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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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DOE OSTI2024

Small‐Molecule Mixed Ionic‐Electronic Conductors for Efficient N‐Type Electrochemical Transistors: Structure‐Function Correlations

Abstract The fundamental challenge in electron‐transporting organic mixed ionic‐electronic conductors (OMIECs) is simultaneous optimization of electron and ion transport. Beginning from Y6‐type/U‐shaped non‐fullerene solar cell acceptors, we systematically synthesize and characterize molecular structures that address the aforementioned challenge, progressively introducing increasing numbers of oligoethyleneglycol (OEG; g) sidechains from 1 g to 3 g, affording OMIECs 1gY, 2gY, and 3gY, respectively. The crystal structure of 1gY preserves key structural features of the Y n series: a U‐shaped/planar core, close π–π molecular stacking, and interlocked acceptor groups. Versus inactive Y6 and Y11, all of the new glycolated compounds exhibit mixed ion‐electron transport in both conventional organic electrochemical transistor (cOECT) and vertical OECT (vOECT) architectures. Notably, 3gY with the highest OEG density achieves a high transconductance of 16.5 mS, an on/off current ratio of ~10 6 , and a turn‐on/off response time of 94.7/5.7 ms in vOECTs. Systematic optoelectronic, electrochemical, architectural, and crystallographic analysis explains the superior 3gY‐based OECT performance in terms of denser n gY OEG content, increased crystallite dimensions with decreased long‐range crystalline order, and enhanced film hydrophilicity which facilitates ion transport and efficient redox processes. Finally, we demonstrate an efficient small‐molecule‐based complementary inverter using 3gY vOECTs, showcasing the bioelectronic applicability of these new small‐molecule OMIECs.

Cho, Yongjoon↗
DOE OSTI2024

Topological Characterization and Uncertainty Visualization of Atmospheric Rivers

Atmospheric rivers (ARs) are long, narrow regions of water vapor in the Earth's atmosphere that transport heat and moisture from the tropics to the mid-latitudes. ARs are often associated with extreme weather events in North America and contribute significantly to water supply and flood risk. However, characterizing ARs has been a major challenge due to the lack of a universal definition and their structural variations. Existing AR detection tools (ARDTs) produce distinct AR boundaries for the same event, making the risk assessment of ARs a difficult task. Understanding these uncertainties is crucial to improving the predictability of AR impacts, including their landfall areas and associated precipitation, which could cause catastrophic flooding and landslides over the coastal regions. In this work, we develop an uncertainty visualization framework that captures boundary and interior uncertainties, i.e., structural variations, of an ensemble of ARs that arise from a set of ARDTs. We first provide a statistical overview of the AR boundaries using the contour boxplots of Whitaker et al. that highlight the structural variations of AR boundaries based on their nesting relationships. We then introduce the topological skeletons of ARs based on Morse complexes that characterize the interior variation of an ensemble of ARs. We propose an uncertainty visualization of these topological skeletons, inspired by MetroSets of Jacobson et al. that emphasizes the agreements and disagreements across the ensemble members. Through case studies and expert feedback, we demonstrate that the two approaches complement each other, and together they could facilitate an effective comparative analysis process and provide a more confident outlook on an AR's shape, area, and onshore impact.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Rotating-Coil Measurement System for Small-Bore-Diameter Magnet Characterization

Rotating-coil measurement systems are widely used to measure the multipolar fields of particle accelerator magnets. This paper presents a rotating-coil measurement system that aims at providing a complete data set for the characterization of quadrupole magnets with small bore diameters (26 mm). The PCB magnetometer design represents a challenging goal for this type of transducer. It is characterized by an aspect ratio 30% higher than the state of the art, imposed by the reduced dimension of the external radius of the rotating shaft and the necessity of covering the entire magnet effective length (500 mm or higher). The system design required a novel design for the mechanical asset, also considering the innovation represented by the commercial carbon fiber tube, housing the PCB magnetometer. Moreover, the measurement system is based primarily on standard and commercially available components, with simplified control and post-processing software applications. The system and its components are cross-calibrated using a stretched-wire system and another rotating-coil system. The measurement precision is established in a measurement campaign performed on a quadrupole magnet characterized by an inner bore diameter of 45 mm.

42 ENGINEERING↗
DOE OSTI2025

Packages of Distributed Energy Technologies Demonstrating Demand Flexibility at Community Scale

The combination of increased electric load growth across all sectors, deferred electrical infrastructure investment, and other factors resulting in variable electric power supply, has created technical challenges to maintaining a resilient and reliable grid. Many federal, regional, and local efforts are in play to modernize the electric grid, including advancing building technologies and distributed energy resources (DERs) that are utilizing smarter controls to become responsive to both occupant and grid needs. This report reviews ten pilot projects demonstrating how groups of buildings combined with behind-the-meter (BTM) DERs such as electric vehicle (EV) charging, battery storage, flexible HVAC and domestic hot water systems, and photovoltaic systems can reliably and cost effectively provide grid services. Each of the ten pilot projects aim to deliver both energy efficiency and demand flexibility (DF) while supporting load growth. The ten demonstration teams are piloting flexible DER packages across diverse communities of residential and commercial buildings to address a variety of regional grid needs. The outcomes of these pilot projects will be used to inform future scaling through utility program development. This paper characterizes the ten teams, showcasing the decision-making process used by each group to develop their packages (Section 2), the grid services they plan to deliver (Section 3), the types of DER packages selected for deployment within building sectors (Section 4) and trends between building sector, DER types, and grid services In order to achieve community scale benefits, the pilot projects must utilize aggregated control mechanisms for coordinating buildings and DERs together. Several types of coordinated control architectures have evolved amongst the teams, influenced by use type, existing market conditions, and integration type. Three coordinated controls architectures have been characterized, highlighting their use cases, benefits, challenges, and tradeoffs in their design. These insights can aid utilities, control vendors, and developers in scaling community-level energy systems (Paul, 2024). Ultimately, the technology packages selected by the ten teams will be coordinated to provide power system services, also known as grid services. Insights from these demonstrations will be useful for grid operators, regulators, aggregators and other stakeholders as they look to deploy demand flexible resources as grid services in the future. The grid services that each team is targeting for demonstration are described in Section 3 and Section 4. Methods for evaluating the grid services have been described in the paper Metrics for Evaluating Grid Service Provision from Communities of Grid-interactive and Efficient Buildings and other DER (MacDonald, 2023). To identify technology packages for demonstration, Section 2 shows that project teams used a range of analysis approaches, including building energy modeling, AMI data analysis, cost-benefit frameworks, and utility pilot data. Some teams emphasized technical modeling to quantify grid impacts and demand reduction potential, while others prioritized economic evaluations, stakeholder input, or exploratory pilots to inform deployment decisions. This diversity reflects the need to tailor selection methods to project goals, available data, and organizational context. Section 5 discusses trends between the DER technologies deployed and the grid service provisions from each team. Residential buildings (multifamily and single family) lean towards technologies that enhance energy efficiency (e.g. weatherization upgrades, smart thermostats) and onsite power generation integration (e.g. solar PV). Commercial building demonstrations prioritize technologies that ensure operational reliability (e.g. battery storage) and centralized energy management systems and optimization solutions. Teams that are deploying controllable storage-based technologies are more likely to provide grid services that require a near real-time response. Teams incorporating load shifting technologies like smart thermostats with HEMs are likely to include energy markets participation and customer bill management offerings. Campus demonstrations are adopting diverse sets of DERs to emphasize renewable generation, paired with centralized control. This section also describes technologies that were considered during project planning but ultimately excluded from final deployment. These demonstrations reveal that effective DER package design should be tailored to building type, customer segment, and construction vintage. Multifamily buildings benefit from centralized HVAC upgrades and supervisory controls, while single-family homes are well-suited for individualized technologies like solar, storage, and smart home energy monitors. Commercial and campus settings prioritize EMIS integration and load optimization. New construction enables cost-effective integration of DER-ready infrastructure, whereas retrofits require deployments aligned with owner and tenant value streams. For utility program planners, early coordination with developers and building owners, paired with segmented and modular program offerings, can improve adoption, scalability, and grid impact.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2024

LSBGnet: an improved detection model for low-surface brightness galaxies

ABSTRACT The Chinese Space Station Telescope (CSST) is scheduled to launch soon, which is expected to provide a vast amount of image potentially containing low-surface brightness galaxies (LSBGs). However, detecting and characterizing LSBGs is known to be challenging due to their faint surface brightness, posing a significant hurdle for traditional detection methods. In this paper, we propose LSBGnet, a deep neural network specifically designed for automatic detection of LSBGs. We established LSBGnet-SDSS model using data set from the Sloan Digital Sky Survey (SDSS). The results demonstrate a significant improvement compared to our previous work, achieving a recall of 97.22 per cent and a precision of 97.27 per cent on the SDSS test set. Furthermore, we use the LSBGnet-SDSS model as a pre-training model, employing transfer learning to retrain the model with LSBGs from Dark Energy Survey (DES), and establish the LSBGnet-DES model. Remarkably, after retraining the model on a small DES sample, it achieves over 90 per cent precision and recall. To validate the model’s capabilities, we utilize the trained LSBGnet-DES model to detect LSBG candidates within a selected 5 sq. deg area in the DES footprint. Our analysis reveals the detection of 204 LSBG candidates, characterized by a mean surface brightness range of $23.5\ \mathrm{ mag}\ \mathrm{ arcsec}^{-2}\le \bar{\mu }_{\text{eff}}(g)\le 26.8\ \mathrm{ mag}\ \mathrm{ arcsec}^{-2}$ and a half-light radius range of 1.4 arcsec ≤ r1/2 ≤ 8.3 arcsec. Notably, 116 LSBG candidates exhibit a half-light radius ≥2.5 arcsec. These results affirm the remarkable performance of our model in detecting LSBGs, making it a promising tool for the upcoming CSST.

Su, Hao (ORCID:0009000778888301)↗
DOE OSTI2024

Nondestructive Analysis of Commercial Batteries

Electrochemical batteries play a crucial role for powering portable electronics, electric vehicles, large-scale electric grids, and future electric aircraft. However, key performance metrics such as energy density, charging speed, lifespan, and safety raise significant consumer concerns. Enhancing battery performance hinges on a deep understanding of their operational and degradation mechanisms, from material composition and electrode structure to large-scale pack integration, necessitating advanced characterization methods. These methods not only enable improved battery performance but also facilitate early detection of substandard or potentially hazardous batteries before they cause serious incidents. Here, this review comprehensively examines the operational principles, applications, challenges, and prospects of cutting-edge characterization techniques for commercial batteries, with a specific focus on in situ and operando methodologies. Furthermore, it explores how these powerful tools have elucidated the operational and degradation mechanisms of commercial batteries. By bridging the gap between advanced characterization techniques and commercial battery technologies, this review aims to guide the design of more sophisticated experiments and models for studying battery degradation and enhancement.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Nanotechnology for catalysis and solar energy conversion

This roadmap on Nanotechnology for Catalysis and Solar Energy Conversion focuses on the application of nanotechnology in addressing the current challenges of energy conversion: 'high efficiency, stability, safety, and the potential for low-cost/scalable manufacturing' to quote from the contributed article by Nathan Lewis. This roadmap focuses on solar-to-fuel conversion, solar water splitting, solar photovoltaics and bio-catalysis. It includes dye-sensitized solar cells (DSSCs), perovskite solar cells, and organic photovoltaics. Smart engineering of colloidal quantum materials and nanostructured electrodes will improve solar-to-fuel conversion efficiency, as described in the articles by Waiskopf and Banin and Meyer. Semiconductor nanoparticles will also improve solar energy conversion efficiency, as discussed by Boschloo et al in their article on DSSCs. Perovskite solar cells have advanced rapidly in recent years, including new ideas on 2D and 3D hybrid halide perovskites, as described by Spanopoulos et al 'Next generation' solar cells using multiple exciton generation (MEG) from hot carriers, described in the article by Nozik and Beard, could lead to remarkable improvement in photovoltaic efficiency by using quantization effects in semiconductor nanostructures (quantum dots, wires or wells). These challenges will not be met without simultaneous improvement in nanoscale characterization methods. Terahertz spectroscopy, discussed in the article by Milot et al is one example of a method that is overcoming the difficulties associated with nanoscale materials characterization by avoiding electrical contacts to nanoparticles, allowing characterization during device operation, and enabling characterization of a single nanoparticle. Besides experimental advances, computational science is also meeting the challenges of nanomaterials synthesis. The article by Kohlstedt and Schatz discusses the computational frameworks being used to predict structure–property relationships in materials and devices, including machine learning methods, with an emphasis on organic photovoltaics. The contribution by Megarity and Armstrong presents the 'electrochemical leaf' for improvements in electrochemistry and beyond. In addition, biohybrid approaches can take advantage of efficient and specific enzyme catalysts. These articles present the nanoscience and technology at the forefront of renewable energy development that will have significant benefits to society.

14 SOLAR ENERGY↗
DOE OSTI2022

Energy-resolved mass spectrometry as a tool for identification of lignin depolymerization products

Lignin is the largest source of bio-based aromatic compounds in nature, and its valorization is essential to the sustainability of lignocellulosic biorefining. Characterizing lignin-derived compounds remains challenging due to the heterogeneity of this biopolymer. Tandem mass spectrometry is a promising tool for lignin structural analytics, as fragmentation patterns of model compounds can be extrapolated to identify characteristic moieties in complex samples. This work extends previous resonance excitation type collision-induced dissociation (CID) methods that identified lignin oligomers containing β-Ο-4, β-5, and β-β bonds, to also identify characteristics of 5-5, β-1, and 4-Ο-5 dimers, enabled by quadrupole time-of-flight (QTOF) CID with energy-resolved mass spectrometry (ERMS). Overall, beam type ERMS offers in-depth structural information and could ultimately contribute to tools for high-throughput lignin dimer identification.

09 BIOMASS FUELS↗
DOE OSTI2022

Understanding the structure and composition of recalcitrant oligosaccharides in hydrolysate using high-throughput biotin-based glycome profiling and mass spectrometry

Novel Immunological and Mass Spectrometry Methods for Comprehensive Analysis of Recalcitrant Oligosaccharides in AFEX Pretreated Corn Stover. Lignocellulosic biomass is a sustainable alternative to fossil fuel and is extensively used for developing bio-based technologies to produce products such as food, feed, fuel, and chemicals. The key to these technologies is to develop cost competitive processes to convert complex carbohydrates present in plant cell wall to simple sugars such as glucose, xylose, and arabinose. Since lignocellulosic biomass is highly recalcitrant, it must undergo a combination of thermochemical treatment such as Ammonia Fiber Expansion (AFEX), dilute acid (DA), Ionic Liquid (IL) and biological treatment such as enzyme hydrolysis and microbial fermentation to produce desired products. However, when using commercial fungal enzymes during hydrolysis, only 75–85% of the soluble sugars generated are monomeric sugars, while the remaining 15–25% are soluble recalcitrant oligosaccharides that cannot be easily utilized by microorganisms. Previously, we successfully separated and purified the soluble recalcitrant oligosaccharides using a combination of charcoal and celite-based separation followed by size exclusion chromatography and studies their inhibitory properties on enzymes. We discovered that the oligosaccharides with higher degree of polymerization (DP) containing methylated uronic acid substitutions were more recalcitrant towards commercial enzyme mixtures than lower DP and neutral oligosaccharides. Here, we report the use of several complementary techniques that include glycome profiling using plant biomass glycan specific monoclonal antibodies (mAbs) to characterize sugar linkages in plant cell walls and enzymatic hydrolysate, matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) using structurally-informative diagnostic peaks offered by negative ion post-secondary decay spectra, gas chromatography followed by mass spectrometry (GC–MS) to characterize oligosaccharide sugar linkages with and without derivatization. Since oligosaccharides (DP 4–20) are small, it is challenging to mobilize these molecules for mAbs binding and characterization. To overcome this problem, we have applied a new biotin-coupling based oligosaccharide immobilization method that successfully tagged most of the low DP soluble oligosaccharides on to a micro-plate surface followed by specific linkage analysis using mAbs in a high-throughput system. This new approach will help develop more advanced versions of future high throughput glycome profiling methods that can be used to separate and characterize oligosaccharides present in biomarkers for diagnostic applications.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Mechanical Characterization of Loblolly Pine

Biorefineries are faced with various material flow challenges during feeding and handling, due to inherent variability and inhomogeneity of biomass feedstocks. This impacts the efficiency of refinery processes and unit operations. Proper characterization of bulk properties allows for optimal process design and reduction of overall costs. This work is aimed at evaluating the physical and mechanical properties that impact bulk flow of loblolly pine. Cyclic axial compression tests are performed to elucidate consolidation behavior under different stress conditions. The results are then used to develop correlations between material parameters (particle size, tissue type, moisture content) and Elastic Modulus of bulk samples.

09 BIOMASS FUELS↗
DOE OSTI2023

In Situ Attenuated Total Reflectance Infrared Spectroelectrochemistry (ATR-IR-SEC) for the Characterization of Molecular Redox Processes on Surface-Proximal Doped Silicon ATR Crystal Working Electrodes

In situ mid-infrared spectroscopy is a powerful technique for understanding the mechanism of CO 2 reduction (CO 2 R) catalysts because it enables the direct detection of catalytic intermediates and products. Moreover, spectroelectrochemistry (SEC), the coupling of spectroscopy with electrochemistry, allows spectroscopic changes to be correlated with applied potentials to reveal potential-dependent intermediates that are often relevant to photoelectrochemical reactions. Hybrid photoelectrodes, comprised of a narrow bandgap semiconductor, like silicon (Si), with a covalently-linked molecular catalyst, are a promising platform for sunlight-driven catalysis, but characterization of the catalytic mechanism(s) is challenging under photoelectrochemical conditions, particularly when the catalyst is present in monolayer or less concentrations. Here, we have developed a new strategy to use multiple-reflection attenuated total reflectance IR spectroscopy (ATR-IR) coupled with electrochemistry to characterize catalysts directly integrated with a semiconductor surface under applied potential. We show that by surface-proximal n-type or p-type doping of the top ~100-200 nm of the crystal surface, Si ATR crystals can be used simultaneously as the internal reflection element and semiconductor working electrode for ATR-IR-SEC measurements. The surface-proximal doping strategy yields a quasi-equipotential surface with excellent infrared transparency that would have been compromised by free carrier absorption if the crystal was uniformly doped. This approach permits the catalytically-active functionalized surface to be directly probed without modification and overcomes signal-to-noise limitations of other strategies that use separately deposited working electrodes on Si ATR crystals. Proof-of-concept ATR-IR-SEC spectra were collected during the reduction and oxidation of monolayers of Re- and Ru-based transition metal carbonyl complexes, respectively, verifying the viability of the technique to probe redox processes associated with CO 2 R catalysts on Si electrode surfaces with high sensitivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Polymer Deconstruction and Redesign Strategies for Plastics Recycling

Advancing plastics recycling requires both the selective deconstruction of existing polymers and the design of new materials that enable efficient reuse without loss of performance. This perspective highlights an integrated approach that is rooted in polymer chemistry, catalysis, and process engineering which can enable a circular plastics economy. Here, we outline recent advances in catalytic, solvolytic, and enzymatic pathways for plastic deconstruction, and examine the molecular design principles driving next-generation recyclable-by-design and bio-based polymers. Despite these advances, major knowledge gaps remain in understanding the evolution of polymer morphology and catalyst structure during deconstruction, assessing deconstruction processes with realistic polymers, and offering redesigned polymers with competitive cost and environmental advantage over conventional plastics. United States Department of Energy (U.S. DOE) national laboratories offer unique capabilities to address these challenges through in situ and operando characterization, high-throughput experimentation, environmental studies, technoeconomic and life cycle assessment, scale-up support, and collaboration networks. Advances made in understanding plastic deconstruction mechanisms and structure-property correlations of redesigned polymers inform emerging research directions including autonomous experimentation, real-time feedback-enabled process optimization, and protein engineering for enzymatic depolymerization.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Photo‐Induced Charge State Dynamics of the Neutral and Negatively Charged Silicon Vacancy Centers in Room‐Temperature Diamond

Abstract The silicon vacancy (SiV) center in diamond is drawing much attention due to its optical and spin properties, attractive for quantum information processing and sensing. Comparatively little is known, however, about the dynamics governing SiV charge state interconversion mainly due to challenges associated with generating, stabilizing, and characterizing all possible charge states, particularly at room temperature. Here, multi‐color confocal microscopy and density functional theory are used to examine photo‐induced SiV recombination — from neutral, to single‐, to double‐negatively charged — over a broad spectral window in chemical‐vapor‐deposition (CVD) diamond under ambient conditions. For the SiV 0 to SiV ‐ transition, a linear growth of the photo‐recombination rate with laser power at all observed wavelengths is found, a hallmark of single photon dynamics. Laser excitation of SiV ‒ , on the other hand, yields only fractional recombination into SiV 2‒ , a finding that is interpreted in terms of a photo‐activated electron tunneling process from proximal nitrogen atoms.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

The Hoyle Family: The Search for Alpha-Condensate States in Light Nuclei

Our present understanding of the structure of the Hoyle state in 12 C and other near-threshold states in α-conjugate nuclei is reviewed in the framework of the α-condensate model. The 12 C Hoyle state, in particular, is a candidate for α-condensation, due to its large radius and α-cluster structure. The predicted features of nuclear α-particle condensates are reviewed along with a discussion of their experimental indicators, with a focus on precision break-up measurements. Two experiments are discussed in detail, firstly concerning the break-up of 12 C and then the decays of heavier nuclei. With more theoretical input, and increasingly complex detector setups, precision break-up measurements can, in principle, provide insight into the structures of states in α-conjugate nuclei. However, the commonly-held belief that the decay of a condensate state will result in Nα-particles is challenged. We further conclude that unambiguously characterizing excited states built on α-condensates is difficult, despite improvements in detector technology.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2022

Modification of conventional peak shapes to accurately represent spectral asymmetry: High-Resolution X-ray photoelectron spectra of [C 4 C 1 Pyrr][NTf 2 ] and [C 8 C 1 Im][NTf 2 ] ionic liquids

X-ray photoelectron spectroscopy (XPS) is one of the most widely used techniques for surface characterization. Analysis of XPS data is challenging and requires the analyst to fit the data with synthetic line shapes to reach physically meaningful interpretations. Experimental spectral envelopes, however, are complex and display asymmetric features that are often ignored or attributed to additional chemical components. The high-resolution XPS spectra of [C 4 C 1 Pyrr][NTf 2 ] and [C 8 C 1 Im][NTf 2 ] all exhibit a degree of asymmetry which is systematically observed at the higher binding energy side of photoemission envelopes. Here, we present the development of a refined fitting procedure for XPS spectra of these ionic liquid-based systems which include (a) Shirley background offset necessary to account for the insulator-like region and (b) spectral asymmetry in C 1s and N 1s regions. Further, Shirley and trapezoid components are applied to compensate for inelastic scattering taking place during electron transitions as high as 7.8 eV above the start of the fitting region in C 1s high-resolution spectrum. To demonstrate the fitness of this model, we present an analysis of a 2:1 mixture of [C 4 C 1 Pyrr][NTf 2 ]: [C 8 C 1 Im][NTf 2 ].

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Structural Changes in Metal Chalcogenide Nanoclusters Associated with Single Heteroatom Incorporation

Atomically precise nanoclusters (NCs) are promising building blocks for designing materials and interfaces with unique properties. By incorporating heteroatoms into the core, the electronic and magnetic properties of NCs can be precisely tuned. To accurately predict these properties, density functional theory (DFT) is often employed, making the rigorous benchmarking of DFT results particularly important. In this study, we present a benchmarking approach based on metal chalcogenide NCs as a model system. We synthesized a series of bimetallic, iron-cobalt chalcogenide NCs [Co 6-x Fe x S 8 (PEt 3 ) 6 ] + (x = 0-6) (PEt = triethyl phosphine) and investigated the effect of heteroatoms in the octahedral metal chalcogenide core on their size and electronic properties. Using ion mobility-mass spectrometry (IM-MS), we observed a gradual increase in the collision cross section (CCS) with an increase in the number of Fe atoms in the core. DFT calculations combined with trajectory method CCS simulations successfully reproduced this trend, revealing that the increase in cluster size is primarily due to changes in metal-ligand bond lengths, while the electronic properties of the core remain largely unchanged. Moreover, this method allowed us to exclude certain multiplicity states of the NCs, as their CCS values were significantly different from those predicted for the lowest-energy structures. Here, this study demonstrates that gas-phase IM-MS is a powerful technique for detecting subtle size differences in atomically precise NCs, which are often challenging to observe using conventional NC characterization methods. Accurate CCS measurements are established as a benchmark for comparison with theoretical calculations. The excellent correspondence between experimental data and theoretical predictions establishes a robust foundation for investigating structural changes of transition metal NCs of interest to a broad range of applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Using Multiple Isotope-Labeled Infrared Spectra for the Structural Characterization of an Intrinsically Disordered Peptide

Intrinsically disordered proteins (IDPs) rapidly interconvert between conformers, requiring an ensemble description. This complicates their experimental characterization, and force field limitations pose challenges for their simulation. Here, in this work, we use isotope-labeled and unlabeled infrared (IR) spectra to reweight simulated ensembles of the elastin-like peptide GVGVPGVG, a paradigmatic disordered peptide. By comparing the results obtained with different spectra, we explicitly show that the weights are underdetermined by the ensemble averaged data. We identify which labels and frequency regions maximize structural information while minimizing sensitivity to simulation error and show that these regions report on whether the peptide makes specific interactions. Our work shows the importance of incorporating simulations and simulated spectra at the planning stages of isotope-labeled IR experiments and more generally provides a framework for interpreting IR data for IDPs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗