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At least 739 records · Page 41

Technical basis for the reduction of the maximum temperature TGA-MS analysis of oxide samples from the 3013 destructive examination program

Thermogravimetric analysis with mass spectroscopy of the evolved gas (TGA-MS) is used to quantify the moisture content of materials in the 3013 destructive examination (3013 DE) surveillance program. Salts frequently present in the 3013 DE materials volatilize in the TGA and condense in the gas lines just outside the TGA furnace. The buildup of condensate can restrict the flow of purge gas and affect both the TGA operations and the mass spectrometer calibration. Removal of the condensed salts requires frequent maintenance and subsequent calibration runs to keep the moisture measurements by mass spectroscopy within acceptable limits, creating delays in processing samples. In this report, the feasibility of determining the total moisture from TGA-MS measurements at a lower temperature is investigated. A temperature of the TGA-MS analysis which reduces the complications caused by the condensation of volatile materials is determined. Analysis shows that an excellent prediction of the presently measured total moisture value can be made using only the data generated up to 700 °C and there is a sound physical basis for this estimate. It is recommended that the maximum temperature of the TGA-MS determination of total moisture for the 3013 DE program be reduced from 1000 °C to 700 °C. It is also suggested that cumulative moisture measurements at 550 °C and 700°C be substituted for the measured value of total moisture in the 3013 DE database. Using these raw values, any of predictions of the total moisture discussed in this report can be made.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of a fast framing detector for electron microscopy

A high frame rate detector system is described that enables fast real-time data analysis of scanning diffraction experiments in scanning transmission electron microscopy (STEM). This is an end-to-end development that encompasses the data producing detector, data transportation, and real-time processing of data. The detector will consist of a central pixel sensor that is surrounded by annular silicon diodes. Both components of the detector system will synchronously capture data at almost 100 kHz frame rate, which produces an approximately 400 Gb/s data stream. Low-level preprocessing will be implemented in firmware before the data is streamed from the National Center for Electron Microscopy (NCEM) to the National Energy Research Scientific Computing Center (NERSC). Live data processing, before it lands on disk, will happen on the Cori supercomputer and aims to present scientists with prompt experimental feedback. This online analysis will provide rough information of the sample that can be utilized for sample alignment, sample monitoring and verification that the experiment is set up correctly. Only a compressed version of the relevant data is then selected for more in-depth processing.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Reliability analysis in the Office of Safety, Environmental, and Mission Assurance (OSEMA)

The technical personnel in the SEMA office are working to provide the highest degree of value-added activities to their support of the NASA Langley Research Center mission. Management perceives that reliability analysis tools and an understanding of a comprehensive systems approach to reliability will be a foundation of this change process. Since the office is involved in a broad range of activities supporting space mission projects and operating activities (such as wind tunnels and facilities), it was not clear what reliability tools the office should be familiar with and how these tools could serve as a flexible knowledge base for organizational growth. Interviews and discussions with the office personnel (both technicians and engineers) revealed that job responsibilities ranged from incoming inspection to component or system analysis to safety and risk. It was apparent that a broad base in applied probability and reliability along with tools for practical application was required by the office. A series of ten class sessions with a duration of two hours each was organized and scheduled. Hand-out materials were developed and practical examples based on the type of work performed by the office personnel were included. Topics covered were: Reliability Systems - a broad system oriented approach to reliability; Probability Distributions - discrete and continuous distributions; Sampling and Confidence Intervals - random sampling and sampling plans; Data Analysis and Estimation - Model selection and parameter estimates; and Reliability Tools - block diagrams, fault trees, event trees, FMEA. In the future, this information will be used to review and assess existing equipment and processes from a reliability system perspective. An analysis of incoming materials sampling plans was also completed. This study looked at the issues associated with Mil Std 105 and changes for a zero defect acceptance sampling plan.

Kauffmann, Paul J.↗

Coordinated Analysis of an Ion Irradiated Carbonaceous Chondrite Suggests Complex Space Weathering Effects

Surfaces of airless planetary bodies are exposed to micrometeorite bombardment and solar wind irradiation which alter the microstructural, compositional, and optical properties of regoliths over time. These processes are collectively known as space weathering, and they complicate the interpretation of remote sensing data and the subsequent characterization of airless surfaces. Within the next 5 years, NASA’s OSIRIS-REx (Origins, Spectral Interpretation, Resource Identification, Security, Regolith Explorer) and JAXA (Japan Aerospace Exploration Agency)’s Hayabusa2 missions will return samples from C-type asteroids Bennu and Ryugu, respectively. Compared to the Moon and S-type asteroids, our understanding of the space weathering of C-complex asteroids is limited. In order to maximize scientific return from remote sensing data and to prepare for the analysis of returned samples from these missions, we must better understand the effects of space weathering on hydrated, organic-rich materials. We can do so by simulating these processes in the laboratory. In this study, we simulate solar wind exposure through ion irradiation of the CM2 carbonaceous chondrite Murchison - a suitable analog for C-complex asteroids. Here, we present coordinated analyses of a sample before and after ion irradiation.

Laczniak, D. L.↗

Silicon solar cell process development, fabrication, and analysis

Two large cast ingots were evaluated. Solar cell performance versus substrate position within the ingots was obtained and the results are presented. Dendritic web samples were analyzed in terms of structural defects, and efforts were made to correlate the data with the performance of solar cells made from the webs.

Yoo, H. I.↗

X-ray computed tomography-based porosity analysis: Algorithms and application for porous woody biomass

The properties of lignocellulosic biomass, such as bulk physical, thermal, and mechanical properties, as well as the mobility of enzymes or catalysts, are largely affected by porosity, pore structures, and pore size distribution. While X-ray computed tomography (CT) has been introduced to effectively produce 3D volumetric images of material microstructure, a quantitative porosity analysis from the 3D images has never been done. This work introduces a first-of-its-kind X-ray CT-based quantitative porosity analysis method and applies the developed toolkit to characterize the internal porosity distribution of loblolly pine. A sample loblolly pine chip was scanned by a nano-resolution X-ray CT system and digitally reconstructed after a sequence of image processing operations. Here, a comprehensive porosity analysis was then performed to quantify the envelope porosity, the spatial distribution of local porosity, and the directional porosity. Solutions to the various challenges in image processing, porosity calculation, and large data handling are provided.

42 ENGINEERING↗

Synthesis and electromagnetic properties of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide composites

Graphical abstract: Due to combining different functions and characteristics of individual materials, hybrid nanocomposite materials can strengthen their applications. Magnetic-conductive nanocomposites are the promising materials with electromagnetic loss, which have synergetic behavior between magnetic and conductive materials. It is the first time to report the synthesis of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide (BF/TD) composites by the gel-precursor self-propagating combustion process. The influence of mass ratio of BF and TD on the electromagnetic properties of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide composites was studied. The tgδ{sub μ} and tgδ{sub ε} of BF–TD composites. - Highlights: • It is the first time to report BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide composites. • The composites are prepared by the gel-precursor self-propagating combustion. • The electromagnetic properties could be adjusted by the mass ratio of BF and TD. • The introduction of TD enhances the dielectric loss and widens the frequency bands. • BF/TD composites will be microwave absorption materials with wide frequency band. - Abstract: Doped BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide composites have been prepared by the gel-precursor self-propagating combustion process. The characterization of the composites are performed by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), Differential thermal analysis-thermo gravimetry (DTA–TG), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM) and network analyzer. Both XRD and FT-IR indicate that the doped BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide composites are successfully synthesized and there are some interactions between BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19} and titanium dioxide. DTA–TG analysis of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide composites shows that the composite gel decomposition process mainly includes two stages: the first stage is the crystallized water and the residual moisture evaporation; the second stage is the nitrate and citric acid decomposition reaction. SEM demonstrates that the doped BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19}/titanium dioxide solid solution has formed. The magnetic parameters indicate that the electromagnetic properties of the composites could be well adjusted by the mass ratio of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19} and titanium dioxide. When the mass ratio of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19} and titanium dioxide is 4:5, the composites have the best magnetic loss. The composites with the mass ratio 6:5 of BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19} and titanium dioxide. BaFe{sub 11.92}(LaNd){sub 0.04}O{sub 19} and titanium dioxide possess good dielectric loss. The introduction of titanium dioxide enhances the dielectric loss and widens the frequency bands. The composites will be promising microwave absorption materials with wide frequency band.

36 MATERIALS SCIENCE↗

Omics-Lethal Human Viruses, West Nile Experiment WGCN002

The purpose of this experiment was to evaluate the host response to wild-type West Nile virus infectious clone (WNV-NY99 clone 382) and mutant (WNVE218A) virus infection. Sample data was obtained from mouse granule cell neurons for mRNA and miRNA expression analysis. See Experiment WGCN003 for corresponding independent biological replicate study. Secondary host-associated viral dataset downloads contain one or more statistically processed (normalization data transformation) quantitative dataset collections resulting in qualitative expression analyses of primary host-pathogen experimental study designs. Transcriptomics dataset downloads have a direct relationship to a primary sample submission corresponding to a specific West Nile virus infection.

59 BASIC BIOLOGICAL SCIENCES↗

Omics-Lethal Human Viruses, West Nile Experiment WGCN003

The purpose of this experiment was to evaluate the host response to wild-type West Nile virus infectious clone (WNV-NY99 clone 382) and mutant (WNVE218A) virus infection. Sample data was obtained from mouse granule cell neurons for mRNA and miRNA expression analysis. See Experiment WGCN002 for corresponding independent biological replicate study. Secondary host-associated viral dataset downloads contain one or more statistically processed (normalization data transformation) quantitative dataset collections resulting in qualitative expression analyses of primary host-pathogen experimental study designs. Transcriptomics dataset downloads have a direct relationship to a primary sample submission corresponding to a specific West Nile virus infection.

59 BASIC BIOLOGICAL SCIENCES↗

Omics-Lethal Human Viruses, West Nile Experiment WDC011

The purpose of this experiment was to evaluate the host response to wild-type West Nile virus (WNVMT) and mutant (WNVE218A) virus infection. Sample data was obtained from primary mouse myeloid dendritic cells for mRNA expression analysis. See Experiment WDC010 (GSE74628) for corresponding independent biological replicate study. Secondary host-associated viral dataset downloads contain one or more statistically processed (normalization data transformation) quantitative dataset collections resulting in qualitative expression analyses of primary host-pathogen experimental study designs. Transcriptomics dataset downloads have a direct relationship to a primary sample submission corresponding to a specific West Nile virus infection.

59 BASIC BIOLOGICAL SCIENCES↗

Thermal analysis of calcium sulfate dihydrate sources used to manufacture gypsum wallboard

Gypsum wallboard has been used for over 100 years as a barrier to the spread of fire in residential and commercial structures. The gypsum molecule, CaSO 4 ·2H 2 O, provides two crystalline waters that are released upon heating providing an endothermic effect. Manufacturers have recognized that the source of the gypsum ore is a factor that affects all aspects of its performance; thus, it is hypothesized that the impurities present in the gypsum ore are the causes of the performance differences. Differential Thermal Analysis/Thermogravimetric Analysis (DTA/TGA) and X-ray Diffraction (XRD) were used in this paper to compare and characterize samples of gypsum ore representing sources of natural, synthetic from a Flue Gas Desulfurization process (FGD) and blends thereof. The hemihydrate phase of representative natural, FGD, and reagent grade calcium sulfate were rehydrated with distilled water and evaluated by DTA/TGA. Analysis of the data shows distinct areas of similarity separated by the conversion to anhydrite ~250 °C. Compositional reconstructions based on DTA/TGA and XRD data were compared and although, the results were comparable, the DTA/TGA suggests thermally active compounds that were not detected by XRD. Anhydrite, silica and halite were reported by XRD but were not thermally reactive in the temperature range evaluated by DTA/TGA (ambient to 1050 °C). Finally, the presence of carbonate compounds (e.g., calcite and dolomite) were indicated by XRD and estimated from the thermal decomposition reaction ~700 °C.

36 MATERIALS SCIENCE↗

Specification of FIPD Fission Gas Chemistry Data

The current FIPD library contains two main sets of fission gas chemistry data. The first set is data collected during the Integral Fast Reactor (IFR) program from 1984 to 1994, using a gas mass spectrometry system located in the Analytical Laboratory (AL) at Argonne National Laboratory-West (Argonne-West). Throughout this period, numerous fission gas release and chemistry datasets were gathered from a variety of metallic fuel pins. The fission gas was sampled by the Gas Assay, Sample and Recharge (GASR) System in the Hot Fuel Examination Facility (HFEF) and transferred to the AL to perform gas composition and isotopic abundance analysis. The second set is data collected after the IFR program. The fission gas samples were also collected by the GASR system at the HFEF, but analyzed using a similar gas mass spectrometer located in Pacific Northwest National Laboratory (PNNL). Many fuel pins irradiated in Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF) were measured, including the fuel pins for the MFF series of experiments, designed to qualify metal fuel for use as driver fuel in the FFTF and X496 experiment. For either set of data, fission gas was sampled with the gas sampling line in GASR using sample bottles after the capsule/element volume has been determined and the system is still full of radioactive gas. The sample bottles were then transferred to the sample packaging cylinder or an approved storage location pending transfer to the AL or prepared for shipment to another laboratory (such as PNNL) for analysis of the collected gas as directed on the GASR data form, other approved form. The receiving laboratories (AL or PNNL) required their Analytical Service Request form to be completed prior to sample transfer. Typical sample transfer processes were initiated at HFEF by the principal or process engineer. The laboratories performing the analyses (AL or PNNL) use the sample bottle numbers as well as a sample number produced by the respective laboratory. HFEF and the responsible experimenter tracked the sample using the analysis number, the gas bottle number, and the fuel pin number.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Kriging-Based Inverse Uncertainty Quantification of BISON Fission Gas Release Model

Nuclear reactor fuel performance analysis studies the thermo-mechanical behavior of fuel rods and verify their compliance with safety criteria under both normal operation and accidental conditions. One of the major concerns in fuel performance analysis is the behavior of the fission gases xenon and krypton in uranium dioxide fuel, which significantly affect the thermo-mechanical performance of the nuclear fuel rods employed in current LWRs. Previously, the modeling of fission gas release (FGR) in nuclear fuel performance codes have been relying on empirical models which are not applicable beyond their range of calibration. Recently a more efficient and flexible physics-based FGR and swelling model that can describe a wider range of reactor operation conditions have been implemented in fuel performance code BISON. In this work, we performed Bayesian calibration to inversely quantify the uncertainties associated with the 5 tuning parameters in BISON FGR model, based on the time-dependent FGR measurement data from Riso-AN3 benchmark. It takes around 1 hour and 40 minutes for BISON to simulate the Riso-AN3 benchmark with a moderate mesh size using 32 processors. As hundreds of thousands of BISON simulations are needed during Markov Chain Monte Carlo (MCMC) sampling, running BISON directly is not a viable solution. Therefore we propose to use Kriging-based metamodels to replace BISON during MCMC sampling. Surrogate model is an approximation of the input/output relation of a computer code/model. It is also called metamodel, response surface, emulator. Surrogate models usually take much less computational time than the original model (like BISON) while maintaining the input/output relation of the original model to a desirable accuracy. Constructing the metamodels normally requires small number of executions of the original model. Once validated, metamodels can be used to perform uncertainty and sensitivity analysis, Bayesian calibration, optimization, etc.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Convection effects on Skylab experiments M551, M552, and M553, phase C report

This report described an analysis of Skylab Experiments M551 (Metals Melting), M552 (Exothermic Brazing), and M553 (Sphere Forming). The primary objective is the study of convection in the molten metals and their attendant solidification theory. Particular attention is given to clarifying the effects of reduced gravity on molten metal flow and solidification. Based on an analysis of physical forces and solidification theory expected for ground-based and Skylab processing, low-g variations were predicted for each experiment. A comparison was then made with the Skylab results available to date. Both metallurgical analyses of other investigators and movies of ground-based and Skylab samples were utilized. Several low-g variations in Skylab processed materials were successfully predicted based on expected variations in physical forces and fluid convection. The same analysis also successfully predicted several features in the Skylab-processed materials which were identical to terrestrially-processed materials. These results are summarized in the conclusion section for each experiment.

Bourgeois, S. V.↗

Electron microscopy analyses and electrical properties of the layered Bi{sub 2}WO{sub 6} phase

The bismuth tungstate Bi{sub 2}WO{sub 6} was synthesized using a classical coprecipitation method followed by a calcination process at different temperatures. The samples were characterized by X-ray diffraction, simultaneous thermogravimetry and differential thermal analysis (TGA/DTA), scanning and transmission electron microscopy (SEM, TEM) analyses. The Rietveld analysis and electron diffraction clearly confirmed the Pca2{sub 1} non centrosymmetric space group previously proposed for this phase. The layers Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} have been directly evidenced from the HRTEM images. The electrical properties of Bi{sub 2}WO{sub 6} compacted pellets systems were determined from electrical impedance spectrometry (EIS) and direct current (DC) analyses, under air and argon, between 350 and 700 °C. The direct current analyses showed that the conduction observed from EIS analyses was mainly ionic in this temperature range, with a small electronic contribution. Electrical change above the transition temperature of 660 °C is observed under air and argon atmospheres. The strong conductivity increase observed under argon is interpreted in terms of formation of additional oxygen vacancies coupled with electron conduction. - Graphical abstract: High resolution transmission electron microscopy: inverse fast Fourier transform giving the layered structure of the Bi{sub 2}WO{sub 6} phase, with a representation of the cell dimensions (b and c vectors). The Bi{sub 2}O{sub 2}{sup 2+} and WO{sub 4}{sup 2−} sandwiches are visible in the IFFT image. - Highlights: • Using transmission electron microscopy, we visualize the layered structure of Bi{sub 2}WO{sub 6}. • Electrical analyses under argon gas show some increase in conductivity. • The phase transition at 660 °C is evidenced from electrical modification.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Improved instrumentation for intensity-, wavelength-, temperature-, and magnetic field-resolved photoconductivity spectroscopy

We report instrumentation for photovoltage and photocurrent spectroscopy over a larger continuous range of wavelengths, temperatures, and applied magnetic fields than other instruments described in the literature: 350 nm≤λ≤1700 nm, 1.8 K≤T≤300 K, and B≤9 T. This instrument uses a modulated monochromated incoherent light source with total power<30 μW in combination with an LED in order to probe selected regions of non-linear responses while maintaining low temperatures and avoiding thermal artifacts. The instrument may also be used to measure a related property, the photomagnetoresistance. We demonstrate the importance of normalizing measured responses for variations in light power and describe a rigorous process for performing these normalizations. We discuss several circuits suited to measuring different types of samples and provide analysis for converting measured values into physically relevant properties. Uniform approaches to measurement of these photoproperties are essential for reliable quantitative comparisons between emerging new materials with energy applications. - Highlights: • A novel instrument for measuring photoconductivity and photocurrents of materials and devices. • Continuous parameter space: 350 nm≤λ≤1700, 1.8 K≤T≤300 K, and B≤9 T. • Methodology for treating non-linear responses and variable lamp intensity. • Mathematical detail for extracting properties of materials from measured values is provided.

36 MATERIALS SCIENCE↗

Impact of Controlled Storage Conditions on the Hydrolysis and Surface Morphology of Amorphous-UO 3

The hydration and morphological effects of amorphous (A)-UO 3 following storage under varying temperature and relative humidity have been investigated. This study provides valuable insight into U-oxide speciation following aging, the U-oxide quantitative morphological data set, and, overall, the characterization of nuclear material provenance. A-UO 3 was synthesized via the washed uranyl peroxide synthetic route and aged based on a 3-factor circumscribed central composite design of experiment. Target aging times include 2.57, 7.00, 14.0, 21.0, and 25.4 days, temperatures of 5.51, 15.0, 30.0, 45.0, and 54.5 °C, and relative humidities of 14.2, 30.0, 55.0, 80.0, and 95.8% were examined. Following aging, crystallographic changes were quantified via powder X-ray diffraction and an internal standard Rietveld refinement method was used to confirm the hydration of A-UO 3 to crystalline schoepite phases. The particle morphology from scanning electron microscopy images was quantified using both the Morphological Analysis of MAterials software and machine learning. Results from the machine learning were processed via agglomerative hierarchical clustering analysis to distinguish trends in morphological attributes from the aging study. Significantly hydrated samples were found to have a much larger, plate-like morphology in comparison to the unaged controls. Predictive modeling via a response surface methodology determined that while aging time, temperature, and relative humidity all have a quantifiable effect on A-UO 3 crystallographic and morphological changes, relative humidity has the most significant impact.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Analysis of high field effects on the steady-state current-voltage response of semi-insulating 4H-SiC for photoconductive switch applications

A model-based analysis of the steady-state, current-voltage response of semi-insulating 4H-SiC is carried out to probe the internal mechanisms, focusing on electric field driven effects. Relevant physical processes, such as multiple defects, repulsive potential barriers to electron trapping, band-to-trap impact ionization, and field-dependent detrapping, are comprehensively included. Results of our model match the available experimental data fairly well over orders of magnitude variation in the current density. A number of important parameters are also extracted in the process through comparisons with available data. Finally, based on our analysis, the possible presence of holes in the samples can be discounted up to applied fields as high as ∼275 kV/cm.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗