroscopy data from the Ti L_2,3 edge show the presence of mixed Ti oxidation states with ~ 15–20% of Ti as Ti^(3+) in hibonite, suggesting a direct substitution of Ti^(3+) ↔ Al^(3+) in hibonite. The remaining ~ 80–85% of Ti is present as Ti^(4+) and corresponding EDX analyses are consistent with the well-known coupled substitution 2Al^(3+) ↔ Ti^(4+) + Mg^(2+) being the major mechanism for Ti and Mg substitution in hibonite. The formation of planar defects in hibonite occurred during high-temperature nebular condensation or melting/crystallization processes. The occurrence of non-stoichiometric hibonite in the Allende CAI deviates from the mineral formation sequence predicted from equilibrium condensation models. Overall, our atomic resolution TEM observations signify non-equilibrium, kinetic-controlled crystal growth during the high-temperature formation of refractory solids in the early solar nebula.

hibonite↗