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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 955 records · Page 53
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

The formation and evolution of Ni 2 Cr precipitates in Ni–Cr model alloys as a function of stoichiometry characterized by synchrotron x-ray diffraction

Ni-based alloys containing significant amounts of Cr, may precipitate new phases during long-term service at elevated temperatures. In Ni–Cr model alloys, the formation of Ni 2 Cr has been found to impact the material properties, including the strength and ductility after isothermal aging below the critical temperature of 590°C. In this work, we quantify the formation and evolution of long-range ordering in four Ni–Cr binary model alloys (Ni/Cr = 1.8, 2.0, 2.2, 2.4) after isothermal aging up to 10,000h at temperatures between 373 and 475°C. The alloys were characterized by hardness testing and synchrotron-based x-ray diffraction to quantify the impact of Ni 2 Cr phase fraction and precipitate size on mechanical properties. After 500h of isothermal aging, the formation of Ni 2 Cr was detected in all four alloys at 475°C. In the stochiometric alloy samples (Ni/Cr = 2.0), the formation of Ni 2 Cr was found after 500 and 3000h aging at 418 and 373°C, respectively. We found that the matrix lattice contraction and Ni 2 Cr phase fraction both saturate after early aging times. This is in stark contrast to the hardness and Ni 2 Cr precipitate size that both continue to increase with increasing aging time. Our results highlight that changes in hardness correlate linearly with Ni 2 Cr precipitate size rather than phase fraction. This important structure-property relationship can potentially help define Ni–Cr-based component lifetimes directly through an understanding of how Ni 2 Cr formation impacts strength and ductility. Here, we find that a precipitation hardening model for critical resolved shear stress with weakly coupled dislocations shows good agreement with the material property changes quantified from experimental measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Effects of elevated temperature exposure on the residual stress state and microstructure of PVD Cr coatings on SiC investigated via in situ X-ray diffraction and transmission electron microscopy

Pure Cr coatings are being considered as corrosion-resistant layers for SiC-SiC f composite fuel cladding in light water reactors. The residual stress state and interdiffusion behavior of Cr coatings deposited on SiC substrates using bipolar high-power impulse magnetron sputtering (B-HiPIMS) and direct current impulse magnetron sputtering (DCMS) were studied using in situ X-ray diffraction experiments at 300 °C, 700 °C, and 1200 °C. After elevated temperature exposure, evolution of the coating microstructure and coating/substrate interdiffusion was characterized by transmission electron microscopy. The compressive residual stress of the dense B-HiPIMS coating at room temperature was gradually relieved at 300 °C, while the stress transitioned to a tensile state at 700 °C. Grain growth of the Cr coating and a Cr–SiC interdiffusion layer consisting of newly formed Cr–C and Cr–Si phases were observed in the B-HiPIMS coating after exposure at 700 °C. The phases in the interdiffusion layer were identified to be Cr 7 C 3 , Cr 3 Si, and Cr 5 Si 3 C x experimentally and by thermodynamic predictions. For the DCMS coating, however, changes in residual stress and microstructure at the elevated temperatures were limited by the inherent porosity and inhomogeneous structure of the as-deposited coating. At 1200 °C, both coating types interacted rapidly with the underlying SiC substrate in the early stages of the experiment. The results from this study suggest that the characteristics of the Cr coatings do not significantly change at the reactor operating temperature of 300 °C, while changes in microstructure and stress state are expected in off-normal conditions of 700 °C and 1200 °C. Finally the results from this study suggest the B-HiPIMS coating is best-suited as a protective coating for SiC fuel cladding.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Understanding the asymmetric orientations and stress states in polycrystalline NiTi SMA by in-situ synchrotron-based high-energy X-ray diffraction

The stress-induced martensite transformations (SIMTs) dramatically affect the recoverable strain and mechanical response of polycrystalline NiTi. An in-depth understanding of the propagation manner and orientation preference of SIMTs is therefore crucial. Here, in this work, we present a unique asymmetric anisotropy of SIMTs and lattice strains induced by Lüders-type deformation in polycrystalline NiTi, achieved through a combination of in-situ synchrotron X-ray diffraction and uniaxial tensile loading and unloading experiments. Our experimental findings reveal that in polycrystalline NiTi under uniaxial deformation, the asymmetry of SIMTs is attributed to the inhomogeneous strain field caused by the Lüders-type mechanism. The asymmetrical SIMT starts with the forward Lüder band and disappears along with the backward Lüder band. The austenite with the favored orientation of $\langle$110$\rangle$ A //loading direction (LD) transformed and recovered back at a higher rate compared to other orientations during both loading and unloading.

36 MATERIALS SCIENCE↗
DOE OSTI2019

High temperature neutron diffraction investigation of U 3 Si 2

The U-Si system is actively undergoing studies due to its promise as a component of an accident tolerant nuclear fuel. In this work, the crystal structure of the U 3 Si 2 compound in the U-Si system was investigated as a function of temperature from room temperature to 1298 K for a sample of approximately 42.02 at.% Si composition and 1373 K for a sample with approximately 42.10 at.% Si using high temperature time-of-flight neutron diffraction on the High-Pressure Preferred Orientation (HIPPO) diffractometer at Los Alamos Neutron Science Center (LANSCE). The simultaneous Rietveld refinement of five histograms from the five HIPPO detector backs (40°, 60°, 90°, 120°, and 145°) provided datasets for the lattice parameters, anisotropic atomic displacement parameters, and atomic positions as a function of temperature. To explore the possibility of a homogeneity range, two sample compositions were analyzed, a 40.02 at.% Si (near stoichiometric) and a potentially hyperstoichiometric (40.10 at.% Si) sample. While minor differences in the anisotropic atomic displacement parameters between the two samples were observed, over the entire investigated temperature range no additional phases were found indicative of a single phase sample and the ability of the U 3 Si 2 compound to accommodate nonstoichiometry, suggesting that the U 3 Si 2 compound is not a line compound confirming previous determinations. However, the differences observed in the average coefficient of linear thermal expansion identified between the two compositions warrant future investigation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Understanding the interaction of extension twinning and basal-plate precipitates in Mg-9Al using precession electron diffraction

Precession electron diffraction is used to characterize the interaction between ${10\bar{1}2}$ tensile twins and basal plate-like precipitates in a post-deformed, precipitate-dispersed Mg-9Al micropillar. We observed a heterogeneous distribution of precipitates in the micropillar sample, which enabled the study of the different stages involved in twin precipitate interactions. We show that twin nucleation was promoted, taking place on the surface, as well as from the interior of the micropillar. Twin tip propagation and twin growth were hindered by the precipitates. Twin tips either were arrested by precipitates and new twins formed on the other side of the precipitate, or continued to grow around the precipitate without the re-nucleation events. During twin thickening, the precipitates did not significantly alter the shear-dominant twin boundary migration mechanism, as evidenced by the relatively flat twin boundaries around the partially embedded precipitates. However, the twin boundary migration was retarded by the precipitates, especially in regions confined by closely-spaced precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Detector requirements and simulation results for the EIC exclusive, diffractive and tagging physics program using the ECCE detector concept

This article presents a collection of simulation studies using the ECCE detector concept in the context of the EIC’s exclusive, diffractive, and tagging physics program, which aims to further explore the rich quark–gluon structure of nucleons and nuclei. To successfully execute the program, ECCE proposed to utilize the detector system close to the beamline to ensure exclusivity and tag ion beam/fragments for a particular reaction of interest. Preliminary studies confirm the proposed technology and design satisfy the requirements. Further, the projected physics impact results are based on the projected detector performance from the simulation at 10 or 100 fb -1 of integrated luminosity. Additionally, insights related to a potential second EIC detector are documented, which could serve as a guidepost for future development.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

The diffractive contribution to deep inelastic lepton-proton scattering: Implications for QCD momentum sum rules and parton distributions

The cross section for deep inelastic lepton-proton scattering (DIS) ℓp→ℓ'p'X includes a diffractive deep inelastic (DDIS) contribution ℓp→ℓ'p'X, in which the proton remains intact with a large longitudinal momentum fraction x F greater than 0.9 and small transverse momentum. The DDIS events, which can be identified with Pomeron exchange in the t-channel, account for approximately 10% of all of the DIS events. Thus, when one measures DIS, one automatically includes the leading-twist Bjorken-scaling DDIS events as a contribution to the DIS cross section, whether or not the final-state proton p' is detected. In such events, the missing momentum fraction x p ' ~0.9 carried by the final-state proton p' in the DDIS events could be misidentified with the light-front momentum fraction carried by sea quarks or gluons in the protons' Fock structure. As we shall show in this article, the underlying QCD Pomeron-exchange amplitude which produces the DDIS events does not obey the operator product expansion nor satisfy momentum sum rules. Thus we conclude that the quark and gluon distributions measured in DIS experiments will be misidentified, unless the measurements explicitly exclude the DDIS events and that a correct determination of the parton distribution functions (PDFs) derived from the DIS data requires the explicit subtraction of the DDIS contribution from the full DIS cross section.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Measuring Ti-7Al slip system strengths at elevated temperature using high-energy X-ray diffraction

Full stress tensors of over four hundred individual grains in a titanium alloy specimen (Ti-7Al) are tracked during continuous uniaxial deformation through the elasto-plastic transition at 355°C. The experiment is facilitated by a unique radiative heating furnace and load frame designed for in-situ high-energy X-ray diffraction measurements. Average strengths of multiple slip system families are calculated directly from the ensemble grain stress data. Overall, results show that elevated temperature lowers the strength of basal slip systems relative to prismatic slip systems, reduces the degree of flow softening due to precipitate shearing, and decreases the first-order pyramidal slip system work-hardening rate.

36 MATERIALS SCIENCE↗
DOE OSTI2017

In situ nanobeam electron diffraction strain mapping of planar slip in stainless steel

Nanobeam electron diffraction strain mapping has been used to measure the strain evolution in stainless steel under in situ deformation. As the amount of deformation increases, the leading dislocation of a planar slip band leaves behind a residual strain in the form of a small lattice expansion. Dislocation analysis confirmed that the dislocations involved were <011> type. Even though, the characteristic residual strain of planar slip has often been observed, it has never before been directly measured. Our conclusions provide a view into the dynamic mechanisms of planar slip, and showcase the possibilities of multidimensional in situ imaging.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The effect of helium implantation on the deformation behaviour of tungsten: X-ray micro-diffraction and nanoindentation

Here, the effect of helium-implantation-induced defects on deformation behaviour is examined by comparing spherical nano-indents in unimplanted and helium-implanted regions of a tungsten single crystal. Helium-implantation increases hardness and causes large pileups. 3D-resolved X-ray micro-diffraction uniquely allows examination of the complex lattice distortions beneath specific indents. In the ion-implanted material we find reduced lattice rotations and residual strains due to indentation, indicating a more confined plastic zone. Together, our observations suggest that helium-induced defects initially act as efficient obstacles to dislocation motion, but are weakened by the subsequent passage of dislocations, causing a reduction in work hardening capacity.

36 MATERIALS SCIENCE↗
DOE OSTI2018

In-situ synchrotron X-ray diffraction study of dual-step strain variation in laser shock peened metallic glasses

Atomic-structure evolution is significant in understanding the deformation mechanism of metallic glasses. Here, we firstly find a dual-step atomic strain variation in laser-shock-peened (LSPed) metallic glasses during compression tests by using in-situ synchrotron X-ray diffraction. Under low compressive load, LSP-deformed zone’s atomic-structure shows low Young’s Modulus (E); with load increase, atomic-structure are re-hardened, showing high E. An atomic deformation mechanism is proposed by using flow unit model, that LSP could induce interconnected flow units and 2 homogenize the atomic-structure. Furthermore, these interconnected flow units are metastable and start to annihilate during compressive loading, causing the dual-step atomic strain variation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

An in situ neutron diffraction study of plastic deformation in a Cu 46.5 Zr 46.5 Al 7 bulk metallic glass composite

Micro-mechanical behaviors of a Cu 46.5 Zr 46.5 Al 7 bulk metallic glass composite in the plastic regime were investigated by continuous in situ neutron diffraction during compression. Three stages of the plastic deformation were observed according to the work-hardening rate. Here, the underlying natures of the work hardening, correlating with the lattice/microscopic strain evolution, are revealed for the three stages: (1) the initiation of shear bands, (2) the phase load transferring from the amorphous phase to the B2 phase and (3) the accelerated martensitic transformation and the work hardening of the polycrystalline phases promoted by the rapid propagation of the shear bands.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Signatures of the unique microstructure of additively manufactured steel observed via diffraction

A series of measurements were designed to gain confidence in the interpretation of the peak breadth in diffraction patterns collected from additively manufactured material, which has a novel microstructure in comparison to the well understood microstructure of wrought materials. Stainless steels made with two additive manufacturing techniques were compared to wrought material. Similar patterns observed in the scattering vector dependence for additively manufactured and deformed wrought materials suggested that the broadening in both materials was related to dislocations. Finally, this was confirmed by heat-treatment, during which both materials exhibited recovery due to the annealing of dislocations at the same temperature.

304L stainless-steel↗
DOE OSTI2018

Anisotropic lattice expansion determined during flash sintering of BiFeO 3 by in-situ energy-dispersive X-ray diffraction

BiFeO 3 has a Curie temperature (T C ) of 825 °C, making it difficult to sinter with conventional methods while maintaining the purity of the material, as unavoidably secondary phases appear at temperatures above T c . Flash sintering is a relatively new technique that saves time and energy compared to other sintering methods. BiFeO 3 was flash sintered at 500 °C to achieve 90% densification. In-situ energy dispersive X-ray diffraction (EDXRD) reflected that the material did not undergo any phase transformation, having been sintered well below the T C . Interestingly, anisotropic lattice expansion in the materialwas observed when the sample was exposed to the electric field.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Stresses within rare-earth doped yttria-stabilized zirconia thermal barrier coatings from in-situ synchrotron X-ray diffraction at high temperatures

There is a growing interest for smart coatings that can be integrated into turbine engines for in-situ temperature measurements or health monitoring. The addition of rare-earth dopants into standard thermal barrier ceramic top coat materials is used to obtain luminescent coatings that enable spectral measurements, for real-time temperature or health monitoring. The thermomechanical performance and durability of such novel coating compositions in extreme environments still remains to be evaluated. Consequently, the ability to manufacture sensor coatings which present suitable thermal properties needs to be demonstrated. For this study, highly luminescent erbium and europium doped yttria-stabilized zirconia and state-of-the-art yttria-stabilized zirconia coatings manufactured by air plasma spray were characterized to determine the effects of the embedded rareearth dopants on coating internal strain and stress and to quantify and compare their high temperature response using synchrotron X-ray diffraction. In-situ depth-resolved strain measurements were performed at 15 μm intervals along the depth of the coatings to evaluate materials response at key locations, specifically at layer interfaces. In-plane stress was calculated for the coatings and a finite element model was implemented to supplement the results and enable further predictions. The results show that the sensor coatings that were manufactured in this work revealed only minor variations in the strain response of sensor coatings under a typical thermal cycle and especially at temperatures closer to that of gas turbine operating conditions, compared to state-of-the-art coatings. This work demonstrates the viability of manufacturing rare-earth doped yttria-stabilized zirconia coatings that provide beneficial spectroscopic monitoring capabilities while having minimal impact on the thermomechanical response of the thermal barrier coatings.

Air plasma spray↗
DOE OSTI2017

Aberration corrected STEM by means of diffraction gratings

In the past 15 years, the advent of aberration correction technology in electron microscopy has enabled materials analysis on the atomic scale. This is made possible by precise arrangements of multipole electrodes and magnetic solenoids to compensate the aberrations inherent to any focusing element of an electron microscope. In this paper, we describe an alternative method to correct for the spherical aberration of the objective lens in scanning transmission electron microscopy (STEM) using a passive, nanofabricated diffractive optical element. This holographic device is installed in the probe forming aperture of a conventional electron microscope and can be designed to remove arbitrarily complex aberrations from the electron's wave front. In this work, we show a proof-of-principle experiment that demonstrates successful correction of the spherical aberration in STEM by means of such a grating corrector (GCOR). Our GCOR enables us to record aberration-corrected high-resolution high-angle annular dark field (HAADF-) STEM images, although yet without advancement in probe current and resolution. Finally, improvements in this technology could provide an economical solution for aberration-corrected high-resolution STEM in certain use scenarios.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

Towards bend-contour-free dislocation imaging via diffraction contrast STEM

Dislocation imaging using transmission electron microscopy (TEM) has been an invaluable tool for characterizing crystallographic defects in metals. Compared to conventional TEM imaging, diffraction contrast imaging scanning transmission electron microscopy (DCI STEM) with appropriate setting can provide better defect contrast with almost negligible bend contour artifacts, enabling more effective analysis of dislocation structures. Here, we investigated why STEM can suppresses bend contour, and how dislocation contrast behaves along with different STEM imaging parameters. Using a body-centered cubic HT-9 ferritic/martensitic alloy as an example, a simple procedure and operational theory are described at the beginning to help set up DCI STEM experiments. Comparing with conventional TEM and the STEM strictly complying with the principle of reciprocity, we found that a pair of STEM convergence and collection semi-angles, α S and β S , a few milliradians in size is essential for bend-contour-free defect imaging. It works in concert such that the convergence STEM probe opens up the reciprocal space, and then a comparable collection region evens out the rocking-curve oscillation and alleviates bend contours from the reciprocal space. This fundamental advantage is unique in DCI STEM. Practical guidelines regarding STEM parameters and specimen orientation and thickness are then provided for DCI STEM dislocation imaging. Lastly, we show that coupling DCI STEM with spectrum images of electron energy loss spectroscopy and of energy-dispersive X-ray Spectroscopy offers a comprehensive characterization of crystallographic defects and chemical information of complex microstructures.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Atomic resolution convergent beam electron diffraction analysis using convolutional neural networks

Two types of convolutional neural network (CNN) models, a discrete classification network and a continuous regression network, were trained to determine local sample thickness from convergent beam diffraction (CBED) patterns of SrTiO 3 collected in a scanning transmission electron microscope (STEM) at atomic column resolution. Acquisition of atomic resolution CBED patterns for this purpose requires careful balancing of CBED feature size in pixels, acquisition speed, and detector dynamic range. The training datasets were derived from multislice simulations, which must be convolved with incoherent source broadening. Sample thicknesses were also determined using quantitative high-angle annular dark-field (HAADF) STEM images acquired simultaneously. The regression CNN performed well on sample thinner than 35 nm, with 70% of the CNN results within 1 nm of HAADF thickness, and 1.0 nm overall root mean square error between the two measurements. The classification CNN was trained for a thicknesses up to 100 nm and yielded 66% of CNN results within one classification increment of 2 nm of HAADF thickness. Our approach depends on methods from computer vision including transfer learning and image augmentation.

36 MATERIALS SCIENCE↗