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DOE OSTI2025

Formation trajectories of solution-processed perovskite thin films from mixed solvents

The engineering of mixed-solvent formulations and their evaporation conditions are key to reproducible perovskite coatings for high-performance photovoltaics. Here, we report a lumped-parameter evaporation model to predict the evolution of a perovskite ink liquid film over time (solvent ratio, solute concentration, and film thickness). The drying-rate model is validated via in situ film-thickness measurements, and the predicted transient liquid film state is mapped as a process path. These methods allow for the prediction of process sensitivity to local environmental factors and the understanding and visualization of a broader processing parameter space enabled through the coupling of process and ink engineering. Process maps are applied to create a new framework for scalable perovskite coating development with a goal of improving the reproducibility and transferability of perovskite fabrication. This approach is demonstrated with blade-coated FA 0.83 Cs 0.17 PbI 3 photovoltaic devices, improving the photovoltaic conversion efficiency from 17.5% ± 1.7% to 20.3% ± 0.6%.

14 SOLAR ENERGY↗

DOE OSTI2021

High-Performance Catalytic Four-Channel Hollow Fibers with Highly Dispersed Nickel Nanoparticles Prepared by Atomic Layer Deposition for Dry Reforming of Methane

In this study, highly dispersed nickel (Ni) nanoparticles (NPs) with an average particle size of 4.3 nm were uniformly deposited on the outer surface, the inner channel surface, and inside the pores of 20-cm long 4-channel α-Al 2 O 3 hollow fibers (HFs) by atomic layer deposition (ALD) for dry reforming of methane (DRM). Cerium oxide (CeO 2 ) was added to promote the catalytic performance of Ni/Al 2 O 3 -HF catalysts. Rationally designed filling methods, by tuning the reactor size and inert fillings, can reduce the catalyst bed voidage in a fixed bed reactor for better reactant gas distribution, effectively utilize the Ni reactive sites, and achieve excellent catalytic performance. It was found that the CeO 2 -promoted Ni/Al 2 O 3 -HF catalyst was highly active and highly stable without deactivation during an overall 400-hr DRM test at 850 ºC. CeO 2 with reversible valence states could participate in surface reactions; especially, the formation of CeAlO 3 provided sufficient surface Ce 3+ for CO 2 activation and enhanced the stability and reusability of the HF catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Decontamination of SARS-CoV-2 and Other RNA Viruses from N95 Level Meltblown Polypropylene Fabric Using Heat under Different Humidities

In March of 2020, the World Health Organization declared a pandemic of coronavirus disease 2019 (COVID-19), caused by the severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2). The pandemic led to a shortage of N95-grade filtering facepiece respirators (FFRs), especially surgical-grade N95 FFRs for protection of healthcare professionals against airborne transmission of SARS-CoV-2. We and others have previously reported promising decontamination methods that may be applied to the recycling and reuse of FFRs. In this study we tested disinfection of three viruses, including SARS-CoV-2, dried on a piece of meltblown fabric, the principal component responsible for filtering of fine particles in N95-level FFRs, under a range of temperatures (60–95 °C) at ambient or 100% relative humidity (RH) in conjunction with filtration efficiency testing. We found that heat treatments of 75 °C for 30 min or 85 °C for 20 min at 100% RH resulted in efficient decontamination from the fabric of SARS-CoV-2, human coronavirus NL63 (HCoV-NL63), and another enveloped RNA virus, chikungunya virus vaccine strain 181/25 (CHIKV-181/25), without lowering the meltblown fabric’s filtration efficiency.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2014

Coupled-cavity terahertz quantum cascade lasers for single mode operation

We demonstrate the operation of coupled-cavity terahertz frequency quantum-cascade lasers composed of two sub-cavities separated by an air gap realized by optical lithography and dry etching. This geometry allows stable, single mode operation with typical side mode suppression ratios in the 30–40 dB range. We employ a transfer matrix method to model the mode selection mechanism. The obtained results are in good agreement with the measurements and allow prediction of the operating frequency.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2014

Instrumentation: Nondestructive Examination for Verification of Canister and Cladding Integrity. FY2014 Status Update

This report documents FY14 efforts for two instrumentation subtasks under storage and transportation. These instrumentation tasks relate to developing effective nondestructive evaluation (NDE) methods and techniques to (1) verify the integrity of metal canisters for the storage of used nuclear fuel (UNF) and to (2) verify the integrity of dry storage cask internals.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1998

A Data Base of Nutrient Use, Water Use, CO2 Exchange, and Ethylene Production by Soybeans in a Controlled Environment

A data set is given describing daily nutrient and water uptake, carbon dioxide (CO2) exchange, ethylene production, and carbon and nutrient partitioning from a 20 sq m stand of soybeans (Glycine max (L.) Merr. cv. McCall] for use in bioregenerative life support systems. Stand CO2 exchange rates were determined from nocturnal increases in CO2 (respiration) and morning drawdowns (net photosynthesis) to a set point of 1000 micromol/ mol each day (i.e., a closed system approach). Atmospheric samples were analyzed throughout growth for ethylene using gas chromatography with photoionization detection (GC/PH)). Water use was monitored by condensate production from the humidity control system, as well as water uptake from the nutrient solution reservoirs each day. Nutrient uptake data were determined from daily additions of stock solution and acid to maintain an EC of 0.12 S/m and pH of 5.8. Dry mass yields of seeds, pods (without seeds), leaves, stems, and roots are provided, as well as elemental and proximate nutritional compositions of the tissues. A methods section is included to qualify any assumptions that might be required for the use of the data in plant growth models, along with a daily event calendar documenting set point adjustments and the occasional equipment or sensor failure.

Wheeler, R. M.↗

NASA NTRS2010

Analysis of Jupiter's Oval BA: A Streamlined Approach

We present a novel method of constructing streamlines to derive wind speeds within jovian vortices and demonstrate its application to Oval BA for 2001 pre-reddened Cassini flyby data, 2007 post-reddened New Horizons flyby data, and 1998 Galileo data of precursor Oval DE. Our method, while automated, attempts to combine the advantages of both automated and manual cloud tracking methods. The southern maximum wind speed of Oval BA does not show significant changes between these data sets to within our measurement uncertainty. The northern maximum dries appear to have increased in strength during this time interval, tvhich likely correlates with the oval's return to a symmetric shape. We demonstrate how the use of closed streamlines can provide measurements of vorticity averaged over the encircled area with no a priori assumptions concerning oval shape. We find increased averaged interior vorticity between pre- and post-reddened Oval BA, with the precursor Oval DE occupying a middle value of vorticity between these two.

Sussman, Michael G.↗

DOE OSTI2025

Non-destructive evaluation and machine learning methods for inspection of spent nuclear fuel canisters: A state-of-the-art review

Nuclear energy is among the cleanest and most efficient energy sources currently available. The operation of nuclear power plants (NPPs) produces large amounts of high-level radioactive waste known as spent nuclear fuel (SNF). Currently, large amounts of SNF is stored in dry cask storage systems (DCSSs) for extended interim storage until a permanent disposal solution becomes available. During the extended interim storage, the DCSS, particularly the SNF canisters, may degrade and abnormal conditions may occur. Therefore, non-destructive evaluation (NDE) and machine learning (ML) approaches are necessary for inspection of SNF canisters. This paper presents a state-of-the-art review of literature by summarizing recent progress made on the applications of NDE and ML for inspection of SNF canisters. Sixteen NDE methods are examined and compared: visual inspection, ultrasonic guided waves (UGWs), laser-based approaches, acoustic emission (AE), eddy current testing (ECT), non-invasive acoustic sensing, dynamic modal testing, cosmic ray muons tomography, neutron imaging, gamma rays detection, fiber optical sensors, through-wall communications, X-ray computed tomography (CT), vibrothermography, monoenergetic photon sources, and surface acoustic wave (SAW) sensors. The technology readiness level (TRL) for each method is assessed and compared. Recent publications on ML-enhanced visual inspection, AE, non-invasive acoustic sensing, dynamic modal testing, and neutron imaging for SNF canisters are summarized and future research needs are identified. In conclusion, this review article provides a convenient reference on the state-of-the-art applications of NDE and ML methods for inspection of SNF canisters.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

A novel freeform extrusion fabrication process for producing solid ceramic components with uniform layered radiation drying

An extrusion-based additive manufacturing process, called the Ceramic On-Demand Extrusion (CODE) process, for producing three-dimensional ceramic components with near theoretical density is introduced in this paper. Heere in this process, an aqueous paste of ceramic particles with a very low binder content (<1 vol%) is extruded through a moving nozzle at room temperature. After a layer is deposited, it is surrounded by oil (to a level just below the top surface of most recent layer) to preclude non-uniform evaporation from the sides. Infrared radiation is then used to partially, and uniformly, dry the just-deposited layer so that the yield stress of the paste increases and the part maintains its shape. The same procedure is repeated for every layer until part fabrication is completed. Several sample parts for various applications were produced using this process and their properties were obtained. The results indicate that the proposed method enables fabrication of large, dense ceramic parts with complex geometries.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Alternative Canister Processing Operations at an Interim Storage Facility - 16617

The US Department of Energy (DOE) is laying the groundwork for implementing interim storage of spent nuclear fuel (SNF) in response to recommendations by the Blue Ribbon Commission on America's Nuclear Future in their report to the Secretary of Energy published January 2012. These efforts include planning for a Pilot Interim Storage Facility (ISF) and a Larger ISF. In March 2014, the DOE employed the CB and I team to evaluate design alternatives for cask handling operations and storing SNF at an ISF. The report, 'Generic Design Alternatives for Dry Storage of Used Nuclear Fuel', (Alternatives Report) evaluates different aspects of an ISF, including a study on alternative approaches for processing SNF canisters such as different cask handling methods and configurations which might be used to transfer canisters from shipping casks into storage locations at an ISF. The purpose of this paper is to report on the development of alternative cask handling operations that have been evaluated for the receipt and storage of the SNF at an initial Pilot ISF and a Larger ISF. This design study is relevant for host communities considering near-term development of a Pilot ISF. DOE-sponsored system analyses indicate that a processing rate of up to 3,000 MTU/yr (approximately 230 to 300 canisters) would be needed for a single Larger ISF (less if more than one ISF were developed) to remove SNF from commercial nuclear plants in a reasonable amount of time. The study evaluated different canister processing operation methodologies in order to reduce the complexity, cost, and personnel exposure associated with processing operations at an ISF. The conclusions from this design study could help to inform the selection of future canister processing operations for an ISF. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Simulation of Proposed Heat Treatment Methods for the Sister Rods

The High Burnup Spent Fuel Data Project (the 'project'), sponsored by the U.S. Department of Energy (DOE) Office of Nuclear Energy (NE), is focused on experimentally evaluating the effects of long-term dry storage and transportation on high burnup (HBU) pressurized water reactor (PWR) fuel (>45 gigawatt days per metric ton uranium). The goals of the project are to provide confirmatory data for analytical model validation and potential improvement; to provide input to future dry storage cask design; to support license renewals and new licenses for Independent Spent Fuel Storage Installation facilities; and to support transportation licensing for high burnup used fuel. In support of these project goals, an instrumented TN-32B bolted-lid cask (the Research Project Cask or RPC) at the North Anna reactor site will be loaded with intact, HBU PWR fuel assemblies (Project Assemblies) having four different kinds of cladding: standard Zircaloy-4, low-tin Zircaloy-4, ZIRLO{sup R}, and M5{sup R}. In approximately ten years, the instrumented cask will be opened for inspection and several fuel rods from the Project Assemblies will be characterized. The project has also removed 25 'sister rods' from assemblies at North Anna: 9 directly from the project assemblies and 16 from similarly constructed and operated HBU assemblies. The 25 sister rods are all high burnup and cover the range of domestically-used cladding alloys. The 25 sister rods were shipped to Oak Ridge National Laboratory (ORNL) in early 2016 for detailed non-destructive examinations (NDE) followed by destructive examination (DE). Examination of the sister rods will provide a baseline for comparison with the cask rods and will allow for separate effects testing. Dry storage canister loading is completed under water in a designated area of the plant's spent fuel pool. In preparation for dry storage, the fuel assemblies and canister cavity must be drained and dried. Typically, the highest temperatures experienced by the fuel during dry storage are encountered either during drying or transfer of the canister to the storage pad; therefore, as a part of the sister rod testing these temperatures will be simulated in the lab to produce samples that are representative of the peak cladding temperature the fuel experiences either during drying, transfer, or storage. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

SU-D-204-05: Fitting Four NTCP Models to Treatment Outcome Data of Salivary Glands Recorded Six Months After Radiation Therapy for Head and Neck Tumors

Purpose: To estimate the radiobiological parameters of four popular NTCP models that describe the dose-response relations of salivary glands to the severity of patient reported dry mouth 6 months post chemo-radiotherapy. To identify the glands, which best correlate with the manifestation of those clinical endpoints. Finally, to evaluate the goodness-of-fit of the NTCP models. Methods: Forty-three patients were treated on a prospective multiinstitutional phase II study for oropharyngeal squamous cell carcinoma. All the patients received 60 Gy IMRT and they reported symptoms using the novel patient reported outcome version of the CTCAE. We derived the individual patient dosimetric data of the parotid and submandibular glands (SMG) as separate structures as well as combinations. The Lyman-Kutcher-Burman (LKB), Relative Seriality (RS), Logit and Relative Logit (RL) NTCP models were used to fit the patients data. The fitting of the different models was assessed through the area under the receiver operating characteristic curve (AUC) and the Odds Ratio methods. Results: The AUC values were highest for the contralateral parotid for Grade ≥ 2 (0.762 for the LKB, RS, Logit and 0.753 for the RL). For the salivary glands the AUC values were: 0.725 for the LKB, RS, Logit and 0.721 for the RL. For the contralateral SMG the AUC values were: 0.721 for LKB, 0.714 for Logit and 0.712 for RS and RL. The Odds Ratio for the contralateral parotid was 5.8 (1.3–25.5) for all the four NTCP models for the radiobiological dose threshold of 21Gy. Conclusion: It was shown that all the examined NTCP models could fit the clinical data well with very similar accuracy. The contralateral parotid gland appears to correlated best with the clinical endpoints of severe/very severe dry mouth. An EQD2Gy dose of 21Gy appears to be a safe threshold to be used as a constraint in treatment planning.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2016

Capillary pressure – saturation relationships for gas shales measured using a water activity meter

Hydraulic fracturing of gas shale formations involves pumping a large volume of fracking fluid into a hydrocarbon reservoir to fracture the rock and thus increase its permeability. The majority of the fracking fluid introduced is never recovered and the fate of this lost fluid, often called “leak off,” has become the source of much debate. Information on the capillary pressure – saturation relationship for each wetting phase is needed to simulate leak off using numerical reservoir models. The petroleum industry commonly employs air – water capillary pressure – saturation curves to predict these relationships for mixed wet reservoirs. Traditional methods of measuring this curve are unsuitable for gas shales due to high capillary pressures associated with the small pores present. Still, a possible alternative method is the water activity meter which is used widely in the soil sciences for such measurements. However, its application to lithified material has been limited. Here, this study utilized a water activity meter to measure air – water capillary pressures (ranging from 1.3 to 219.6 MPa) at several water saturation levels in both the wetting and drying directions. Water contents were measured gravimetrically. Seven types of gas producing shale with different porosities (2.5–13.6%) and total organic carbon contents (0.4–13.5%) were investigated. Nonlinear regression was used to fit the resulting capillary pressure – water saturation data pairs for each shale type to the Brooks and Corey equation. Data for six of the seven shale types investigated were successfully fitted (median R 2 = 0.93), indicating this may be a viable method for parameterizing capillary pressure – saturation relationships for inclusion in numerical reservoir models. As expected, the different shale types had statistically different Brooks and Corey parameters. However, there were no significant differences between the Brooks and Corey parameters for the wetting and drying measurements, suggesting that hysteresis may not need to be taken into account in leak off simulations.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2019

Working fluid selection for organic Rankine cycle power generation using hot produced supercritical CO 2 from a geothermal reservoir

Geothermal heat mining simulations using supercritical CO 2 (sCO 2 ) were performed in this research. Working fluid selection criteria for power generation using sCO 2 from a geothermal reservoir are then presented for subcritical, superheated and supercritical organic Rankine cycles (ORCs). Meanwhile, method of working fluid classification for ORC is proposed. To get the most feasible ORC design, this study introduces the concept of “turning point” for isentropic and dry working fluids, as well as minimum turbine inlet temperature for wet working fluids. A thermodynamic model was developed with capabilities to obtain the optimal working fluid mass flow rate, evaporation temperature, superheated temperature, and supercritical pressure, to evaluate the thermal performance of the three ORC approaches using hot produced sCO 2 . With this model, thirty potential working fluids with critical temperatures in the range from 50 to 225 °C were screened for utilizing hot produced sCO 2 considering physical properties, environmental and safety impacts, and thermodynamic performances. Finally, the thermodynamic results were compared for all possible working fluids.

15 GEOTHERMAL ENERGY↗

DOE OSTI2012

Heavy metals in liquid pig manure in light of bacterial antimicrobial resistance

Heavy metals are regularly found in liquid pig manure, and might interact with bacterial antimicrobial resistance. Concentrations of heavy metals were determined by atomic spectroscopic methods in 305 pig manure samples and were connected to the phenotypic resistance of Escherichia coli (n=613) against 29 antimicrobial drugs. Concentrations of heavy metals (/kg dry matter) were 0.08-5.30 mg cadmium, 1.1-32.0 mg chrome, 22.4-3387.6 mg copper, <2.0-26.7 mg lead, <0.01-0.11 mg mercury, 3.1-97.3 mg nickel and 93.0-8239.0 mg zinc. Associated with the detection of copper and zinc, resistance rates against {beta}-lactams were significantly elevated. By contrast, the presence of mercury was significantly associated with low antimicrobial resistance rates of Escherichia coli against {beta}-lactams, aminoglycosides and other antibiotics. Effects of subinhibitory concentrations of mercury on bacterial resistance against penicillins, cephalosporins, aminoglycosides and doxycycline were also demonstrated in a laboratory trial. Antimicrobial resistance in the porcine microflora might be increased by copper and zinc. By contrast, the occurrence of mercury in the environment might, due to co-toxicity, act counter-selective against antimicrobial resistant strains.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2012

Manganese and Ceria Sorbents for High Temperature Sulfur Removal from Biomass-Derived Syngas -- The Impact of Steam on Capacity and Sorption Mode

Syngas derived from biomass and coal gasification for fuel synthesis or electricity generation contains sulfur species that are detrimental to downstream catalysts or turbine operation. Sulfur removal in high temperature, high steam conditions has been known to be challenging, but experimental reports on methods to tackle the problem are not often reported. We have developed sorbents that can remove hydrogen sulfide from syngas at high temperature (700 C), both in dry and high steam conditions. The syngas composition chosen for our experiments is derived from statistical analysis of the gasification products of wood under a large variety of conditions. The two sorbents, Cu-ceria and manganese-based, were tested in a variety of conditions. In syngas containing steam, the capacity of the sorbents is much lower, and the impact of the sorbent in lowering H{sub 2}S levels is only evident in low space velocities. Spectroscopic characterization and thermodynamic consideration of the experimental results suggest that in syngas containing 45% steam, the removal of H{sub 2}S is primarily via surface chemisorptions. For the Cu-ceria sorbent, analysis of the amount of H{sub 2}S retained by the sorbent in dry syngas suggests both copper and ceria play a role in H{sub 2}S removal. For the manganese-based sorbent, in dry conditions, there is a solid state transformation of the sorbent, primarily into the sulfide form.

09 BIOMASS FUELS↗

DOE OSTI2022

Hot-melt extrudability of amorphous solid dispersions of flubendazole-copovidone: An exploratory study of the effect of drug loading and the balance of adjuvants on extrudability and dissolution

The FDA-approved anthelmintic flubendazole has shown potential to be repositioned to treat cancer and dry macular degeneration; however, its poor water solubility limits its use. Amorphous solid dispersions may overcome this challenge, but the balance of excipients may impact the preparation method and drug release. Here, we evaluate the influence of adjuvants and drug loading on the development of an amorphous solid dispersion of flubendazole-copovidone by hot-melt extrusion. The drug, copovidone, and adjuvants (magnesium stearate and hydroxypropyl cellulose) mixtures were statistically designed, and the process was performed in a twin-screw extruder. The study showed that flubendazole and copovidone mixtures were highly extrudable, except when drug loading was high (>40%). Furthermore, magnesium stearate positively impacted the extrusion and was more effective than hydroxypropyl cellulose. The extruded materials were evaluated by modulated differential scanning calorimetry and X-ray powder diffraction, obtaining positive amorphization and physical stability results. Pair distribution function analysis indicated the presence of drug rich domains with medium-range order structure and no evidence of polymer-drug interaction. All extrudates presented faster dissolution (HCl, pH 1.2) than pure flubendazole, and both adjuvants had a notable influence on the dissolution rate. In conclusion, hot-melt extrusion may be a viable option to obtain stable flubendazole: copovidone amorphous dispersions.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2014

Survey of mercury, cadmium and lead content of household batteries

Highlights: • A well selected sample of 146 batteries was analysed for its heavy metals content. • A comparison was made between heavy metals contents in batteries in 2006 and 2011. • No significant change after implementation of the new EU Batteries Directive. • Severe differences in heavy metal contents were found in different battery-types. - Abstract: The objective of this work was to provide updated information on the development of the potential impact of heavy metal containing batteries on municipal waste and battery recycling processes following transposition of the new EU Batteries Directive 2006/66/EC. A representative sample of 146 different types of commercially available dry and button cells as well as lithium-ion accumulators for mobile phones were analysed for their mercury (Hg)-, cadmium (Cd)- and lead (Pb)-contents. The methods used for preparing the cells and analysing the heavy metals Hg, Cd, and Pb were either developed during a former study or newly developed. Several batteries contained higher mass fractions of mercury or cadmium than the EU limits. Only half of the batteries with mercury and/or lead fractions above the marking thresholds were labelled. Alkaline–manganese mono-cells and Li-ion accumulators, on average, contained the lowest heavy metal concentrations, while zinc–carbon batteries, on average, contained the highest levels.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗