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DOE OSTI2024

Oxidation Penetration in Nuclear Graphite

Study results are presented for seven grades of graphite where 21 cylindrical samples were oxidized to a nominal level of mass loss. Low mass loss samples exhibited ~3% oxidative mass loss, intermediate ~8%, and high ~11%. Flat sample surfaces were covered during oxidation to minimize oxidation penetration at the top and bottom of each sample. Oxidized samples had their diameters reduced stepwise in 1 mm or 2 mm increments. Residual samples were weighed, geometric dimensions were recorded, and Archimedes measurements were taken at each step. Preliminary comparative graphical analysis is presented to illustrate the resultant density gradients observed. Raw tabular data are also provided.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Nanoindentation mapping defects filtration for heterogeneous materials using generative adversarial networks

Advanced composite materials with multiple phases and heterogeneous microstructure necessitate spatial mapping characterization of elastic modulus to develop constitutive relations and overall mechanical response. Such modulus mapping can be obtained using the nanoindentation technique, where the indenter tip raster over the selected microstructure region. Typically, a surface preparation procedure is done in the specimens to ensure proper contact between the indenter tip and sample surface. However, a near-perfect surface finish is unachievable in heterogeneous materials, primarily with ceramic reinforcements, due to the differential material removal rate during polishing. Thus, the nanoindenter records localized erroneous measurements due to differences in surface roughness and corresponding force response. This study establishes a novel deep learning-based strategy to rectify incorrect experimental spatial measurements acquire during nanoindentation modulus mapping. Here, the integrated bicubic interpolation and generative adversarial networks (GANs) model was trained using 14 ceramic and 18 metallic data sets, each comprising 65,536 measurements. The developed algorithm was validated against experimental measurements on four unknown specimens. The standard deviation in measured elastic modulus reduces by ~50% in ceramics and ~72% in metallic samples. This computational framework proposes a novel approach to reducing uncertainty in materials’ properties using state-of-the-art computer vision techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Comparison of Results for Quarter 1 Surface Water Split Samples Collected at the Nuclear Fuel Services Site, Erwin, Tennessee

Oak Ridge Associated Universities (ORAU), under the Oak Ridge Institute for Science and Education (ORISE) contract, collected split surface water samples with Nuclear Fuel Services (NFS) representatives on August 22, 2012. Representatives from the U.S. Nuclear Regulatory Commission and Tennessee Department of Environment and Conservation were also in attendance. Samples were collected at four surface water stations, as required in the approved Request for Technical Assistance number 11-018. These stations included Nolichucky River upstream (NRU), Nolichucky River downstream (NRD), Martin Creek upstream (MCU), and Martin Creek downstream (MCD). Both ORAU and NFS performed gross alpha and gross beta analyses. The comparison of results using the duplicate error ratio (DER), also known as the normalized absolute difference. A DER ≤ 3 indicates that, at a 99% confidence interval, split sample results do not differ significantly when compared to their respective one standard deviation (sigma) uncertainty. The NFS split sample report does not specify the confidence level of reported uncertainties. Therefore, standard two sigma reporting is assumed and uncertainty values were divided by 1.96. A comparison of split sample results, using the DER equation, indicates one set with a DER greater than 3. A DER of 3.1 is calculated for gross alpha results from ORAU sample 5198W0003 and NFS sample MCU-310212003. The ORAU result is 0.98 ± 0.30 pCi/L (value ± 2 sigma) compared to the NFS result of -0.08 ± 0.60 pCi/L. Relatively high DER values are not unexpected for low (e.g., background) analyte concentrations analyzed by separate laboratories, as is the case here. It is noted, however, NFS uncertainties are at least twice the ORAU uncertainties, which contributes to the elevated DER value. Differences in ORAU and NFS minimum detectable activities are even more pronounced. comparison of ORAU and NFS split samples produces reasonably consistent results for low (e.g., background) concentrations.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2013

COMPARISON OF RESULTS FOR QUARTER 2 SURFACE WATER SPLIT SAMPLES COLLECTED AT THE NUCLEAR FUEL SERVICES SITE, ERWIN, TENNESSEE

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2014

Accurate formula for dissipative interaction in frequency modulation atomic force microscopy

Much interest has recently focused on the viscosity of nano-confined liquids. Frequency modulation atomic force microscopy (FM-AFM) is a powerful technique that can detect variations in the conservative and dissipative forces between a nanometer-scale tip and a sample surface. We now present an accurate formula to convert the dissipation power of the cantilever measured during the experiment to damping of the tip-sample system. We demonstrated the conversion of the dissipation power versus tip-sample separation curve measured using a colloidal probe cantilever on a mica surface in water to the damping curve, which showed a good agreement with the theoretical curve. Moreover, we obtained the damping curve from the dissipation power curve measured on the hydration layers on the mica surface using a nanometer-scale tip, demonstrating that the formula allows us to quantitatively measure the viscosity of a nano-confined liquid using FM-AFM.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2013

COMPARISON OF RESULTS FOR QUARTER 4 SURFACE WATER SPLIT SAMPLES COLLECTED AT THE NUCLEAR FUELS SERVICES SITE, ERWIN, TN

Oak Ridge Associated Universities (ORAU), under the Oak Ridge Institute for Science and Education (ORISE) contract, collected split surface water samples with Nuclear Fuel Services (NFS) representatives on June 12, 2013. Representatives from the U.S. Nuclear Regulatory Commission (NRC) and the Tennessee Department of Environment and Conservation were also in attendance. Samples were collected at four surface water stations, as required in the approved Request for Technical Assistance number 11-018. These stations included Nolichucky River upstream (NRU), Nolichucky River downstream (NRD), Martin Creek upstream (MCU), and Martin Creek downstream (MCD). Both ORAU and NFS performed gross alpha and gross beta analyses, and Table 1 presents the comparison of results using the duplicate error ratio (DER), also known as the normalized absolute difference. A DER ≤ 3 indicates at a 99% confidence interval that split sample results do not differ significantly when compared to their respective one standard deviation (sigma) uncertainty (ANSI N42.22). The NFS split sample report specifies 95% confidence level of reported uncertainties (NFS 2013). Therefore, standard two sigma reporting values were divided by 1.96. In conclusion, most DER values were less than 3 and results are consistent with low (e.g., background) concentrations. The gross beta result for sample 5198W0014 was the exception. The ORAU gross beta result of 6.30 &plusmn 0.65 pCi/L from location NRD is well above NFS's non-detected result of 1.56 &plusmn 0.59 pCi/L. NFS's data package includes no detected result for any radionuclide at location NRD. At NRC's request, ORAU performed gamma spectroscopic analysis of sample 5198W0014 to identify analytes contributing to the relatively elevated gross beta results. This analysis identified detected amounts of naturally-occurring constituents, most notably Ac-228 from the thorium decay series, and does not suggest the presence of site-related contamination.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2013

COMPARISON OF RESULTS FOR QUARTER 3 SURFACE WATER SPLIT SAMPLES COLLECTED AT THE NUCLEAR FUEL SERVICES SITE, ERWIN, TENNESSEE

Oak Ridge Associated Universities (ORAU), under the Oak Ridge Institute for Science and Education (ORISE) contract, collected split surface water samples with Nuclear Fuel Services (NFS) representatives on March 20, 2013. Representatives from the U.S. Nuclear Regulatory Commission and the Tennessee Department of Environment and Conservation were also in attendance. Samples were collected at four surface water stations, as required in the approved Request for Technical Assistance number 11-018. These stations included Nolichucky River upstream (NRU), Nolichucky River downstream (NRD), Martin Creek upstream (MCU), and Martin Creek downstream (MCD). Both ORAU and NFS performed gross alpha and gross beta analyses, and Table 1 presents the comparison of results using the duplicate error ratio (DER), also known as the normalized absolute difference. A DER {<=} 3 indicates that at a 99% confidence interval, split sample results do not differ significantly when compared to their respective one standard deviation (sigma) uncertainty (ANSI N42.22). The NFS split sample report does not specify the confidence level of reported uncertainties (NFS 2013). Therefore, standard two sigma reporting is assumed and uncertainty values were divided by 1.96. In conclusion, most DER values were less than 3 and results are consistent with low (e.g., background) concentrations. The gross beta result for sample 5198W0012 was the exception. The ORAU result of 9.23 &plusmn 0.73 pCi/L from location MCD is well above NFS's result of -0.567 &plusmn 0.63 pCi/L (non-detected). NFS's data package included a detected result for U-233/234, but no other uranium or plutonium detection, and nothing that would suggest the presence of beta-emitting radionuclides. The ORAU laboratory reanalyzed sample 5198W0012 using the remaining portion of the sample volume and a result of 11.3 &plusmn 1.1 pCi/L was determined. As directed, the laboratory also counted the filtrate using gamma spectrometry analysis and identified only naturally occurring or ubiquitous man-made constituents, including beta emitters that are presumably responsible for the elevated gross beta values.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2013

Comparison of results for quarter 5 surface water split samples collected at the nuclear fuel services site Erwin Tennessee

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Using SF 6 and Xe to Monitor Gas Migration Through Explosion-Generated Fracture Networks

Here we describe a field study where tracer gas was injected into a subsurface cavity created by a small chemical explosion beneath the water table. The main objective of the study is to compare the migration of sulfur hexafluoride (SF 6 ) and xenon (Xe) through an explosion-generated fracture network and to study the influence of ground water on gas transport. A mixture of tracer gases (50% of SF 6 and 50% of Xe) was injected on 31 October 2018 and gas sampling continued until 8 November 2018. We observe similar trends in SF 6 and Xe concentrations at four ground surface sampling sites. The changes in the SF 6 /Xe ratios with time show that more SF 6 than Xe is observed during the barometric pressure lows when the absolute measured concentrations are highest. Conversely, the ratio SF 6 /Xe is less than 1 during the high-pressure intervals when absolute measured concentrations are low. The results of the experiment suggest that during barometric pressure lows the tracer is migrating to the surface primarily by advective gas phase transport, whereas during barometric pressure highs, advection is suppressed and near-surface evaporation of interstitial pore fluid with tracer dissolved in it becomes more important. Thus, the results of the experiment show that the gas concentrations at the surface are controlled by the combined effects of the gas dissolution into pore water and the barometric pressure fluctuations.

58 GEOSCIENCES↗

NASA NTRS2019

Microbial Monitoring of Astromaterials Curation Labs Reveals Inter-Lab Diversity

The Astromaterials Curation Division at NASA’s Johnson Space Center houses seven sample collections stored in separate clean rooms to avoid cross-contamination. Prior to receiving new sample collections from carbon rich asteroids, we instituted a monitoring program to characterize the microbial ecology of these labs and to understand how organisms could interact with and potentially contaminate current and future collections. Methods: Beginning in Oct. 2017 we sampled the Meteorite (ISO 7 equivalent) and Pristine Lunar (ISO 5 equivalent) labs on a monthly basis. Surface samples were collected using dry swabs. Air samples were collected using an impactor style air sampler. Cultivable organisms were identified and characterized. Aliquots of each sample were also preserved for DNA sequencing. For each sampling event recovery rate was calculated as the percentage of samples showing microbial growth1. Fungal colonies were selected for amino acid extraction and analysis via Ultra- Performance Liquid Chromatography with Fluorescence Detection and Mass Spectrometry.

Regberg, A. B.↗

DOE OSTI2014

Atomic Force Microscope Controlled Topographical Imaging and Proximal Probe Thermal Desorption/Ionization Mass Spectrometry Imaging

This paper reports on the development of a hybrid atmospheric pressure atomic force microscopy/mass spectrometry imaging system utilizing nano-thermal analysis probes for thermal desorption surface sampling with subsequent atmospheric pressure chemical ionization and mass analysis. The basic instrumental setup and the general operation of the system were discussed and optimized performance metrics were presented. The ability to correlate topographic images of a surface with atomic force microscopy and a mass spectral chemical image of the same surface, utilizing the same probe without moving the sample from the system, was demonstrated. Co-registered mass spectral chemical images and atomic force microscopy topographical images were obtained from inked patterns on paper as well as from a living bacterial colony on an agar gel. Spatial resolution of the topography images based on pixel size (0.2 m x 0.8 m) was better than the resolution of the mass spectral images (2.5 m x 2.0 m), which were limited by current mass spectral data acquisition rate and system detection levels.

Ovchinnikova, Olga S↗

NASA NTRS1992

Analysis of surfaces from the LDEF A0114, phase 2

Analysis of surfaces from the Long Duration Exposure Facility (LDEF) continued during the reporting period. Work has continued on profilometry measurements of eroded and corroded sample surfaces, optical transmission measurements, analysis of the pinhole camera, and x-ray photoelectron spectroscopy (XPS) analysis of some samples. Papers that have appeared or have been accepted for publications are listed. Several of these papers and an abstact are included.

Gregory, John C.↗

DOE OSTI2018

Room temperature decomposition of dimethyl methylphosphonate on cuprous oxide yields atomic phosphorus

Organophosphorus compounds have a wide range of reactivity depending on the coordination and oxidation state of the P atom. Due to their toxicity, certain organophosphonates are used as pesticides, herbicides, and, notoriously, as chemical nerve agents. The organophosphonate decomposition mechanism depends strongly on the substrate material, which motivates careful analysis of a range of potential materials for decontamination and sensing applications. Here, we present a study of the decomposition of dimethyl methylphosphonate (DMMP), a simulant molecule for the nerve agent sarin, on polycrystalline cuprous oxide surfaces (Cu 2 O). We use ambient pressure X-ray photoelectron spectroscopy (APXPS) and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy to monitor the pressure-dependent surface chemistry during exposure to DMMP vapor. At room temperature, we observe extensive degradation of DMMP, which includes the formation of reduced P products on the sample surface. We identify five unique P-containing species in the P 2p APXPS spectra, including atomic P and a surface-bound phosphinate [O=PH(OCH 3 )Osingle bondCu]. Here we propose a DMMP decomposition pathway whereby accumulation of this phosphinate species leads to an autocatalytic reaction on the Cu 2 O surface which yields reduced P species. After DMMP exposure, heating the Cu 2 O sample to 265°C leads to complete removal of all carbonaceous species and accumulation of a phosphate layer with stoichiometry similar to P 2 O 5 . These results introduce a new mechanism of room-temperature DMMP decomposition on metal oxides, which could be leveraged for the design of tailored metal oxide materials for catalyzing organophosphonate decomposition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Results for the Fourth Quarter 2012 Tank 50 WAC Slurry Sample: Chemical and Radionuclide Contaminants

This report details the chemical and radionuclide contaminant results for the characterization of the 2012 Fourth Quarter sampling of Tank 50 for the Saltstone Waste Acceptance Criteria (WAC).1 Information from this characterization will be used by Waste Solidification Engineering (WSE) to support the transfer of low-level aqueous waste from Tank 50 to the Salt Feed Tank in the Saltstone Facility in Z-Area, where the waste will be immobilized. This information is also used to update the Tank 50 Waste Characterization System. The following conclusions are drawn from the analytical results provided in this report: The concentration of the reported chemical and radioactive contaminants were less than their respective WAC Limits and Targets, unless noted in this section. Norpar 13 and Isopar L have higher detection limits 5 compared with the Saltstone WAC 1 . The data provided in this report is based upon the concentrations in the sub-sample, and due to the limited solubility in aqueous solution, may not represent the concentrations of the analytes in Tank 50. Diisooctyl adipate (or diisooctyl hexanedioate) was measured at 1.30E+00 mg/L in one of two replicate measurements conducted on an at-depth sample. a The organic analysis of the at-depth sample was conducted at the request of SRR. 4 This analyte was below the detection limit in the surface sample. The low insoluble solids content increases the measurement uncertainty for insoluble species.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Effects of structural defects on optical properties of In x Ga 1-x N layers and quantum wells

This review concentrates on the microstructure of In x Ga 1-x N layers and quantum wells (QWs) in relation to their optical properties. The microstructure of In x Ga 1-x N, with a constant In(x) concentration, shifts with layer thickness. Only layers below 100 nm for x = 0.1 are nearly defect-free. A photoluminescence peak is observed at 405 nm, in line with ~10% In, suggesting band-edge luminescence. Layers with greater thickness and In content present a corrugated surface with numerous structural defects, including V-defects, causing redshifts and multi-peaks in photoluminescence up to 490 nm. These defects, resembling those in GaN, lead to a corrugated sample surface. Atomic force microscopy shows a 3.7-fold larger corrugation in samples with 20 QWs compared to those with 5 QWs measured on 2 × 2 μm 2 areas. Like in GaN, dual growth on different crystallographic planes results in varied QW thicknesses, influencing optical traits of devices made from In x Ga 1-x N layers. The purpose of this review and the chosen subject is to highlight the significant contribution of Wladek Walukiewicz and his group to the current research on the properties of In x Ga 1-x N, which are crucial alloys in the field of optoelectronics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS2013

Examples of Optical Assessment of Surface Cleanliness of Genesis Samples

Optical microscope assessment of Genesis solar wind collector surfaces is a coordinated part of the effort to obtain an assessed clean subset of flown wafer material for the scientific community. Microscopic survey is typically done at 50X magnification at selected approximately 1 square millimeter areas on the fragment surface. This survey is performed each time a principle investigator (PI) returns a sample to JSC for documentation as part of the established cleaning plan. The cleaning plan encompasses sample handling and analysis by Genesis science team members, and optical survey is done at each step in the process. Sample surface cleaning is performed at JSC (ultrapure water [1] and UV ozone cleaning [2]) and experimentally by other science team members (acid etch [3], acetate replica peels [4], CO2 snow [5], etc.). The documentation of each cleaning method can potentially be assessed with optical observation utilizing Image Pro Plus software [6]. Differences in particle counts can be studied and discussed within analysis groups. Approximately 25 samples have been identified as part of the cleaning matrix effort to date.

Rodriquez, Melissa C.↗

DOE OSTI2014

Superhydrophobic Analyte Concentration Utilizing Colloid-Pillar Array SERS Substrates

In order to detect a few molecules present in a large sample it is important to know the trace components in the medicinal and environmental sample. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. Moreover, the following work involves superhydrophobic surfaces that includes silicon pillar arrays formed by lithographic and dewetting protocols. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added to the functionalized pillar array system via soaking. The pillars are used native and with hydrophobic modification. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 10-12 M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up applications in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Surface and bulk effects of K in highly efficient Cu 1-x K x InSe 2 solar cells

To advance knowledge of the beneficial effects of K in Cu(In,Ga)(Se,S) 2 (CIGS) photovoltaic (PV) absorbers, recent Cu-K-In-Se phase growth studies have been extended to PV performance. First, the effect of distributing K throughout bulk Cu 1-x K x InSe 2 absorbers at low K/(K+Cu) compositions (0 = x = 0.30) was studied. Efficiency, open-circuit voltage (VOC), and fill factor (FF) were greatly enhanced for x ~ 0.07, resulting in an officially-measured 15.0%-efficient solar cell, matching the world record CuInSe 2 efficiency. The improvements were a result of reduced interface and bulk recombination, relative to CuInSe 2 (x ~ 0). However, higher x compositions had reduced efficiency, short-circuit current density (J SC ), and FF due to greatly increased interface recombination, relative to the x ~ 0 baseline. Next, the effect of confining K at the absorber/buffer interface at high K/(K+Cu) compositions (0.30 = x = 0.92) was researched. Previous work showed that these surface layer growth conditions produced CuInSe 2 with a large phase fraction of KInSe 2 . After optimization (75 nm surface layer with x ~ 0.41), these KInSe 2 surface samples exhibited increased efficiency (officially 14.9%), VOC, and FF as a result of decreased interface recombination. The KInSe 2 surfaces had features similar to previous reports for KF post-deposition treatments (PDTs) used in world record CIGS solar cells - taken as indirect evidence that KInSe 2 can form during these PDTs. Both the bulk and surface growth processes greatly reduced interface recombination. However, the KInSe 2 surface had higher K levels near the surface, greater lifetimes, and increased inversion near the buffer interface, relative to the champion bulk Cu 1-x K x InSe 2 absorber. These characteristics demonstrate that K may benefit PV performance by different mechanisms at the surface and in the absorber bulk.

14 SOLAR ENERGY↗