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DOE OSTI2021

Dynamic Effects and Hydrogen Bonding in Mixed-Halide Perovskite Solar Cell Absorbers

The organic component (methylammonium) of CH 3 NH 3 PbI 3- x Cl x -based perovskites shows electronic hybridization with the inorganic framework via H-bonding between N and I sites. Femtosecond dynamics induced by core excitation are shown to strongly influence the measured X-ray emission spectra and the resonant inelastic soft X-ray scattering of the organic components. The N K core excitation leads to a greatly increased N-H bond length that modifies and strengthens the interaction with the inorganic framework compared to that in the ground state. The study indicates that excited-state dynamics must be accounted for in spectroscopic studies of this perovskite solar cell material, and the organic-inorganic hybridization interaction suggests new avenues for probing the electronic structure of this class of materials. Furthermore, it is incidentally shown that beam damage to the methylamine component can be avoided by moving the sample under the soft X-ray beam to minimize exposure and that this procedure is necessary to prevent the creation of experimental artifacts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Approaching PetaVolts per Meter Plasmonics Using Structured Semiconductors

A newly uncovered class of plasmons in the strongly excited limit opens access to unprecedented Petavolts per meter electromagnetic fields with wide-ranging, transformative impact. Unlike conventional plasmons, such plasmons are constituted by non-perturbative, large-amplitude oscillations of the ultradense, delocalized free electron Fermi gas inherent in conductive media. Here structured semiconductors doped to have an appropriate conduction electron density are introduced to tune the properties of the Fermi gas for matched excitation of large-amplitude plasmons using readily available electron beams which enables immediate experimental validation. Specifically, an electrostatic, surface “crunch-in” plasmon is collisionlessly excited by the beam launched inside a tube. Strong excitation due to matching results in relativistic oscillations of the electron gas and unravels unique phenomena. Relativistically induced ballistic electron transport comes about due to relativistic multifold increase in the mean free path and also leads to unconventional heat deposition beyond Ohm’s law. This explains the absence of observed damage or solid-plasma formation in past experiments on conductive samples interacting with electron bunches shorter than 10-13 seconds. Furthermore, relativistic momentum leads to copious tunneling of electron gas across the surface, which then crunches inside the tube. Relativistic effects along with large, localized electron density variations underlying these modes necessitate kinetic approach to theoretical and computational modeling. Kinetic model presented here demonstrates experimental viability of observing tens of gigavolts per meter plasmonic fields excited by matching readily available electron beams to plasmons in semiconductors with 1018cm-3 free electron density, and paves the way for Petavolts per meter plasmonics.

42 ENGINEERING↗

DOE OSTI2020

Microstructure Experiments-Enabled MARMOT Simulations of SiC/SiC-based Accident Tolerant Nuclear Fuel System

We have undertaken an experimental-computational project that addresses a few key technology gaps associated with the use of SiC/SiC composites for light water reactor fuel cladding. Two principal endeavors in this project are to assess the irradiation-induced microstructural changes and swelling in SiC/SiC composites, and to characterize and model the porous oxide surface layer (when exposed to steam) along SiC recession that is detrimental to the clad integrity under accident conditions. The project tasks are: (i) ion irradiation and characterization (University of Tennessee, Knoxville), (ii) mechanical tests and analysis (University of South Carolina), (iii) steam exposure tests (Oak Ridge National Laboratory), (iv) electron microscopy and spectroscopic characterization (NC State University), (v) x-ray microscopy and reconstruction (University of South Carolina and NC State University), (vi) phase field modeling and simulations (NC State University and Idaho National Laboratory). The effects of 10 MeV Au ion irradiation at 350°C on the microstructure evolution in SiC/SiC composites are investigated at doses up to 400 displacements per atom (dpa) at the University of Tennessee, Knoxville. Atomic force microscopy and optical profilometry reveal irradiation induced axial and radial shrinkage of the fibers for doses greater than 10 dpa. Based on detailed electron microscopy characterization, the primary cause of the fiber shrinkage is attributed to irradiation-induced loss of carbon packets. Additionally, the multilayer PyC interface is observed to portray high resistance to irradiation damage. The mechanical response and failure mechanisms of un-irradiated samples is also assessed through loading tests and X-ray imaging at the University of South Carolina. Steam exposure tests are performed at the Oak Ridge National Laboratory in a facility that represents a reactor pressure vessel under a loss-of-coolant-accident scenario. The samples that are analyzed methodically in this report are tested for 32/31 hours at 1200°C with a velocity of 0.25 cm/s for the pressures: 0.1 MPa, 0.45 MPa, 0.92 MPa and 1.38 MPa. Scanning/transmission electron microscopy analysis conducted at the NC State University (NCSU) shows that the oxide layer thickness increases with the steam pressure. While the oxide layer is crystalline (α- cristobalite) for the pressures 0.45 MPa, 0.92 MPa and 1.38 MPa, the layer is amorphous at 0.1 MPa. Results from Raman spectroscopy have also confirmed the formation of α-cristobalite phase of SiO₂. The abrupt increase in the integrated Raman intensity ratio between steam pressures 0.1 and 0.45 MPa suggests the onset of accelerated crystallization. Non-destructive three dimensional X-ray microscopy/tomography (XCT) and computational image processing techniques are employed by the University of South Carolina to probe the porous oxidation features on SiC samples at varying pressures. Interestingly, most pores are observed to be located away from the surface as well as the oxide-SiC interface. The average oxide layer thickness assessed from the XCT analysis is seen to be in excellent agreement with the values determined through scanning electron microscopy analysis for the highest pressures where the oxide layer is relatively more uniform. A phase-field model developed by the NC State University and Idaho National Laboratory for simulating oxidation of SiC by steam captures the paralinear kinetics of SiC oxidation with a high degree of fidelity. Results from quasi-one-dimensional and two dimensional simulations show that the pores with oxidizing species lead to a higher volatilization rate. These simulations indicate that the enhanced apparent volatilization rates at higher pressures observed in experiments can be rationalized by the increased volatilization from the pores. The project team has also successfully developed the capability to import images from experiments for realistic evolution of the oxidizing microstructure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1976

Gas interaction effects on lunar bonded particles and their implications

Results are reported for an experimental investigation of gas-interaction effects on different Apollo 11 and Apollo 12 lunar-soil samples containing bonded particles. In the experiments, lunar fines were exposed to pure O2, pure water vapor, HCl, NH3, N2, HCOOH, and CH3NH2, in order to observe whether bonded particles would separate. In addition, repeated gas adsorption/desorption measurements were performed to determine the nature and reactive properties of the particle surfaces, and surface areas were measured for comparison with analogous terrestrial samples to determine whether the surface areas of highly radiation-damaged particles were larger or smaller. It is found that N2 is apparently ineffective in separating bonded particles and that the ratio of Apollo 11 to Apollo 12 bonded particles separated by a particular gas exposure ranges from 2.5 to 3.0. Possible reasons for differences in material surface properties at the two Apollo sites are considered, and it is concluded that material from a certain depth at some other site was transported to the Apollo 12 site and mixed with the original material in recent years (considerably less than 2000 years ago).

Mukherjee, N. R.↗

NASA NTRS1978

Compression of rehydratable vegetables and cereals

Characteristics of freeze-dried compressed carrots, such as rehydration, volatile retention, and texture, were studied by relating histological changes to textural quality evaluation, and by determining the effects of storage temperature on freeze-dried compressed carrot bars. Results show that samples compressed with a high moisture content undergo only slight structural damage and rehydrate quickly. Cellular disruption as a result of compression at low moisture levels was the main reason for rehydration and texture differences. Products prepared from carrot cubes having 48% moisture compared favorably with a freshly cooked product in cohesiveness and elasticity, but were found slightly harder and more chewy.

Burns, E. E.↗

NASA NTRS1993

Below band-gap laser ablation of diamond for transmission electron microscopy

A 248 nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250-micron-thick substrate was achieved in about 15 min at normal incidence. While the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon-ion milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets characteristic of such type 1a diamonds.

George, T.↗

NASA NTRS2015

3-D Printed Ultem 9085 Testing and Analysis

The purpose of this document is to analyze the mechanical properties of 3-D printed Ultem 9085. This document will focus on the capabilities, limitations, and complexities of 3D printing in general, and explain the methods by which this material is tested. Because 3-D printing is a relatively new process that offers an innovative means to produce hardware, it is important that the aerospace community understands its current advantages and limitations, so that future endeavors involving 3-D printing may be completely safe. This document encompasses three main sections: a Slosh damage assessment, a destructive test of 3-D printed Ultem 9085 samples, and a test to verify simulation for the 3-D printed SDP (SPHERES Docking Port). Described below, 'Slosh' and 'SDP' refer to two experiments that are built using Ultem 9085 for use with the SPHERES (Synchronized Position Hold, Engage, Reorient, Experimental Satellites) program onboard the International Space Station (ISS) [16]. The SPHERES Facility is managed out of the National Aeronautics and Space Administration (NASA) Ames Research Center in California.

Aguilar, Daniel↗

NASA NTRS1993

Below Band-Gap Laser Ablation of Diamond for Transmission Electron Microscopy

A 248-nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250 micron thick substrate was achieved in about 15 minutes at normal incidence. Whilst the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets

Posthill, J. B.↗

NASA NTRS2001

Dynamic Fatigue of ULE Glass

Ultra Low Expansion (ULE) glass is used in a number of applications which require a low thermal expansion coefficient. One such application is telescope mirror elements. An allowable stress can be calculated for this material based upon modulus of rupture data; however, this does not take into account the problem of delayed failure. Delayed failure, due to stress corrosion can significantly shorten the lifetime of a glass article. Knowledge of the factors governing the rate of subcritical flaw growth in a given environment enables the development of relations between lifetime, applied stress and failure probability for the material under study. Dynamic fatigue is one method of obtaining the necessary information to develop these relationships. In this study, the dynamic fatigue method was used to construct time-to-failure diagrams for both 230/270 ground and optically polished samples. The grinding and polishing process reduces the surface flaw size and subsurface damage, and relieves residual stress by removing materials with successively smaller grinding media. This resulted in an increase in the strength of the optic during the grinding and polishing sequence. There was also an increase in the lifetime due to grinding and polishing. It was found that using the fatigue parameters determined from the 230/270 grit surface are not significantly different from the optically polished values. Although the lower bound of the polished samples is more conservative, neither time-to-failure curves lie beyond the upper or lower bound of the confidence limits. Therefore, designers preferring conservative limits could use samples without residual stress present (polished samples) to determine the fatigue parameters and inert Weibull parameters from samples with the service condition surface, to determine time-to-failure of the optical element.

Tucker, Dennis S.↗

DOE OSTI2021

Genomic reconstruction of fossil and living microorganisms in ancient Siberian permafrost

Abstract Background Total DNA (intracellular, iDNA and extracellular, eDNA) from ancient permafrost records the mixed genetic repository of the past and present microbial populations through geological time. Given the exceptional preservation of eDNA under perennial frozen conditions, typical metagenomic sequencing of total DNA precludes the discrimination between fossil and living microorganisms in ancient cryogenic environments. DNA repair protocols were combined with high throughput sequencing (HTS) of separate iDNA and eDNA fraction to reconstruct metagenome-assembled genomes (MAGs) from ancient microbial DNA entrapped in Siberian coastal permafrost. Results Despite the severe DNA damage in ancient permafrost, the coupling of DNA repair and HTS resulted in a total of 52 MAGs from sediments across a chronosequence (26–120 kyr). These MAGs were compared with those derived from the same samples but without utilizing DNA repair protocols. The MAGs from the youngest stratum showed minimal DNA damage and thus likely originated from viable, active microbial species. Many MAGs from the older and deeper sediment appear related to past aerobic microbial populations that had died upon freezing. MAGs from anaerobic lineages, including Asgard archaea, however exhibited minimal DNA damage and likely represent extant living microorganisms that have become adapted to the cryogenic and anoxic environments. The integration of aspartic acid racemization modeling and metaproteomics further constrained the metabolic status of the living microbial populations. Collectively, combining DNA repair protocols with HTS unveiled the adaptive strategies of microbes to long-term survivability in ancient permafrost. Conclusions Our results indicated that coupling of DNA repair protocols with simultaneous sequencing of iDNA and eDNA fractions enabled the assembly of MAGs from past and living microorganisms in ancient permafrost. The genomic reconstruction from the past and extant microbial populations expanded our understanding about the microbial successions and biogeochemical alterations from the past paleoenvironment to the present-day frozen state. Furthermore, we provided genomic insights into long-term survival mechanisms of microorganisms under cryogenic conditions through geological time. The combined strategies in this study can be extrapolated to examine other ancient non-permafrost environments and constrain the search for past and extant extraterrestrial life in permafrost and ice deposits on Mars.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Sample spinning to mitigate polarization artifact and interstitial-vacancy imbalance in ion-beam irradiation

Accelerator-based ion-beam irradiation has been widely used to mimic the effects of neutron radiation damage in nuclear reactors. However, ion radiation is most often monodisperse in the incoming ions’ momentum direction, leading to excessive polarization in defect distribution, while the scattering under neutron irradiation is often more isotropic and has less radiation-induced polarization. Mitigation of the excess-polarization as well as the damage non-uniformity artifact might be crucial for making the simulation of neutron radiation by ion-beam radiation more realistic. In this work, a general radiation polarization theory in treating radiation as external polar stimuli is established to understand the natural material responses in different contexts, and the possibility to correct the defect polarization artifact in ion-beam irradiation. Inspired by Magic Angle Spinning in Nuclear Magnetic Resonance, we present a precise sample spinning strategy to reduce the point-defect imbalance effect in ion-beam irradiation. It can be seen that with optimized surface inclination angle and the axis of sample rotation, the vacancy-interstitial population imbalance, as well as the damage profile non-uniformity in a designated region in the target are both reduced. It is estimated that sample spinning frequency on the order of kHz should be sufficient to scramble the ion momentum monodispersity for commonly taken ion fluxes and dose rates, which is experimentally feasible.

36 MATERIALS SCIENCE↗

NASA NTRS2023

The Effect of Oxidation in Environmental Barrier Coatings Subject to Foreign Object Damage

Oxidation and foreign object damage (FOD) are two key failure modes for environmental barrier coatings (EBCs). For EBCs with a silicon (Si) bond coat, a thermally grown oxide (TGO) layer forms at the EBC –bond coat interface. The TGO layer is considered the weak interface, and directly influences the life of the EBC. Moreover, FOD has been shown to cause significant subsurface damage resulting in delamination or spallation of the EBC which can occur at the EBC -bond coat interface or the bond coat -substrate interface. The purpose of this work is to investigate the synergistic effects of oxidation and FOD in a ytterbium disilicate (𝑌𝑏2𝑆𝑖2𝑂7) EBC. FOD testing is conducted on as-deposited and steam oxidized samples at room temperature using a 1.59-mm hardened steel ball projectile. The resulting damage is characterized by optical profilometry and scanning electron microscopy (SEM). Additionally, a quasi-static, mechanical assessment of the EBC bond strength in the presence of a growing TGO is presented.

environmental barrier coatings (EBCs)↗

NASA NTRS2014

Insights into Regolith Dynamics from the Irradiation Record Preserved in Hayabusa Samples

The rates of space weathering processes are poorly constrained for asteroid surfaces, with recent estimates ranging over 5 orders of magnitude. The return of the first surface samples from a space-weathered asteroid by the Hayabusa mission and their laboratory analysis provides "ground truth" to anchor the timescales for space weathering. We determine the rates of space weathering on Itokawa by measuring solar flare track densities and the widths of solar wind damaged rims on grains. These measurements are made possible through novel focused ion beam (FIB) sample preparation methods.

Keller, Lindsay P.↗

NASA NTRS2015

Experimentally Shocked and Altered Basalt: Laboratory Analogs for Calibration of Mars Remote Sensing and In Situ Data

Calciumphosphate (likely chloroapatite) is formed in the alteration experiments and is more abundant in the altered and shocked sample probably due to increased surface area exposed to alteration fluids resulting from shock damage in the form of both brittle and structural deformation to the starting material (Figs 1 & 3). Apatite forms in basic conditions so the closed system alteration experiment must be buffered by the basalt starting material to create a fluid chemistry environment evolving from neutral at the start to alkaline after 21 days at 160 C. Plagioclase feldspar in the unshocked sample (Fig. 2) has undergone a solid-state transformation to maskelynite, a disordered phase that is not manifest in the XRD pattern of the shocked sample (Fig.4). Olivine and ulvospinel that are present in the starting material can be detected by XRD in the shocked and altered sample (Fig. 4). Tungsten from the sample holder used in the shock experiments dominates the XRD pattern of the shocked and altered sample (Fig. 4). Samples were weighed after the alteration experiments to determine mass loss and predict the amount of material available for the planned analyses from the shock experiments. Within the constraints of these experiments, mass loss is negligible. The samples will next be characterized by Moessbauer and Vis-Near IR spectroscopy, the results of which will be compared to the Mars Exploration Rovers and Mars Reconnaissance Orbiter data sets respectively.

Bell, M. S.↗

NASA NTRS1987

Shock effects and argon loss in samples of the Leedey L6 chondrite experimentally shocked to 29-70 GPa pressures

The recovery of polished 600-micron-thick 7-mm-diameter disk samples and powder samples of the Leedey L6 chondrite from 29-70-GPa experimental shocks is investigated experimentally under vacuum conditions, with a focus on the possible direct shock loss of radiogenic Ar. The results of petrographic examination of the shocked samples and Ar isotope measurements are presented in tables, graphs, and micrographs and characterized in detail. The principal damage mechanisms are identified as mechanical disaggregation and increasing cataclasis, with little melting. The degassing of radiogenic Ar is found to be relatively modest and to increase with shock pressure and sample porosity; it is attributed to a combination of mechanical grain disruption and feldspar melting. It is inferred that Ar loss in naturally shocked materials (especially those showing few signs of melting) probably occurs during extended exposure to high temperatures during impact formation.

Bogard, Donald↗

NASA NTRS2015

Experimentally Shocked and Altered Basalt: Laboratory Analogs for Calibration of Mars Remote Sensing and In Situ Data

Calcium phosphate (likely chloroapatite) is formed in the alteration experiments and is more abundant in the altered and shocked sample probably due to increased surface area exposed to alteration fluids resulting from shock damage in the form of both brittle and structural deformation to the starting material (Figs 1 & 3). Apatite forms in basic conditions so the closed system alteration experiment must be buffered by the basalt starting material to create a fluid chemistry environment evolving from neutral at the start to alkaline after 21 days at 160 degrees Centigrade. Plagioclase feldspar in the unshocked sample (Fig. 2) has undergone a solid-state transformation to maskelynite, a disordered phase that is not manifest in the X-ray diffraction pattern of the shocked sample (Fig.4). Olivine and ulvospinel that are present in the starting material can be detected by X-ray diffraction in the shocked and altered sample (Fig. 4). Tungsten from the sample holder used in the shock experiments dominates the X-ray diffraction pattern of the shocked and altered sample (Fig. 4). Samples were weighed after the alteration experiments to determine mass loss and predict the amount of material available for the planned analyses from the shock experiments. Within the constraints of these experiments, mass loss is negligible. The samples will next be characterized by Moessbauer and Vis-Near Infrared spectroscopy, the results of which will be compared to the Mars Exploration Rovers and Mars Reconnaissance Orbiter data sets respectively.

Bell, M. S.↗

NASA NTRS1995

Telescience operations with the solar array module plasma interaction experiment

The Solar Array Module Plasma Interactions Experiment (SAMPIE) is a flight experiment that flew on the Space Shuttle Columbia (STS-62) in March 1994, as part of the OAST-2 mission. The overall objective of SAMPIE was to determine the adverse environmental interactions within the space plasma of low earth orbit (LEO) on modern solar cells and space power system materials which are artificially biased to high positive and negative direct current (DC) voltages. The two environmental interactions of interest included high voltage arcing from the samples to the space plasma and parasitic current losses. High voltage arcing can cause physical damage to power system materials and shorten expected hardware life. parasitic current losses can reduce power system efficiency because electric currents generated in a power system drain into the surrounding plasma via parasitic resistance. The flight electronics included two programmable high voltage DC power supplies to bias the experiment samples, instruments to measure the surrounding plasma environment in the STS cargo bay, and the on-board data acquisition system (DAS). The DAS provided in-flight experiment control, data storage, and communications through the Goddard Space Flight Center (GSFC) Hitchhiker flight avionics to the GSFC Payload Operations Control Center (POCC). The DAS and the SAMPIE POCC computer systems were designed for telescience operations; this paper will focus on the experiences of the SAMPIE team regarding telescience development and operations from the GSFC POCC during STS-62. The SAMPIE conceptual development, hardware design, and system verification testing were accomplished at the NASA Lewis Research Center (LeRC). SAMPIE was developed under the In-Space Technology Experiment Program (IN-STEP), which sponsors NASA, industry, and university flight experiments designed to enable and enhance space flight technology. The IN-STEP Program is sponsored by the Office of Space Access and Technology (OSAT).

Wald, Lawrence W.↗

DOE OSTI2020

Characterising Ion-Irradiated FeCr: Hardness, Thermal Diffusivity and Lattice Strain

Ion-irradiated FeCr alloys are useful for understanding and predicting neutron damage in the structural steels of future nuclear reactors. Previous studies have largely focused on the structure of irradiation induced defects, probed by transmission electron microscopy (TEM), as well as changes in mechanical properties. Across these studies, a wide range of irradiation conditions has been employed on samples with different processing histories, which complicates the analysis of the relationship between defect structures and material properties. Furthermore, key properties, such as irradiation-induced changes in thermal transport and lattice strain, are little explored. Here we present a systematic study of Fe3Cr, Fe5Cr and Fe10Cr binary alloys implanted with 20 MeV Fe3+ ions to nominal doses of 0.01 dpa and 0.1 dpa at room temperature. Nanoindentation, transient grating spectroscopy (TGS) and X-ray micro-beam Laue diffraction were used to study the changes in hardness, thermal diffusivity and strain in the material as a function of damage and Cr content. Our results suggest that Cr leads to an increased retention of irradiation-induced defects, causing substantial changes in hardness and lattice strain. However, thermal diffusivity varies little with increasing damage and instead degrades significantly with increasing Cr content in the material. We find significant lattice strains even in samples exposed to a nominal displacement damage of 0.01 dpa. The defect density predicted from the lattice strain measurements is significantly higher than that observed in previous TEM studies, suggesting that TEM may not fully capture the irradiation-induced defect population. (C) 2020 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

FeCr alloys↗