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DOE OSTI2023

Design of Monolithic Bi-Layer High-Z PAL-Si Hard X-ray CMOS Image Sensors for Quantum Efficiency Enhancement

This article experimentally investigates the inception of an innovative hard X-ray photon energy attenuation layer (PAL) to advance high-energy X-ray detection (20–50 keV). A bi-layer design with a thin film high-Z PAL on the top and Si image sensor on the bottom has previously demon-strated quantum yield enhancement via computational methods by the principle of photon energy down conversion (PEDC), where high-energy X-ray photon energies are attenuated via inelastic scattering down to ≤10 keV, which is suitable for efficient photoelectric absorption by Si. Quantum yield enhancement has been experimentally confirmed via a preliminary demonstration using PAL-integrated Si-based CMOS image sensors (Si CIS). Furthermore, substituting the high-Z PAL with a lower-Z material—Sn—and alternatively coupling it with a conventional scintillator ma-terial—Lutetium-yttrium oxyorthosilicate (LYSO)—have been compared to demonstrate the most prominent efficacy of monolithic integration of high-Z PAL on Si CIS to detect hard X-rays, paving the way for next-generation high-energy X-ray detection methods.

47 OTHER INSTRUMENTATION↗

DOE OSTI2019

Very High Refractive Index Transition Metal Dichalcogenide Photonic Conformal Coatings by Conversion of ALD Metal Oxides

Materials for nanophotonic devices ideally combine ease of deposition, very high refractive index, and facile pattern formation through lithographic templating and/or etching. In this work, we present a scalable method for producing high refractive index WS 2 layers by chemical conversion of WO 3 synthesized via atomic layer deposition (ALD). These conformal nanocrystalline thin films demonstrate a surprisingly high index of refraction (n > 3.9), and structural fidelity compatible with lithographically defined features down to ~10 nm. Although this process yields highly polycrystalline films, the optical constants are in agreement with those reported for single crystal bulk WS 2 . Subsequently, we demonstrate three photonic structures - first, a two-dimensional hole array made possible by patterning and etching an ALD WO 3 thin film before conversion, second, an analogue of the 2D hole array first patterned into fused silica before conformal coating and conversion, and third, a three-dimensional inverse opal photonic crystal made by conformal coating of a self-assembled polystyrene bead template. Furthermore these results can be trivially extended to other transition metal dichalcogenides, thus opening new opportunities for photonic devices based on high refractive index materials.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Alternate Methods for Cleaning Zirconium Plate

The United States High Performance Research Reactor Conversion Program identified the need to transition from highly enriched uranium fuel to lowly enriched uranium fuel for high power research and civil reactors. One of the fuel configurations selected for these reactors was a uranium (U) foil alloyed with 10% molybdenum (Mo). The U-10Mo fuel foil was then covered with a zirconium (Zr) interlayer and pressed into an aluminum cladding. Idaho National Laboratory prescribed a need to remove surface oxidation on the Zr prior to bonding it with U-10Mo fuel foil. To determine the best method of oxidation removal, a variety of polishing methods, including hand polishing with a diamond paste or Scotch-Brite™ pads, mechanically wet-polishing with abrasive belts, and chemical etching with hydrofluoric/nitric acid mixtures, were investigated on pre-polished Zircaloy 702 sheets purchased directly from the manufacturer. No change in surface roughness was detected using any of these methods relative to the as-received material. In fact, scanning electron microscopy detected grit from hand polishing with Amplex Grade 30 waste soluble diamond paste and Scotch-Brite™ pads. Visible staining was found, and fluorine detected via X-ray photoelectron spectroscopy on the flash etching samples. These contaminants were not seen on the as-received material. In addition to the need to remove the oxide layer on the Zr prior to co-rolling, there are concerns that the Neolube debonding agent on the co-rolling can may contaminate the Zr surface after co-rolling. The experimental results found that zirconium in contact with Neolube coated steel plates was easily cleaning with ethanol wiping after heat treated and no carbide inclusions remained on the surface. Overall, all cleaning methods tested did not significantly change the surface roughness of the plates or reduce the oxide layer present on the zirconium. Carbon was found on all the samples, before and after cleaning, except for the flash etch samples which detected fluorine instead. The insignificant changes seen in the cleaned plates relative to the as received plates question the need for cleaning prior to rolling. Further investigation in the requirements for cleaning at this step is recommended. Current methods for cleaning the surface after hot rolling with alcohol appear sufficient. After hot rolling, if Neolube does peel off the can and onto the zirconium coated foil surface, a dry abrasive or diamond paste polish is not recommended due to the chance of abrasive being embedded into the surface. However, the ability of an etchant to lift the lubricant off the zirconium surface indicates that a spot etch method could work to clean specific spots where Neolube is present, if the need arises.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Simultaneous Ligand Exchange Fabrication of Flexible Perovskite Solar Cells using Newly Synthesized Uniform Tin Oxide Quantum Dots

Halide perovskite solar cells (HPSCs) have a significant potential for future photovoltaic systems because of a high power conversion efficiency (PCE) exceeding 23% using solution processing methods. A low-temperature processed oxide layer is a challenging issue for large-scale manufacture of flexible and low-cost HPSCs. Here, we propose a simple reverse micelle-water injection method for highly dispersed ligand-capped ultrafine SnO2 quantum dots (QD). Interestingly, we observed that the ligands, which help in the formation of a uniform SnO2 QD thin film, spontaneously exchange for halide through a perovskite solution, and finally we form a suitable SnO2 QD-halide junction for high-performance HPSCs. The flexible HPSC with the SnO2 QD-halide junction formed via the ligand exchange exhibits a high PCE of 17.7% using a flexible substrate. It also shows an excellent flexibility, where the initial PCE is maintained within 92% after 1000 bending cycles with a bending radius of 18 mm.

14 SOLAR ENERGY↗

DOE OSTI2025

Artificial to Spiking Neural Networks Conversion with Calibration in Scientific Machine Learning

Here, we introduce a method to convert physics-informed neural networks (PINNs), commonly used in scientific machine learning, to spiking neural networks (SNNs), which are expected to have higher energy efficiency compared to traditional artificial neural networks (ANNs). We first extend the calibration technique of SNNs to arbitrary activation functions beyond ReLU, making it more versatile, and we prove a theorem that ensures the effectiveness of the calibration. We successfully convert PINNs to SNNs, enabling computational efficiency for diverse regression tasks in solving multiple differential equations, including the unsteady Navier–Stokes equations. We demonstrate great gains in terms of overall efficiency, including separable PINNs (SPINNs), which accelerate the training process. Overall, this is the first work of this kind and the proposed method achieves relatively good accuracy with low spike rates.

PINN↗

DOE OSTI2020

Hanford Site Composite Analysis Data Package: Exposure Scenarios and Radionuclide Specific Dose Conversion Factors

This data package summarizes the exposure assumptions, equations, and methods used to calculate radionuclide-specific unit dose factors and the radiological doses for both groundwater and atmospheric pathways as a part of the updated Hanford Site Composite Analysis (CA). An All Pathways Representative Person exposure scenario is considered to evaluate exposure via both groundwater and atmospheric transport pathways. The radiological dose assessments for both groundwater and atmospheric pathways are included in the performance assessments (PAs) for various Waste Management Areas at the Hanford Site. This data package calculates exposure route-specific and total unit dose factors for CA-specific radionuclides of concern based on the exposure assumptions used in the CA and PAs. This data package also presents the results and comparison of the radionuclide-specific unit dose factors based on the exposure assumptions used in the revised Hanford Site Composite Analysis and Hanford Site performance assessments for low-level waste disposal facilities.

61 RADIATION PROTECTION AND DOSIMETRY↗

DOE OSTI2022

Hanford Site Composite Analysis Data Package: Exposure Scenarios and Radionuclide Specific Dose Conversion Factors.

This data package summarizes the exposure assumptions, equations, and methods used to calculate radionuclide-specific unit dose factors and the radiological doses for both groundwater and atmospheric pathways as a part of the revised Hanford Site Composite Analysis. An All-Pathways Representative Person exposure scenario is considered to evaluate exposure via both groundwater and atmospheric transport pathways. The radiological dose assessments for both groundwater and atmospheric pathways are included in the performance assessments for various Waste Management Areas at the Hanford Site. This data package calculates exposure route-specific and total unit dose factors for composite-analysis-specific radionuclides of concern based on the exposure assumptions used in the composite analysis and performance assessments. This data package presents the results and comparison of the radionuclide-specific unit dose factors based on the exposure assumptions used in the revised composite analysis and various performance assessments.

61 RADIATION PROTECTION AND DOSIMETRY↗

DOE OSTI2018

Biomass conversion to fuels and chemicals

This disclosure relates to compositions and methods for converting biomass to various chemical intermediates and final products including fuels. Aspects include the depolymerization of lignin, cellulose, and hemicellulose to a wide slate of depolymerization compounds that can be subsequently metabolized by genetically modified bacterium, and converted to cis,cis-muconic acid. Other aspects include the use of monometallic catalysts for converting the cis,cis-muconic acid to commodity chemicals and fuels, for example adipic acid and/or nylon.

09 BIOMASS FUELS↗

DOE OSTI2019

Biomass conversion to fuels and chemicals

09 BIOMASS FUELS↗

DOE OSTI2024

Indirect Liftoff Mechanism for High‐Throughput, Single‐Source Laser Scribing for Perovskite Solar Modules

A high‐throughput, single‐source laser scribing method exploiting a transparent conducting oxide (TCO) indirect liftoff mechanism is developed to produce serially interconnected perovskite solar modules. The TCO‐based indirect liftoff mechanism relies solely on laser absorption in the front transparent electrode material reducing thermal damage to the overlying layers and allowing for fast scribing speeds with low‐cost μs‐pulse duration fiber laser systems. Minimal resistive power losses are observed with the method compared to conventional ablative laser scribes, maintaining the power conversion efficiencies of small‐area devices (≈0.2 cm 2 ) across significantly larger deposition areas (≈1 cm 2 ). Finally, demonstrating > 3 m s −1 processing speeds, TCO‐based liftoff provides the highest throughput laser scribing method for thin‐film photovoltaic devices produced on glass/TCO substrates, capable of processing large‐area perovskite solar modules at a manufacturing scale.

14 SOLAR ENERGY↗

DOE OSTI2018

Modeling of proton-induced radioactivation background in hard X-ray telescopes: Geant4-based simulation and its demonstration by Hitomi ’s measurement in a low Earth orbit

Hard X-ray astronomical observatories in orbit suffer from a significant amount of background due to radioactivation induced by cosmic-ray protons and/or geomagnetically trapped protons. Within the framework of a full Monte Carlo simulation, we present modeling of in-orbit instrumental background which is dominated by radioactivation. To reduce the computation time required by straightforward simulations of delayed emissions from activated isotopes, we insert a semi-analytical calculation that converts production probabilities of radioactive isotopes by interaction of the primary protons into decay rates at measurement time of all secondary isotopes. Therefore, our simulation method is separated into three steps: (1) simulation of isotope production, (2) semi-analytical conversion to decay rates, and (3) simulation of decays of the isotopes at measurement time. This method is verified by a simple setup that has a CdTe semiconductor detector, and shows a 100-fold improvement in efficiency over the straightforward simulation. To demonstrate its experimental performance, the simulation framework was tested against data measured with a CdTe sensor in the Hard X-ray Imager onboard the Hitomi X-ray Astronomy Satellite, which was put into a low Earth orbit with an altitude of 570 km and an inclination of 31°, and thus experienced a large amount of irradiation from geomagnetically trapped protons during its passages through the South Atlantic Anomaly. The simulation is able to treat full histories of the proton irradiation and multiple measurement windows. As a result, the simulation results agree very well with the measured data, showing that the measured background is well described by the combination of proton-induced radioactivation of the CdTe detector itself and thick Bi 4 Ge 3 O 12 scintillator shields, leakage of cosmic X-ray background and albedo gamma-ray radiation, and emissions from naturally contaminated isotopes in the detector system.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2019

Total Protein Analysis in Algae via Bulk Amino Acid Detection: Optimization of Amino Acid Derivatization after Hydrolysis with O -Phthalaldehyde 3-Mercaptopropionic Acid (OPA-3MPA)

The analysis of protein in algal biomass is one of the most critical areas of commercial development of algae characterization for nutritional or other high value applications. A new rapid and accurate method is required that can be widely implemented and that is free from interferences from the complex algal biomass matrix. We developed a simple spectrophotometric method for primary amino acid quantification bulk measurement in an acid hydrolyzed algal biomass preparation, as an alternative to the more labor-intensive amino HPLC acid analysis or less specific nitrogen-to-protein conversion. We have validated an O -phthalaldehyde (OPA)-based derivatization method, showing accurate and linear quantification for standard reference amino acids as well as mixtures, mimicking the amino acid complexity found in algal biomass. The presence of interferences that may be derived from the complex biomass biochemical composition was tested during the method validation phase. We document the application of a novel method of OPA derivatization with 3-mercaptopropionic acid (3MPA) to determine the total amino acid content of harvested algal biomass collected from different, controlled cultivation conditions and demonstrated a within 10% accuracy against a reference measurement of amino acid content in at least 4 species and 10 algal biomass samples, across early, mid, and late-stages of cultivation.

09 BIOMASS FUELS↗

DOE OSTI2024

De novo Materials Design of Catalytic Surface Motifs for Water-Gas-Shift (Final Progress Report DOE Grant DE-SC0019281)

This project was aimed at developing innovative theoretical methods and models to understand essential catalysis-relevant issues such as CO 2 conversion, fuel cells, and lithium batteries. Through collaborations with experimentalists, we strive to develop new quantum and machine learning methods for the understanding of surface and interfacial chemistry that can empower the design of energy and sustainability systems. Overall, our work under this grant brings cross-disciplinary insights into catalytic materials, microenvironments, and other conditions, which can serve to provide design rules for the next generation of catalysts.

25 ENERGY STORAGE↗

DOE OSTI2020

Sustainable energy and fuels from biomass: a review focusing on hydrothermal biomass processing

Fossil fuels are being replaced with renewable energy resources (biomass and biomass waste, solar, geothermal, wind, etc.) to ensure sustainable development, reduce the dependence on fossil fuels, address environmental challenges including climate change. Today, biomass produces 5 × 10 19 kJ of energy/year, which corresponds to 10% of the annual global energy consumption. Considering the variety of biomass resources, this value is predicted to reach 150 × 10 19 kJ by 2050. Biomass may become even more important for use as an energy resource and chemical raw material in the 21st century. Hydrothermal biomass conversion stands out as a promising and alternative technology. Methods such as traditional gasification and pyrolysis require dry biomass. Hydrothermal techniques have been developed to eliminate the cost and time required for drying biomass. The purpose of this process is to decompose biomass with a high moisture content into small molecules and reduce its oxygen content to obtain liquid fuels or valuable chemicals. Finally, this review presents the current and future state of energy, energy sources, biomass properties and biomass conversion technologies with a focus on hydrothermal technologies.

09 BIOMASS FUELS↗

DOE OSTI2021

Reaching the Excitonic Limit in 2D Janus Monolayers by In Situ Deterministic Growth

Abstract Named after the two‐faced Roman god of transitions, transition metal dichalcogenide (TMD) Janus monolayers have two different chalcogen surfaces, inherently breaking the out‐of‐plane mirror symmetry. The broken mirror symmetry and the resulting potential gradient lead to the emergence of quantum properties such as the Rashba effect and the formation of dipolar excitons. Experimental access to these quantum properties, however, hinges on the ability to produce high‐quality 2D Janus monolayers. Here, these results introduce a holistic 2D Janus synthesis technique that allows real‐time monitoring of the growth process. This prototype chamber integrates in situ spectroscopy, offering fundamental insights into the structural evolution and growth kinetics, that allow the evaluation and optimization of the quality of Janus monolayers. The versatility of this method is demonstrated by synthesizing and monitoring the conversion of SWSe, SNbSe, and SMoSe Janus monolayers. Deterministic conversion and real‐time data collection further aid in conversion of exfoliated TMDs to Janus monolayers and unparalleled exciton linewidth values are reached, compared to the current best standard. The results offer an insight into the process kinetics and aid in the development of new Janus monolayers with high optical quality, which is much needed to access their exotic properties.

2D materials↗

DOE OSTI2018

LncRNA EPIC1 protects human osteoblasts from dexamethasone-induced cell death

Highlights: • Dexamethasone (Dex) increases Lnc-EPIC1 expression in human osteoblasts. • Lnc-EPIC1 expression is elevated in necrotic femoral head tissues of Dex-taking patients. • Ectopic Lnc-EPIC1 overexpression protects human osteoblasts from Dex. • Lnc-EPIC1 siRNA potentiates Dex-induced cytotoxicity in human osteoblasts. • Myc is the primary target of Lnc-EPIC1 in human osteoblasts. Dexamethasone (Dex) can induce injury to human osteoblasts. Long non-coding RNA (LncRNA) EPIC1 (Lnc-EPIC1) is a novel Myc-interacting LncRNA. Its effect on Dex-treated human osteoblasts is studied here. In OB-6 osteoblastic cells and primary human osteoblasts, treatment with Dex increased expression of Lnc-EPIC1. Its expression is also elevated in the necrotic femoral head tissues of Dex-taking patients. Ectopic overexpression of Lnc-EPIC1 inhibited Dex-induced apoptosis and programmed necrosis in OB-6 cells and primary human osteoblasts. Reversely, Lnc-EPIC1 silencing by targeted siRNA potentiated Dex-induced cytotoxicity. Myc is the target of Lnc-EPIC1 in osteoblasts. Exogenous overexpression of Myc protected OB-6 cells from Dex. Conversely, Myc knockout by CRISPR-Cas-9 method abolished Lnc-EPIC1-induced OB-6 cytoprotection against Dex. Together, Lnc-EPIC1 expression protects human osteoblasts from Dex possible via regulation of Myc.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2023

Insights into co-pyrolysis of polyethylene terephthalate and polyamide 6 mixture through experiments, kinetic modeling and machine learning

The non-isothermal pyrolysis of polyethylene terephthalate (PET), polyamide 6 (PA6), and their mixtures was studied in a thermogravimetric analyzer at different heating rates. Temperature of maximum decomposition (T max ) decreased by 25–45 °C and 35–55 °C for the PET:PA6 mixtures (3:1, 1:1, 1:3) compared to PET and PA6, respectively. The kinetic analysis was initially carried out using isoconversional method. However, the dependency of activation energy on conversion was observed for the co-pyrolysis of PET and PA6 that suggested the occurrence of multi-step reactions in the mixtures. Distributed activation energy model (DAEM) was used in this study to describe the multistep reactions occurring during pyrolysis of PET:PA6 mixtures. Here, in this work, a four-parallel reaction DAEM was developed to describe the pyrolysis kinetics of PET:PA6 mixtures. The apparent mean activation energies (E o ) for PET, PA6, and mixtures varied in the range of 244–255, 140–215, and 138–255 kJ mol –1 , respectively. The mass loss profiles of PET and PA6 mixtures were also modeled using artificial neural network (ANN). Out of 155 ANN models, the best prediction was made by ANN511 with R 2 greater than 0.997 for both test and unseen data. The interaction effects observed through TGA experiments and subsequent kinetic analysis were further assessed in terms of product composition using analytical pyrolysis coupled with gas chromatograph/mass spectrometer (Py-GC/MS). Co-pyrolysis of PET and PA6 resulted in the formation of new aromatic compounds with nitrogen-containing functional groups, which were not detected when PET or PA6 were pyrolyzed individually.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Performance characterization of nanofiltration, reverse osmosis, and ion exchange technologies for acetic acid separation

A major obstacle to widespread implementation of bio-based fuels and chemicals is the lack of efficient and costeffective separation methods. To purify acetic acid produced by biochemical conversion of biomass via anaerobic digestion, this work employs two commonly used separation technologies: (1) ion-exchange (IX) resin and (2) pressure-driven membranes. This study tested five commercially available strong- and weak-base anion-exchange resins and five commercially available nanofiltration (NF) and reverse osmosis (RO) membranes. The pH of the feed solution significantly affected adsorption capacity. At pH 6.3, a strong-base IX resin (IRN-78) performed best (95.1% acetate removal). With strong-base IX resins, the Langmuir isotherm model fit well, whereas for weak-base IX resins, the Freundlich isotherm provided a better fit. A pseudo-second-order kinetic model fit well for both IRN-78 and IRA-67. Regarding membrane separation, RO (BW30XFR membrane) achieved the highest rejection (98.6% acetate rejection), whereas an NF membrane (NF*) achieved the best combination of permeate flux (105 L/(h∙m 2 )) and rejection (83.1% acetate rejection). For membrane performance, the experimental data were fit using the solution diffusion model. Increased pH in the feed solution lowered permeate flux but increased acetic acid rejection. Finally, then the acetic acid concentration in the feed solution increased, both permeate flux and acetic acid rejection decreased for membrane NF*.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗