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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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At least 217 records · Page 12

Single crystal purification reduces trace impurities in halide perovskite precursors, alters perovskite thin film performance, and improves phase stability

Impurities present in commercially available halide perovskite precursors are known to affect photovoltaic performance. Here, we employ bulk single crystal growth of FAPbI 3 using solvent orthogonality induced crystallization (SONIC) to remove a broad set of extrinsic impurities from commercially available halide perovskite precursors, as verified by detailed chemical analysis. Following SONIC purification, FAPbI 3 films made from PbI 2 of originally low purity (99%) and high purity (99.99%) show improved phase purity and stability under light and heat relative to films made from raw precursors or precursors purified via retrograde powder crystallization (RPC) in 2-methoxyethanol, a method commonly utilized in recent reports of the highest-efficiency perovskite solar cells. In conclusion, single-crystal purification of precursors improves film stability under operational stressors, and the large enhancements in material purity provide a cleaner slate for improved isolation of compositional and additive effects on perovskite phase stability.

14 SOLAR ENERGY↗

Modeling of Sagging for 3D Printed Layers During the Curing Process

Here, a printed layer of silica-enforced poly(dimethylsiloxane)-co-(diphenylsiloxane) is modeled as a two-phase system consisting of air and polymer with an interface set up during the printing process. The structural geometry changes mostly due to the action of surface tension, while all material properties are strongly temperature dependent. Polymer flow is described using equations of the extended Herschel–Bulkley model, with parameters strongly dependent on temperature and degree of curing. Parameters of the model are determined using flow sweep measurements and separate experiments with vertical structure sagging at different temperatures. The curing process is modeled using dependencies between the curing rate, degree of curing, and temperature obtained in studies by differential scanning calorimetry. The developed model is used for simulations of printed structure deformations with different initial and boundary conditions.

36 MATERIALS SCIENCE↗

Mixed Plastics Waste Valorization through Tandem Chemical Oxidation and Biological Funneling

Mixed plastics waste represents an abundant and largely untapped feedstock for the production of valuable products. The chemical diversity and complexity of these materials, however, present major barriers to realizing this opportunity. In this work, we show that metal-catalyzed autoxidation depolymerizes comingled polymers into a mixture of oxygenated small molecules that are advantaged substrates for biological conversion. We engineer a robust soil bacterium, Pseudomonas putida, to funnel these oxygenated compounds into a single exemplary chemical product, either ..beta..-ketoadipate or polyhydroxyalkanoates. This hybrid process establishes a strategy for the selective conversion of mixed plastics waste into useful chemical products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Highly Flexible Dielectric Films from Solution Processable Covalent Organic Frameworks**

Covalent organic frameworks (COFs) are known to be a promising class of materials for a wide range of applications, yet their poor solution processability limits their utility in many areas. Here we report a pore engineering method using hydrophilic side chains to improve the processability of hydrazone and β-ketoenamine-linked COFs and the production of flexible, crystalline films. Further, mechanical measurements of the free-standing COF films of COF-PEO-3 (hydrazone-linked) and TFP-PEO-3 (β-ketoenamine-linked), revealed a Young's modulus of 391.7 MPa and 1034.7 MPa, respectively. The solubility and excellent mechanical properties enabled the use of these COFs in dielectric devices. Specifically, the TFP-PEO-3 film-based dielectric capacitors display simultaneously high dielectric constant and breakdown strength, resulting in a discharged energy density of 11.22 J cm -3 . This work offers a general approach for producing solution processable COFs and mechanically flexible COF-based films, which hold great potential for use in energy storage and flexible electronics applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

SuFExable polymers with helical structures derived from thionyl tetrafluoride

Sulfur(VI) fluoride exchange (SuFEx) is a category of click chemistry that enables covalent linking of modular units through sulfur(VI) connective hubs. The efficiency of SuFEx and the stability of the resulting bonds have led to polymer chemistry applications. Now, we report the SuFEx click chemistry synthesis of several structurally diverse SOF 4 -derived copolymers based on the polymerization of bis(iminosulfur oxydifluorides) and bis(aryl silyl ethers). This polymer class presents two key characteristics. First, the [-N=S(=O)F-O-] polymer backbone linkages are themselves SuFExable and undergo precise SuFEx-based post-modification with phenols or amines to yield branched functional polymers. Second, studies of individual polymer chains of several of these new materials indicate helical polymer structures. The robust nature of SuFEx click chemistry offers the potential for post-polymerization modification, enabling the synthesis of materials with control over composition and conformation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Importance of Engineered and Learned Molecular Representations in Predicting Organic Reactivity, Selectivity, and Chemical Properties

Machine-readable chemical structure representations are foundational in all attempts to harness machine learning for the prediction of reactivities, selectivities, and chemical properties directly from molecular structure. The featurization of discrete chemical structures into a continuous vector space is a critical phase undertaken before model selection, and the development of new ways to quantitatively encode molecules is an active area of research. Here, we highlight the application and suitability of different representations, from expert-guided “engineered” descriptors to automatically “learned” features, in different prediction tasks relevant to organic and organometallic chemistry, where differing amounts of training data are available. These tasks include statistical models of stereo- and enantioselectivity, thermochemistry, and kinetics developed using experimental and quantum chemical data. The use of expert-guided molecular descriptors provides an opportunity to incorporate chemical knowledge, domain expertise, and physical constraints into statistical modeling. In applications to stereoselective organic and organometallic catalysis, where data sets may be relatively small and 3D-geometries and conformations play an important role, mechanistically informed features can be used successfully to obtain predictive statistical models that are also chemically interpretable. We provide an overview of several recent applications of this approach to obtain quantitative models for reactivity and selectivity, where topological descriptors, quantum mechanical calculations of electronic and steric properties, along with conformational ensembles, all feature as essential ingredients of the molecular representations used. Alternatively, more flexible, general-purpose molecular representations such as attributed molecular graphs can be used with machine learning approaches to learn the complex relationship between a structure and prediction target. This approach has the potential to out-perform more traditional representation methods such as “hand-crafted” molecular descriptors, particularly as data set sizes grow. One area where this is particularly relevant is in the use of large sets of quantum mechanical data to train quantitative structure–property relationships. A general approach toward curating useful data sets and training highly accurate graph neural network models is discussed in the context of organic bond dissociation enthalpies, where this strategy outperforms regression using precomputed descriptors. Finally, we describe how graph neural network predictions can be incorporated into mechanistically informed statistical models of chemical reactivity and selectivity. Once trained, this approach avoids the expensive computational overhead associated with quantum mechanical calculations, while maintaining chemical interpretability. We illustrate examples for which fast predictions of bond dissociation enthalpy and of the identities of radicals formed through cleavage of a molecule’s weakest bond are used in simple physical models of site-selectivity and reactivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A multi-stage single photochrome system for controlled photoswitching responses

The ability of molecular photoswitches to convert on/off responses into large macroscale property change is fundamental to light-responsive materials. However, moving beyond simple binary responses necessitates the introduction of new elements that control the chemistry of the photoswitching process at the molecular scale. To achieve this goal, we designed, synthesized and developed a single photochrome, based on a modified donor–acceptor Stenhouse adduct (DASA), capable of independently addressing multiple molecular states. The multi-stage photoswitch enables complex switching phenomena. To demonstrate this, we show spatial control of the transformation of a three-stage photoswitch by tuning the population of intermediates along the multi-step reaction pathway of the DASAs without interfering with either the first or final stage. This allows for a photonic three-stage logic gate where the secondary wavelength solely negates the input of the primary wavelength. Finally, these results provide a new strategy to move beyond traditional on/off binary photochromic systems and enable the design of future molecular logic systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structural modification of fentanyls for their retrospective identification by gas chromatographic analysis using chloroformate chemistry

Abstract The one-step breakdown and derivatization of a panel of nine fentanyls to yield uniquely tagged products that can be detected by Electron Ionization Gas Chromatography-Mass Spectrometry (EI-GC-MS) is presented. The method involves the treatment of the synthetic opioids with 2,2,2-trichloroethoxycarbonyl chloride (TrocCl) at 60 °C for 3 h in dichloromethane and furnishes two products from one fentanyl molecule that can be used to retrospectively identify the original opioid. Parameters that were studied and fully optimized for the method included temperature, solvent, nature of scavenging base and reaction time. One of the two resulting products from the reaction bears the trichloroethoxycarbonyl (Troc) tag attached to the norfentanyl portion of the original opioid and greatly aids in the opioid detection and identification process. The methodology has been applied to the chemical modification of a panel of nine fentanyls and in all cases the molecular ion peak for the Troc-norfentanyl product bearing the distinctive trichloroethyl isotopic signature can be clearly observed. The method’s LLOD was determined to be 10 ng/mL while its LLOQ was found to be 20 ng/mL. This methodology represents the first application of chloroformates in the chemical modification of this class of synthetic opioids that are notoriously inert to common derivatization strategies available for GC–MS analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Chemical Design of Organic Interface Modifiers for Highly Efficient and Stable Perovskite Solar Cells

Perovskite solar cells (PSCs) have demonstrated rapid progress in their power conversion efficiencies (PCEs) - from 3.8% in 2009 to 25.7% in 2022 - and they have received considerable attention as a promising future photovoltaic (PV) technology. However, the operational stability of PSCs is still inadequate to satisfy the standards for commercial applications. Interface engineering has become one of the most important strategies to push PSCs' efficiency and stability for practical use. Among the various interface engineering approaches, organic interface modifiers (OIMs) have been frequently used by the PSC field to address the issues limiting PSC stability at high efficiency levels. In this perspective, the chemical structures of state-of-the-art OIMs are discussed, and their characteristics are reviewed, as well as the impact on device performance associated with key device interfaces (e.g., metal oxide/perovskite and organic transport layer/perovskite interfaces) from a chemical and materials engineering point of view is discussed. Finally, design considerations and the authors' perspective are discussed, on the basis of representative literature examples, for building new, customized organic OIMs to further improve PSC efficiency and stability toward commercialization.

14 SOLAR ENERGY↗

Porous Materials for Water Purification

Water pollution is a growing threat to humanity due to the pervasiveness of contaminants in water bodies. Significant efforts have been made to separate these hazardous components to purify polluted water through various methods. However, conventional remediation methods suffer from limitations such as low uptake capacity or selectivity, and current water quality standards cannot be met. Recently, advanced porous materials (APMs) have shown promise in improved segregation of contaminants compared to traditional porous materials in uptake capacity and selectivity. These materials feature merits of high surface area and versatile functionality, rendering them ideal platforms for the design of novel adsorbents. Here, this Review summarizes the development and employment of APMs in a variety of water treatments accompanied by assessments of task-specific adsorption performance. Finally, we discuss our perspectives on future opportunities for APMs in water purification.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A scalable and autoclavable oxygen nanosensor platform for metabolic monitoring of Saccharomyces cerevisiae in a bioreactor and other in situ systems

Polymer-encapsulated dye nanoparticle sensors are a valuable approach to achieving in situ analyte measurements with luminescence; however, typical emulsion-based nanosensors are poorly suited for large-scale biological samples due to limitations of synthesis scalability and stability. Branched polyethylenimine (PEI) is a versatile polymer scaffold ideal for constructing nanoparticles with various covalently conjugated moieties due to their high density of reactive primary amines, high water solubility, and biological stability. In this work, we used branched polyethylenimine as a scaffold-based approach for making a stable and scalable ratiometric oxygen sensor. Pt (II) tetracarboxyporphine was used as an oxygen-sensing dye and coumarin 343 as a reference dye, all covalently linked to the PEI scaffold producing a product that could withstand sterilization procedures and easily be scaled. To minimize toxicity from the PEI scaffold, we conjugated it with 2000 MW PEG. The applicability of the sensors was demonstrated in a 200 mL Saccharomyces cerevisiae yeast culture, using orthogonal luminescent and electrochemical oxygen measurements to validate sensor response and measure the metabolic activity of the yeast in our culture. Further, this approach was able to match the sensitivity of our electrochemical measurements while improving upon drawbacks of other luminescent methods of oxygen detection, demonstrating effective monitoring for at least 20 h. Our scaffold-based approach is a modular and easily translatable technology that could be useful in various biotechnological applications.

59 BASIC BIOLOGICAL SCIENCES↗

Accelerated carbonation and structural transformation of blast furnace slag by mechanochemical alkali-activation

Alternative cements and production routes are necessary to offset the considerable global CO 2 emissions of Portland cement production. The combination of alkali-activation and mechanochemical milling in a CO 2 rich atmosphere is a promising green direction for synthesizing cementitious material as it upcycles hazardous material (slag) while capturing wt% of CO 2 during synthesis. We investigate the resulting structural transformations incurred during synthesis and hydration using a suite of characterization techniques including solid-state 27 Al, 29 Si, and 13 C NMR. The local aluminosilicate network structure of the processed clinker is best described by a melilite-type structure. Upon hydration, the network polymerizes to form a calcium, sodium aluminosilicate hydrate gel. The synthesis route also creates various metastable carbonates and bicarbonates from captured CO 2 and alkali-additives that transform into stable carbonate phases like calcite, aragonite, and gaylussite, after hydration. These findings indicate accelerated carbonation reactions occur during clinker production and demonstrates novelty as a green cement technology.

36 MATERIALS SCIENCE↗

Sol-gel processing of a covalent organic framework for the generation of hierarchically porous monolithic adsorbents

Covalent organic frameworks (COFs) have emerged as a versatile material platform for such applications as chemical separations, chemical reaction engineering, and energy storage. Their inherently low mechanical stability, however, frequently renders existing methods of pelletization ineffective, contributing to pore collapse, pore blockage, or insufficient densification of crystallites. Here, we present a process for the shaping and densifying of COFs into robust centimeter-scale porous monoliths without the need for templates, additives, or binders. This process minimizes mechanical damage from shear-induced plastic deformation and further provides a network of interparticle mesopores that we exploit in accessing analyte capacities above those achievable from the intrinsic COF structure. Using a lattice-gas model, we accurately capture the monolithic structure across the mesoporous range and tie pore architecture to performance in both gas-storage and -separation applications. Collectively, these results represent a substantial step in the practical applicability of COFs and other mechanically weak porous materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An investigation on the impact of halidization on substituted dimethoxybenzenes

Functionalized organic molecules are emerging as charge storage materials in electrochemical technologies as the breadth and diversity of the organic design space offers the possibility of purpose-built materials with property sets optimized for a particular application. First developed as overcharge protection materials in lithium-ion batteries, substituted dialkoxybenzenes represent a potentially promising molecular platform for advancing soluble charge storage materials. In this study, we systematically substitute a series of halide groups at the 2- and 5-positions of the 1,4-dimethoxybenzene core, investigate the impact the halide groups have on molecular properties using electrochemical and spectroscopy methods, and compare these results to those of 2,5-dimethyl-1,4-dimethoxybenzene (25DDB), a previously reported derivative. In general, we observe that introduction of heavy halogen atoms leads to decreased gravimetric capacity as compared to 25DDB, but concomitantly improves solubility and redox potentials. As the halide functional group increases in size, the active material becomes less stable in its oxidized state as evinced by both cyclic voltammetry and bulk electrolysis cycling. None of the halogenated species are as stable as 25DDB indicating that these materials may be better suited for applications with more rapid cycling conditions (e.g., redox shuttling). More broadly, these results may serve as a useful data set for computational methods for materials discovery and optimization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Gas-solid reaction pathway for chlorination of rare earth and actinide metals using hydrogen and chlorine gas

Hydriding and chlorination of buttons of metallic cerium have been tested as a head-end step to separating metal impurities from actinides. The objective here was to achieve complete conversion to chlorides while maintaining high surface area via small particles and open porosity. Hydriding by reaction with 100% H 2 gas at 573 K was successful at reducing cm-scale metal buttons into small particles/fragments. This step was followed by reaction with flowing 99.5% anhydrous Cl 2 gas at temperatures ranging from 423 to 573 K for 60 min. In experiments reported here, up to 92% conversion to cerium chloride was achieved from reacting with the anhydrous chlorine gas. The final chloride product has high porosity coupled with small particle sizes (microns to 1600 μm), which makes it suitable for subsequent purification processes. Higher chlorine concentrations in the gas favor higher conversion to chloride. The optimal temperature to achieve high chlorination is 523 K. Oxygen is a minor impurity in the chlorine gas which appears to prevent complete chlorination from being achieved.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Phosphate amendment drives bloom of RNA viruses after soil wet-up

Soil rewetting after a dry period results in a surge of activity and succession in both microbial and DNA virus communities. Less is known about the response of RNA viruses to soil rewetting—while they are highly diverse and widely distributed in soil, they remain understudied. We hypothesized that RNA viruses would show temporal succession following rewetting and that phosphate amendment would influence their trajectory, as viral proliferation may cause phosphorus limitation. Using 39 time-resolved metatranscriptomes and amplicon data, 2190 RNA viral populations were identified across five phyla, with 26 % of these predicted to infect bacteria, and 11 % fungi. Only 1.2 % of viral populations had annotated capsid genes, suggesting most persist via intracellular replication without a free virion phase. Phosphate amendment altered RNA viral community composition within the first week and amended vs. unamended communities remained distinguishable for up to three weeks. While the overall host community remained stable, certain bacterial populations showed reduced abundance in phosphate-amended soils, likely due to increased viral lysis, as RNA bacteriophages proliferated significantly. Notably, 60 % of the viruses with increased abundance under phosphate amendment belonged to basal Lenarviricota clades rather than well-known groups like Leviviricetes. We estimate RNA bacteriophage infections may affect 10 7 –10 9 bacteria per gram of soil, aligning with the total bacterial population (10 7 –10 10 g -1 soil), suggesting that RNA phages significantly influence bacterial communities post-wet-up, with phosphorus availability modulating this effect.

59 BASIC BIOLOGICAL SCIENCES↗

Data Set Analysis to Reduce Uncertainty in Formula Assignments of Ultrahigh Resolution Mass Spectra

Environmental samples contain a vast array of organic compounds with diverse elemental compositions and heteroatom content. Molecular formula assignments of ultrahigh resolution mass spectra (HRMS) hold promise for elucidating the molecular composition of these compounds. However, the need to account for an assortment of heteroatoms increases the uncertainty associated with individual assignments – and ultimately the ecological, biological, and biogeochemical insights gleaned from the assignments. To address this challenge, we introduce a formula assignment strategy that leverages HRMS data sets to improve assignment confidence, filter false assignments, and mitigate bias in assignment routines. The strategy, implemented using CoreMS, first identifies the highest confidence assignment for a recurring ion in a data set by assessing the mass accuracy and isotopologue similarity of all assignments to the ion across the data set. The second component of the strategy examines the consistency of mass errors for an assigned ion throughout a data set and flags formulas with statistically unlikely deviations in mass error. Here, we illustrate the application and utility of the strategy by comparing its results against documented misassignment patterns within a set of oceanographic samples that were measured with 21 T Fourier Transform Ion Cyclotron Resonance Mass Spectrometry. Because the efficacy of our strategy improves with data set size, it is particularly useful for enhancing assignment confidence in large HRMS data sets common in studies of environmental systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗