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DOE OSTI2022

The complex structural and chemical nature of monolithic U-10Mo fuel and Zr barrier layer

Nanoscale microstructural characterization by advanced transmission electron microscopy techniques on a U-10Mo/Zr barrier layer monolithic fuel plate was performed to evaluate the microstructural evaluation after high burn-up. Gas bubble superlattice evolution, grain restructuring, and evolution of the Zr interaction layer is investigated through detailed electron microscopy characterization. The use of automated crystallographic orientation mapping to irradiated U-10Mo fuel highlights that the restructured ultra-fine grains are separated by high angle grain boundaries at a burn up of 4.42 × 10 21 fissions/cm 3 . Additionally, advanced chemical analysis and multi-variable statistical analysis shows spatial clustering of solid fission product precipitates. Finally, characterization of a newly observed porous nanocrystalline Zr region in the barrier layer is studied. Finally, this work provides insights into the grain subdivision and restructuring process while using advanced microscopy techniques to analyze fission products in neutron-irradiated U-10Mo fuel.

36 MATERIALS SCIENCE↗

NASA NTRS1981

Electron-temperature dependence of dissociative recombination of electrons with N2/+/.N2 dimer ions

The variation with electron temperature of the dissociative recombination of electrons with N2(+).N2 dimer ions is investigated in light of the importance of such ions in the lower ionosphere and in laser plasmas. Dissociative recombination coefficients were determined by means of a microwave afterglow mass spectrometer technique for electron temperatures from 300-5600 K and an ion and neutral temperature of 300 K. The recombination coefficient is found to be proportional to the -0.41 power of the electron temperature in this range, similar to that observed for the CO(+).CO dimer ion and consistent with the expected energy dependence for a fast dissociative process.

Whitaker, M.↗

NASA NTRS1994

Three-dimensional reconstruction of coronal mass ejections

Computer assisted tomography (CAT) techniques are used to reconstruct the three dimensional shape of coronal mass ejections in the interplanetary medium. Both the Helios 2 spacecraft zodiacal-light photometers and the Solwind coronograph measure changes in Thomson scattering of sunlight from electrons. The technique from near-perpendicular Solwind and Helios views are applied to determine the density of a mass ejection which left the solar surface on 24 May 1979. The coronograph and the Helios perspective views are not simultaneous; the Solwind observations extend outward to sky plane distances of only 10 of the solar radius, whereas the Helios 16 photometer observes to as close as 17 of the solar radius from the sun. The solution is obtained by assuming outward radial expansion and that the coronal mass ejections (CME's) have the same speed everywhere at the same height. The analyses show that CME's are extensive three dimensional structures (the CME of 24 May appears approximately shell) like in three dimensions.

Jackson, Bernard V.↗

NASA NTRS2026

Polarized Resonant Soft X-ray Scattering (P-RSoXS) as a New Technique for Characterizing Amorphous Astromaterials

In the coming years, samples will be returned from several asteroids, the lunar surface, and the first material returned directly from the Martian surface. Previous in-situ and remote studies indicate these samples will contain abundant amorphous or weakly crystalline materials. However, detailed characterization and quantification of these amorphous materials remains challenging. Conventional techniques, including electron microscopy and X-ray diffraction, provide important information on material structure, but are generally limited to crystalline materials. Polarized resonant soft X-ray scattering (P-RSoXS) is a synchrotron-based X-ray scattering technique that has been used to characterize and quantify weakly crystalline systems, including soft materials. This research aims to translate this technique to geologic and extraterrestrial materials, building off the knowledge of using P-RSoXS to interrogate soft materials. P-RSoXS is well-suited to interrogate geologic materials, which are often multiphase, heterogeneous systems with crystalline and amorphous components, and domain sizes on the order of tens of nanometers. It is anticipated that future work will help reveal new chemical and structural information in geologic materials. Maturation of this preliminary work to develop P-RSoXS to characterize astromaterial-relevant samples will provide new understanding of the secondary processes responsible for the development of amorphous astromaterials and further elucidate our knowledge of the geologic history and past alteration processes.

Joshua H Litofsky↗

DOE OSTI2025

Stimulating β -Series Precipitation in Mg–Nd Alloys Via Microalloying: A Comparison of Electron Microscopy and Small-Angle Scattering Techniques

The Mg–Nd alloy system is of particular interest in the development of high-strength, lightweight structural alloys due to the formation of strengthening metastable Mg–Nd β-series precipitates during heat treatment. The strengthening is primarily provided by a combination of the β''' and β 1 precipitation. It is therefore important to understand how the precipitation behavior can be enhanced by other common alloying elements. In this work, the effects of 0.2 wt pct Zn and Ca on β-series precipitation were studied. Small-angle/ultra-small-angle X-ray scattering (SAXS/USAXS) techniques in combination with scanning transmission electron microscopy (STEM) were used to study the evolution of precipitation microstructure. Here, it is found that the Zn additions refine the precipitates, leading to an increase in hardness with aging at 200 °C. On the other hand, the Ca additions result in an acceleration in the formation of larger β 1 precipitates and chains which provides less strengthening. The β 1 chains are surrounded by precipitate-free zones (PFZs) that further contribute to the decreases in hardness observed in the over-aged condition. This paper demonstrated that SAXS/USAXS provides a powerful tool for an in situ study of the early stages of precipitation in the Mg–Nd-based alloys.

36 MATERIALS SCIENCE↗

NASA NTRS1974

Vibrational relaxation in expanding N2 and air

New N2 vibrational temperature data, obtained in expanding N2 and air using the electron beam technique, are analyzed permitting the vibrational relaxation times to be determined as a function of temperature. In addition, the effects on N2 vibrational relaxation times of direct vibrational energy transfer between N2 and H2O, between N2 and O2, and between N2 and free electrons introduced from arc contaminants are analyzed. The vibrational relaxation times determined from the present measurements agree with those measured in the expanding flows of shock tunnels and impact tubes. These expanding data also agree with relaxation times observed in acoustical resonant cavities where alternating compressions and expansions take place. The relaxation times in expanding flows (vib-tran exchange process) are found to be approximately 50 times faster than those measured in the compressing flow of shock tubes (tran-vib exchange process). This evidence strongly supports the concept that one relaxation time distribution cannot be applied to both exchange processes.

Sebacher, D. I.↗

NASA NTRS1979

Experimental Investigation of Launch Vehicle Transient Input Simulation in Payload Tests

The technique of electronically simulating the structural dynamics of a launch vehicle in transient tests of payloads using multiple vibration excitation systems was investigated. The development of computer programs to determine transfer functions, synthesize shaker forcing functions, and control vibration exciters is described. A demonstration test using the techniques was described and results are presented. The evaluation of the potential for applying this technique to large Shuttle payloads is discussed.

Rader, P.↗

DOE OSTI2022

Tunable plasmon-enhanced second-order optical nonlinearity in transition-metal dichalcogenide nanotriangles (Final Report for SC0008712)

The control of light-matter interaction at the nanoscale is a grand challenge that cuts across modern photonics, plasmonics, and optoelectronics. The development of simulation tools for predictive modeling of nanostructured light emitters and absorbers is critical to successfully tackling this grand challenge. Existing state-of-the-art tools are not suitable for the following reasons: a) Phenomenological models of materials, commonly employed in the full-wave solutions to Maxwell’s equations, are fit to experimental data for bulk materials and fall short when attempting to analyze nanostructures. b) Nonlinearities in optical response can arise solely from nanostructuring, and require time-dependent quantum electronic transport techniques to capture. c) Emergent materials with exotic and tunable physical properties are increasingly used, but their properties are very sensitive to the substrate, impurities, and edge termination, and require an accurate description of interband and intraband processes, as well as dissipation. d) Microscopic modeling of electronic transport usually employs simplified electrodynamics, and realistic models that couple full electronic transport with full-wave electrodynamics are needed for accurate photonics simulations. The objective of this project was to computational tools that will overcome the limitations faced by current modeling tools and provide an unprecedented level of accuracy for predictive modeling of light-matter interaction at the nanoscale.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Environmentally Assisted Cracking Research for Current and Advanced Nuclear Structural Materials

Understanding environmentally assisted cracking is an important aspect of nuclear materials research, as it provides information about failure mechanisms that lead to safety concerns or shutdowns. Idaho National Laboratory has ongoing research to understand how materials behave in the harsh nuclear environments for both the current fleet of light water reactors, as well as advanced reactors, where materials are exposed to more extreme environments. Corrosion and cracking of current materials, advanced materials, and materials formed through advanced manufacturing techniques are being examined, with particular interest in irradiation effects on corrosion and cracking, as well as the effects of environmental impurities. Testing, such as stress corrosion cracking, corrosion fatigue, and in-situ crack growth measurements, as well as a suite of characterization tools, including electron microscopy techniques and x-ray computed tomography, are being utilized to better understand the material response, limitations, and cracking mechanisms to ensure safe and reliable nuclear plants.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Laser-driven ultrafast transmission electron microscopy

Recent advances in lasers and electron optics technology have allowed transmission electron microscopes to achieve high spatial and temporal resolution, making them capable of tracking atoms, charges and spin motions down to the attosecond and nanometre scales. This Primer discusses the most common and practical experimental implementation of time-resolved transmission electron microscopy and the stroboscopic mode for evaluating ultrafast reversible dynamics. An in-depth discussion of photo-induced near-field electron microscopy, a technique unique to laser-assisted electron microscopy, is also provided, covering its prospective applications in the study of coherent phenomena in quantum materials. The experimental strategies and limitations in investigating the structural dynamics of materials and nanostructures by imaging, diffraction and spectroscopy are also described in detail, with a direct comparison with more conventional and established techniques. Here, we provide key information for new researchers who intend to use ultrafast transmission electron microscopy to address new challenges in specific materials science, condensed matter and nanophotonics.

Transmission electron microscopy↗

DOE OSTI2020

Synthesis of Macroscopic Single Crystals of Ge 2 Sb 2 Te 5 via Single-Shot Femtosecond Optical Excitation

Using in situ electron diffraction techniques, we demonstrate that femtosecond optical excitation above a threshold fluence of the amorphous, as-deposited, phase change material Ge 2 Sb 2 Te 5 creates large, 100 μm scale single crystals. This is 2 orders of magnitude larger than previously reported grains synthesized via photoexcitation. Transmission electron microscopy shows that these large crystals are dewetted regions with a face-centered cubic structure. Energy-dispersive X-ray spectroscopy indicates that the crystals have the same composition as the initial amorphous phase. In this work, we present a theoretical model which shows that this arises from a crossover from a nucleation-dominated crystallization regime to a growth-dominated crystallization regime, and we show that the measured grain size is consistent with Johnson–Mehl–Avrami–Kolmogorov (JMAK) crystallization theory for temperatures near the melting temperature. The ability to grow macroscopic single crystals from an amorphous material, and on arbitrary amorphous substrates, opens up a large area of potential applications, as well as new opportunities for tuning the nucleation, growth, and switching characteristics of phase-change materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Effect of Electronic Shot Noise on Dynamic Measurements using Optical Techniques: Examples from Rayleigh Scattering and Unsteady PSP

Electronic shot noise is an unavoidable reality in all optical techniques that depend on measuring light intensity. For steady-state, time-averaged measurements the impact of shot noise can be easily reduced by increasing the exposure time, or by averaging over multiple-exposures. That is not the case for unsteady measurements, where time histories of light intensity variations need to be created either by high-speed photography (unsteady PSP) or via photoelectron counting (spectrally resolved Rayleigh scattering) over short time durations using a photo-multiplier tube (PMT) and photon counting electronics. Electronic shot noise introduces a fixed amount of random error, which can overwhelm the light intensity variation caused by turbulent fluctuations. Spectrum computed from such time series shows a fixed noise floor that is independent of the number of data points in the time series. For a fixed optical system, where the collected power of the luminescent light (uPSP), or the scattered light (Rayleigh) is fixed, one needs to resort to special techniques to obtain enough signal-to noise ratio (SNR). For the uPSP application it is shown that averaging of the adjacent pixels improves SNR; although this may lead to a sacrifice of spatial resolution. A second means is to increase the exposure time, which leads to a lowering of the frequency range. For the Rayleigh application, improvements of SNR can be achieved via two different cross-correlation based approaches. The first involves measuring the light intensity using two PMTs using short, contiguous gates; thereby, creating two time-series of data. The second one involves collecting one long time-series of data using one set of measurement device, followed by an odd-even splitting into two time series. When the two time-series are cross-correlated, and a power spectrum is calculated, a significant reduction in the shot noise floor can be achieved. Examples from measurements of density and velocity fluctuations spectra from two different Rayleigh setup are presented to demonstrate the process.

uPSP↗

NASA NTRS2011

Space Shuttle GN and C Development History and Evolution

Completion of the final Space Shuttle flight marks the end of a significant era in Human Spaceflight. Developed in the 1970 s, first launched in 1981, the Space Shuttle embodies many significant engineering achievements. One of these is the development and operation of the first extensive fly-by-wire human space transportation Guidance, Navigation and Control (GN&C) System. Development of the Space Shuttle GN&C represented first time inclusions of modern techniques for electronics, software, algorithms, systems and management in a complex system. Numerous technical design trades and lessons learned continue to drive current vehicle development. For example, the Space Shuttle GN&C system incorporated redundant systems, complex algorithms and flight software rigorously verified through integrated vehicle simulations and avionics integration testing techniques. Over the past thirty years, the Shuttle GN&C continued to go through a series of upgrades to improve safety, performance and to enable the complex flight operations required for assembly of the international space station. Upgrades to the GN&C ranged from the addition of nose wheel steering to modifications that extend capabilities to control of the large flexible configurations while being docked to the Space Station. This paper provides a history of the development and evolution of the Space Shuttle GN&C system. Emphasis is placed on key architecture decisions, design trades and the lessons learned for future complex space transportation system developments. Finally, some of the interesting flight operations experience is provided to inform future developers of flight experiences.

Zimpfer, Douglas↗

NASA NTRS2000

Laser Welding in Electronic Packaging

The laser has proven its worth in numerous high reliability electronic packaging applications ranging from medical to missile electronics. In particular, the pulsed YAG laser is an extremely flexible and versatile too] capable of hermetically sealing microelectronics packages containing sensitive components without damaging them. This paper presents an overview of details that must be considered for successful use of laser welding when addressing electronic package sealing. These include; metallurgical considerations such as alloy and plating selection, weld joint configuration, design of optics, use of protective gases and control of thermal distortions. The primary limitations on use of laser welding electronic for packaging applications are economic ones. The laser itself is a relatively costly device when compared to competing welding equipment. Further, the cost of consumables and repairs can be significant. These facts have relegated laser welding to use only where it presents a distinct quality or reliability advantages over other techniques of electronic package sealing. Because of the unique noncontact and low heat inputs characteristics of laser welding, it is an ideal candidate for sealing electronic packages containing MEMS devices (microelectromechanical systems). This paper addresses how the unique advantages of the pulsed YAG laser can be used to simplify MEMS packaging and deliver a product of improved quality.

Source record↗

NASA NTRS2014

A Coordinated Focused Ion Beam/Ultramicrotomy Technique for Serial Sectioning of Hayabusa Particles and Other Returned Samples

Recent sample return missions, such as NASA's Stardust mission to comet 81P/Wild 2 and JAXA's Hayabusa mission to asteroid 25143 Itokawa, have returned particulate samples (typically ~5-50 μm) that pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on how the samples are prepared for analysis. This also holds true for other extraterrestrial materials, including interplanetary dust particles, micrometeorites and lunar regolith grains. Traditionally, particulate samples have been prepared using microtomy techniques (e.g., [1]). However, for hard mineral particles ≳20 μm, microtome thin sections are compromised by severe chatter and sample loss. For these difficult samples, we have developed a hybrid technique that combines traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for the in situ investigation of grain surfaces and interiors. Using this method, we have increased the number of FIB-SEM prepared sections that can be recovered from a particle with dimensions on the order of tens of μms. These sections can be subsequently analyzed using a variety of electron beam techniques. Here, we demonstrate this sample preparation technique on individual lunar regolith grains in order to study their space-weathered surfaces. We plan to extend these efforts to analyses of individual Hayabusa samples.

Berger, E. L.↗

NASA NTRSDate not supplied

Examination of Lunar Regolith Simulants By SEM-EDS and Imaging Raman Spectroscopy

The Artemis series lunar missions will include sample returns from the lunar south pole. Lunar regolith simulants (RS) generated in the lab provide opportunities to compare two surface science techniques: scanning electron microscopy (SEM-EDS) and Raman induced surface spectroscopy. The results will also be applicable for supporting future commercial lunar payload services (CLPS) and Artemis surface. Surface characterization contributes to continued development of lunar regolith studies and adds to various regolith databases. In characterizing various lunar regolith simulants, part of the aim should be to standardize techniques and utilize anticipated methods available for astromaterials studied during, or returned from, upcoming missions, particularly samples collected from the Moon’s south pole and permanently shadowed regions (PSRs).. An initial survey of available simulants has been started with Raman scanning process for particle counting the results of which will enrich the NASA-JSC Simulant Development Lab (SDL) simulant properties database and the Colorado School of Mines Planetary Simulant Data Base. An SEM-EDS dataset of raw regolith simulant materials are collected.

Raman Microscopy↗

DOE OSTI2024

3D Nanocrystallography and the Imperfect Molecular Lattice

Crystallographic analysis relies on the scattering of quanta from arrays of atoms that populate a repeating lattice. While large crystals built of lattices that appear ideal are sought after by crystallographers, imperfections are the norm for molecular crystals. Additionally, advanced X-ray and electron diffraction techniques, used for crystallography, have opened the possibility of interrogating micro- and nanoscale crystals, with edges only millions or even thousands of molecules long. These crystals exist in a size regime that approximates the lower bounds for traditional models of crystal nonuniformity and imperfection. Accordingly, data generated by diffraction from both X-rays and electrons show increased complexity and are more challenging to conventionally model. New approaches in serial crystallography and spatially resolved electron diffraction mapping are changing this paradigm by better accounting for variability within and between crystals. The intersection of these methods presents an opportunity for a more comprehensive understanding of the structure and properties of nanocrystalline materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2024

A Coordinated Mineralogical and Oxygen Isotopic Study of Refractory Ca-Al-Rich Inclusions

Refractory Ca-Al-rich inclusions (CAIs) in primitive chondritic meteorites represent the oldest solids that formed in our Solar System. Coordinated analyses using multiple ion and electron-beam techniques are vital to fully understand complex nebular and asteroidal processes that CAIs may have experienced in the context of the formation and early evolution of our Solar System. We report the results of a coordinated mineralogical and oxygen isotopic study of unique grossite bearing CAIs from reduced CV (Vigarano type) carbonaceous chondrites using transmission electron microscopy and secondary ion mass spectrometry. Grossite (CaAl 4 O 7 ) occurs in cores of nodules in fine grained CAIs that likely represent aggregates of nebular condensates. In many occurrences, grossite has been partially replaced by hercynite [(Fe,Mg,Zn)Al 2 O 4 ], which displays complex microstructures and compositions, and magnetite nanoparticles. This grossite alteration likely occurred via crystallographically controlled metasomatic reactions with Zn, Fe-rich aqueous fluids on the parent asteroid. The constituent phases of grossite bearing CAIs show heterogeneous oxygen isotopic compositions . That is, grossite and perovskite are 16 O poor and melilite is variably 16 O-depleted in contrast to solar like, 16 O-rich hibonite and spinel. The observed oxygen isotopic distribution is interpreted as a result of mineralogically controlled oxygen isotopic exchange with an 16 O-poor fluid on the parent asteroid. Collectively, we conclude that the presence of limited fluids played an important role in preferential alteration of grossite to hercynite and magnetite and various degrees of 16 O depletion in grossite, perovskite, and melilite during thermal metamorphism on the CV chondrite parent asteroid.

Jangmi Han↗