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At least 235 records · Page 13

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DOE OSTI2024

Cast Film Production with Polyethylene Recycled from a Post-Industrial Printed Multilayer Film by Solvent-Targeted Recovery and Precipitation

The solvent-targeted recovery and precipitation (STRAP) process separates and recovers the constituent resins in multilayer plastic packaging films by selective polymer dissolution. In this work, three different experimental methods were considered to recover a polyethylene (PE) resin from a printed multilayer film by STRAP. The methods consisted of (1) a filter bag system, (2) a Soxhlet extraction, and (3) a jacketed dissolution vessel. Cast films were produced with the PE recovered from each method and were analyzed for color, mechanical properties, and number of impurities. High-quality recycled PE cast films can be produced by increasing the solvent to plastic ratio, including a filter pore size of 100 μm, and optimizing temperature control in STRAP. Furthermore, this study demonstrates that STRAP polymers can be recycled back into plastic films, enabling the potential circularity of these packaging materials.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Structure of Gas Phase Monohydrated Nicotine: Implications for Nicotine’s Native Structure in the Acetylcholine Binding Protein

In this work, we report a joint experimental–theoretical study of the never reported before structure and infrared spectra of gas phase monohydrated nicotine (NIC) and nornicotine (NOR) and use them to assign their protonation sites. NIC’s biological activity is strongly affected by its protonation site, namely, the pyrrolidine (Pyrro-NICH + , anticipated active form) and pyridine (Pyri-NICH + ) forms; however, these have yet to be directly experimentally determined in either the nicotinic acetylcholine receptor (nAChR, no water present) or the acetylcholine-binding protein (AChBP, a single water molecule is present) but can only be inferred to be Pyrro-NICH + from the intermolecular distance to the neighboring residues (i.e., tryptophan). Our temperature-controlled double ion trap infrared spectroscopic experiments assisted by the collisional stripping method and high-level theoretical calculations yield the protonation ratio of Pyri:Pyrro = 8:2 at 240 K for the gas phase NICH + ···(H 2 O) complex, which resembles the molecular cluster present in the AChBP. Therefore, a single water molecule in the gas phase enhances this ratio in NICH + relative to the 3:2 for the nonhydrated gas phase NICH + in a trend that contrasts with the almost exclusive presence of Pyrro-NICH + in aqueous solution. In contrast, the Pyri-NORH + protomer is exclusively observed, a fact that may correlate with its weaker biological activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

A Robust Methodology to Elucidate Kinetics of Room Temperature Electrochemical Propane Adsorption on Platinum

Electrocatalytic activation of alkanes can further decarbonize chemical manufacturing by leveraging affordable renewable electricity and readily available shale gas reserves in the United States. Earlier works have identified the unique role of Pt in adsorbing and activating alkanes, like propane, at room temperature in acidic, aqueous electrolytes, revealing spontaneous formation of deeply dehydrogenated propane-derived surface species with an intact C 3 - backbone. Although an adsorption mechanism was hypothesized, it has not been explicitly investigated to date, preventing the quantification of kinetic rate parameters. A robust methodology to investigate and benchmark propane adsorption kinetics on Pt is critical for the rational design of electrocatalysts that exhibit higher selectivity toward desired partially oxidized products. Herein, we analyze an oxidative current transience that appears during the adsorption of propane on Pt in aqueous electrochemical conditions and develop a methodology that elucidates the adsorption mechanism and enables quantification of rate parameters such as order dependences and apparent activation barriers. This method yields an expected first-order dependence with respect to propane concentration at low coverage and reveals a second-order dependence with respect to the concentration of surface active sites. Additionally, the apparent activation barrier for propane adsorption was calculated using an Arrhenius analysis of the current transience under temperature control. The experimentally measured activation barrier of 35 kJ mol –1 is in excellent agreement with the theoretical barrier calculated by density functional theory (DFT). The kinetic analysis was extended, via the use of transition state theory, to extract entropy and enthalpy of activation, yielding consistent results with the proposed two-step adsorption mechanism and DFT calculations. These results demonstrate reliable quantification of kinetic parameters for electrocatalytic activation of C–H bonds in alkanes that can be employed for rational catalyst development for a versatile range of electrocatalytic conditions.

alkane activation↗

DOE OSTI2025

Enhancing Turbulent Mixing and Microphysical Uniformity in a Tall Convection‐Cloud Chamber Through Idealized Heterogeneity of Boundaries

A large convection cloud chamber has been proposed for exploring aerosol–cloud–drizzle interactions under well‐controlled turbulent conditions. Recent theoretical and numerical studies suggest that a convection cloud chamber with two heated and two cooled sidewalls can significantly enhance the liquid water content and thus benefit drizzle initiation. However, a chamber with such a sidewall configuration develops stable stratification and extremely weak turbulence therein. In this study, we conduct large‐eddy simulations of a tall convection chamber with five different sidewall configurations consisting of alternating warm and cold patches. For each configuration, the total surface area of warm patches equals that of cold patches, resulting in the same expected cloud‐free supersaturation based on a flux budget model. Results show that changing the sidewall configuration, while keeping all other factors constant, can substantially enhance turbulent mixing and improve the uniformity of thermodynamic and cloud microphysical properties in the bulk region of the chamber. In addition, turbulence strength is positively correlated with liquid water content and negatively correlated with cloud droplet number concentration, consistent with theoretical predictions. Our results highlight the advantage of building a large cloud chamber using modular patches with individually controllable temperature and humidity to achieve well‐mixed conditions.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Solid-state laser refrigeration of a composite semiconductor Yb:YLiF 4 optomechanical resonator

Photothermal heating represents a major constraint that limits the performance of many nanoscale optoelectronic and optomechanical devices including nanolasers, quantum optomechanical resonators, and integrated photonic circuits. Here, we demonstrate the direct laser refrigeration of a semiconductor optomechanical resonator >20 K below room temperature based on the emission of upconverted, anti-Stokes photoluminescence of trivalent ytterbium ions doped within a yttrium-lithium-fluoride (YLF) host crystal. Optically-refrigerating the lattice of a dielectric resonator has the potential to impact several fields including scanning probe microscopy, the sensing of weak forces, the measurement of atomic masses, and the development of radiation-balanced solid-state lasers. In addition, optically refrigerated resonators may be used in the future as a promising starting point to perform motional cooling for exploration of quantum effects at mesoscopic length scales, temperature control within integrated photonic devices, and solid-state laser refrigeration of quantum materials.

42 ENGINEERING↗

DOE OSTI2025

Fast product release requires active-site water dynamics in carbonic anhydrase

Water plays an essential role in enzyme structure, stability, and the substantial rate enhancement of enzyme catalysis. However, direct observations linking enzyme catalysis and active-site water dynamics pose a significant challenge due to experimental difficulties. By integrating an ultraviolet (UV) photolysis technique with temperature-controlled X-ray crystallography, we track the catalytic pathway of carbonic anhydrase II (CAII) at 1.2 Å resolution. This approach enables us to construct molecular movies of CAII catalysis, encompassing substrate (CO 2 ) binding, conversion from substrate to product (bicarbonate), and product release. In the catalytic pathway, we identify an unexpected configuration in product binding and correlate it with sub-nanosecond rearrangement of active-site water. Based on these experimental observations, we propose a comprehensive mechanism of CAII and describe the detailed structure and dynamics of active-site water in CAII. Our findings suggest that CAII has evolved to utilize the structure and fast dynamics of the active-site waters for its diffusion-limited catalytic efficiency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Maximizing long-term biohydrogen production with Clostridium thermocellum for high solids conversion of lignocellulosic biomass

Biological hydrogen production from lignocellulosic biomass sustainably couples organic waste reduction with renewable energy generation. Efficient conversion is challenged by the structural complexity of lignocellulose and resulting recalcitrance to enzymatic degradation. Clostridium thermocellum natively breaks down biomass with highly effective hemi-/cellulases systems (i.e., cellulosomes) and generates hydrogen in anaerobic cultivation, creating a compelling platform for lignocellulosic biohydrogen production. Achieving commercially viable production rates requires balancing high biomass loading and throughput against uniform mixing conditions required for enzyme dispersion, pH and temperature control, and efficient hydrogen and metabolite removal in continuous operation. To address these barriers to process intensification, we implemented novel reactor and process designs for high-solids lignocellulosic biomass fermentations using the C. thermocellum KJC19-9 strain, genetically engineered for co-utilization of cellulose and hemicellulose sugars (i.e., xylose). Via computational fluid dynamics (CFD) modeling and experimental validation, we achieved a >50% improvement in biohydrogen production with an improved anchor-type impeller morphology, coupled to a threefold reduction in agitation rate. To further reduce rheological constraints and accumulation of toxic metabolites, we then transitioned the process to sequencing fed-batch operation. The resulting process generated 24.87 L H 2 L −1 from 160 g L −1 of deacetylated and mechanically refined (DMR)-pretreated corn stover biomass over 16 days while solubilizing >95% of influent cellulose and hemicellulose, setting a new performance benchmark for continuous production of biohydrogen from lignocellulose.

08 HYDROGEN↗

DOE OSTI2022

Effect of substrate temperature on sputter-deposited boron carbide films

Sputter deposition of B4C films with tailored physical properties remains a challenge. Here, we systematically study how substrate temperature influences the properties of B4C films deposited by direct current magnetron sputtering onto planar substrates held at temperatures in the range of 100-510°C. Results show that all films are amorphous stoichiometric B4C, with low O content of ~1 at. %. Films deposited onto substrates at 100°C exhibit high compressive residual stress and decreased mechanical properties. Therefore, for elevated substrate temperatures in the range of 180-510°C, film mass density, surface roughness, Young’s modulus, and hardness are weakly dependent on substrate temperature. However, in this temperature range, an increase in substrate temperature leads to larger residual compressive stress accompanied by a corresponding reduction in the concentration of nanoscale inhomogeneities. At least for the landing atom ballistics conditions studied here, a substrate temperature range of ~185-250°C is optimum for growing films with near-zero intrinsic residual stress. The overall weak substrate temperature dependence of film properties revealed in this work is favorable for the development of a robust deposition process, particularly for the case of deposition onto non-planar substrates where temperature control is often challenging.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Demonstration of improved laser preheat with a cryogenically cooled magnetized liner inertial fusion platform

We report on progress implementing and testing cryogenically cooled platforms for Magnetized Liner Inertial Fusion (MagLIF) experiments. Two cryogenically cooled experimental platforms were developed: an integrated platform fielded on the Z pulsed power generator that combines magnetization, laser preheat, and pulsed-power-driven fuel compression and a laser-only platform in a separate chamber that enables measurements of the laser preheat energy using shadowgraphy measurements. The laser-only experiments suggest that ~89% ± 10% of the incident energy is coupled to the fuel in cooled targets across the energy range tested, significantly higher than previous warm experiments that achieved at most 67% coupling and in line with simulation predictions. The laser preheat configuration was applied to a cryogenically cooled integrated experiment that used a novel cryostat configuration that cooled the MagLIF liner from both ends. Furthermore, the integrated experiment, z3576, coupled 2.32 ± 0.25 kJ preheat energy to the fuel, the highest to-date, demonstrated excellent temperature control and nominal current delivery, and produced one of the highest pressure stagnations as determined by a Bayesian analysis of the data.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

A liquid metal dropper for experiments on the wettability of liquid metals on plasma facing components

A liquid metal dropper has been developed as a part of the Ion-Gas-Neutral Interactions with Surfaces 2 (IGNIS-2) facility at The Pennsylvania State University. The dropper has the capability of directly applying drops to candidate plasma facing materials for nuclear fusion reactors to enable measurements of their liquid metal wetting properties. The results presented here are specific to the use of lithium in the dropper. This paper discusses the design choices of the liquid metal dropper and its chamber, including the heating and temperature control and the dropper’s motorized operation. Lithium drops of masses ranging from 0.05 g up to 0.13 g, equivalent to drop diameters between 5.6 mm to 1 cm, have been consistently dispensed by the dropper. A new algorithm is developed and used to automate the analysis of the contact angle between the liquid drops and substrate material for efficient analysis of video data recorded to study the wetting properties of candidate plasma-facing components.

Instruments & Instrumentation↗

DOE OSTI2026

Design improvements for a recirculating reactor: Enhanced temperature measurement and sample-isolated reactivity in steady-state kinetic studies

Building upon a previous recirculating reactor design [S.A. Tenney, K. Xie, J.R. Monnier, A. Rodriguez, R.P. Galhenage, S. Audrey, D.A. Chen, Rev. Sci. Instrum. 84, 104101 (2013)], we present significant improvements that address key limitations in steady-state kinetic measurements for heterogeneous catalysis. The enhanced reactor design features direct sample heating with a focused IR lamp and temperature measurement in direct contact with the sample, enabling more accurate temperature control and improved kinetic analysis. A critical advancement is the isolation of sample reactivity from reactor wall contributions, ensuring that only the sample contributes to measured reaction rates. This was a limitation in earlier designs where the entire reactor contributed to the observed reactivity. The system incorporates a bypass flow cell for direct comparison with powder catalysts under identical conditions using a standard plug-flow reactor configuration. We demonstrate these capabilities through CO oxidation experiments on Pt(111) single crystals and graphene-passivated Pt(111), highlighting the system's ability to differentiate catalytic activity in model systems and directly compare them with high surface area powder catalysts. This reactor is particularly suited for thin films and low surface area catalysts that are not effectively evaluated in traditional flow reactors, especially for samples with low numbers of active sites or slow reaction rates.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Cryogenic and Temperature-Dependent Photoelectron Spectroscopy of Metal Complexes

Negative ion photoelectron spectroscopy (NIPES) coupled with electrospray ionization (ESI) has been proved to be a powerful gas-phase spectroscopic tool for characterizing electronic structures and chemical bonding of a variety of cluster anions and corresponding neutral radicals involved in the condensed phase reactions and transformations. Since the acquisition of cryogenic and temperature-controlling capabilities, broader range of research scope has been covered. This review summarizes our recent investigations on metal complexes employing cryogenic ESI-NIPES that provide us essential information towards understanding complicated condensed phase reactions including hydrocarbon activations and electron transfer reactions, and afford us spectroscopic probe of highly reactive transient species and intimate redox pairs. Special attention has been drawn to connect gas phase photodetachment processes with solution phase redox reactions. Photodetachment of transition metal-EDTA complexes has been systematically investigated to model the sequential oxidation reactions of these species in solutions. The obtained gas phase electron affinity (EA) is compared with the solution redox potential (E1/2) and the metal ionization potential (IP) for several series of homologous metal complexes to emphasize their intrinsic correlations with deviations being largely modulated by different degrees of ligand participations.

Yuan, Qinqin↗

DOE OSTI2026

Experimental evaluation of the vapor box divertor concept with an open vapor box module in Magnum-PSI

A promising approach to handle the intense plasma heat flux in the divertor region of a tokamak is the Vapor Box Divertor (VBD). Here plasma-lithium interaction creates a dense lithium vapor cloud which interacts with the incoming plasma, effectively shielding the tungsten surface beneath, therefore preventing overheating and sputtering of the tungsten and increasing the component’s lifetime. Two key steps must be addressed to validate this concept: investigating plasma-Li interactions and the transport mechanism of the latter in the presence of plasma. To explore this, a Vapor Box Module (VBM) has been designed for use with the linear plasma generator Magnum-PSI. The VBM consists of a series of three cylindrical boxes, with Li being evaporated at a controlled temperature in the central box (CB). Divertor-like plasma enters the VBM from an upstream aperture, interacts with the Li vapor cloud and exits through a downstream aperture ultimately impacting a target equipped with a calorimetry system. Optical diagnostics Thomson scattering, Filtered fast camera Imaging and optical emission spectroscopy provided information on plasma parameters in terms of electron density n e , temperature T e and plasma composition before and after this interaction. A significant reduction in plasma power was observed upon the establishment of lithium vaporization determined via cooling water calorimetry and embedded thermocouples at the downstream target. This resulted in a drop of the target temperature from ∼800 °C to ∼350 °C (57%) at the highest applied power (11.1 MW m −2 ) and CB temperature (∼700 °C). Lithium condensation at the side boxes of the VBM in combination with strong plasma momentum transfer effectively prevented upstream migration of lithium, while enhancing Li transport toward the target. The achievement of the two main goals of reducing plasma power and confining the Li in the VBM, are consistent with earlier published preliminary SOLPS-ITER simulations. This study shows that the presence of lithium in a VBD-like configuration can result in a strong reduction of power to the target surface, while at the same time the lithium vapor is effectively confined by the VBM, aided by the incoming plasma, preventing its escape from the VBM geometry. This represents a valuable step toward validating the feasibility of the VBD configuration in future fusion reactors.

Magnum-PSI↗

DOE OSTI2022

MAGIS-100 environmental characterization and noise analysis

We investigate and analyze site specific systematics for the MAGIS-100 atomic interferometry experiment at Fermi National Accelerator Laboratory. As atom interferometers move out of the laboratory environment passive and active mitigation for noise sources must be implemented. To inform the research and development of the experiment design, we measure ambient temperature, humidity, and vibrations of the installation site. We find that temperature fluctuations will necessitate enclosures for critical subsystems and a temperature controlled laser room for the laser system. We also measure and analyze the vibration spectrum above and below ground for the installation site. The seismic vibration effect of gravity gradient noise is also modeled using input from a low-noise seismometer at multiple locations and a mitigation scheme is studied using a stochastic simulation and characterized by a suppression factor.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Design of the cryogenic moderator system for the second target station

The Second Target Station (STS) at Oak Ridge National Laboratory will be a 700 kW pulsed spallation neutron source designed to provide the world's highest brightness cold neutron beams. In order to produce the required neutron performance, two compact liquid hydrogen moderators are located adjacent to the tungsten spallation target and must be supplied with less than 20 K hydrogen and a para hydrogen fraction of 99.8% or greater. The Cryogenic Moderator System (CMS) will consist of a single hydrogen loop feeding the two moderators in series cooled by a helium refrigerator with a cooling capacity of 2.5 kW at 17 K. The hydrogen loop consists of a hydrogen circulator, hydrogen helium heat exchanger, ortho-para converter, accumulator, transfer lines and heater. The design of the hydrogen loop is based on the CMS design of the First Target Station at the Spallation Neutron Source and some of the component designs may be reused. General hydrogen temperature control is provided by controlling the flowrate of helium to the heat exchanger. The hydrogen loop will have a constant flowrate of 0.5 L/s and remove a nuclear heat load of about 850 W from the two moderators, which is deposited both directly in the hydrogen and the adjacent hydrogen containing structures. Because the nuclear heat load is accelerator driven, the hydrogen system must remain stable when the heat load is removed instantaneously during beam trips. System stability is maintained passively with the accumulator and actively with the heater. Ionizing radiation which interacts with the liquid hydrogen drives backconversion of the hydrogen from parahydrogen to orthohydrogen. The STS moderator performance is very sensitive to small fractions of orthohydrogen requiring an ortho-para converter to maintain the hydrogen supplied to the moderators at near equilibrium parahydrogen concentration. STS CMS is in the early stage of preliminary design and current focus is evaluating component sizing and system stability during beam transients.

Janney, Jim↗

DOE OSTI2022

Hidden variable in the electrocaloric effect of ferroics

Caloric effects allow for temperature control through adiabatic application of external fields and are actively explored for solid-state refrigeration. The common wisdom is that the application of ultrahigh fields enhances the effects, thus providing a route to their practical applications. Here, using the ferroelectric relaxor (Ba, Ca)(Ti, Zr)O 3 , we demonstrate that in ferroics, which are the prime candidates for such application, this is not true in general and that caloric effects can be enhanced through the reduction of the applied field. The explanation of such a counterintuitive response is in the dependence of the electrocaloric effect on the effective poling field that can be regarded as a “hidden” variable of the caloric effects.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Experimental determination of precision, resolution, accuracy and trueness of time-of-flight neutron diffraction strain measurements

We discuss a simple statistical analysis which yields the precision, resolution, accuracy and trueness of diffraction-based lattice strain measurements. The procedure consists of measuring the thermal expansion induced in each component of an ideal, non-reacting, two-component, crystalline powder sample in situ. One component, with a high coefficient of thermal expansion (CTE), serves as an internal thermometer. The quantities of interest are obtained by determining the smallest, statistically significant, thermal lattice strain which can be detected through diffraction analysis in the second, low CTE, component in response to controlled temperature changes. This procedure also provides a robust check of the alignment of the diffraction system and is able to reveal the presence of systematic errors. The application of this technique to a time-of-flight engineering diffractometer/strain scanner is presented.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2021

Collaborative Decision Approach for Electricity Pricing-demand Response Stackelberg Game

Demand response programs are considered as a valuable resource in smart grids that provide several advantages of load shifting, peak load reduction, mediating intermittency of renewable energy integration, etc. Flexible price-based incentives have been recognized as a critical strategy in motivating and compensating consumers' load adjustment actions for successful implementation of demand response. Game theoretical approaches, especially Stackelberg games are popularly adopted to model the relationship between electricity price and customers' demand response and solved by the classical centralized backward induction (BI) method. However, the BI method generally requires convexity of the follower's model for necessary optimality conditions, and the computational time of any centralized approach increases sharply with larger problem instances. In this paper, the Stackelberg game of electricity pricing-demand response between a distribution system operator (DSO) and load aggregators (LAs) is decomposed based on a collaborative optimization (CO) framework, where each LA is treated as a discipline with its own domain constraints (e.g. building temperature control), while the DSO at the system level tries to reduce the solution discrepancy and guide the searching towards optimality. Several groups of comparison experiments have demonstrated the effectiveness of the proposed collaborative decision approach in solving the demand response game.

Chen, Yang↗