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All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Fracture Toughness Evaluation for Spent Nuclear Fuel Clad Systems Using Spiral Notch Torsion Fracture Toughness Test

Many radioactive materials within the nuclear fuel cycle present a significant hazard. Such materials include spent nuclear fuel, high-level waste, legacy waste and other nuclear materials. These materials are often held in long-term storage as an interim stage within their lifecycle, including reuse or disposal. Safety and security of spent nuclear fuel (SNF) interim storage installations and follow-on SNF transportations to its final repository sites are very important, due to a great concentration of fission products, actinides and activation products. Fracture mechanics approach in applying to SNF system reliability investigation, especially for the high burn up (HBU) SNF, during SNF long term dry storage or SNF transportation is necessary due to the inherited flaws and inhomogeneity structures existed in a SNF system from the reactor operation. For instance, such as hydride and oxide formation, surface flaw induced by SNF assembly contact interactions, or internal flaws induced by pellet-clad mechanical interaction (PCMI). However, none of the existing fracture toughness data deal with fuel cladding specific geometry or SNF material conditions, such as cladding structure with the segment fuel pellets configuration and the PCMI mechanism. Consequently, the application of existing fracture toughness data to SNF system reliability investigation can be error prone; thus, the development of an industry-wide consensus fracture mechanics approach is needed. The objective of this research is to develop an in-situ fracture mechanics testing protocol, including the associated analytical procedure, that is suitable for evaluating the SNF fracture toughness. Fracture toughness data was obtained under quasi-static fracture loading using Oak Ridge National Laboratory (ORNL) developed Spiral Notch Torsion Test (SNTT) technology carried out on a biaxial tension/torsion tester. These data will be used to support SNF reliability investigation during long-tern SNF dry storage stage or in the follow-on SNF system transport to the final repository sites. SNTT has been a recent breakthrough in measuring fracture toughness for different materials, including metals, ceramics, concrete and polymers composites. Due to its high geometry constraint and unique loading condition, SNTT can be used to measure the fracture toughness with smaller specimens without concern of size effects. The application of SNTT to brittle materials has been proved to be successful. The micro-cracks induced by original notches in brittle materials could ensure crack growth in SNTT samples. Therefore, no fatigue pre cracks are needed for brittle materials specimens. The application of SNTT to the ductile material to generate valid toughness data will require a test sample with sufficient pre-crack length to increase the sample localized constraint at crack front. Fatigue pre-crack growth techniques with the associated compliance function estimated was developed for estimating the crack penetration depth to monitor the fatigue crack growth evolution. In order to extend SNTT approach to a thin shell cladding structure material, a new testing protocol and the associated analytical procedure for estimating the SNF fracture toughness was developed. The detailed SNTT approach and its estimated fracture toughness for the Zr-4 cladding structure with segment alumina inserts are presented in this report. The SNTT test results indicate that SNTT method is a reliable test approach with good repeatability in applying to Zr-4 cladding material. For the medium and the short crack length, the estimate J Q upon fracture for the baseline Zr-4 cladding is at 285.7 lb/in with 2-sigma uncertainty of 18.59 lb/in., and the associated K Q is at 61.4 Ksi√in. For a long crack length, the crack initialization orientation is apparently deviated from the principle tensile stress contour – 45° spiral crack front (i.e., Mode I + Mode III failure mechanism); and the estimated J Q is at 108 lb/in., the associated K Q is at 37.7 Ksi√in. The estimate Mode I J Q (along the 45° pitch principle tensile stress contour) is at 200 lb/in.; which indicate a significant reduction in the fracture toughness in a tubing structure under mixed mode loading condition, Mode I + Mode III, compared to that of Mode I (tensile stress dominated) alone.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

CCN Measurements at Urban Site during CoURAGE

Cloud condensation nuclei (CCN) measurements were collected during CoURAGE from March - June 2025 at the BSEC urban atmospheric chemistry supersite (39.32057 N, 76.6246 W). CCN number concentrations (# cm-3) were obtained at a frequency of 1 second using a cloud condensation nuclei counter (CCN-100, Droplet Measurement Technologies). The CCN counter was operated in stepping mode, measuring CCN over a range of supersaturations from 0.2 to 1.0%. The settings of the instrument were set such that the supersaturation increased in increments of 0.2% up to the maximum supersaturation, and then decreased in increments of 0.2% down to the minimum supersaturation in a repeating cycle. The supersaturation of the instrument was calibrated weekly using ammonium sulfate. The weekly calibrated supersaturation values have been applied to the data. Data during transitions between supersaturation values were removed and replaced with a value of -999. Transitions are defined as the first 210 seconds after a new supersaturation value to ensure the instrument has stabilized following a change in supersaturation. Data were also flagged with a value of -999 if there were concerns with the function of the instrument, specifically the presence of alarm codes, fogging of the optical particle counter (1st stage monitor > 0.4 V), or a sheath to sample flow ratio outside the expected range (< 9 or > 11).

CCN number density↗
DOE OSTI2021

Isotopic analysis of sub-nanogram neodymium loads using new ATONA™ amplifiers

The long-term gains of the ATONA™ amplifiers are shown to have less than 1 ppm variability. Repeat measurements of the JNdi-1 reference material demonstrate the ability of the ATONA™ amplification technology to make measurements of 143 Nd/ 144 Nd ratios with 23 ppm external reproducibility on 100-pg loads. The effect of increasing integration time on analytical reproducibility is also displayed as increasing integration time from 10 to 30s reduced the external measurement uncertainty from 37 to 23 ppm. These measurements represent an improvement of more than a factor of 3 in external measurement reproducibility relative to previously published 143 Nd/ 144 Nd measurements of 100-pg loads. Furthermore, this new technology will allow for the measurement of smaller samples for precise isotope ratios and open new avenues of research in the geological and nuclear forensic communities.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2025

Dry Deactivation of Sodium Metal in a Molten LiCl-KCl-CsCl-NaCl System

An experimental study was performed with the objective of investigating and characterizing a dry technique for deactivation of sodium metal in a molten salt system. The study was performed in three parts. First, proof-of-principle testing of the technique was performed at bench scale. It involved loading and melting tens of grams of clean sodium metal atop a pool of LiCl-KCl-CsCl eutectic at ∼300°C and then adding ammonium chloride particles while mixing. The ammonium chloride reacted with sodium to form sodium chloride and nitrogen/hydrogen off-gases. The sodium chloride assimilated into the salt pool, forming a quaternary salt mixture of LiCl-KCl-CsCl-NaCl. The proof-of-principle testing repeatedly exhibited complete deactivation of the loaded sodium metal. Second, characterization of a LiCl-KCl-CsCl-NaCl system was performed using differential scanning calorimetry to produce a partial phase diagram of LiCl-KCl-CsCl eutectic versus NaCl, which identified the liquidus, solidus, and two-phase regions of the quaternary system. Third, the dry deactivation technique was demonstrated at kg-scale in an inert atmosphere radiological glovebox with sodium metal that was previously separated in the same glovebox from uranium metal in unirradiated blanket elements for the Fermi-1 nuclear reactor. The quaternary salt product at the end of the demonstration was sampled and showed complete deactivation of the sodium metal. Here, in short, this study qualified a technique to completely deactivate batches of sodium metal in the absence of air or water. While this study focused on the deactivation of sodium metal, including bond sodium from unirradiated blanket elements, the technique is applicable to other sources of sodium metal, such as sodium metal from batteries. Furthermore, the technique could also be extended to other alkali metal systems, including lithium, sodium, potassium, rubidium, cesium, and mixtures thereof.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Electronic structure at coarse-grained resolutions from supervised machine learning

Computational studies aimed at understanding conformationally dependent electronic structure in soft materials require a combination of classical and quantum-mechanical simulations, for which the sampling of conformational space can be particularly demanding. Coarse-grained (CG) models provide a means of accessing relevant time scales, but CG configurations must be back-mapped into atomistic representations to perform quantum-chemical calculations, which is computationally intensive and inconsistent with the spatial resolution of the CG models. A machine learning approach, denoted as artificial neural network electronic coarse graining (ANN-ECG), is presented here in which the conformationally dependent electronic structure of a molecule is mapped directly to CG pseudo-atom configurations. By averaging over decimated degrees of freedom, ANN-ECG accelerates simulations by eliminating backmapping and repeated quantum-chemical calculations. The approach is accurate, consistent with the CG spatial resolution, and can be used to identify computationally optimal CG resolutions.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Examining Nuisance Aerosol Detections in Light of the Origin of the Screening Process (November 2021)

The evolution of philosophy and computations in the International Data Center (IDC) related to aerosol samples have had profound impacts on the number of recorded detections in the network since routine operations began in 2000. Key decisions from policymakers have been the list of triggering radionuclides, the scheme for categorizing these into interest levels 1-5, and an algorithm for determining when an anthropogenic isotope is seen so often that it is no longer interesting, known as the Exponential Weighted Moving Average (EWMA). These are described in the Operations Manual of the IDC. Key parameters that are controlled by the IDC but for which the IDC receives occasional input from policymakers include the constants in EWMA and the peak significance threshold for individual gamma rays, the latter of which directly leads to determination of the presence or absence of a radionuclide in a sample. There are also changes in computations which the IDC makes and informs policy makers about, such as changes in how background is computed, which could also affect the ease of detecting a peak – real or false. Rather than focus on the quantitative changes due to computation changes, this work records some thinking on how isotopes and peak significance levels were chosen, and the resulting detections seen over 18 years during the buildup of the International Monitoring System (IMS). These detections are considered on a global scale to try to determine the relative impact on monitoring, and in some cases, the nature of their existence. Repeated detections of 131I and 133I are the most troublesome, but they are not so frequent to be a major problem for the Verification Regime. These detections could probably be handled adequately using scientific methods currently under development for xenon backgrounds. It is also somewhat problematic that top-level analysis of aerosol backgrounds has not been reported previous to this. The steep increase in the rate of detections after 2016 are a concern, either in the actual backgrounds or from changes in the calculations methods used to generate the Reviewed Radionuclide Report (RRR.) Final conclusions of the authors are that the computational stability of the RRR is very important. With computational stability, changes can be usefully analyzed as being due to changes in radioactivity in Earth’s atmosphere This report is a distillation into text of a talk given in the Radionuclide Experts Group (RNEG) in Vienna during Working Group B (WGB) in February of 2019. This report does not directly contain any IDC data, only summaries by year, or by isotope, or by location. No specific IDC detection by time, location, or isotope is included.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Filtration Performance of Layering Masks and Face Coverings and the Reusability of Cotton Masks after Repeated Washing and Drying

In this study, filtration efficiency of different respirators, face masks, and a 2-ply cotton handkerchief bandana was compared for particles in the size range of 60 nm-4 um under a "perfect fit" condition. The filtration efficiency at the most penetrating particle size of 0.3 um on average ranged from 83-99% for N95 and KN95 respirators, 42-88% for surgical masks, 16-23% for cloth masks, and 9% for bandana. We also investigated the effects of using double surgical masks or layering a cloth mask over various surgical masks in terms of their filtration characteristics. In most of these combinations, the filtration efficiency improved by ~25% for particles 0.3-1 um in diameter without any substantial change in the filter quality factor when compared to the highest of the individual mask results. To investigate the reusability of cotton cloth masks, 2-layer cotton fabric sample coupons were machine washed and dried for 52 cycles leading to an increase in inhalation resistance (~20 Pa) without affecting size-resolved filtration efficiency. Scanning electron microscopy revealed that washing and drying led to the gradual deconstruction of cotton fibers at the scale of several micrometers to hundreds of nanometers in the form of delamination of the fiber wall and fibrillation of the nanofiber constituents. Results indicate that cloth masks may be layered over surgical masks for additional benefits, and that cloth masks made out of cotton fabric can be washed and reused numerous times without a significant loss in filtration efficiency.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2024

Multiscale modeling of HBV infection integrating intra- and intercellular viral propagation to analyze extracellular viral markers

Chronic infection with hepatitis B virus (HBV) is caused by the persistence of closed circular DNA (cccDNA) in the nucleus of infected hepatocytes. Despite available therapeutic anti-HBV agents, eliminating the cccDNA remains challenging. Thus, quantifying and understanding the dynamics of cccDNA are essential for developing effective treatment strategies and new drugs. However, such study requires repeated liver biopsy to measure the intrahepatic cccDNA, which is basically not accepted because liver biopsy is potentially morbid and not common during hepatitis B treatment. We here aimed to develop a noninvasive method for quantifying cccDNA in the liver using surrogate markers in peripheral blood. We constructed a multiscale mathematical model that explicitly incorporates both intracellular and intercellular HBV infection processes. The model, based on age-structured partial differential equations, integrates experimental data from in vitro and in vivo investigations. By applying this model, we roughly predicted the amount and dynamics of intrahepatic cccDNA within a certain range using specific viral markers in serum samples, including HBV DNA, HBsAg, HBeAg, and HBcrAg. Our study represents a significant step towards advancing the understanding of chronic HBV infection. The noninvasive quantification of cccDNA using our proposed method holds promise for improving clinical analyses and treatment strategies. By comprehensively describing the interactions of all components involved in HBV infection, our multiscale mathematical model provides a valuable framework for further research and the development of targeted interventions.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Durable and Low-Cost Fractal Structured Multifunctional Coatings for Next-Generation CSP

Fractal coatings on various low-cost and high-temperature metallic substrates such as SS316, SS347, In800H, In740H, In625, Haynes 230, etc. were fabricated employing our patented novel electrodeposition process at various deposition potentials and deposition times, as well as chemical etching. The best combination of the materials and processing conditions were co-optimized for the reliable and repeatable fabrication of the multifunctional coatings. Surface morphologies were examined using SEM and AFM, and fractal characterization was done using a 3D optical surface profiler. Fractal dimension was used to identify successful fabrication and material parameters. The mechanical durability of the coatings was evaluated using several standardized tests, such as sand abrasion (ASTM D968) and adhesion (ASTM D3359), to fully characterize and demonstrate the mechanical durability of the fabricated surfaces. HTF immersion tests on the fractal multifunctional coatings were conducted based on a modification of the ASTM D870, which is established for static water immersion testing. To calculate the corrosion rates and descaled weight loss of the samples subjected to thermal exposure for different time durations (100 h, 300 h, 500 h, and optionally 750 h) to estimate the corrosion rate. While protecting the substrates from corrosion is an important goal, an allied goals is also to examine the post-corrosion temperature stability and properties of the molten salts themselves due to the dissolution of the constituents of the alloys and the corrosion products from the coatings that cause “fouling” of the molten salts. Fouling characteristics of the different molten salt HTFs exposed to coated and uncoated substrates were investigated. Finally, considering a prototype molten salt/sCO2 heat exchanger, cost/performance model is developed to demonstrate that the coatings on low-cost alloys such as stainless steel provide lower levelized cost of heat exchanger compared to high nickel content Ha230.

14 SOLAR ENERGY↗
DOE OSTI2019

EGS Collab Experiment 1: Microseismic Monitoring

The U.S. Department of Energy's Enhanced Geothermal System (EGS) Collab project aims to improve our understanding of hydraulic stimulations in crystalline rock for enhanced geothermal energy production through execution of intensely monitored meso-scale experiments. The first experiment is being performed at the 4850 ft level of the Sanford Underground Research Facility (SURF), approximately 1.5 km below the surface at Lead, South Dakota. Here we report on microseismic monitoring of repeated stimulation experiments and subsequent flow tests between two boreholes in the Poorman Formation. Stimulations were performed at several locations in the designated injection borehole at flow rates from 0.1 to 5 L/min over temporal durations from minutes to hours. Microseismic monitoring was performed using a dense 3D sensor array including two cemented hydrophone strings with 12 sensors at 1.75 m spacing accompanied by 18 3-C accelerometers, deployed in 6 monitoring boreholes, completely surrounding the stimulation region. Continuous records were obtained over a two-month period using a novel dual recording system consisting of a conventional 96 channel exploration seismograph and a high-performance 64 channel digitizer sampling sensors at 4 and 100 kHz respectively. Using a standard STA/LTA triggering algorithm, we detected thousands of microseismic events with recorded energy in a frequency range generally above 3 kHz and up to 40 kHz. The locations of these events are consistent with creation of a hydraulic fracture and additional reactivation of pre-existing structures. Using manual pick refinement and double-difference relocation we are able to track the fracture growth to high precision. We estimate the times and locations of the fracture intersecting a monitoring and the production borehole using microseismic events. They are in excellent agreement with independent measurements using distributed temperature sensing, in-situ strain observations and measurements of conductivity changes. This submission includes a microearthquake catalog, raw event files, a subset of the continuous microseismic monitoring data collected during stimulations and flow test activity on 05/22/2018, 05/23/2018, 05/24/2018, 05/25/2018, 06/25/2018, 07/19/2018, 07/20/2018, 12/7/2018, 12/20/2018, and 12/21/2018 (in binary format), and a binary file interpreter to read the continuous microseismic monitoring data. A Stanford Geothermal Workshop paper is also included to describe microseismic monitoring activities at SURF during these periods.

15 GEOTHERMAL ENERGY↗
DOE OSTI2019

Oxy-fluorophosphate glass doped SmO{sup 3+} as solid state dosimeter via spectroscopic techniques

In the present work, collective studies on optical, structural and magnetic properties of 0.5% SmO{sup 3+} ions in new easily melting fluorophosphate glass of the basic composition 70P{sub 2}O{sub 5}–20AlF{sub 3}–10NaF were carried out. The same combined spectral measurements (UV–Vis, FTIR, and ESR) were repeated after successive gamma irradiation. These collective spectral studies are expected to throw some insight on the effect of host fluorophosphate glass on these selected spectral properties of samarium ions together with identifying the effects of gamma irradiation on both the host fluorophosphate glass and on samarium ions and reaching to the resultant generated induced defects. The experimental results exhibit that, the slope of the UV–Vis line is sufficiently high in order to this tool is preferable to be elected as a suitable tool for the dosimetric purpose for this glass composition. The results in this manuscript propose that it is possible to use these techniques to determine if the glass sample may be used as solid-state dosimeters for gamma dose measurements in the range from 0.1 up to 15 kGy due to their linearity with the absorbed dose, color change, low fading for time periods up to 25 days and good response reproducibility.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Identifying the Role of Magnesium Content in Assessing the Electrochemical Performance of (CoCuMgNiZn)O

High-entropy oxides (HEOs) featuring 5 or more metals in approximately equimolar ratios, such as the prototypical rock-salt-structured (CoCuMgNiZn)O, have attracted interest for their potential to display material properties superior to oxides with combinations of 4 or fewer of the component metals. In particular, (CoCuMgNiZn)O has shown promise as an anode for lithium-ion batteries with a high specific capacity retention over extended cycling. Previous studies have suggested that magnesium, despite being electrochemically inert, provides a crucial contribution to the favorable performance of this HEO by stabilizing the crystal structure through repeated charge–discharge cycles. This paper probes the extent and mechanism of the magnesium effect by using a facile microwave-assisted hydrothermal synthesis method to vary the level of Mg content. Moreover, we extensively characterized the product with techniques such as 4D-STEM and ICP-OES, which have not previously been applied in combination with this material, in order to elucidate the relationships among chemical composition, nanostructure, and performance. Here, we show that the level of Mg incorporation is positively correlated with long-term stability and negatively correlated with rate capacity, and that the latter effect yields a stronger influence upon the overall performance, with the best-performing sample possessing a Mg quantity equivalent to ∼1/5 that of an equimolar concentration. This finding demonstrates not only that the variation of individual elemental levels offers a promising and relatively unexplored avenue to optimize the electrochemical performance of HEO materials but also that it should not be assumed that equimolar compositions of constituent elements are necessarily the best.

36 MATERIALS SCIENCE↗
DOE OSTI2020

First Examination of Irradiated Fuel with Pulsed Neutrons at LANSCE (Preliminary Results)

We present preliminary results on the characterization of an irradiated U-lOZr-lPd fuel sample that was prepared from the irradiated AFC-3A-R5A sample. U-lOZr metallic fuels are researched as host materials for potential transmutation fuels and the addition of palladium strives to bind lanthanides, thus preventing fuel-cladding chemical interactions (FCCI). These interactions limit the lifetime of metallic fuels and are caused by migration of lanthanide fission products to the periphery of the fuel slug, where they start to interact with the D9 or HT9 steel cladding, ultimately leading to failure of the mechanical integrity of the cladding. Neutrons offer bulk characterization of irradiated materials for which X-ray tomography methods are not suitable due to the immense gamma background emitted from the samples. In particular pulsed neutrons provide information from the ability to resolve the neutron energy using their time-of-flight and thus the potential to utilize neutron absorption resonance to characterize the spatial distribution of isotopes. This, in turn, may allow to characterize the distribution of fission and neutron capture products non-destructively and may ultimately be applied to the bulk of an irradiation capsule prior to destructive post-irradiation examination to identify regions of interest. To allow the characterization of entire irradiation capsules, a cask is under development in the advanced post-irradiation work package at LANL and progress on this development was reported elsewhere. In parallel, an irradiated U-lOZr-lPd sample cut from the AFC-3AR5A irradiation was shipped to LANL and will be fully characterized with an NSUF funded rapid turnaround experiment (RTE) in the 2020 LANSCE run cycle. The sample emits at a dose rate of ~3R/hr on contact and is therefore manageable with remote handling, without requiring a cask. The disk-shaped material is larger than samples prepared for analysis using electron or X-ray methods and is therefore an intermediate step towards characterization of bulk samples at LANSCE. However, since it covers the full diameter of the irradiated fuel slug, some insight on redistribution of elements, spatially resolved information on microstructure, e.g. phase composition and texture, will be possible using the pulsed neutron-based methods developed for fuel characterization at LANSCE. This report describes the development of procedures to handle the sample at LANSCE as well as preliminary data and results from tests conducted in December 2019 on the energy-resolved neutron imaging (ERNI) beam line at flight path 5 and the high pressure-preferred orientation diffractometer (HIPPO) at LANSCE. This effort is a collaboration between LANL, INL, and ORNL. To compare our capabilities with prior work, we present an overview of previously reported bulk characterization of irradiated or spent fuels. The overview addresses neutron diffraction and neutron absorption resonance spectroscopy, both of which have only few reported applications on irradiated or spent nuclear fuel, as well as neutron radiography. This literature review was already described in a previous report but is repeated here to put our current efforts in context of previous work.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Rapid sample delivery for megahertz serial crystallography at X-ray FELs

Liquid microjets are a common means of delivering protein crystals to the focus of X-ray free-electron lasers (FELs) for serial femtosecond crystallography measurements. The high X-ray intensity in the focus initiates an explosion of the microjet and sample. With the advent of X-ray FELs with megahertz rates, the typical velocities of these jets must be increased significantly in order to replenish the damaged material in time for the subsequent measurement with the next X-ray pulse. Here in this paper, this work reports the results of a megahertz serial diffraction experiment at the FLASH FEL facility using 4.3 nm radiation. The operation of gas-dynamic nozzles that produce liquid microjets with velocities greater than 80 m s -1 was demonstrated. Furthermore, this article provides optical images of X-ray-induced explosions together with Bragg diffraction from protein microcrystals exposed to trains of X-ray pulses repeating at rates of up to 4.5 MHz. Finally, the results indicate the feasibility for megahertz serial crystallography measurements with hard X-rays and give guidance for the design of such experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Psilocybin: crystal structure solutions enable phase analysis of prior art and recently patented examples

Psilocybin {systematic name: 3-[2-(dimethylamino)ethyl]-1 H -indol-4-yl dihydrogen phosphate} is a zwitterionic tryptamine natural product found in numerous species of fungi known for their psychoactive properties. Following its structural elucidation and chemical synthesis in 1959, purified synthetic psilocybin has been evaluated in clinical trials and has shown promise in the treatment of various mental health disorders. In a recent process-scale crystallization investigation, three crystalline forms of psilocybin were repeatedly observed: Hydrate A, Polymorph A, and Polymorph B. The crystal structure for Hydrate A was solved previously by single-crystal X-ray diffraction. This article presents new crystal structure solutions for the two anhydrates, Polymorphs A and B, based on Rietveld refinement using laboratory and synchrotron X-ray diffraction data, and density functional theory (DFT) calculations. Utilizing the three solved structures, an investigation was conducted via Rietveld method (RM) based quantitative phase analysis (QPA) to estimate the contribution of the three different forms in powder X-ray diffraction (PXRD) patterns provided by different sources of bulk psilocybin produced between 1963 and 2021. Over the last 57 years, each of these samples quantitatively reflect one or more of the hydrate and anhydrate polymorphs. In addition to quantitatively evaluating the composition of each sample, this article evaluates correlations between the crystal forms present, corresponding process methods, sample age, and storage conditions. Furthermore, revision is recommended on characterizations in recently granted patents that include descriptions of crystalline psilocybin inappropriately reported as a single-phase `isostructural variant.' Rietveld refinement demonstrated that the claimed material was composed of approximately 81% Polymorph A and 19% Polymorph B, both of which have been identified in historical samples. In this article, we show conclusively that all published data can be explained in terms of three well-defined forms of psilocybin and that no additional forms are needed to explain the diffraction patterns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Intrinsic Ion Transport Properties of Block Copolymer Electrolytes

Knowledge of intrinsic properties is of central importance for materials design and assessing suitability for specific applications. Self-assembling block copolymer electrolytes (BCEs) are of great interest for applications in solid-state energy storage devices. A fundamental understanding of ion transport properties, however, is hindered by the difficulty in deconvoluting extrinsic factors, such as defects, from intrinsic factors, such as the presence of interfaces between the domains. Here, we quantify the intrinsic ion transport properties of a model BCE system consisting of poly(styrene-block-ethylene oxide) (SEO) and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) salt using a generalizable strategy of depositing thin films on interdigitated electrodes and self-assembling fully connected parallel lamellar structures throughout the films. Comparison between conductivity in homopolymer poly(ethylene oxide) (PEO)-LiTFSI electrolytes and the analogous conducting material in SEO over a range of salt concentrations (r, molar ratio of lithium ion to ethylene oxide repeat units) and temperatures reveals that between 20% and 50% of the PEO in SEO is inactive. Using mean-field theory calculations of the domain structure and monomer concentration profiles at domain interfaces-both of which vary substantially with salt concentration-the fraction of inactive PEO in the SEO, as derived from conductivity measurements, can be quantitatively reconciled with the fraction of PEO that is mixed with greater than a few volume percent of polystyrene. Despite the detrimental interfacial effects for ion transport in BCEs, the intrinsic conductivity of the SEO studied here (ca. 10 -3 S/cm at 90 degrees C, r = 0.085) is an order of magnitude higher than reported values from bulk samples of similar molecular weight SEO (ca. 10 -4 S/cm at 90 degrees C, r = 0.085). Finally, this work provides motivation and methods for pursuing improved BCE chemical design, interfacial engineering, and processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Performance of pumped counterflow virtual impactors to study aerosol interactions with laboratory generated warm clouds

Pumped Counterflow Virtual Impactors (PCVI) are designed to separate aerosols based on aerodynamic diameter, which is particularly useful for isolating cloud droplets and ice crystals from smaller particles. However, the PCVI transmission efficiency (TE) values reported in the literature show considerable variability, and little information is available on the TEs for cloud liquid droplets. Here, we determined the optimal flow conditions for PCVI sampling for different activation ratios from the MTU Pi-cloud chamber, highlighting the conditions that maximize droplet residual sampling while minimizing interstitial transmission. Even for a lower limit cloud activation ratio = 1:10, an add flow of 1.5 LPM achieves a residual fraction greater than 0.80, with a droplet TE of ∼15% for typical Pi-Chamber droplets with diameters between 3.5 to 10 µm. This framework can be adapted for field cloud measurements based on the cloud conditions of interest. TE for cloud droplets under flow conditions at which ∼99% of the unactivated submicron particles were removed was substantially lower between 8 and 16% than for supermicron dry particles (∼30 to 40% for 3 µm polystyrene latex spheres). In addition, we conducted a comparison of the performances of three similar PCVI units to assess repeatability for dry aerosols and cloud droplets. All three PCVIs performed similarly in rejecting submicron particles smaller than the desired cutoff diameter. One of the units showed lower TEs due to a misalignment of the internal orifice. We discuss a procedure that improved alignment and performance.

54 ENVIRONMENTAL SCIENCES↗