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At least 631 records · Page 35
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Focused Ion Beam analysis of non radioactive samples [PowerPoint]

The presentation includes various images to illustrate the analysis. Helios G4 Plasma FIB: Xe ion columns mills material 30 times faster than Ga; Options include: Energy Dispersive Spectroscopy (EDS), Wavelength Dispersive spectroscopy (WDS) Electron backscattered Diffraction (EBSD), Time of Flight Sims (ToF SIMS), Inert gas/vacuum sample transfer system; Excels at micromachining and collecting 3D datasets using various detection systems.

42 ENGINEERING↗
DOE OSTI2021

Examination of Intergranular Crack on SC0234

The microstructure of the SC0234 weld was evaluated per DA-SPEC-01067, ''General Purpose Heat Source (GPHS) Plutonium-238 Dioxide Fueled Clad Product Specification'' and it was determined that the weld microstructure conformed to the quality requirements. During the examination of weld cross section, the metallographic analysis revealed the presence of a surface crack. Prior visual examination per RPS-TA55-303 had not revealed the crack, nor did the surface photography performed per RPS-TA55-302. The presence of the crack does not violate any of the product specifications called out on DA-SPEC-01067. Although there is a well-documented history of weld hot crack susceptibility in the early development of the DOP-26 iridium alloy, a surface crack such as this had not been documented during welding at Los Alamos. In the interest of better understanding the cause; the product engineer/program recommended further examination of the crack. This report discusses the examination of the crack found in the weld cross section of simulant clad SC0234. Metallography, Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy techniques (EDS) where used in the analysis of the crack and the surrounding weld microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2021

High Throughput In-Line Coating Metrology Development for Solid Oxide Fuel Cell Manufacturing

Coatings play key roles in solid oxide fuel cell (SOFC) stack durability. For example, diffusion barrier coatings on Cr-containing interconnect and balance of plant (BOP) components protect electrodes from Cr poisoning over the long operational lifetimes (>10,000 hours) of the fuel cell stack. Common defects in coatings, such as cracks, pinholes, and porosity, result in a failure to protect the electrodes, resulting in shorter operational lifetime and thus higher cost. It is very unlikely, even in the best coating process, that all these defects can be mitigated, hence identifying critical defects in parts, and removing defective parts from production before they can damage the stack, becomes paramount. Furthermore, these quality control techniques must be operational in the production/assembly line (in-line), i.e., high throughput and non-destructive, and cost effective. Redox Power Systems, LLC (Redox) together with the National Renewable Energy Laboratory (NREL) developed much needed high throughput, in-line metrology techniques for protective coatings. The overall goal of the project is to lower cost while increasing robustness, reliability, and endurance of SOFC stacks. To accomplish this, we had several objectives, including: to identify key coating and substrate defects that lead to coating failure through the use of detailed characterization methods (e.g., microscopy, XRD, EDS, electrochemistry); to assess capabilities of in-line metrology techniques, e.g., optical profilometry (Redox) and thermography (NREL), to probe these defects, or evidence thereof; demonstrate long-term performance of “defect-free” protective coatings, as identified by in-line metrology, in solid oxide fuel cell (SOFC) stack operation. In the first part of this project, the ability to identify key defects expected to lead to coating and SOFC degradation using in-line metrology tools were evaluated. Coated interconnect samples with controlled defect types and populations were tested under conditions similar to SOFC operation, followed by detailed post-test analysis to reveal the defects responsible for observed degradation. In the second part of the project, the optimal in-line metrology techniques and methodologies were used to map the defect distribution in full-size interconnects with critical defects intentionally allowed to exist in some cases. These interconnects underwent SOFC testing for extended periods (up to ~3,000 hours) followed by post-test analysis to evaluate the effectiveness of in-line metrology techniques in mitigating MCO coating related degradation. Key accomplishments in this project included the following: Demonstrated ASR of < 0.05 ohm-cm 2 at 650 °C for 1,000 hours with low defect (determined by in-line metrology) interconnect samples (average ASR=37 milliohms-cm 2 after over 1,000 hours). Demonstrated that low defect coatings on interconnects (as screened using in-line metrology) have low volatilization of chromium at ~650 °C for 1,000 hours as detected using Cr-getter material (< 5 at% increase above baseline); 1022 hour duration tests under humidified, elevated temperature (750 °C rather than 650 °C) compared a base case against different coating thicknesses. Demonstrated capability to identify initial key defects of interest with in-line metrology techniques using up to 8 cm by 10 cm having coatings with and without intentional defects of interest using thermal imaging and optical profilometry. Correlated key defects identified using metrology techniques with observed coating performance (e.g., ASR and Cr volatility). Conducted several 4 cm by 4 cm cell tests using MCO-interconnects that were pre-screened using some of the metrology techniques developed in the project (e.g., optical profilometry). An analysis of ASR measurements were able to show that defect-free coatings resulted in the anticipated performance in the cell tests.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2021

Wear in particle based CSP systems from particle abrasion and attrition at high temperature

High temperature particle-based receivers offer distinct advantages over conventional molten salt receivers due to their ability to achieve temperatures above 700 ºC, direct absorption of solar energy as they fall through a beam of concentrated sunlight, and the relative ease of storage (and retrieval using a secondary working fluid) in insulated storage tanks. The use of particles, however, also raises concerns with material degradation from the flow of hot or cold particles through discharge hoppers or along the inner receiver surfaces and other system components (e.g. tubes, valves etc.), depending on operating mode of the receiver. The flow of particles over surfaces may result in loss of material from abrasive wear, impact erosion from impingement under gravitational fall and particle attrition as particles fall and move on top of each other. In the present study, the performance of candidate materials and particles were evaluated through a series of abrasion erosion and particle attrition experiments at room temperature as well as at 800 °C. Candidate materials were subject to abrasive wear from particles at low particle to material velocities inside a resistance heated kiln, and analyzed for changes in mass and surface morphology using cross-sectional scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) tests. The wear rate for different specimens was noted to be largely driven by the strength of chromia scales built on the specimens from exposure to high temperature. Particle attrition measurements explored the susceptibility of particles to breakdown from particle to particle interaction and the generation of fines from this process. At the low velocities expected in particle based CSP plants, the particles tested exhibited near negligible breakdown. However, changes in the particle hardness at 800 ºC resulted in a significantly higher particle breakdown to sizes <40 microns raising potential environmental concerns. In addition to particle breakdown, it was also noted that the sample had oxides from the stainless steel test setup mixed in with the particles. Similar oxides can be expected to turn up in the utility scale particle based CSP plants as well. The presence of oxide was also noted to affect the solar absorptivity of the mixture compared to a clean initial specimen, potentially resulting in a change in the overall efficiency of the CSP plant.

14 SOLAR ENERGY↗
DOE OSTI2021

Deformation Mechanism of Age Hardened Alloy 709 Materials

This report provides an in-depth study of the microstructures of creep-deformed Alloy 790 materials. Five specimens, all creep-tested at 600°C under 330 MPa to failure, were investigated. The creep specimens were machined from plates fabricated by different melt practices, Argon Oxygen Decarburization (AOD), or AOD followed by Electroslag remelting (ESR), and different heat treatments: 1100 or 1150°C Solution Anneal (SA), and some with additional Precipitation Treatment (PT) of 775°C for 10 hours. TEM samples were made from the gauge and the grip sections of each creep-deformed specimen. Bright-field (BF) imaging, high-angle annular dark field (HAADF) imaging, and energy dispersive x-ray spectroscopy (EDS) using a scanning transmission electron microscope (STEM) were carried out on all the samples.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2021

Hospice Landscape Report

In July 2018, CMS requested assistance from Oak Ridge National Laboratory (ORNL) to provide expert data science support aimed at developing algorithms for data mining of medical data for operational and payment purposes. The project is intended to be exploratory: work is aimed at alleviating challenges associated with improper payments, specifically audit methodologies and targeting and changes to risk scores. Project goals include developing new, sophisticated methods for audit targeting and improved profile– payment error correlations, specifically focused on Medicare Part C, the program under which MAOs provide health care services to beneficiaries. ORNL conducted RADV analyses against RAPS and EDS data as well as a hospice landscape analysis per a January 2015 dataset that included Medicare beneficiaries who were in hospice in 2017 and 2018. Ongoing work under this project also involves development of predictive models for RADV investigations and hospice landscape.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2021

Intentional Uranium Tagging for Material Provenance and Pathway Forensics (LA19-Intentional-Forensics-NDD3Bb) (Annual Report for FY21)

This report describes the outcomes of the third and final year of a project to research the feasibility of tagging uranium materials, especially nuclear fuels. The experimental focus remained on metallic uranium forms under prospective surface and bulk tagging scenarios. Overall, the results showed that the tags could be successfully imparted and characterized in both as-built and degraded conditions. This was in line with expectations coming into this project, indicating promise for both surface and bulk tagging of metallic forms of uranium. Multiple surface tagging techniques and detection strategies were explored in FY21, with an emphasis on improving tag quality, readability, and detection in the field. Non-radioactive materials were used as a testbed. Selective deposition via laser beam was determined to be successful in imparting a readable titanium deposit on a stainless steel base plate, and can be read with high resolution characterization techniques (e.g., scanning electron microscopy) and field capable tools (e.g., eddy current testing). Other deposition techniques, such as selective deposition via electron beam and photoluminescent tags, were explored in FY21, and while success for these techniques would be dependent on additional work, these techniques showed potential for surface tagging applications. To survey bulk taggant elements for bulk uranium metal, 16 tagging elements were spread among 18 depleted uranium castings (4 baseline, 3 mix, 1 dilution, and 10 recycle). Most of these were made and characterized in FY21. Taggant acceptability was based upon manufacturability, detectability, and persistence from the standpoint of two detection options: bulk chemical analysis (for “chemical taggants”) and microstructural analysis (for “second phase taggants”). Taggant detection in both up-front manufacturing and in the face of “degradations” such as dilution, mixing, and recycling was generally good. Two independent laboratories carried out chemical analysis on most of the castings, and often at several locations within a casting, and the results are discussed. Scanning electron microscopy+EDS microanalysis revealed the second phases mostly contained the expected tagging elements. The shapes and 2 spatial distributions of these micron-sized carbides, oxides, and intermetallic particles offers opportunities for further science-based investigation and tagging optimization. Overall, V and Co currently appear as the best choices for chemical taggants while Al, Ti, Mn, Co, Pd, and Tb all look good as second phase taggants. The other elements considered here – Sc, Ni, Ge, Nb, Ce, Ta, W, Ir, and Au – while not being ruled out, require more study to become viable options. It is of special note that in the recycling study only one of the 12 elements fell out of detection even after 10 meltings, demonstrating their persistence. An Appendix tabulates all chemical analysis results to enable more quantitative and statistical studies of detection opportunities and limitations, as a part of a related project.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Reassessing the Market—Computation Interface to Enhance Grid Security and Efficiency

The goal of this project is to reconsider core market and reliability processes that can potentially yield to transformative advances in power grid security, reliability, and efficiency. Current electric power market designs are strongly a function of computing capabilities and limitations that were available in the mid-to-late 1990s, circa deregulation. This includes constructs such as: (1) a 2-tiered day-ahead/real-time market construct; and (2) linearized (“DC”) real power flow approximations in dispatch and pricing. At that time, state-of-the-art computational capabilities could at the limit address deterministic mixed-integer programming formulations of unit commitment (UC) and linear programming formulations of economic dispatch (ED) at limited fidelity and scale. Such constraints forced limited look-ahead time-horizons, crude approximations of AC power flow physics and operations, and artificial partitioning between day-ahead markets, hour(s)-ahead reliability processes, and real-time markets. Consequently, these limitations have resulted in limited security and reliability with increasing out-of-market payments, particularly as uncertainty associated with renewables and distributed energy resources grows.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2022

Synthesis and Characterization of Silicon Carbide Ceramic Composites with CeO 2 Powder

This study pioneers the fabrication and characterization of silicon carbide (SiC) containing cerium dioxide (CeO 2 ). CeO 2 powder was tested as a surrogate for actinide oxide waste forms such as uranium dioxide (UO 2 ) and plutonium dioxide (PuO 2 ). Several syntheses were evaluated with varying amounts of preceramic polymer (SMP-10 resin) and CeO 2 containing either SiC fiber, carbon fiber, or no fibers. Scanning electron microscopy (SEM) was used to characterize morphology and compositional differences, and energy-dispersive x-ray spectroscopy (EDS) was used to provide semiquantitative elemental analysis. In addition, each sample was characterized by density, powder x-ray diffraction (pXRD), and Raman spectroscopy. Samples containing nearly more than four times CeO 2 powder than SMP-10 resin by mass had the best properties. This research establishes a unique synthesis for SiC containing high concentrations of CeO 2 powder to illustrate how it may be managed as a potential waste form.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Development of Quantum Computing Interconnect Based on Aerosol Jet Printing and Electrochemical Deposition of Rhenium

The electrodeposition of rhenium on to a metal seed layer on flexible substrates is presented as a means to creating superconducting flexible cable connectors in an enabling plug-and-play approach for quantum computing. Cryogenic quantum electronics are currently connected using masses of stainless-steel coaxial cables that are bulky, rigid - both in form and design - and lead to significant joule heating, thermal noise, and cross talk. Here, we present an unprecedented approach to integrate an aerosol jet printed (AJP) metal seed layer with rhenium electrodeposition on a flexible substrate in the advancement of superconducting interconnect technologies. Silver and gold were printed using the ‘Nanojet’ aerosol jet printer on Kapton films. Adhesion of gold was found to be far superior to that of silver and adhesion on roughened Kapton surpassed that of its smooth counterpart. Electrodeposition of rhenium was successful on both silver and gold and an amorphous Re film was confirmed by XRD. Results for both materials are presented however due to the poor adhesion of silver to Kapton it was ruled out as a viable candidate. Composite materials were characterized by profilometry, EDS, XRD and FIBSEM. Electrical measurements of the composite at ambient temperature showed a critical temperature (T c ), where the resistance drops to 0, of 5.8 K, well above 4.2 K, the temperature of liquid helium. Stress-strain tests of the Ag-Re and Au-Re composites on roughened and smooth Kapton were completed. Cyclic flexure testing (200 cycles) to 1.25% strain showed smooth Kapton samples reach a stress of ~16 MPa, while Kapton roughened with sandpaper, reaches ~20MPa of stress for the same 1.25% strain.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The study of local overheating and plasma formation on stainless steel z-pinch targets

Plasma formation from intensely ohmically heated conductors is known to be highly non-uniform, as local overheating can be driven by micron-scale imperfections. Detailed understanding of plasma formation is required to predict the performance of magnetically driven physics targets and magnetically-insulated transmission lines (MITLs). Previous LDRD-supported work (projects 178661 and 200269) developed the electrothermal instability (ETI) platform, on the Mykonos facility, to gather high-resolution images of the self-emission from the non-uniform ohmic heating of z-pinch rods. Experiments studying highly inhomogeneous alloyed aluminum captured complex heating topography. To enable detailed comparison with magnetohydrodynamic (MHD) simulation, 99.999% pure aluminum rods in a z-pinch configuration were diamond-turned to ~10nm surface roughness and then further machined to include well-characterized micron-scale "engineered" defects (ED) on the rod's surface (T.J. Awe, et al., Phys. Plasmas 28, 072104 (2021)). In this project, the engineered defect hardware and diagnostic platform were used to study ETI evolution and non-uniform plasma formation from stainless steel targets. The experimental objective was to clearly determine what, if any, role manufacturing, preparation, or alloy differences have in encouraging nonuniform heating and plasma formation from high-current density stainless steel. Data may identify improvements that may be implemented in the fabrication/preparation of electrodes used on the Z machine. Preliminary data shows that difference in manufacturer has no observed effect on ETI evolution, stainless alloy 304L heated more uniformly than alloy 310 at similar current densities, and that stainless steel undergoes the same evolutionary ETI stages as ultra-pure aluminum, with increased emission tied to areas of elevated surface roughness.

36 MATERIALS SCIENCE↗
DOE OSTI2022

DISTRIBUTION OF ION-EXCHANGEABLE RARE EARTH ELEMENTS AND CRITICAL MINERALS IN COAL-HOSTED CLAYS OF THE POWDER RIVER BASIN, WY

Increasing demand for a more robust domestic supply of rare earth elements (REE) and critical minerals (CM) has led to significant investigation into unconventional sources. Coal and coal byproducts from the Powder River Basin (PRB) of Wyoming are potential sources of REE but lack complete characterization of mineral hosts including ion-adsorption clays (IACs). IACs, which provide a substantial portion of the global REE supply, form when hydrated REE complexes are physiosorbed to negatively charged sites on clay surfaces. Typical IAC minerals include kaolinite, illite, and smectite. REE complexes are easily leached from IACs via ion exchange, making them economically attractive. However, research regarding the partitioning behaviors of strategic metals into PRB coal-hosted clays is limited. This project aims to quantify the modes of occurrence and distribution of REE and CM in clay minerals derived from PRB coals. Strategic metals investigated in this project have historic production or promising deposits within the PRB and/or high anticipated supply risk, and include: REE (lanthanides and Y), V, Ti, platinum group elements (PGE; Pt, Pd, Rh, Ru, Ir, Os), Al, Co, Ga, Zr, and W. Semi-quantitative compositional data from portable x-ray fluorescence spectroscopy (pXRF) on coal core from the PRB is consistent with the known correlation between REE and Al content, suggesting increased REE abundance will be found in clay-rich units. pXRF data also identifies elevated V, Ti, Co, and Zr correlated with Al. Preliminary x-ray diffraction (XRD) data indicates kaolinite, illite, and dickite are abundant minerals in overburden and clay-rich partings. Quantitative analysis via inductively coupled plasma mass spectrometry (ICP-MS) provides insights into REE and CM fractionation in coals as we compare trace metal occurrence to variations in mineralogy. Additionally, we apply scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) data to correlate clay size and morphology to trace metal occurrence. Our findings supplement a broader effort to couple REE and CM extraction with existing domestic coal production and contribute to the fundamental understanding of adsorption processes that occur in low-temperature basin environments.

Stuart, Sophia↗
DOE OSTI2022

Survey of the Worldwide Supply Chain of Commodities Needed for a Quantum Technology Program

Quantum Information Science (QIS) is an emerging technology being pursued by fundamental science research groups worldwide, as well as commercial companies and government programs. There are a variety of QIS disciplines, including quantum computing, quantum sensing and quantum encryption. Some of the commodities needed for a robust quantum laboratory are particular to quantum phenomenon, but in general the equipment needed is similar to that needed for a typical high - technology lab (e.g. oscilloscopes, lasers, vacuum chambers, etc.). This study focuses on identifying commodities manufactured worldwide that would be needed for a robust quantum lab. The authors' own knowledge of needed equipment and primary vendors was used as a starting point, follow ed by extensive internet searching and utilization of buyer's guides to create a large spreadsheet of most of the components needed, the company offering the components, and country of manufacture. With this extensive spreadsheet, stakeholders can identify commodities that would be needed for a quantum lab oratory and potentially identify market choke points.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗
DOE OSTI2022

Reduced diffusion and enhanced retention of multiple radionuclides from pore structure characterization of barrier materials for enhanced repository performance

Fluid flow and chemical transport in porous media are the macroscopic consequences of pore structure, which integrates geometry (e.g., pore size and surface area, pore-size distribution) and topology (e.g., pore connectivity). Low-permeability geological media whose pores are poorly interconnected will exhibit the characteristics of anomalous diffusion and sample size-dependent effective porosity, which will strongly impact long-term net diffusion and retention of radionuclides in geological repository settings involving different host rocks and barrier materials. A suite of innovative and complementary experimental approaches is utilized to study the microscopic pore structure and macroscopic fluid flow & chemical transport for a range of host rocks and barrier materials, in addition to standard clay minerals and reference rocks. With a particular focus on quantifying the presence and magnitude of “isolated” pores for a reduced effective porosity in low-permeability geomedia, the integrated methodologies for basic properties and pore structure characterization of these geomedia include X-ray diffraction, thin section petrography, grain size distribution, water immersion porosimetry after vacuum-pulling for full saturation, mercury intrusion porosimetry, nitrogen physisorption, scanning electron microscopy, X-ray computed tomography, and (ultra-)small angle neutron (X-ray) scattering. In addition, custom-designed gas diffusion, tracer recipe involving a range of anionic and cationic chemicals with subsequent analyses by laser ablation and inductively coupled plasma-mass spectrometry, along with batch sorption, column transport, and imbibition tests were conducted for coupled effects of pore structure and chemical retention/transport. From the perspectives of pore structure in conjunction with multiple and complementary approaches to examining a range of sample sizes under different observational scales, we find that the poor pore connectivity is prevalent in low-permeability media (mudstone and crystalline rock) that is related to geological processes (e.g., compaction, diagenesis and thermal maturation). For example, the deep and organic matter-rich mudstones have a much smaller effective porosity than the total porosity (as a result of poor pore connectivity) and associated diffusion coefficient, and the effective porosity & diffusion coefficients are also dependent upon the sample sizes used in the measurement. Similarly, most of the pore space in the shallow mudstone is also controlled by pore-throat diameters in the 5-50 nm range of intergranular pore types from its fine-grained nature, but with an overall good pore connectivity. However, the nm-sized pore space (physically pore-network architecture) and strong sorption capacities (chemical retention from clay minerals) of both shallow and deep mudstones lead to the synergistic retention of cationic radionuclides and their utilities as effective host rocks and barrier materials. Our unique approaches of studying how the micro-scale pore structure affect macro-scale fluid flow, diffusion & retention, and chemical transport produce improved mechanistic understanding, and realistic quantification, of diffusion and retention of typical radionuclides in a range of generic host rocks and barrier materials (clay/shale, salt, crystalline rock, and tuff), with the overall results leading to scientifically-based understanding of enhanced isolation (from both diffusion and retention) of radionuclides and improved confidence on the long-term performance of geological repository to store high-level radioactive wastes. In addition to the training of 25 undergraduates, graduates, and postdocs of UTA, the scientists (organizations) involved in performing this work (e.g., discussion, sample sharing, and operation of SANS and SAXS instruments) include Ed Matteo, Yifeng Wang, and Kristopher Kuhlman (Sandia National Laboratories), Jens Birkholzer, Liange Zheng, Tim Kneafsey, and Sharon Borglin (Lawrence Berkeley National Laboratory), Mavrik Zavarin (Lawrence Livermore National Laboratory), Yukio Tachi and Yuta Fukatsu (Japan Atomic Energy Agency), Mieke de Craen (Euridice, Belgium), Markus Bleuel (NIST), Wei-Ren Chen, Gergely Nagy, Changwoo Do, William Heller, Larry Anovitz, and Kenneth Littrell (ORNL), as well as Jan Illvsky, Ivan Kuzmenko, Ju-Sang Park and Jon Almers (ANL). Key deliverables include a total of 13 peer-reviewed journal articles (nine published and three under review), 23 presentations at scientific conferences (AAPG, AAPG Southwest Section, AGU, Asian Clay Conference, GSA, GSA South-Central Section, IHLRWM, InterPore, International Conference on Chemistry and Migration Behavior of Actinides and Fission Products in the Geosphere, International Conference on Coupled Processes in Fractured Geological Media: Observation, Modeling and Application), and academic institutions (UTA, New Mexico State University; University of Poitiers, France; University of Helsinki, Finland; Uppsala University, Sweden; Istanbul Technical University, Turkey) and other organizations (Andra, France; Posiva Oy, Finland).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Field Testing of Self-Healing Metallic Coatings for Internal Corrosion Protection of Natural Gas Pipelines

Internal corrosion occurs in natural gas pipelines primarily due to the presence of water, carbon dioxide, and hydrogen sulfide. Internal corrosion can eventually result in leakage, cracks, and rupture of the pipeline. The objective of this work is to mitigate internal corrosion in steel pipelines transporting natural gas using cold spray coatings. The corrosion behavior of carbon steel coated with self-healing zinc chromium (ZnCr) and zinc niobium (ZnNb) cold spray coatings was investigated in a natural gas environment. For comparison purposes, hot-dip galvanized steel (HDGS) was tested under the same conditions as cold spray coatings. The field test was performed at the NW Natural gas storage facility in Mist, Oregon. The field test was conducted in a 6-inch diameter pipe transporting wet natural gas out of an underground storage well at 500 psi and 4.4 °C. The coupons were tested for 15 and 32 days under stagnant and flow conditions, respectively. Weight loss method was used to measure the corrosion rate of metallic coatings. Post-corrosion surface characterization was performed on the specimen using a scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS). Crystalline phases were determined by X-ray diffraction (XRD). The field-test results confirmed that the metallic coatings provided corrosion protection of carbon steel exposed to wet natural gas under stagnant and flow conditions. The formation of the ZnCO 3 layer on top of ZnNb and ZnCr coatings led to passivation of the coatings which helps to reduce the self-corrosion. These layers form a barrier for diffusion of corrosive species to the surface.

03 NATURAL GAS↗
DOE OSTI2023

Study on Electrostatic Separation of Quinoline Insolubles from Coal Tar Pitch

The feasibility of electrical separation in the removal of quinoline insoluble (QI) particles from coal tar pitch (CTP) was experimentally investigated. QI particle involvement prohibits the effective fabrication of high-quality value-added products, such as carbon fibers, from CTP. A substantial and sustainable CTP market exists around the world; therefore, a strong incentive exists to develop a viable technical approach to effectively and economically remove QI particles from CTP. The electrical separation method shows promise to achieve this technical goal (Cao et al., 2012). Even with the given setup (wire- cylinder adapted), critical issues remain to be addressed for this method to be applicable to the CTP: (1) identifying the wash oil used in the original QI separation, (2) understanding the mechanism of QI separation, (3) characterizing the deposit, and (4) identifying the QI. This study integrated a set of experimental and analysis techniques into the electrical separation tests to address the aforementioned issues. Key findings are as follows: 1. Electric current responses: • The electric current level of the CTP–wash oil solution reported by Cao et al. (2012) can be attained by using a mixture of 25% quinoline and 75% toluene for the CTPs examined in this study under the same electrical load condition. • The electric current tends to decrease during the test period because of the decreasing number of charged particles. • The reversed field corresponded to the configuration of electrostatic precipitation for positive corona discharge. The high electric field can result in dielectric breakdown and lead to an abrupt current surge. 2 Deposit response and solvent candidates: • Deposit of particles in CTP mixture can be effectively implemented in a wire-cylinder configuration as proposed and examined in this study. • Deposit depends on the solvents. Among the solvents tested, two- and three-part solvents that included quinoline and ethanol (i.e., 25% quinoline and 75% toluene; 50% quinoline and 50% toluene; and 33% wash oil, 33% BTX, and 34% ethanol) produced the highest deposit weight. • The deposit process examined in this study is derived from the charged particles. An appreciable relation exists between deposit weight and electric charge. 3. QI removal efficiency (RE): • The RE of the electrostatic separation can reach as high as 76.2% for Carbores, and 61.6% for Koppers. • The RE can be further enhanced if the field level increases from 0.16 kV/mm that was used in the current study to 0.23 kV/mm, according to the relation established between the RE and the electric field. 4. Testing of the modeling system: • The motion of particles is originally driven by the charge-based electric force in the cases tested. The solid particle separation mechanism is similar to that of QI deposition in CTP. • The mechanical movement of solid particles can be strongly affected by the gravitational and viscous forces in the electric field. 5. EDS analysis and chemical compositions: • The main chemical composition of deposit QI matches that of as-prepared CTP QI. The deposit QI is derived from the same group of the CTP QI. • In addition to carbon, the QI contains oxygen, sodium, aluminum, silicon, iron, and sulfur. The work for the near future is also discussed.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2023

Improving Nb3Sn Cavity Performance Using Centrifugal Barrel Polishing

Nb3Sn superconducting radiofrequency (SRF) cavities have been an ongoing research topic for many years motivated by the potential for higher accelerating gradients and quality factors compared to niobium SRF cavities. The highest performing Nb3Sn cavities are manufactured using tin vapor-diffusion coating, which creates a Nb3Sn film with a surface roughness of around 100-200 nm. This is thought to be one of the limiting factors for the accelerating gradient of Nb3Sn cavities due to enhancement of magnetic field near sharp surface features. To smooth Nb3Sn SRF cavities, we have developed a mechanical polishing procedure which uses centrifugal barrel polishing to smooth the surface followed by a secondary tin coating step to repair the surface. We show that the accelerating field of a Nb3Sn SRF cavity is improved by applying this procedure. We also investigate the quench mechanism of the polished cavity by utilizing temperature mapping to measure which regions of the cavity e xperience heating during RF operation. We then cut samples from these regions and analyze the film microstructure and chemical composition in 3D using EDS and EBSD measurements together with a focused ion-beam (FIB) tomography technique.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2023

Scaling from Flux Towers to Ecosystem Models: Regional Constraints on Carbon Cycle Processes from Atmospheric Carbonyl Sulfide (Final Report)

DOE supported research suggests that gross primary productivity (GPP) is largely underestimated by global earth system models [Welp et al., 2011], reflecting the persistent challenge in extrapolating from local-scale GPP observations to global-scale earth system models. This poor understanding of GPP at large spatial scales is of particular concern in tropical forests. In tropical forests, some earth systems models forecast a powerful feedback between a warming climate and a decline in GPP resulting in forest dieback. While this simulated feedback is intensely debated, we lack robust large-scale constraints on GPP that are needed to resolve this debate. In particular, carbon dioxide measurements provide valuable information on net carbon flux, but not on the gross flux associated with GPP. Here we conducted a study of regional-to-global scale GPP using atmospheric carbonyl sulfide to provide a new constraint on GPP mechanisms in earth system models. Our project activities integrated modeling, in situ measurement, and remote sensing techniques to resolve GPP for the Amazon as well as global scale trends. The results of this work included initiating airborne carbonyl sulfide monitoring in the Amazon, training for postdocs and graduate students at a Hispanic Serving Institution, fundamental advances in carbonyl sulfide budgets [e.g. Hilton et al., Nature Climate Change, 2017], and high-profile publications that focused on GPP trends for the Amazon [Stinecipher et al., GRL, 2022] and global historical GPP trends [Campbell, et al., Nature, 2017]. Based on the suggestion of our DOE program manager, we published a state-of-the-science commentary to the scientific community on GPP monitoring with COS [Campbell et al., EOS, 2017] which was selected as the cover story. DOE support was acknowledged in all reports. The importance of this research to understanding climate change was communicated to the general public through community seminars (Rotary, Public Libraries, State Parks), an op-ed (SF Chronicle), and interviews in the mass media including two stories in the New York Times (4/5/17; 7/30/18), one of which was especially widely read after it was featured in the New York Time’s Quote of the Day.

54 ENVIRONMENTAL SCIENCES↗