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All sources NASA NTRS DOE OSTI

DOE OSTI2022

Gain roll-off in cadmium selenide colloidal quantum wells under intense optical excitation

Colloidal quantum wells, or nanoplatelets, show among the lowest thresholds for amplified spontaneous emission and lasing among solution-cast materials and among the highest modal gains of any known materials. Using solution measurements of colloidal quantum wells, this work shows that under photoexcitation, optical gain increases with pump fluence before rolling off due to broad photoinduced absorption at energies lower than the band gap. Despite the common occurrence of gain induced by an electron–hole plasma found in bulk materials and epitaxial quantum wells, under no measurement conditions was the excitonic absorption of the colloidal quantum wells extinguished and gain arising from a plasma observed. Instead, like gain, excitonic absorption reaches a minimum intensity near a photoinduced carrier sheet density of 2 × 10 13 cm –2 above which the absorption peak begins to recover. To understand the origins of these saturation and reversal effects, measurements were performed with different excitation energies, which deposit differing amounts of excess energy above the band gap. Across many samples, it was consistently observed that less energetic excitation results in stronger excitonic bleaching and gain for a given carrier density. Transient and static optical measurements at elevated temperatures, as well as transient X-ray diffraction of the samples, suggest that the origin of gain saturation and reversal is a heating and disordering of the colloidal quantum wells which produces sub-gap photoinduced absorption.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Samoa Updater: An Application of the Levenberg-Marquardt Method to Update DELFIC Predictions Using Field Measurements

The US Department of Energy (DOE) Forensics Operations (DFO) is a member of the Ground Collections Task Force (GCTF), which is responsible for sample collection of radiological debris for attribution should a nuclear detonation ever occur in the United States. The DFO runs the Defense Land Fallout Interpretive Code (DELFIC) Fallout Planning Tool to predict the deposition of fallout from a nuclear detonation. This prediction is refined using the DELFIC Updater tool, which takes ground measurements and adjusts DELFIC inputs to minimize the difference between prediction and observation, yielding improved predictions of fallout in locations both measured and not yet measured. Samoa, a framework for uncertainty analysis and optimization, is used to improve DELFIC predictive fallout modeling. This new capability using Samoa, dubbed “Samoa Updater,” is compared with the current DELFIC Updater, a brute-force sampling approach. Samoa Updater uses the Levenberg– Marquardt (LM) method, a gradient-based nonlinear least squares approach that uses the functional shape of the input space to increase optimization speed. In simulated test cases Samoa Updater yields faster and more accurate solutions than the current Updater.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2023

Layer-by-Layer-Processed Organic Solar Cells with 18.02% Efficiency Enabled by Regulating the Aggregation of Bottom Polymers

The fabrication of organic solar cells (OSCs) by a layer-by-layer (LBL) method has attracted growing attention in recent years. As already known, the pre-aggregates of conjugated polymers in solution have a profound impact on their microstructure morphology in films. Herein, by simply controlling the solution temperature and annealing processes, the pre-aggregation behavior of D18 polymer in solution can be fine-tuned and the microstructure of D18 bottom layer is well manipulated. The optimized D18 bottom layer can effectively regulate L8-BO upper-layer-forming suitable networks for efficient charge transportation. In addition, a vertical phase separation with a special D/D:A/A structure (P-i-N-type component distribution) is also formed. As a result, compared to the 16.43% power conversion efficiency (PCE) of the bulk heterojunction devices, such control enables bilayer OSC devices based on the polymer D18 and L8-BO to deliver an enhanced PCE of 18.02% with simultaneously improved short-circuit current density, open-circuit voltage, and fill factor. Importantly, it is also demonstrated in these results that the LBL deposition process utilizing the pre-aggregation of polymer and its fiber-network-forming ability is a very promising approach to improve charge dynamics, suppress carrier recombination, and fabricate highly efficient OSCs.

14 SOLAR ENERGY↗

DOE OSTI2025

Deconstructing dynamics of symmetry breaking

The Kibble–Zurek mechanism (KZM) successfully predicts the density of topological defects deposited by the phase transitions, but it is not clear why. Its key conjecture is that, near the critical point of the second-order phase transition, critical slowing down will result in a period when the system is too sluggish to follow the potential that is changing faster than its reaction time. The correlation length at the freeze-out instant $\hat{t}$ when the order parameter catches up with the posttransition broken symmetry configuration is then decisive, determining when the mosaic of broken symmetry domains locks in topological defects. To understand why the KZM works so well, we analyze the Landau–Ginzburg model and show why temporal evolution of the order parameter plays such a key role. In conclusion, the analytical solutions we obtain suggest experimentally accessible observables that can shed light on symmetry-breaking dynamics while testing the conjecture on which the KZM is based.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Solid‐Adsorbed Polymer‐Electrolyte Interphases for Stabilizing Metal Anodes in Aqueous Zn and Non‐Aqueous Li Batteries

Abstract Polymers are known to adsorb spontaneously from liquid solutions in contact with high‐energy substrates to form configurationally complex, but robust phases that often exhibit higher durability than might be expected from the individual physical bonds formed with the substrate. Rational control of the physical, chemical, and transport properties of such interphases has emerged as a fundamental opportunity for scientific and technological advances in energy storage technology but requires in‐depth understanding of the conformation states and electrochemical effect of the adsorbed polymers. Here, we analyze the interfacial adsorption of oligomeric polyethylene glycol (PEG) chains of moderate sizes dissolved in protic and aprotic liquid electrolytes and find that there is an optimum polymer molecular weight of approximately 400 Da at which the highest columbic efficiency is achieved for both Zn and Li deposition. These findings point to a simple, versatile approach for extending the lifetime of batteries.

Jin, Shuo↗

DOE OSTI2024

Making Plasticized Polymer Electrolytes Stable Against Sodium Metal for High‐Energy Solid‐State Sodium Batteries

Solid polymer electrolytes based on plastic crystals are promising for solid-state sodium metal (Na 0 ) batteries, yet their practicality has been hindered by the notorious Na 0 -electrolyte interface instability issue, the underlying cause of which remains poorly understood. Here, in this study, by leveraging a model plasticized polymer electrolyte based on conventional succinonitrile plastic crystals, we uncover its failure origin in Na 0 batteries is associated with the formation of a thick and non-uniform solid electrolyte interphase (SEI) and whiskery Na 0 nucleation/growth. Furthermore, we design a new additive-embedded plasticized polymer electrolyte to manipulate the Na 0 deposition and SEI formulation. For the first time, we demonstrate that introducing fluoroethylene carbonate (FEC) additive into the succinonitrile-plasticized polymer electrolyte can effectively protect Na 0 against interfacial corrosion by facilitating the growth of dome-like Na 0 with thin, amorphous, and fluorine-rich SEIs, thus enabling significantly improved performances of Na//Na symmetric cells (1,800 h at 0.5 mA cm −2 ) and Na//Na 3 V 2 (PO 4 ) 3 full cells (93.0 % capacity retention after 1,200 cycles at 1 C rate in coin cells and 93.1 % capacity retention after 250 cycles at C/3 in pouch cells at room temperature). Our work provides valuable insights into the interfacial failure of plasticized polymer electrolytes and offers a promising solution to resolving the interfacial instability issue.

25 ENERGY STORAGE↗

DOE OSTI2024

Evaluation of Directed Energy Deposition and Laser Powder Bed Fusion Nickel-Based Alloys Process Application Envelopes Based on Performance, Process Economics, Supply Chain Risks, and Reactor-Specific Targeted Components

The goal of the Advanced Materials and Manufacturing Technologies (AMMT) program is to accelerate the deployment of new materials and manufacturing technologies into advanced nuclear-related systems. Although 316H stainless steel fabricated by laser powder bed fusion (LPBF) has already been identified as an alloy that could have a significant effect on various reactor technologies, many other materials and manufacturing techniques are being evaluated. Nickel-based alloys typically offer higher-temperature capabilities compared with advanced stainless steels, and previous reports looked at three Ni-based alloy categories: low-Co alloys with a potential use close to the reactor core; high-temperature, high-strength alloys; and molten salt–compatible alloys. Due to the increasing interest in the low Co 625 alloy for nuclear applications, the alloy was compared at the Oak Ridge National Laboratory (ORNL) with 617, 230, two high-temperature, high-strength solution-strengthened alloys. Hot cracking could not be suppressed for alloy 230, and it was shown that these cracks, which were elongated along the build direction (BD), had a drastic effect on the ductility of alloy 230 at room temperature when specimens were machined perpendicular to the BD. Cracking was not as significant for alloy 617, but still led to significant variation in ductility at room temperature along the build direction. On the contrary, LPBF printing of crack-free alloy 625 was achieved using similar printing parameters, and the alloy looks like a very promising candidate for various reactor technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Solid–Adsorbed Polymer–Electrolyte Interphases for Stabilizing Metal Anodes in Aqueous Zn and Non–Aqueous Li Batteries

Polymers are known to adsorb spontaneously from liquid solutions in contact with high-energy substrates to form configurationally complex, but robust phases that often exhibit higher durability than might be expected from the individual physical bonds formed with the substrate. Rational control of the physical, chemical, and transport properties of such interphases has emerged as a fundamental opportunity for scientific and technological advances in energy storage technology but requires in-depth understanding of the conformation states and electrochemical effect of the adsorbed polymers. Here, we analyze the interfacial adsorption of oligomeric polyethylene glycol (PEG) chains of moderate sizes dissolved in protic and aprotic liquid electrolytes and find that there is an optimum polymer molecular weight of approximately 400 Da at which the highest columbic efficiency is achieved for both Zn and Li deposition. Furthermore, these findings point to a simple, versatile approach for extending the lifetime of batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Mechanistic Study of Controlled Zinc Electrodeposition Behaviors Facilitated by Nanoscale Electrolyte Additives at the Electrode Interface

Nanoparticle organic hybrid materials (NOHMs) are liquid-like materials composed of an inorganic core to which a polymeric canopy is ionically tethered. NOHMs have unique properties including negligible vapor pressure, high oxidative thermal stability, and the ability to bind to reactive species of interest due to the tunability of their polymeric canopy. This makes them promising multifunctional materials for a wide range of energy and environmental technologies, including electrolyte additives for electrochemical energy storage (e.g., flow batteries) and the electrochemical conversion of CO 2 to chemicals and fuels. Due to their unique transport behaviors in fluid systems, an understanding of the near-electrode surface behavior of NOHMs in electrolyte solutions and their effect on electrochemical reactions is still lacking. In this work, the complexation of zinc (Zn) by NOHMs with an ionically tethered polyetheramine canopy (HPE) (NOHM-I-HPE) was studied using attenuated total reflectance Fourier transform infrared and Carbon-13 nuclear magnetic resonance spectroscopy. Additionally, various electrochemical techniques were employed to discern the role of NOHM-I-HPE during zinc electrodeposition, and the results were compared to those of the electrochemical system containing untethered HPE polymers. Our findings confirmed that NOHM-I-HPE and HPE reversibly complex zinc in the aqueous electrolyte. NOHM-I-HPE and HPE were found to block some of the electrode active sites, reducing the overall current density during electrodeposition, while facilitating the formation of smooth zinc deposits, as revealed by surface imaging and diffraction techniques. Observed variations in the current density responses and the degree of passivation created by the NOHM-I-HPE and HPE adsorbed on the electrode surface revealed that their different packing behaviors at the electrode–electrolyte interface influence the zinc deposition mechanism. The presence of the nanoparticle and ordering offered by the NOHMs as well as the structured conformation of the polymeric canopy allowed the formation of void spaces and free volumes for enhanced transport behaviors. Furthermore, these findings provided insights into how structured electrolyte additives such as NOHMs can allow for advancements in electrolyte design for controlled deposition of metal species from energy-dense electrolytes or for other electrochemical reactions.

25 ENERGY STORAGE↗

DOE OSTI2021

Radiological Scouting, Monitoring and Inspection Using Drones

Human populations and natural ecosystems are bound to be exposed to ionizing radiation from the deposition of artificial radionuclides resulting from nuclear accidents, nuclear devices or radiological dispersive devices (“dirty bombs”). On the other hand, Naturally Occurring Radioactive Material industries such as phosphate production or uranium mining, contribute to the on site storage of residuals with enhanced concentrations of natural radionuclides. Therefore, in the context of the European agreements concerning nuclear energy, namely the European Atomic Energy Community Treaty, monitoring is an essential feature of the environmental radiological surveillance. In this work, we obtain 3D maps from outdoor scenarios, and complete such maps with measured radiation levels and with its radionuclide signature. In such scenarios, we face challenges such as unknown and rough terrain, limited number of sampled locations and the need for different sensors and therefore different tasks. We propose a radiological solution for scouting, monitoring and inspecting an area of interest, using a fleet of drones and a controlling ground station. First, we scout an area with a Light Detection and Ranging sensor onboard a drone to accurately 3D-map the area. Then, we monitor that area with a Geiger–Müller Counter at a low-vertical distance from the ground to produce a radiological (heat)map that is overlaid on the 3D map of the scenario. Next, we identify the hotspots of radiation, and inspect them in detail using a drone by landing on them, to reveal its radionuclide signature using a Cadmium–Zinc–Telluride detector. We present the algorithms used to implement such tasks both at the ground station and on the drones. The three mission phases were validated using actual experiments in three different outdoor scenarios. We conclude that drones can not only perform the mission efficiently, but in general they are faster and as reliable as personnel on the ground.

Pinto, Luís Ramos (ORCID:0000000319975484)↗

DOE OSTI2024

Toolpath considerations for DED: Arc and laser welding

Directed energy deposition (DED) is a form of additive manufacturing that uses localized melted metal, similar to traditional arc welding, to construct an object. In comparison to polymer systems, metal systems can exert additional control over the build process through manipulation of the pool of melted metal, called the “melt pool.” This is especially important to maintain appropriate layer heights and create high quality builds. Additionally, metal systems allow site-specific control of the printed part, which enables advanced construction techniques that would otherwise not be possible. However, both of these types of control require support from the slicing software and, potentially, sensor feedback. This chapter will discuss these control processes and their basic implementation in a slicing program. The processes described here lay the foundation for more advanced solutions, particularly sensor feedback, that will be discussed later.

Borish, Michael↗

DOE OSTI2025

Active Divertor Heat Flux Control using Impurity Powder Dropper

Divertor plasma-facing components (PFCs) in a tokamak are typically designed to withstand average steady-state heat loads of about 5–10 MW/m 2 , a limit that applies to both solid and liquid lithium (LL) PFCs. Exceeding these design values can result in surface damage to tungsten PFCs or excessive lithium (Li) evaporation in liquid lithium divertor (LLD) PFCs. Since exceeding the divertor heat load limits has serious consequences, it is therefore prudent to develop a tool to reduce the divertor heat load and bring the heat load to within the design limit without affecting the plasma performance. Active low Z impurity injection such as Li has been suggested as a potential solution to mitigate excess heat flux as suggested previously, given that non-coronal radiation can be quite large ~ 20–30 MJ per mole of injected Li. Li is considered desirable for reducing the edge neutral recycling helping to improve plasma energy confinement. In this paper, we model the Impurity Power Dropper (IPD) to investigate its potential of divertor heat flux control. The IPD is typically located at the top of the tokamak device and uses a vertical drift tube of a few meters. In the 2 m drift tube case, the IPD powder is accelerated to ~ 6 m/sec before reaching the plasma with the upper divertor configuration, matching the condition for the in-board side pellet injection case. By modeling the IPD geometry we determined the IPD powder deposition profile, and thus the non-coronal radiation and ionization profiles in time as well. From the enhanced radiation power loss, it is therefore possible to reduce the divertor heat load using the divertor simulation code. In conclusion, the IPD divertor heat flux control can be tested in the facilities with IPD including ST-40, DIII-D, EAST, WEST and NSTX-U.

Active lithium injection↗

DOE OSTI2025

Tetracene Functionalized Si(111) Achieves Enhanced Solar-to-Chemical Energy Conversion via Molecular Acceptor States

The properties of semiconductor|liquid interfaces play a critical role in determining the efficiency of solar-to-hydrogen (STH) conversion. Here, we investigate how molecular functionalization of Si(111) and Si(111)|TiO 2 surfaces impacts photoelectrochemical (PEC) hydrogen production efficiency. We find that functionalization of ∼3% of the atop sites of Si(111) with either 9-anthracene (Anth) or 5-tetracene (Tet), with the remaining sites passivated by methyl groups, provides substrates with high electronic quality and low surface oxide densities, as determined by X-ray photoelectron spectroscopy (XPS) measurements. Surface photovoltage (SPV) spectroscopy shows that surfaces modified with Anth or Tet exhibit an increased photovoltage, with Tet-functionalized surfaces yielding an additional 192 meV relative to methyl-terminated Si(111), indicating improved charge separation for Si-Tet. Further improvement in onset potential was achieved by replacing a nitrogen-containing TiO 2 atomic layer deposition (ALD) precursor (TDMAT) with a precursor lacking nitrogen (TTIP), which eliminates the parasitic defect band in the TiO 2 overlayer (p-Si(111)-Tet|TTIP-TiO 2 |Pt: V OC = +0.283 ± 0.041 V vs RHE). Density functional theory (DFT) analysis demonstrates that compared with Anth-modified Si(111), the Tet-modified surface exhibits more hybridized Si(111)-Tet states closer to the silicon band edges. Mercury contact current–voltage (I–V, dark) measurements quantified the relative interfacial density of states of Si-Tet, Si-Anth and Si-Me surfaces─revealing that the interfacial state density was highest for Si-Tet. This suggests that such hybridized interfaces serve to capture better photoexcited charge, which enables facile electron transfer to molecular acceptors in solution. Altogether, the data indicate that beneficial hybrid molecular LUMO surface states interacting with the Si conduction band edge results in improved hydrogen evolution (HER) performance for p-Si devices.

Group theory↗

DOE OSTI2022

Developing solid-surface plasma facing components for pilot plants and reactors with replenishable wall claddings and continuous surface conditioning. Part B: required research in present tokamaks

Abstract The companion part A paper (Stangeby et al 2022) reports a number of independent estimates indicating that high-duty-cycle DT tokamaks starting with pilot plants will likely experience rates of net erosion and deposition of solid PFC, plasma facing component, material in the range of 10 3 to 10 4 kg yr −1 , regardless of the material used. The subsequent redeposition of such large quantities of material has the potential for major interference with tokamak operation. Similar levels and issues will be involved if ∼continuous low-Z powder dropping is used for surface conditioning of DT tokamaks, independent of the material used for the PFC armor. In Stangeby et al (2022) (part A) it is proposed that for high-duty-cycle DT tokamaks, non-metallic low-Z refractory materials such as ceramics (graphite, SiC, etc) used as in situ replenishable, relatively thin—of order mm—claddings on a substrate which is resistant to neutron damage could provide a potential solution for protecting the main walls, while reducing the risk of degrading the confined plasma. Assessment of whether such an approach is viable will require information, much of which is not available today. Section 6 of part A identifies a partial list of major physics questions that will need to be answered in order to make an informed assessment. This part B report describes R&D needed to be done in present tokamaks in order to answer many of these questions. Most of the required R&D is to establish better understanding of low-Z slag generation and to identify means to safely manage it. Powder droppers provide a unique opportunity to carry out controlled studies on the management of low-Z slag in current tokamaks, independent of whether their protection tiles use low-Z or high-Z material.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Designing Track for Electrospinning Unit and Cost-Effective Laser Scanning System

Nanofibers are produced in the Targeted Systems Department (TSD) by applying a large voltage to the nanofiber fluid and the collection apparatus known as the electrospinner. The fiber is then shot out of nozzles and collected onto the electrospinner into a nanofiber mat. The problem is that since the nozzle heads are stationary, there is non-uniform deposition of nanofiber on the collection drum leading to variation in thickness of the produced nanofiber mat. To mitigate this issue, a reciprocating mechanism is designed to move the nozzle along the drum collector along with the ability to vary its stroke length. This design was realized using Siemens NX and several parts were printed using a 3D printer, but is, as of writing, untested. Second project involved providing an alternative method to scan a large sample that had undergone certain surface deformation by beam interaction and detect out of plane deformation such as micro-scale swelling and surface roughness. Systems to carry out this scanning already exist; however, they are expensive and produce many files that need to be stitched together and are cumbersome to deal with. The solution is to create a scanning system using an already purchased scanning laser and linear stage motor. The laser and stage motor were combined to produce length results that aligned with a digital microscope but differing height results.

Ruffolo, Leopoldo↗

DOE OSTI2024

Designing a track for an electrospinning unit and cost-effective laser scanning system

Ruffolo, Leopoldo↗

DOE OSTI2025

UV-Vis spectrophotometric determination of rare earth elements (REE) speciation at near-neutral to alkaline pH. Part II: hydrolysis of Er from 25 to 75 °C

Aqueous speciation of rare earth elements (REE) controls their mobilization, fractionation, and enrichment in the natural waters. Geochemical modeling of their speciation is key to improve our understanding of the formation of economic mineral deposits, for developing mineral separation and mine tailing recovery technologies, and for characterizing the geochemistry of thermal water. However, our ability to predict the fate of REE in a wide pH and temperature range is limited by the scarcity of thermodynamic data for the REE hydroxyl complexes. In part I of this study (H. J. Han and A. P. Gysi, Dalton Trans., 2024, 53, 13129–13141), the optical properties of m-cresol purple (mCP) were determined using UV-Vis spectrophotometry between 25 and 75 °C in order to develop a method for deriving the hydrolysis constants of erbium (Er). Here, UV-Vis spectrophotometry experiments were conducted as a function of temperature between 35 and 75 °C to determine the hydrolysis of Er in near-neutral to alkaline solutions using mCP as an in situ pH color indicator. Here, the experiments were conducted with Er concentrations from 0 to ~0.253 mmol kg –1 in low ionic strength solutions (≤0.001 mol kg –1 ).

58 GEOSCIENCES↗

DOE OSTI2022

Automated Process Planning for Embossing and Functionally Grading Materials via Site-Specific Control in Large-Format Metal-Based Additive Manufacturing

The potential for site-specific, process-parameter control is an attribute of additive manufacturing (AM) that makes it highly attractive as a manufacturing process. The research interest in the functionally grading material properties of numerous AM processes has been high for years. However, one of the issues that slows developmental progress in this area is process planning. It is not uncommon for manual programming methods and bespoke solutions to be utilized for site-specific control efforts. This article presents the development of slicing software that contains a fully automated process planning approach for enabling through-thickness, process-parameter control for a range of AM processes. The technique includes the use of parent and child geometries for controlling the locations of site-specific parameters, which are overlayed onto unmodified toolpaths, i.e., a vector-based planning approach is used in which additional information, such as melt pool size for large-scale metal AM processes, is assigned to the vectors. This technique has the potential for macro- and micro-structural modifications to printed objects. A proof-of-principle experiment is highlighted in which this technique was used to generate dynamic bead geometries that were deposited to induce a novel surface embossing effect, and additional software examples are presented that highlight software support for more complex objects.

36 MATERIALS SCIENCE↗