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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Assessment of buffer-IPyC thermomechanical debonding behavior using new experimental strength data in BISON

TRIstructural ISOtropic (TRISO) fuel is a nuclear fuel commonly used in High Temperature Gas-cooled Reactors (HTGRs). A single sub-millimeter-diameter TRISO fuel particle consists of a spherical fuel kernel surrounded by four coating layers: a low-density pyrocarbon buffer layer, an inner pyrolytic carbon (IPyC) layer, a silicon carbide (SiC) layer, and an outer pyrolytic carbon (OPyC) layer. The kernel is commonly made of UO2 or a mixture of uranium carbide and uranium oxide (UCO). During reactor operation, the TRISO coating layers are subjected to irradiation-induced dimensional changes and the associated thermomechanical behavior of each layer. One of the observed behaviors is gap formation between the buffer and IPyC layer due to the porous buffer’s irradiation-induced shrinkage exceeding that of the IPyC layer. Not all irradiated particles will experience buffer-IPyC gap formation. The debonding may be partial, or it may be nearly total. However, from post-irradiation examination of UCO TRISO fuels irradiated as part of the Advanced Gas Reactor (AGR) Fuel Development and Qualification Program, it was concluded that partial buffer-IPyC debonding was the most common type of buffer-IPyC interaction. To predict TRISO thermomechanical performance, multi-physics models have been built that are being continually updated and refined. The BISON code is a finite element-based nuclear fuel performance code that may be used for 1D, 2D, and 3D TRISO particle simulations. This code is used to calculate fuel temperature, kernel swelling, buffer densification, thermal and irradiation creep, fracture, and fission gas production and release. One of the recent additions to the BISON code is the ability to model the process of layer debonding. This paper will focus on the simulation results of the improved BISON debonding model that will utilize updated strengths measured from irradiated AGR TRISO fuel particles. The new experimental strength data from micromechanical tests of irradiated TRISO fuel samples were exercised in the BISON simulations and compared to baseline strength data to assess their applicability in the models. This also includes updated buffer-IPyC bond strengths to simulate layer delamination. Based on current experimental observations it is noted that the buffer-IPyC separation occurs not exactly at the junction of these two layers, but more on the side of the buffer layer. That observation is also implemented in the TRISO interface debonding model. This improved modeling approach using experimental strength data to characterize buffer-IPyC debonding and its potential subsequent cracking will be presented in the paper along with comparisons to available experimental observations.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Novel Instrumentation for Advanced Quantum Chromodynamics Studies with Flavor Sensitivity

The true nature of ordinary matter has always fascinated humankind, whose imagination has been pointed to the right direction since the 5th century BC with the first known atomic theory by Leucippus and Democritus. They described the matter as formed by small, invisible, indivisible, and eternal particles: the atoms. A long investigation followed them, including contributions from several of history?s greatest philosophers and scientists. The progress led to the understanding that atoms have an internal structure consisting of a central nucleus composed of protons and neutrons, surrounded by a cloud of electrons. About 50 years ago, scientists discovered that nucleons also have an internal structure. Through the Deep Inelastic Scattering (DIS) experiments, on which a lepton is scattered off a nucleon, it was possible to access the distribution of partons inside the nucleon along the longitudinal direction defined by the hard-scale probe. It was a crucial step in developing Quantum Chromodynamics (QCD), currently the best theory describing the subatomic matter. Ultimately, DIS was recognized as a limited tool to investigate the nucleon structure because it is mainly sensitive to observables at the probe?s energy scale. In recent decades, theoretical developments have allowed defining soft-scale observables by measuring more complex processes. Reactions such as Semi-Inclusive Deep Inelastic Scattering (SIDIS) with single or di-hadron production, can provide information about the momentum of parton inside the nucleon. In particular, polarized SIDIS allows access to the Transverse-Momentum-Dependent (TMD) parton distributions describing the correlations of the quark and gluon degrees of freedom in transverse momentum and spin. This study can provide three-dimensional imaging of nucleon structure and inner dynamics, as long as the hadronic component in the final state can be measured. Identifying the species of the produced particles provides information on the quark flavor and assumes a crucial role in this context. The thesis describes the work carried out by the author in preparing novel instrumentation for particle identification in the final state of DIS experiments, to support modern analysis of the parton dynamics within the basic confined object (nucleon) with flavor sensitivity. The work has been focused on the CLAS12 spectrometer in operation at Jefferson Laboratory (JLab), Newport News, VA, USA, and the ePIC experiment in preparation for the future Electron-Ion Collider (EIC) at Brookhaven National Laboratory (BNL), Long Island, NY, USA. CLAS12 is a fixed-target experiment using a 12 GeV beam of polarized electrons scattering off polarized nuclear targets. In 2018 and 2022, two Ring Imaging Cherenkov (RICH) detector modules were installed to improve the ?±/K± separation in the high-momentum region (3÷8 GeV/c) of the experiment. The author contributed to the assembly, installation, and com- missioning of the second RICH module, to the efficiency studies of the first module, and to the first SIDIS analysis with high-momentum kaons identified by the RICH. These studies led to the observation of the first spin asymmetry with high-momentum kaons from the CLAS12 experiment, and an initial assessment of the systematic error associated with the hadron identification. ePIC will be the first experiment at the future EIC, the new collider designed to expand the frontiers of QCD. The author was involved in the development of the dual-radiator Ring Imaging Cherenkov (dRICH). This detector will interpolate the measurements of the Cherenkov angles of photons produced by relativistic particles crossing two different radiators to identify charged hadrons. The author contributed to the studies conducted with the dRICH prototype, developing the reconstruction and analysis software and simulations, characterizing the aerogel radiator samples, and being responsible for the tracking system used during the beam tests. The performance obtained by the prototype has been progressively improved and the results are now comparable with the expectation derived from the simulation and satisfy the requirements of the experiment. In Chapter 1, the SIDIS theory is briefly introduced, outlying the connection with the experimental measurement. Chapter 2 includes the description of the CLAS12 RICH, its assembly and installation, and the efficiency study. In Chapter 3, the analysis of the Beam-Spin Asymmetry associated with SIDIS kaons is described. Chapter 4 describes the contribution to the dRICH for EIC, starting from a description of the ePIC experiment and focusing on the studies performed for the dRICH prototype. The conclusions of this work are summarized at the end.

Vallarino, Simone↗
DOE OSTI2023

Mass-induced confinement near the sill of the conformal window

We revisit standard arguments for hyperscaling of the spectrum when a nonzero fermion mass is introduced to a gauge-fermion theory which is conformal in the infrared limit. With some general assumptions, we argue that the induced confinement scale will be significantly enhanced near the edge of the conformal to confining transition. This enhancement can allow for the fermion mass to be arbitrarily small compared to the confinement scale. This scale separation may allow for apparent spontaneous breaking of chiral symmetry within the conformal window, which may be of interest for construction of dilaton effective field theories in this regime.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2024

Development and test of a large-aperture Nb3Sn cos-theta dipole coil with stress management

The stress-managed cos-theta (SMCT) coil is a new concept which was proposed and is being developed at Fermilab in the framework of US Magnet Development Program (US-MDP) for high-field and/or large-aperture accelerator magnets based on low-temperature and high-temperature superconductors. A 120-mm aperture two-layer Nb3Sn SMCT dipole coil has been developed at Fermilab to demonstrate and test the SMCT concept including coil design, fabrication technology and performance. The first SMCT demo coil was fabricated and assembled with 60-mm aperture Nb3Sn coil inside a dipole mirror configuration and tested separately and in series with the insert coil. This paper summarizes the design, parameters, and quench performance of the 120-mm aperture SMCT coil in a dipole mirror configuration.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

NorthStar Helium Cooling System. Final Report on LANL Contribution

From the beginning of NNSA support to the NorthStar development of a production facility for the medical isotope Molybdenum-99 (Mo99), LANL has been responsible for the design and testing of a target and its cooling. The target is comprised of a stack of Mo100 disks separated by coolant flow gaps between the disks and between the first disk and a housing window, which separates the target and its coolant from the vacuum of the beam line. The target, and therefore its cooling requirements, evolved steadily over the years of system development

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2022

Development of an MCP-Based Timing Layer for the LHCb ECAL Upgrade-2

The increase in instantaneous luminosity during the high-luminosity phase of the LHC represents a significant challenge for future detectors. A strategy to cope with high-pileup conditions is to add a fourth dimension to the measurements of the hits, by exploiting the time separation of the various proton–proton primary collisions. According to LHCb simulation studies, resolutions of about 10–20 picoseconds, at least an order of magnitude shorter than the average time span between primary interactions, would be greatly beneficial for the physics reach of the experiment. Microchannel plate (MCP) photomultipliers are compact devices capable of measuring the arrival time of charged particles with the required resolution. The technology of large-area picosecond photodetectors (LAPPDs) is under investigation to implement a timing layer that can be placed within a sampling calorimeter module with the purpose of measuring the arrival time of electromagnetic showers. LAPPD performances, using a Gen-I tile with a delay-line anode and a Gen-II with a capacitively coupled anode, have been measured thoroughly both with laser (wavelength of 405 nm and pulse width of 27.5 ps FWHM) and high-energy electron (1–5.8 GeV) beams. Time resolutions of the order of 30 ps for single photoelectrons and 15 ps for electromagnetic showers initiated by 5-GeV electrons, as measured at the shower maximum, are obtained.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

On the Short-scale Spatial Variability of Electron Inflows in Electron-only Magnetic Reconnection in the Turbulent Magnetosheath Observed by MMS

We investigate the detailed properties of electron inflow in an electron-only reconnection event observed by the four Magnetospheric Multiscale (MMS) spacecraft in the Earth's turbulent magnetosheath downstream of the quasi-parallel bow shock. The lack of ion coupling was attributed to the small-scale sizes of the current sheets, and the observed bidirectional super-Alfvénic electron jets indicate that the MMS spacecraft crossed the reconnecting current sheet on both sides of an active X-line. Remarkably, the MMS spacecraft observed the presence of large asymmetries in the two electron inflows, with the inflows (normal to the current sheet) on the two sides of the reconnecting current layer differing by as much as a factor of four. Furthermore, even though the four MMS spacecraft were separated by less than seven electron skin depths, the degree of inflow asymmetry was significantly different at the different spacecraft. The asymmetry in the inflow speeds was larger with increasing distances downstream from the reconnection site, and the asymmetry was opposite on the two sides of the X-line. We compare the MMS observations with a 2D kinetic particle-in-cell (PIC) simulation and find that the asymmetry in the inflow speeds stems from in-plane currents generated via the combination of reconnection-mediated inflows and parallel flows along the magnetic separatrices in the presence of a large guide field.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2023

Particle Scale Impacts on Deconstruction Energy of Pine Residues

The goal of this Case Study was to quantify the impacts of variable moisture and ash on hammer mill throughput and energy consumption and on generation of fines that are not able to be fed to conversion, as compared to a status quo Base Case system. Also considered was convertible carbon content (minimum carbon specification) and maximum ash content and the delivered feedstock cost impacts of not being able to feed residue not meeting both specifications to the conversion reactor. Laboratory data on the impacts of input particle size and moisture content on the exit particle size were received from FCIC Subtask 5.2: Preprocessing, High Temperature Conversion Preprocessing from their single particle impact population balance modeling study (Tiasha Bhattacharjee, INL). Additional throughput and energy consumption data were obtained from FCIC Subtask 5.2 (Jordan Klinger, INL) for the same grinder with a 6 mm screen in place. These data were utilized to develop the necessary response surface equations to perform throughput analysis using discrete event simulation. Because the ash contents in the separated fines had not been analyzed in the laboratory at the time of the model runs, we chose to assume that the ash distributed proportionally with total mass into the overs and unders in the disk screen following grinding.

energy consumption↗
DOE OSTI2023

Inhibit the strain accumulation for 5V spinel cathode by mitigating the phase separation during high voltage stage

LiNi 0.5 Mn 1.5 O 4 (LNMO) spinel cathode is a potential cathode material for high-power, low-cost lithium-ion batteries (LIBs) due to its low raw material cost, high operating voltage and efficient lithium-ion transport channel. However, LNMO suffers from structural stability due to the two-phase-transformation during charge/discharge process, leading to poor cycling performance. Here, to address the issues, we have constructed a homogeneous aggregated LNMO cathode with a multifaceted primary particle, namely the LNMO with single-crystal secondary particles (SSP LNMO). Ex situ and in situ characterizations including the synchrotron X-ray diffraction, the neutron diffraction and full pouch cell validated that the SSP LNMO exhibit a single solid-solution reactions with a restrained lattice evolution during the delithiation/lithiation process. This is in contrast to the normal LNMO cathode, which demonstrates a significant two-phase transition from spinel Li 1-x Ni 0.5 Mn 1.5 O 4 to rock-salt MnO 2 at high voltage. Therefore, the SSP LNMO has greatly improved cycle life compared to the normal LNMO cathode. Overall, this study demonstrates the possibility of constructing LNMO based on primary-grain morphology modulation to improve the intrinsic stability of LIBs.

25 ENERGY STORAGE↗
DOE OSTI2026

Neutron reconstruction via blips in liquid argon time projection chambers

Neutrons are important final-state particles in neutrino interactions, yet they are not considered or reconstructed in most current neutrino liquid argon time projection chamber (LArTPC) physics analyses. In this paper, we present a simulation-based proof-of-concept study of neutron reconstruction in a generic LArTPC detector. Leveraging isolated, MeV-scale energy deposits, or blips, from neutron inelastic scattering, and using realistic blip response from published experimental results, we demonstrate the capability to identify neutrons and to reconstruct the direction and energy of the final-state neutron system in sub-GeV neutrino interactions. We then explore how neutron-related blip attributes can be used to improve physics studies of neutrino interactions, such as enhancing neutrino-antineutrino separation in atmospheric neutrinos and reverse-horn-current beam neutrinos. This study provides an initial quantification of LArTPC neutron reconstruction capabilities, which we expect to improve with future advancements in blip reconstruction, identification, and classification algorithms, as well as the modeling of neutrons.

Morquecho, Miguel Hernandez [Univ. of Minnesota, M↗
DOE OSTI2022

Structural basis for inhibition of the Cation-chloride cotransporter $\mathrm{NKCC1}$ by the diuretic drug bumetanide

Cation-chloride cotransporters (CCCs) NKCC1 and NKCC2 catalyze electroneutral symport of 1 Na + , 1K + , and 2 Cl - across cell membranes. NKCC1 mediates trans-epithelial Cl - secretion and regulates excitability of some neurons and NKCC2 is critical to renal salt reabsorption. Both transporters are inhibited by the so-called loop diuretics including bumetanide, and these drugs are a mainstay for treating edema and hypertension. Here, our single-particle electron cryo-microscopy structures supported by functional studies reveal an outward-facing conformation of NKCC1, showing bumetanide wedged into a pocket in the extracellular ion translocation pathway. Based on these and the previously published inward-facing structures, we define the translocation pathway and the conformational changes necessary for ion translocation. We also identify an NKCC1 dimer with separated transmembrane domains and extensive transmembrane and C-terminal domain interactions. We further define an N-terminal phosphoregulatory domain that interacts with the C-terminal domain, suggesting a mechanism whereby (de)phosphorylation regulates NKCC1 by tuning the strength of this domain association.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Measurement of Conduction and Valence Bands g -Factors in a Transition Metal Dichalcogenide Monolayer

The electron valley and spin degree of freedom in monolayer transition-metal dichalcogenides can be manipulated in optical and transport measurements performed in magnetic fields. The key parameter for determining the Zeeman splitting, namely, the separate contribution of the electron and hole g factor, is inaccessible in most measurements. Here we present an original method that gives access to the respective contribution of the conduction and valence band to the measured Zeeman splitting. It exploits the optical selection rules of exciton complexes, in particular the ones involving intervalley phonons, avoiding strong renormalization effects that compromise single particle g -factor determination in transport experiments. These studies yield a direct determination of single band g factors. We measure g c1 = 0.86 ± 0.1, g c2 = 3.84 ± 0.1 for the bottom (top) conduction bands and g v = 6.1 ± 0.1 for the valence band of monolayer WSe 2 . These measurements are helpful for quantitative interpretation of optical and transport measurements performed in magnetic fields. In addition, the measured g factors are valuable input parameters for optimizing band structure calculations of these 2D materials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Cylindricity Sensitivity Thermal Model of the AGR-5/6/7 Experiment in the Advanced Test Reactor

The AGR-5/6/7 experiment is currently being irradiated in the Advanced Test Reactor (ATR) at the Idaho National Laboratory and is approximately 70% complete. Several fuel and material irradiation experiments have been planned for the U.S. Department of Energy Advanced Gas Reactor Fuel Development and Qualification Program, which supports the development and qualification of tristructural isotropic (TRISO) coated particle fuel for use in high-temperature gas-cooled reactors. The goals of these experiments are to provide irradiation performance data to support fuel process development, qualify fuel for normal operating conditions, support development of fuel performance models and codes, and provide irradiated fuel and materials for post-irradiation examination and safety testing. Originally planned and named as separate fuel experiments, but subsequently combined into a single test train, AGR-5/6/7 is testing low-enriched uranium oxycarbide TRISO fuel. The AGR-5/6/7 test train has 5 capsules with thermocouples and independent gas control mixtures. Unique to this paper is a sensitivity study concerning the cylindricity of the graphite holders containing the fuel compacts and their eccentricity in relation to the stainless-steel capsule walls. Each capsule has small nubs on the outside used for centering the graphite holder inside the stainless-steel capsule with a small gas gap used to control temperature. Due to machining tolerances of these nubs and vibration wearing the nubs down when the experiment is running in the reactor, the possibility exists that the holder may move around radially. Each capsule is equipped with several thermocouples placed at various radii and depths within each graphite holder. This paper will show the sensitivity of offsetting the graphite holder for various radii in 45-degree increments around the circle with the objective of minimizing the difference between the measured thermocouples and the modeled thermocouple temperatures. Separate gas mixtures of helium/neon are introduced into this gas gap between the holder and capsule wall and changed as necessary to maintain the desired thermocouple temperatures to keep the fuel compacts at constant temperature as the nuclear reactor conditions change. The goal of the sensitivity study is to find a radius and an angle to offset the holder from perfectly centered for each of the five capsules separately. The complex thermal model includes fission heating, gamma heating, radiation heat transfer, and heat transfer via conduction and radiation across the control gaps. Subroutines linked to the thermal model offer an easy method to offset the graphite holder from the capsule walls without remeshing the entire model.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Metallic Coating of Cerium Oxide Microspheres

The ability to remove heat is paramount to nuclear fuel performance and longevity. Retaining fission product and separating fuel from reactor coolant and the environment is also necessary to prevent radiological contamination. Conventional nuclear fuel for commercial light water reactors and radioisotope power systems (RPS) is composed of oxide powders pressed into a pellet (cm-scale) and then sealed into a metal cladding to confine the fuel. What typical fuels lack is a method to surround each particle of nuclear fuel in metal, thus providing a more intimate protection layer for accident tolerance and boosting the thermal extraction from the fuel element. In such a way, metal-coated fuel particles increase heat extraction efficiency over clad-pellet designs while increasing the accident tolerance of the fuel. Metal oxide microspheres have wide-ranging applications, including the realm of fuels for nuclear reactors and RPS. Microspheres of uranium oxide/uranium carbide, mixed uranium/plutonium oxides, transuranics, and thorium fuels have been extensively studied. Pacific Northwest National Laboratory has also demonstrated the production of 238 PuO 2 microspheres for RPS applications. Metal-coated oxide microsphere fuels may also be attractive for other applications such as nuclear thermal rockets, future nuclear reactor designs, and catalysts.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

A Novel Sustainable Process for Multilayer Graphene Synthesis Using CO 2 from Ambient Air

Graphene produced by different methods can present varying physicochemical properties and quality, resulting in a wide range of applications. The implementation of a novel method to synthesize graphene requires characterizations to determine the relevant physicochemical and functional properties for its tailored application. We present a novel method for multilayer graphene synthesis using atmospheric carbon dioxide with characterization. Synthesis begins with carbon dioxide sequestered from air by monoethanolamine dissolution and released into an enclosed vessel. Magnesium is ignited in the presence of the concentrated carbon dioxide, resulting in the formation of graphene flakes. These flakes are separated and enhanced by washing with hydrochloric acid and exfoliation by ammonium sulfate, which is then cycled through a tumble blender and filtrated. Raman spectroscopic characterization, FTIR spectroscopic characterization, XPS spectroscopic characterization, SEM imaging, and TEM imaging indicated that the graphene has fifteen layers with some remnant oxygen-possessing and nitrogen-possessing functional groups. The multilayer graphene flake possessed particle sizes ranging from 2 µm to 80 µm in diameter. BET analysis measured the surface area of the multilayer graphene particles as 330 m 2 /g, and the pore size distribution indicated about 51% of the pores as having diameters from 0.8 nm to 5 nm. This study demonstrates a novel and scalable method to synthesize multilayer graphene using CO 2 from ambient air at 1 g/kWh electricity, potentially allowing for multilayer graphene production by the ton. The approach creates opportunities to synthesize multilayer graphene particles with defined properties through a careful control of the synthesis parameters for tailored applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Thermal Model Heat Rate Predictions of the AGR-5/6/7 Experiment

Several fuel and material irradiation experiments have been planned for the U.S. Department of Energy Advanced Gas Reactor Fuel Development and Qualification Program, which supports the development and qualification of tristructural isotropic (TRISO) coated particle fuel for use in high-temperature gas-cooled reactors. The goals of these experiments are to provide irradiation performance data to support fuel process development, qualify fuel for normal operating conditions, support development of fuel performance models and codes, and provide irradiated fuel and materials for post-irradiation examination and safety testing. Originally planned and named as separate fuel experiments, but subsequently combined into a single test train. AGR-5/6/7 will test low-enriched uranium oxycarbide (UCO – a heterogeneous mixture of uranium oxide and uranium carbide) TRISO fuel. The AGR-5/6 portion of the experiment will provide data to support qualification of the selected reference fuel design, while the AGR-7 portion will serve as a margin test, irradiating the fuel beyond normal operating conditions. During irradiation, the temperature in each capsule is controlled by varying the helium / neon gas mixture flowing through the capsule until the desired thermocouple temperature is reached. Further adjustments can be made by changing the lobe power and the neutron filter. Three neutron filters are available to use as the experiment burns up the fissionable fuel. A thermal finite element model has been created for the five capsules comprising the AGR-5/6/7 experiment. Heat rates from a physics analysis are imported into the model along with fast neutron fluence. Graphite shrinkage due to the fast neutron fluence is incorporated into the model. Gas gaps change as a function of fast neutron fluence. Radiation heat transfer is a major contributor in this model. This is a large model with more than 1 million finite element brick elements. More than 150 different parts are modeled in the finite element model and communicate with each other from a heat transfer sense. More than 50 thermocouples are used in the experiment and are compared to actual measurements. The experiment is composed of five separate stainless steel capsules all welded together. This paper presents a method used to predict the gas mixture in the event that all of the thermocouples fail in a particular capsule. Curve fitting of heat rates from previous cycles and projecting them into the future is the basis of the method.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Development of a compact electron cyclotron resonance accelerator for industrial and security applications

We describe the development of a novel accelerator, an electron Cyclotron Resonance Accelerator (eCRA) [1], to produce high power electron beams and X-ray beams for medical, research, sterilization, and national security applications. The several attractive features of eCRA include: a compact robust room-temperature single-cell RF cavity as the accelerating structure; continuous ampere-level high current output; and production of a self-rastering electron beam, thus eliminating the need for a separate beam scanner. Progress on the eCRA development, including numerical simulation, engineering design, and on-going experimental efforts will be reported here.

43 PARTICLE ACCELERATORS↗
DOE OSTI2021

The pervasive impact of critical fluctuations in liquid–liquid extraction organic phases

Liquid-liquid extraction is an essential chemical separation technique where polar solutes are extracted from an aqueous phase into a nonpolar organic solvent by amphiphilic extractant molecules. A fundamental limitation to the efficiency of this important technology is third phase formation, wherein the organic phase splits upon sufficient loading of polar solutes. The nanoscale drivers of phase splitting are challenging to understand in the complex hierarchically structured organic phases. In this study, we demonstrate that the organic phase structure and phase behavior are fundamentally connected in a way than can be understood with critical phenomena theory. For a series of binary mixtures of trialkyl phosphate extractants with linear alkane diluents, we combine small angle x-ray scattering and molecular dynamics simulations to demonstrate how the organic phase mesostructure over a wide range of compositions is dominated by critical concentration fluctuations associated with the critical point of the third phase formation phase transition. These findings reconcile many longstanding inconsistencies in the literature where small angle scattering features, also consistent with such critical fluctuations, were interpreted as reverse micellar-like particles. Altogether, this study shows how the organic phase mesostructure and phase behavior are intrinsically linked, deepening our understanding of both and providing a new framework for using molecular structure and thermodynamic variables to control mesostructure and phase behavior in liquid-liquid extraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗