Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “diffraction pattern”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 523 records · Page 29
All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

Chaos and Beyond in a Water Filled Ultrasonic Resonance System

Finite amplitude ultrasonic wave resonances in a one-dimensional liquid-filled cavity, formed by a narrow band transducer and a plane reflector, are reported. The resonances are observed to include not only the expected harmonic and subharmonic signals (1,2) but chaotic signals as well. The generation mechanism requires attaining a threshold value of the driving amplitude that the liquid-filled cavity system becomes sufficiently nonlinear in response. The nonlinear features of the system were recently investigated via the construction of an ultrasonic interferometer having optical precision. The transducers were compressional, undamped quartz and lithium niobate crystals having the frequency range 1-10 MHz, driven by a high power amplifier. Both an optical diffraction system to characterize the diffraction pattern of laser light normally incident to the cavity and a receiving transducer attached to an aligned reflector with lapped flat and parallel surfaces were used to assess the generated resonance response in the cavity. At least 5 regions of excitation are identified.

Lazlo, Adler↗
NASA NTRS2020

Optical Characterization of Laser Retroreflector Arrays for Lunar Landers

Laser Retroreflector Array for Lunar Landers (LRALL) is a small optical instrument designed to provide a target for precision laser ranging from a spacecraft in lunar orbit, enabling geolocation of the lander and its instrument suite and establishing a fiducial maker on the lunar surface. Here we describe the optical performance of LRALL at visible and near-infrared wavelengths. Individual corner cube reflectors (CCRs) within LRALL were tested for surface flatness and dihedral angle values. We also imaged the far-field diffraction patterns of individual CCRs as well as the entire retroreflector array over the range of possible incident angles to extract the optical cross section as a function of viewing angle. We also measured the optical properties of one of the CCRs over the lunar temperature range (100 K to 380 K) and found no significant temperature-dependent variance. The test results show LRALL meets the design criteria and can be ranged to from elevation angles above 30° with respect to the instrument base from an orbital laser altimeter such as the Lunar Orbiter Laser Altimeter (LOLA) on the Lunar Reconnaissance Orbiter (LRO). This work summarizes the test data and serves as a guide for future laser ranging to these retroreflector arrays.

Daniel R Cremons↗
NASA NTRSDate not supplied

Alignment and Verification Testing of the GPS LRA Test Bed

The LRCTF (Laser Ranging Characterization and Test Facility) is a unique facility built at NASA GSFC to provide thermal-optical testing of the next generation GPS LRA (Global Positioning Satellite’s Laser Retroreflector Array) laser ranging target. The 400mm diameter target is an array consisting of 48 total internal reflection retroreflectors and has an optical cross section requirement of 100 MSM (million square meters). To verify that the array meets this requirement during on-orbit conditions, the LRCTF is equipped with a 400mm test beam, a data product output consisting of full aperture FFDPs (Far Field Diffraction Patterns) and a thermal chamber. The FFDPs are used to calculate the OCS. This paper will describe the facility design, alignment approach, and verification process.

Patricia Lyons↗
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↗
DOE OSTI2022

The Complexity and Challenges of Irradiation-Induced Phase Instability Phenomenon in Nuclear Power Plant Components

High energy irradiation by neutrons or ions of metastable austenitic 300-series steels appears to initiate formation of bcc-phases with different morphology and elemental composition compared to that of retained ferrite. Extensive formation of specific Fe-rich ferrite was observed on the grain boundaries of annealed Russian steel 12Cr18Ni10Ti, an analog of AISI 321, after irradiation in the center-core region of sodium-cooled BN-350 fast reactor (SFR) doses up to 57 dpa at ~1×10-6dpa/sec. The ferrite fraction determined from scanning electron microscopy (SEM) closely matched the magnetic fraction determined using a ferritscope confirmed by X-ray diffraction analysis and selected area diffraction patterns. Chemical composition of the secondary phases was determined by energy dispersive X-ray analysis using transmission electron microscope, showing Fe-rich ferrite domains. Fe-ion irradiation (2.3 MeV) was used to study the accumulation of ferrite and martensite phases at higher dpa rates. The very high etchability of these ferrite particles in alcohol-based solutions may signal a very high etching in hot water, leading to accelerated intergranular cracking, especially upon long-term exposure during extended plant lifetimes.

D a, Merezhko↗
DOE OSTI2023

Development of Large-Volume-Diamond Anvil Cell for Neutron Diffraction: The Neutron Diamond Anvil Cell Project at ORNL

10 years ago, Dave Mao, director of EFree (energy frontier research in extreme environments), a DOE energy frontier recognized the importance of neutron science for energy research. The subsequent establishment of a neutron group within EFree lead to the establishment of an “Instrument Development Team” for SNAP, the High-Pressure beamline at the Spallation Neutron Source at Oak Ridge National Laboratory in Tennessee. The idea was to develop novel high pressure techniques to expand the pressure range for neutron diffraction. A goal was set to reach half megabar levels (50 GPa), which at the time was considered as extremely challenging. Here we will give a brief overview of the developments during the last decade in this novel area of research. Fortunately, during this period multi carat diamond anvils have become available mainly by the chemical vapor deposition process (CVD), making research in this pressure range and beyond rather routine. This paper shows the latest developments in large anvil designs, compact multiple ton diamond cells and some examples of high-quality neutron diffraction patterns of sample sizes far below conventional levels.

Boehler, Reinhard↗
DOE OSTI2023

Super-resolution optical microscope

A super-resolution microscope avoids the need for complex phase plate optics normally used to produce a doughnut-shaped depletion beam by employing low-intensity regions of common diffraction patterns such as an Airy disk.

Kolkowitz, Shimon↗
DOE OSTI2025

Time at Temperature Abstract and Intern Poster

Current NRC regulations for BWR operations dictate that any occurrence reaching the point of Departure from Nucleate Boiling (DNB) disqualifies the use of the fuel rod for further reactor operation. That criteria does not account for duration of rate of the power increase, the corresponding effects on material properties or rewetting that may occur. Previous Anticipated Operational Occurrences (AOOs) show short durations power increase that may require limited amounts of heat removal. Industrial experience has shown evidence that fuel can reach dryout yet continue to safely operate in regular reactor conditions. The gap in research into such occurrences is the motivation for a series of experiments, including this current work. Time-at-Temperature experiments aim to identify and characterize the microstructural changes in Zircaloy-2 under oxygen-free high temperatures. This work uses the FlashDSC instrument to rapidly ramp up and down the temperature of a focus ion beam (FIB) prepared large area lift-out (LALO) of Zircaloy-2 at a rate of 10,000 K/s to desired values. The focus is to characterize the microstructure evolution, if any, of Zircaloy-2 that may impact its performance under typical BWR conditions. This characterization includes analyzing grain structure and size, secondary phase particle (SPPs) size, shape, composition, and location using Transmission Electron Microscopy (TEM). Further data collection and analysis is in progress including diffraction pattern indexing and 4D STEM processing. While current results focus on the testing and characterizing unirradiated material, future plans include expansion to irradiated material to explore the effects of rapid transition rates seen in DNB and dryout conditions on irradiationg damage and defect annealing.

36 - MATERIALS SCIENCE↗
DOE OSTI2026

Time at Temperature Experiments on Neutron Irradiated Zircaloy-2 using Conventional & Flash DSC

Dryout events in Boiling Water Reactors (BWRs) are currently treated by NRC regulations as automatic disqualification for continued fuel rod operation, even though this criterion does not account for the rate or duration of power increases, associated changes in material behavior, or the possibility of rewetting. Operational history from Anticipated Operational Occurrences (AOOs) shows that short, transient power excursions often demand only modest heat removal, and industry experience suggests that fuel can briefly enter dryout yet return to safe, stable operation. The lack of detailed understanding of the material response during such events motivates the present series of experiments. This study uses unique and innovative methods to investigate microstructural evolution in irradiated Zircaloy-2 exposed to high temperatures in inert environments. Differential Scanning Calorimetry (DSC) and FlashDSC are combined to build a comprehensive experimental framework capable of identifying the a–ß phase transformation in zirconium and examining defect annealing under steep thermal gradients. FlashDSC enables rapid heating and cooling of Focused Ion Beam (FIB)–prepared large-area lift-outs (LALOs) of irradiated Zircaloy-2 at rates of 1,000 K/s to peak temperatures of 600°C, 750°C, and 900°C. The goal is to determine whether these conditions produce measurable microstructural changes that could influence cladding performance in typical BWR environments. Microstructural characterization includes quantifying dislocation density and assessing secondary phase particle (SPP) size and distribution using Transmission Electron Microscopy (TEM). Ongoing analysis, such as diffraction pattern indexing and 4D STEM processing, will further refine these observations.

36 - MATERIALS SCIENCE↗
NASA NTRS1999

X-Ray Diffraction Techniques for a Field Instrument: Patterns of Lithologic Provences

Future exploration of Mars will attempt to shed light on the mineralogy of surface materials. Instruments deployed from remote platforms should have the capability to conduct both intensive analyses as well as rapid, reconnaissance surveys while they function in the martian environment as surrogate geologists. In order to accommodate the reconnaissance mode of analysis and to compensate for analytical limitations imposed by the space-flight conditions, data analysis methods are being developed that will permit interpretation of data by recognition of signatures or "fingerprints". Specifically, we are developing a technique which will allow interpretation of diffraction patterns by recognition of characteristic signatures of different lithologic provences. This technique allows a remote vehicle to function in a rapid-scan mode using the lithologic signature to determine where a more thorough analysis is needed. An x-ray diffraction pattern is characterized by the angular positions of diffracted x-rays, x-ray intensity levels and background radiation levels. These elements may be used to identify a generalized x-ray signature. Lithologic signatures are being developed in two ways. A signature is composed using the ideal powder diffraction indices from the mineral assembledge common to a specific lithologic provence. This is then confirmed using a laboratory diffraction pattern of a whole rock powder. Preliminary results comparing the diffraction signatures of the major mineral assembledges common to basalt, carbonate, and evaporite basin deposits indicate that lithologies are differentiable as a "fingerprint". Statistical analyses are being performed to establish the confidence levels of this technique.

Marshall, J.↗
DOE OSTI2022

Laser-induced patterning for a diffraction grating using the phase change material of Ge 2 Sb 2 Te 5 (GST) as a spatial light modulator in X-ray optics: a proof of concept

The proposed X-ray spatial light modulator (SLM) concept is based on the difference of X-ray scattering from amorphous and crystalline regions of phase change materials (PCMs) such as Ge 2 Sb 2 Te 5 (GST). In our X-ray SLM design, the “ on” and “ off” states correspond to a patterned and homogeneous state of a GST thin film, respectively. The patterned state is obtained by exposing the homogeneous film to laser pulses. In this paper, we present patterning results in GST thin films characterized by microwave impedance microscopy and X-ray small-angle scattering at the Stanford Synchrotron Radiation Lightsource.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Coexistence of vitreous and crystalline phases of H 2 O at ambient temperature

Formation of vitreous ice during rapid compression of water at room temperature is important for biology and the study of biological systems. Here, we show that Raman spectra of rapidly compressed water at greater than 1 GPa at room temperature exhibits the signature of high-density amorphous ice, whereas the X-ray diffraction (XRD) pattern is dominated by crystalline ice VI. To resolve this apparent contradiction, we used molecular dynamics simulations to calculate full vibrational spectra and diffraction patterns of mixtures of vitreous ice and ice VI, including embedded interfaces between the two phases. We show quantitatively that Raman spectra, which probe the local polarizability with respect to atomic displacements, are dominated by the vitreous phase, whereas a small amount of the crystalline component is readily apparent by XRD. The results of our combined experimental and theoretical studies have implications for detecting vitreous phases of water, survival of biological systems under extreme conditions, and biological imaging. The results provide additional insight into the stable and metastable phases of H 2 O as a function of pressure and temperature, as well as of other materials undergoing pressure-induced amorphization and other metastable transitions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

High‐speed 4‐dimensional scanning transmission electron microscopy using compressive sensing techniques

Abstract Here we show that compressive sensing allows 4‐dimensional (4‐D) STEM data to be obtained and accurately reconstructed with both high‐speed and reduced electron fluence. The methodology needed to achieve these results compared to conventional 4‐D approaches requires only that a random subset of probe locations is acquired from the typical regular scanning grid, which immediately generates both higher speed and the lower fluence experimentally. We also consider downsampling of the detector, showing that oversampling is inherent within convergent beam electron diffraction (CBED) patterns and that detector downsampling does not reduce precision but allows faster experimental data acquisition. Analysis of an experimental atomic resolution yttrium silicide dataset shows that it is possible to recover over 25 dB peak signal‐to‐noise ratio in the recovered phase using 0.3% of the total data. Lay abstract : Four‐dimensional scanning transmission electron microscopy (4‐D STEM) is a powerful technique for characterizing complex nanoscale structures. In this method, a convergent beam electron diffraction pattern (CBED) is acquired at each probe location during the scan of the sample. This means that a 2‐dimensional signal is acquired at each 2‐D probe location, equating to a 4‐D dataset. Despite the recent development of fast direct electron detectors, some capable of 100kHz frame rates, the limiting factor for 4‐D STEM is acquisition times in the majority of cases, where cameras will typically operate on the order of 2kHz. This means that a raster scan containing 256^2 probe locations can take on the order of 30s, approximately 100‐1000 times longer than a conventional STEM imaging technique using monolithic radial detectors. As a result, 4‐D STEM acquisitions can be subject to adverse effects such as drift, beam damage, and sample contamination. Recent advances in computational imaging techniques for STEM have allowed for faster acquisition speeds by way of acquiring only a random subset of probe locations from the field of view. By doing this, the acquisition time is significantly reduced, in some cases by a factor of 10‐100 times. The acquired data is then processed to fill‐in or inpaint the missing data, taking advantage of the inherently low‐complex signals which can be linearly combined to recover the information. In this work, similar methods are demonstrated for the acquisition of 4‐D STEM data, where only a random subset of CBED patterns are acquired over the raster scan. We simulate the compressive sensing acquisition method for 4‐D STEM and present our findings for a variety of analysis techniques such as ptychography and differential phase contrast. Our results show that acquisition times can be significantly reduced on the order of 100‐300 times, therefore improving existing frame rates, as well as further reducing the electron fluence beyond just using a faster camera.

Robinson, Alex W.↗
DOE OSTI2022

Psilocybin: crystal structure solutions enable phase analysis of prior art and recently patented examples

Psilocybin {systematic name: 3-[2-(dimethylamino)ethyl]-1 H -indol-4-yl dihydrogen phosphate} is a zwitterionic tryptamine natural product found in numerous species of fungi known for their psychoactive properties. Following its structural elucidation and chemical synthesis in 1959, purified synthetic psilocybin has been evaluated in clinical trials and has shown promise in the treatment of various mental health disorders. In a recent process-scale crystallization investigation, three crystalline forms of psilocybin were repeatedly observed: Hydrate A, Polymorph A, and Polymorph B. The crystal structure for Hydrate A was solved previously by single-crystal X-ray diffraction. This article presents new crystal structure solutions for the two anhydrates, Polymorphs A and B, based on Rietveld refinement using laboratory and synchrotron X-ray diffraction data, and density functional theory (DFT) calculations. Utilizing the three solved structures, an investigation was conducted via Rietveld method (RM) based quantitative phase analysis (QPA) to estimate the contribution of the three different forms in powder X-ray diffraction (PXRD) patterns provided by different sources of bulk psilocybin produced between 1963 and 2021. Over the last 57 years, each of these samples quantitatively reflect one or more of the hydrate and anhydrate polymorphs. In addition to quantitatively evaluating the composition of each sample, this article evaluates correlations between the crystal forms present, corresponding process methods, sample age, and storage conditions. Furthermore, revision is recommended on characterizations in recently granted patents that include descriptions of crystalline psilocybin inappropriately reported as a single-phase `isostructural variant.' Rietveld refinement demonstrated that the claimed material was composed of approximately 81% Polymorph A and 19% Polymorph B, both of which have been identified in historical samples. In this article, we show conclusively that all published data can be explained in terms of three well-defined forms of psilocybin and that no additional forms are needed to explain the diffraction patterns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗