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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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At least 793 records · Page 44
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Neutron diffraction study of magnetic ordering in high pressure phases of rare earth metal holmium

The magnetic ordering in rare earth metals is well established for ambient pressure crystal structures, however, little is known about the magnetic ordering in their corresponding high-pressure crystalline modifications. Holmium (Ho) was studied in a large-volume diamond anvil cell at the Spallation Neutron Source to high-pressure up to 20 GPa and to low-temperature to 10 K. We have conducted two independent high-pressure low-temperature experiments under non-hydrostatic and quasi-hydrostatic pressure conditions respectively. The ambient pressure hexagonal close packed (hcp) phase of holmium shows two magnetic transitions below 10 GPa one to an incommensurate Antiferromagnetic (AFM) phase and another to a conical-Ferromagnetic (c-FM) phase. In contrast, alpha-Samarium-type (α-Sm) phase above 10 GPa and the double hexagonal close packed (dhcp) phase above 19 GPa show only one FM transition marked by the appearance of a magnetic peak at 3 Å and the concurrent enhancement of nuclear peaks below 30 K. Finally, these new transitions observed by neutron diffraction can be accounted by a commensurate superlattice formation along c-axis in both the α-Sm-type phase and the dhcp phase.

36 MATERIALS SCIENCE↗
DOE OSTI2023

In-situ investigation of strengthening and strain hardening mechanisms of Cu-added medium-Mn steels by synchrotron-based high-energy X-ray diffraction

A novel Cu-added medium-Mn steel with a chemical composition of Fe–0.27C–9.1Mn–1.86Al–3.3Cu (wt.%) was designed and subjected to intercritical annealing (IA) temperature range from 620 °C to 680 °C for 1 h. The ultimate tensile strength (UTS) increases and the yielding strength (YS) decreases with the IA temperature increasing. The YS of 824 MPa, UTS of 1222 MPa, total elongation (TE) of 55%, and product of strength and elongation (PSE) of 67.2 GPa·% are achieved after IA at 660 °C. Transmission electron microscopy confirmed that Cu-rich nanoparticles precipitate in the ferrite. The in-situ high-energy X-ray diffraction (HE-XRD) experiments show that at the beginning of plastic deformation, both austenite and ferrite bear the applied load. The load is mainly undertaken by martensite with effective transformation-induced plasticity (TRIP) effect triggered. The YS of ferrite is significantly higher than that of austenite. The individual contribution of solid solution strengthening, grain refinement strengthening, dislocation strengthening, and precipitation strengthening in ferrite and austenite is analyzed. The discrepancy between the YS of ferrite and austenite is mainly attributed to the precipitation strengthening due to the Cu-rich nanoparticles precipitation. The moderate mechanical stability and the collaboration of TRIP and twinning-induced plasticity (TWIP) effects of austenite contributed to the enhanced strain hardening capability and resulted in large ductility.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Correlating energy density induced residual stress, porosity, and mechanical property variations in directed energy deposition using neutron diffraction and imaging techniques

In a directed energy deposition (DED) process, the energy density deposited into the materials drives the structure and properties. The energy density is influenced by several printing parameters, such as laser power, hatch spacing, scanning speed, etc. In this study, 316L stainless steels samples were fabricated with varying hatch spacing aiming to induce variations in sample microstructure and properties. A combination of techniques including engineering neutron diffraction, neutron computed tomography, and tensile testing, were employed to correlate the structure and macroscopic properties. Porosity was predominantly observed at the bottom of the deposited materials and was effectively reduced by decreased hatch spacing. Correlatively, compressive residual stress was observed at the bottom of the specimens, while internal stress is largely determined by the hatch spacing. The residual stress in general decreases as the hatch spacing decreases. The maximum ultimate tensile strength (UTS) was found to increase from 517.4 to 528.6 MPa with a strain increased from 0.847 to 0.897 as the hatch spacing decreased from 0.45 to 0.42 mm. However, further increase in energy density by reducing the hatch spacing resulted in a significant decrease in UTS (as low as 452 MPa). This work provides new insights from bulk non-destructive techniques into correlating energy density induced residual stress, porosity, and mechanical property variations in directed energy deposition.

316L stainless steel↗
DOE OSTI2025

Probing the high-pressure densification of amorphous silica nanomaterials using SBA-15: An investigation into the paradoxical nature of the first sharp diffraction peak

The densification and X-ray scattering of mesoporous silica (SBA-15) were measured simultaneously under gigapascal (GPa) pressures. The results are compared to previous work on amorphous silica (aSiO 2 ) and demonstrate the feasibility of measuring the densification of aSiO 2 nanomaterials with small angle X-ray scattering (SAXS) in-situ in a diamond anvil cell. Compared to fused silica, the position of the SBA-15 first sharp diffraction peak (FSDP) is 7 times more sensitive to pressure and has a transition in its pressure dependance at a lower pressure (~2 GPa vs.~13 GPa). SBA-15 has two densification regimes, low-density amorphous and highdensity amorphous, which have equations of state comparable to low-density amorphous and high-density amorphous fused silica. Further, the transition between these two regimes occurs at a lower pressure than for fused silica (~1.5 GPa vs.~13 GPa). The results suggest that there is no direct relationship between the FSDP position and the aSiO 2 density during compression.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

High-energy x-ray diffraction microscopy study of deformation microstructures in neutron-irradiated polycrystalline Fe-9%Cr

In this paper, we used far-field high-energy x-ray diffraction microscopy (FF-HEDM) to measure in 3D the spatial distributions of the sizes, orientations, and residual strains of grains and subgrains formed by room-temperature tensile deformation in a neutron-irradiated (450 °C, 0.01dpa) Fe-9Cr specimen and its unirradiated counterpart. We found that neutron irradiation under this condition alone had no effect on the grain size distribution. After deformation, grains fragmented into subgrains in both unirradiated and irradiated specimens: the irradiated specimen contained a few large subgrains which co-existed with many smaller subgrains, while the unirradiated specimen contained small subgrains with a relatively uniform size distribution. Prior to deformation, the irradiated specimen had higher residual strain spread compared to its unirradiated counterpart, while after deformation to the maximum uniform elongation, the strain distributions among subgrains were similar between the unirradiated and irradiated specimens. The FF-HEDM measurements provide new insight into the effects of neutron irradiation on the mechanical response of Fe-Cr ferritic alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2020

An Electron Backscatter Diffraction Analysis of Grain Boundary Initiated Discontinuous Precipitation in U-10Mo

The effect of varied thermomechanical processing on discontinuous precipitation (DP) in U-10Mo was investigated, with specific emphasis on understanding the role of grain boundary misorientation in DP. Varied prior homogenization heat treatment and thermomechanical processing resulted in differences in both the fraction of DP and the colony width, and was attributed to variations in the grain boundary misorientation distribution. Regardless of the degree of DP-based transformation, extensive growth of DP colonies was dominant on 30°–45° misorientation boundaries. Interestingly, misorientation histograms of the deformed and annealed specimens suggest the processing steps involved may have inhibited DP colony growth along a small fraction of these high angle boundaries. Large-area electron backscatter diffraction montages coupled with high resolution mapping suggest symmetric {110}-type interfaces may be important considerations for mitigating extensive DP growth in this alloy system.

Discontinuous Precipitation, Uranium, Electron Bac↗
DOE OSTI2023

Phase transformations and thermal expansion coefficients of unirradiated U-X wt.% Zr (X = 6, 10, 20, 30) measured via neutron diffraction

This work characterizes the crystallographic evolution of unirradiated U-X wt.% Zr (X = 6, 10, 20, 30) while cooling from equilibration, single phase γ-U-Zr, at 900 °C to ambient temperature using time-of-flight neutron diffraction. The β-U phase was unobserved during cooling at 1 °C/min in all alloys. All alloys followed the phase transformation pathway of γ-U-Zr→γ-U-Zr+α-U→α-U +δ-UZr2 with an observed miscibility gap in γ-U-Zr. The α-U and δ-UZr2 transformation took place simultaneously in the U-30 wt.% Zr sample. These findings strengthen the need to re-approach the U-Zr phase diagram in entirety. Bulk volumetric CTEs agree well with published data, strengthening the quantification of lattice-specific CTEs reported in this study. A compositionally dependent discontinuity in thermal expansion, increasing in magnitude with decreasing U content, occurs during the γ-U-Zr→α-U+δ-UZr2 transformation. The γ-U-Zr lattice parameter was measured to have a compositional dependency.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Phase quantification in low carbon Nb-Mo bearing steel by electron backscatter diffraction technique coupled with kernel average misorientation

Highlights: • The microstructures in a low carbon Nb-Mo bearing steel have been investigated. • EBSD combined with a (KAM) map has been used for quantification. • The effects of step size and kernel size on quantification are systemically discussed. • The result indicates that the kernel size should be close to the sub-structure of the granular bainite. - Abstract: An efficient and accurate method is developed for microstructural quantification of complex phases in a low carbon Nb-Mo bearing steel, of which optical micrographs show that it consists of granular bainite and a small amount of ferrite. Our previous work, proposing a method to measure the misorientation angles via electron backscatter diffraction (EBSD) to differentiate granular bainite and ferrite, has been reported. That method is accurate for phase quantification but laborious for the characterization process. To resolve this difficulty, in this study, EBSD combined with a kernel average misorientation (KAM) map is used for phase characterization. Comparisons are made among KAM maps with different kernel sizes (300 to 600 nm) and various step sizes (100 to 600 nm). It is found that a kernel size close to the sub-structure size of granular bainite (500 nm) is optimal for phase identification, while varied step sizes produce relatively invariant results. Therefore, KAM maps can be used for fast and reliable phase quantification, provided that an appropriate kernel size and a large step size are used.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Elevated temperature transmission Kikuchi diffraction in the SEM

Highlights: • The potential of high temperature in-situ TKD characterization is demonstrated. • High quality Kikuchi patterns can be obtained at high temperature. • The very local heat of the MEMS-based heating system minimises infrared radiation. • TKD is a suitable technique for in-situ studies of solid state dewetting. - Abstract: Transmission Kikuchi diffraction (TKD) facilitates automated orientation mapping of thin films in scanning electron microscopes (SEM). In this study TKD is applied for the first time to perform in-situ annealing experiments on gold thin films deposited on a MEMS-based heating system. The very local heating associated with this system enables reliable TKD measurements at elevated temperatures without notable disturbance from infrared radiation. The dewetting of an Au thin film into Au nanoparticles upon heating is followed with orientation mapping in a temperature range between 20 °C and 900 °C. The local thickness variation associated with the dewetting is observed qualitatively by observing the intensity of the transmitted beam, which decreases as the film thickness increases locally. The results of this study reveal that TKD is a well suited technique to study thin-film stability and solid state dewetting. Moreover, the outcome of this methodological study provides a baseline for further in-situ crystallographic studies of electron transparent samples in the SEM.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Electron backscatter diffraction helps direct calculation of magnetocrystalline anisotropy energy in API 5L steels

Highlights: • Experimental evidence of the capability of EBSD to accurately estimate MAE of API 5L steels. • MAE can be calculated directly from raw EBSD data for reduced sample sizes. • Number of grains sufficient to estimate MAE from EBSD is in the order of several hundreds. • The use of equivalent orientations increases drastically the accuracy of MAE estimations. • EBSD helps explain origin of the observed correlation between MAE and Barkhausen noise. - Abstract: This paper shows evidence of the capability of electron backscatter diffraction (EBSD) to accurately estimate the magnetocrystalline anisotropy energy (MAE) of API 5L steels. The crystallographic texture of five circular steel samples was characterized by X-ray global texture and EBSD microtexture measurements. The average MAE of each one of these samples was estimated from the set of individual grain orientations obtained from orientation maps measured by EBSD. The angular dependence of EBSD-derived MAE was compared with predictions made from X-ray texture and Barkhausen noise (BHN) measurements. The average MAE determined from the EBSD data is in good agreement with the predictions made from X-ray and BHN measurements for all the studied samples. This agreement can be explained by the fact that the number of grains used to predict the average MAE from the EBSD results was statistically sufficient to reproduce the MAE predicted by the other two methods. The EBSD measurement strategy for the accurate MAE estimation was established in terms of parameters such as the number of individual grain orientations to be measured, the sample's texture acuity and grain size, the use of equivalent orientations given by the statistical orthorhombic symmetry of the studied samples, and different measurement planes.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Non-destructive compositional and microstructural characterization of Sardinian Bronze Age swords through Neutron Diffraction

Highlights: • Determination of the manufacturing technique of some “Sa Idda” swords • New data on their provenience • Determination of: alloy composition, dendritic segregation, mineralization phase - Abstract: The Monte Sa Idda type swords belong to a well characterized typological class, whose origin has long been debated and seems to coincide with the Iberian Peninsula. The name comes from the site of the first discovery of a hoard containing this type of swords, among other bronze artefacts, namely Monte Sa Idda, Decimoputzu-Cagliari, Italy. The swords were produced through fusion inside a casting mould. Such kind of casting mould has not been found in Sardinia, and this may suggests that finished objects were either imported or made using clay or sand casting mould. Moreover, the discovery of these types of sword, in hoards and in votive deposits, raises the problem of their functional use. It is unknown if the blades were intended to be used as weapons, and therefore subjected to cold working necessary for thinning and sharpening of the blade, or as ceremonial objects. In order to answer to these questions, a neutron diffraction experiment was performed on three swords belonging to the Monte Sa Idda type. The results obtained are presented and discussed in the paper.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Quantifying the inter- and intra-granular stresses and their effects on deformation behaviors for the polycrystalline hexagonal beryllium by neutron diffraction

Highlights: • The inter- and intra-granular stresses are quantified for the polycrystalline hexagonal metal beryllium. • Composite behavior of the internal stresses is revealed in the polycrystalline beryllium. • Those internal stresses show the obvious grain-orientation dependence. • Those stresses can be significantly tuned by the temperature and strain rate effects. • The dislocation slip and twinning are quantified together with the inter- and intra-granular stored energies. - Abstract: The internal stresses developing at different length scales play the important role in materials performance. This importance has been well recognized for the cubic metals, however, not for the hexagonal close-packed (hcp) ones. The present work investigates the intergranular and intragranular stresses in the polycrystalline hexagonal beryllium by neutron diffraction. The correlation between those internal stresses and the deformation mechanism is revealed, and the strain rate and temperature effects on those stresses are presented. A composite behavior of intergranular and intragranular stresses is observed, which can be significantly tuned by the temperature and strain rate effects. The intergranular stress and stored energy are large for the soft-oriented grains (SOGs), while the intragranular stress and stored energy are large for the hard-oriented ones (HOGs). Both of those stresses are significantly high for the dynamic strain rate while they are relatively low for the elevated temperature. The large internal stresses in the dynamically compressed specimen should be attributed to the large number of twins and high density of dislocations. Different HOGs-SOGs configurations are proposed on the light of those observations, which might facilitate the properties controlling and extend the application scope for the hcp metal beryllium.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Grain-resolved temperature-dependent anisotropy in hexagonal Ti-7Al revealed by synchrotron X-ray diffraction

Hexagonal metals have anisotropic coefficients of thermal expansion causing grain-level internal stresses during heating. High energy x-ray diffraction microscopy, a non-destructive, in situ, micromechanical and microstructural characterization technique, has been used to determine the anisotropic coefficients of thermal expansion (CTEs) for Ti-7Al. Two samples of polycrystalline α-phase Ti-7Al were continuously heated from room temperature to 850 °C while far-field HEDM scans were collected. The results showed a change in the ratio of the CTEs in the ‘a’ and ‘c’ directions which explains discrepancies found in the literature. The CTE additionally appears to be affected by the dissolution of α 2 precipitates. Analysis of the grain-resolved micromechanical data also shows reconfiguration of the grain scale stresses likely due to anisotropic expansion driving crystallographic slip.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Creep properties of advanced austenitic steel 709 determined through short experiments under in-situ neutron diffraction followed by TEM characterization

Here in this study, the creep mechanisms at play in Alloy 709 (Fe-20Cr-25Ni) are investigated by performing short-term creep-type tests under in-situ neutron diffraction experiments. Short tests are performed in the temperature range of 500 to 900 °C under constant load with a load ranging from 50 to 150 MPa. The creep exponent and activation energy are determined using the Bird-Mukherjee-Dorn relation and compared to that obtained from conventional longer creep tests from the literature. Scanning transmission electron microscopy (S/TEM) of the post-creep microstructure indicates that interaction of dislocations with precipitates are a dominant mechanism at play. Furthermore, local elemental mapping indicated chemical segregation at grain boundaries and formation of complex precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Local lattice distortion in NiCoCr, FeCoNiCr and FeCoNiCrMn concentrated alloys investigated by synchrotron X-ray diffraction

Severe lattice distortion is presumptively considered as a core effect of high-entropy alloys, but quantitative measurements are still missing. Here, we demonstrate that the lattice distortion in high-entropy alloys can be quantitatively analyzed based on pair distribution function obtained from synchrotron X-ray diffraction. By applying this method to equiatomic NiCoCr, FeCoNiCr and FeCoNiCrMn concentrated alloys, we found that the local lattice distortion in the NiCoCr (0.23%) and FeCoNiCrMn (0.24%) alloys are comparable while negligible in the FeCoNiCr alloy (0.04%). Furthermore, the origin of local lattice distortion in the NiCoCr and FeCoNiCrMn concentrated alloys was discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Coherent diffraction study of calcite crystallization during the hydration of tricalcium silicate

The aim of this work is using Bragg coherent X-ray diffraction imaging (BCDI) to study the calcite crystallization during carbonation of hydrated tricalcium silicate (C 3 S). Portland cement is a very complex synthesized product whose 50–70% mass is composed of C 3 S, which is the most important phase to produce calcium silicate hydrates and calcium hydroxide. Hence, its hydration contributes greatly to the hydration of cement and later to the carbonation of cement products when it reacts with CO 2 , often from the air, to form calcium carbonates. BCDI has emerged in the last decade as a promising high-resolution lens-less imaging approach for characterization of various samples. It has made significant progress with the development of X-ray sources and phase-retrieval algorithms. BCDI allows for imaging the whole three-dimensional structure of micro- and sub-micro- crystalline materials and can show the strain distribution at the nanometer spatial resolution. Finally, results show that calcite crystallization follows a through-solution reaction and the growth model of the calcite crystal can be explained by using “phase domain” theory. In conclusion, during carbonation, calcite crystals grow by increasing the number of phase domains within them while the domain size remains at about 200–300 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Helium-implantation-induced lattice strains and defects in tungsten probed by X-ray micro-diffraction

Tungsten is the main candidate material for plasma-facing armour components in future fusion reactors. Bombardment with energetic fusion neutrons causes collision cascade damage and defect formation. Interaction of defects with helium, produced by transmutation and injected from the plasma, modifies defect retention and behaviour. Here we investigate the residual lattice strains caused by different doses of helium-ion-implantation into tungsten and tungsten-rhenium alloys. Energy and depth-resolved synchrotron X-ray micro-diffraction uniquely permits the measurement of lattice strain with sub-micron 3D spatial resolution and ~10 -4 strain sensitivity. Increase of helium dose from 300 appm to 3000 appm increases volumetric strain by only ~2.4 times, indicating that defect retention per injected helium is ~3 times higher at low helium doses. This suggests defect retention is not a simple function of implanted helium dose, but strongly depends on material composition and presence of impurities. Conversely, analysis of W-1 wt% Re alloy samples and of different crystal orientations shows that both the presence of rhenium, and crystal orientation, have a comparatively small effect on defect retention. These insights are key for the design of armour components in future reactors where it will be essential to account for irradiation-induced dimensional change when predicting component lifetime and performance.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Residual stress distribution in an additively manufactured complex structure by neutron diffraction measurement

Residual stress in an aerodynamically shaped Ni-based superalloy airfoil fabricated by laser powder bed fusion was measured by neutron diffraction. The experiment was conducted by considering the complex shape, implementing computer aided experiment planning, and automatic alignment at each rapid measurement. The 3-dimensional (3D) residual stress distribution in the airfoil is presented in this work, which lacks symmetry due to the complex geometry of the airfoil. In conclusion, the results provide theoretical thermal processing models a complete residual stress dataset of simulation validation on 3D shape complex structure.

Residual stress↗