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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

Differential Mobility Spectrometry on the ISS: Successes and Current Concerns

With the construction of the International Space Station (ISS), crew members moved from the relatively short flights of the Space Shuttle (~ 2 weeks) to missions lasting months to a year. As such, environmental monitoring needs also changed, transitioning from a reliance on archival sampling to a combination of archival sampling and in-flight data collection. In the case of trace volatile organic compound (VOC) monitoring, this in-flight monitoring was performed early on by the Volatile Organic Analyzer (VOA), a gas chromatograph-ion mobility spectrometer, which operated on the ISS for 7 years. This large, fixed-position analyzer was replaced by Air Quality Monitors (AQMs), a pair of small gas chromatograph-differential mobility spectrometers, in the spring of 2013. During their initial half decade of use, and covering multiple sets of units, the AQMs performed well, meeting all of their validation criteria and generally showing excellent accuracy when compared to the now-reduced archival samples. These instruments were also used to perform a survey of the US Operating Segment (US Lab Module, European Columbus Module, and Japanese Pressurized Module), confirming that the atmosphere in this segment is well-mixed. The AQMs were also able to provide important information in contingency situations, such as confirming that no ammonia was present on the ISS following alarms suggesting that the coolant loops had leaked in January 2015. As the fleet of AQMs has aged, though, issues of concern have arisen. These have ranged from pervasive electronics board problems to loss of sensitivity due to carbon dioxide to incorrect identification of compounds. Some of these issues are unavoidable due to the nature of the AQM’s use and preparation prior to flight. However, with the extension of the ISS to 2030 (well past its original 2024 lifetime), the fleet of AQMs will be asked to perform longer, requiring solutions to some of the inherent problems. In this presentation, we will discuss the history of the AQM on the ISS with a focus on more recent results. These results show both the continued usefulness of the AQM for atmospheric monitoring and also the current concerns, including: 1) the incorrect identification of benzene, 2) reporting of elevated isopropanol concentrations, and 3) the loss of the reactant ion peak (RIP) that must be resolved in order for the instrument to continue to serve as the primary trace VOC monitor on the ISS.

William T. Wallace↗
DOE OSTI2020

Impact of dual-layer solid-electrolyte interphase inhomogeneities on early-stage defect formation in Si electrodes

While intensive efforts have been devoted to studying the nature of the solid-electrolyte interphase (SEI), little attention has been paid to understanding its role in the mechanical failures of electrodes. Here we unveil the impact of SEI inhomogeneities on early-stage defect formation in Si electrodes. Buried under the SEI, these early-stage defects are inaccessible by most surface-probing techniques. With operando full field diffraction X-ray microscopy, we observe the formation of these defects in real time and connect their origin to a heterogeneous degree of lithiation. This heterogeneous lithiation is further correlated to inhomogeneities in topography and lithium-ion mobility in both the inner- and outer-SEI, thanks to a combination of operando atomic force microscopy, electrochemical strain microscopy and sputter-etched X-ray photoelectron spectroscopy. Our multi-modal study bridges observations across the multi-level interfaces (Si/LixSi/inner-SEI/outer-SEI), thus offering novel insights into the impact of SEI homogeneities on the structural stability of Si-based lithium-ion batteries. Severe structural deformation during (de)lithiation is the main factor limiting the stability of Si anodes in Li-ion batteries. Here, a multi-modal approach is used to visualize these deformations in their early-stage and link them to inhomogeneities in the dual-layer solid-electrolyte interphase.

25 ENERGY STORAGE↗
DOE OSTI2021

Potentiometric entropy and operando calorimetric measurements reveal fast charging mechanisms in PNb 9 O 25

The Wadsley–Roth compound PNb 9 O 25 is a promising fast charging lithium ion battery anode material with high operating voltage to prevent solid electrolyte interface formation. Here, in this work, we present potentiometric entropy measurements featuring signatures of semiconductor-to-metal transition and intralayer ordering upon lithiation in the anode material PNb 9 O 25 that could not be observed with in situ X-ray diffraction. In addition, the instantaneous heat generation rates at the PNb 9 O 25 working electrode and at the lithium metal counter electrode during galvanostatic cycling were measured individually for the first time by operando isothermal calorimetry. The heat generation rate decreased at the PNb 9 O 25 electrode upon lithiation due to the decrease in electrical resistivity caused by the semiconductor-to-metal transition observed in potentiometric entropy measurements. Furthermore, the heat generation rate at the lithium metal electrode was positive during delithiation due to the exothermic plating of Li + ions on the lithium metal counter electrode associated with dendrite formation. Furthermore, calorimetric measurements established that the entropy change dominated the reversible heat generation rate at each electrode. Finally, the contribution of enthalpy of mixing was relatively small even at high C-rates thanks to the high Li + ion mobility in PNb 9 O 25 confirming its promises as a fast charging anode material.

25 ENERGY STORAGE↗
NASA NTRS1983

Eclipse-related measurements of middle-atmosphere electrical parameters

Measurements of electrical conductivity and its constituent parameters, charge density and ion mobility, are presented for the solar eclipse rocket campaign conducted at Red Lake, Ontario, Canada. Three parachute-borne probes (two Gerdien condensers and a blunt probe) were flown during the eclipse which occurred on 26 February 1979. Additional payloads launched at other times provided important supplemental background measurements. The entire launch series occurred during aurorally active conditions, as indicated by the probe measurements. Specifically, positive conductivity enhancements above 45 km demonstrate the dominance of auroral ionization as a source for positive ions in the region. Such effects evidenced during the eclipse make it difficult to determine the extent to which the decrease in positive conductivity above 60 km is eclipse-related. The negative conductivity component associated with free electrons displays solar dependence both during the eclipse and for the other measurement periods. In spite of the aurorally active conditions, rapid electron loss was observed during totality, thus indicating the importance of non-ionizing solar effects on electrons in the region.

Mitchell, J. D.↗
NASA NTRS2006

Miniature Ion-Array Spectrometer

A figure is shown that depicts a proposed miniature ion-mobility spectrometer that would share many features of design and operation of the instrument described in another article. The main differences between that instrument and this one would lie in the configuration and mode of operation of the filter and detector electrodes. A filter electrode and detector electrodes would be located along the sides of a drift tube downstream from the accelerator electrode. These electrodes would apply a combination of (1) a transverse AC electric field that would effect differential transverse dispersal of ions and (2) a transverse DC electric field that would drive the dispersed ions toward the detector electrodes at different distances along the drift tube. The electric current collected by each detector electrode would be a measure of the current, and thus of the abundance of the species of ions impinging on that electrode. The currents collected by all the detector electrodes could be measured simultaneously to obtain continuous readings of abundances of species. The downstream momentum of accelerated ions would be maintained through neutralization on the electrodes; the momentum of the resulting neutral atoms would serve to expel gases from spectrometer, without need for a pump.

Hartley, Frank T.↗
DOE OSTI2020

Spray Mechanism of Contained-Electrospray Ionization

Analytical characteristics of contained electrospray ionization (ESI) are summarized in terms of its potential to modify the analyte solution during the stages of droplet formation to provide opportunities to generate native versus denatured biomolecular gas-phase ions, without the need for bulk-phase analyte modifications. The real-time modification of the charged microdroplets occurs in a cavity that is included in the outlet of the contained-ESI ion source. Close examination of the inside of the cavity using a high-speed camera revealed the formation of discrete droplets as well as thin liquid films in the droplets wake. When operated at 20 psi N2 pressure, the droplets were observed to move at an average speed of 8 mm/s providing ~1 s mixing time in a 10 mm cavity length. Evidence is provided for the presence of highly reactive charged droplets based on myoglobin charge state distribution, apo-myoglobin contents, and ion mobility drift time profiles under different spray conditions. Mechanistic insights for the capture of vapor-phase reagents and droplet dynamics as influenced by different operational modes are also described.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1999

A Second-Generation Volatile Organic Analyzer for the International Space Station

Early in the development of the Crew Health Care System (CHECS) for the International Space Station (ISS), it was recognized that detection of target volatile organic compounds would be a key component of the air monitoring strategy. Experiences during the NASA/Mir program supported the decision to include a real-time volatile organic analyzer (VOA) aboard ISS to help assess the impact of air quality events on crew health and determine the effectiveness of decontamination efforts. Toward this end, a joint development by the Toxicology Laboratory at Johnson Space Center and Graseby Dynamics produced a VOA that has been delivered and is ready for the first 5 years of ISS operation. The first-generation VOA selection criteria included minimizing size, weight, and power consumption while maintaining analytical performance. Measuring available technologies against these criteria, a VOA system based upon gas chromatography/ion mobility spectrometry (GC/IMS) was selected in the mid-90's. However, as NASA looks forward to later-stage ISS operations and to new frontiers such as human exploration of Mars, the ISS VOA (weighing 43 kg and consuming 160 watts) must be replaced by a smaller, less resource-intensive device. This paper will present a possible second-gene ration VOA based upon the same technology as the first-generation unit. Utilizing GC/IMS technology again will permit the instrumental data and experience gained during the initial phase of ISS to be applied to later ISS phases and advanced spacecraft missions. During the past 3 years, efforts to reduce the size of ion mobility spectrometers have been pursued by Graseby Dynamics, the manufacturer of the first-generation VOA. The concept of operation, expected analytical performance, and estimated size of a fully functional second-generation VOA based upon GC/mini-IMS technology will be presented. Furthermore, results of initial laboratory evaluations will be shown.

Limero, Thomas↗
DOE OSTI2025

Operando Neutron Imaging of Lithium Flux and Gradient Cathode Design for Enhanced Kinetics in High‐Loading All‐Solid‐State Li─S Batteries

All-solid-state Li–sulfur batteries (ASSLSBs) are considered promising candidates for next-generation energy storage owing to their inherent safety, high energy density, and abundant sulfur resources. However, slow redox kinetics greatly limit sulfur utilization during solid-solid sulfur reactions, leading to significant challenges to achieve efficient performance in high-mass-loading ASSLSBs. Here, operando neutron image is employed to directly visualize, for the first time, that sluggish Li + transport kinetics and the uneven distribution of Li + during cathodic reactions are critical factors limiting sulfur conversion. To address this issue, gradient cathode architectures comprising three and five layers are designed, in which catholyte concentrations are strategically varied to optimize Li-ion flux and enhance ionic conductivity of the whole composite cathode electrode. Operando neutron imaging distinctly visualizes and confirms that three-layer gradient approach significantly enhances Li-ion mobility, resulting in more uniform redox reactions and greatly improved sulfur utilization compared to traditional non-gradient structures. Consequently, the three-layer gradient cathode achieves superior rate performance and reduced electrode polarization at high sulfur mass loadings of 4.5 and 6.0 mg cm −2 . Furthermore, the applicability and scalability of this design are demonstrated in a five-layer gradient cathode architecture, achieving an impressive discharge specific capacity increase from 656 mAh g −1 (three-layer gradient) to 1232 mAh g −1 at 1/20 C for ultra-high sulfur loading of 7.5 mg cm −2 . In conclusion, this innovative gradient cathode design offers substantial advancements in understanding and overcoming Li-ion transport limitations, paving the way toward practical, high-energy-density ASSLSBs.

25 ENERGY STORAGE↗
NASA NTRS2007

Potential for Measurement of Trace Volatile Organic Compounds in Closed Environments Using Gas Chromatograph/Differential Mobility Spectrometer

For nearly 3.5 years, the Volatile Organic Analyzer (VOA) has routinely analyzed the International Space Station (ISS) atmosphere for a target list of approximately 20 volatile organic compounds (VOCs). Additionally, an early prototype of the VOA collected data aboard submarines in two separate trials. Comparison of the data collected on ISS and submarines showed a surprising similarity in the atmospheres of the two environments. Furthermore, in both cases it was demonstrated that the VOA data can detect hardware issues unrelated to crew health. Finally, it was also clear in both operations that the VOA s size and resource consumption were major disadvantages that would restrict its use in the future. The VOA showed the value of measuring VOCs in closed environments, but it had to be shrunk if it was to be considered for future operations in these environments that are characterized by cramped spaces and limited resources. The Sionex Microanalyzer is a fraction of the VOA s size and this instrument seems capable of maintaining or improving upon the analytical performance of the VOA. The two design improvements that led to a smaller, less complex instrument are the Microanalyzer s use of recirculated air as the gas chromatograph s carrier gas and a micromachined detector. Although the VOA s ion mobility spectrometer and the Microanalyzer s differential mobility spectrometer (DMS) are related detector technologies, the DMS was more amenable to micromachining. This paper will present data from the initial assessment of the Microanalyzer. The instrument was challenged with mixtures that simulated the VOCs typically detected in closed-environment atmospheres.

Limero, Thomas↗
DOE OSTI2020

Revealing High Na-Content P2-Type Layered Oxides as Advanced Sodium-Ion Cathodes

Layered Na-based oxides with the general composition of Na x TMO 2 (TM: transition metal) have attracted significant attention for their high compositional diversity that provides tunable electrochemical performance for electrodes in sodium-ion batteries. The various compositions bring forward complex structural chemistry that is decisive for the layered stacking structure, Na-ion conductivity, and the redox activity, potentially promising new avenues in functional material properties. In this work, we have explored the maximum Na content in P2-type layered oxides and discovered that the high-content Na in the host enhances the structural stability; moreover, it promotes the oxidation of low-valent cations to their high oxidation states (in this case Ni 2+ ). This can be rationalized by the increased hybridization of the O(2p)-TM(3d-e g *) states, affecting both the local TM environment as well as the interactions between the NaO 2 and TMO 2 layers. These properties are highly beneficial for the Na storage capabilities as required for cathode materials in sodium-ion batteries. It leads to excellent Na-ion mobility, a large storage capacity (>100 mAh g –1 between 2.0-4.0 V), yet preventing the detrimental sliding of the TMO 2 layers (P2–O2 structural transition), as reflected by the ultralong cycle life (3000 (dis)charge cycles demonstrated). These findings expand the horizons of high Na-content P2-type materials, providing new insights of the electronic and structural chemistry for advanced cathode materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Rapid Targeted Quantitation of Protein Overexpression with Direct Infusion Shotgun Proteome Analysis (DISPA-PRM)

While much effort has been placed on comprehensive quantitative proteome analysis, certain applications demand measurement of only a few target proteins from complex systems. Traditional approaches to targeted proteomics rely on nano-liquid chromatography (nLC) and targeted mass spectrometry (MS) methods, e.g., parallel reaction monitoring (PRM). However, the time requirement for nLC can limit throughput of targeted proteomics. To achieve rapid and high-throughput targeted methods, here we show that nLC separations can be eliminated and replaced with direct infusion shotgun proteome analysis (DISPA) using high-field asymmetric waveform ion mobility spectrometry (FAIMS) with PRM. We demonstrate application of DISPA-PRM for rapid targeted quantification of bacterial enzymes utilized in the production of biofuels by monitoring temporal expression in 72 metabolically engineered bacterial cultures in under 2.5 hours, with a measured dynamic range >1200-fold. Here, we conclude that DISPA-PRM presents a valuable innovative tool with results comparable to nLC-MS/MS, enabling fast and rapid detection of targeted proteins in complex mixtures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Tailoring Disordered/Ordered Phases to Revisit the Degradation Mechanism of High‐Voltage LiNi 0.5 Mn 1.5 O 4 Spinel Cathode Materials

Abstract In the spinel oxide cathode family, LiNi 0.5 Mn 1.5 O 4 (LNMO) shows a high operating voltage (≈4.7 V vs Li/Li + ) and excellent Li‐ion mobility with stable 3D conducting channels. Ni/Mn cation disordered and ordered phases usually coexist in LNMO materials, and they have distinct structural and electrochemical properties, resulting in different battery performances for LNMO materials with different phase compositions. Identifying the correlation between phase compositions and electrochemical properties is of significance to the improvement of battery performance and understanding of degradation mechanisms. Herein, the disordered/ordered phase compositions in LNMO materials are tailored by post‐annealing strategies and their impacts on electrochemical performance and degradation mechanisms from the surface to the bulk are systematically investigated. The ordered phase increases rapidly as Mn 3+ is oxidized to Mn 4+ through a post‐annealing process. LNMO with an intermediate fraction of disordered and ordered phases gives rise to improved cycling stability. This article further reports that a high ordered phase fraction can preferentially protect Ni from dissolution during cycling. However, these results suggest that the transition metal dissolution and surface structural change of LNMO do not exhibit a direct correlation with cycling stability. These results indicate the capacity fading mainly correlates with the bulk structural distortion, leading to decreased Li‐ion kinetics.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Highly selective ion separations based on counter-flow electromigration in nanoporous membranes

Highly selective ion separations are vital for recovering important salts, and membrane-based techniques may enable environmentally friendly ion separations that operate continuously. This study demonstrates that simply opposing convective flow with electromigration in track-etched membranes leads to remarkable selectivities among monovalent ions. Because the membrane-pore diameters are orders of magnitude larger than the ion diameters, advection moves all ions at the same velocity, whereas electrophoretic velocities are proportional to ion mobilities. Thus during counter-flow cation electromigration, less mobile cations have lower electromigration velocity components and pass through porous membranes more rapidly than more mobile cations. Using membranes with 400 nm pores, counter-flow electromigration gives Li + /K + selectivities of 100 and Li + /Na + selectivities around 30 in mixed-salt studies. In this work, numerical simulations based on the extended Nernst-Planck equation agree with trends in experimental data and highlight the importance of high Péclet numbers, high current-to-flow ratios, and uniform current distributions for achieving high selectivities. Importantly, experimental separations give high selectivities at 0.3 M ionic strength and low Li + /K + ratios, which suggest these methods may also work in brine solutions. Nevertheless, energy costs for such separations are high.

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

OzMALDI: A Gas-Phase, In-Source Ozonolysis Reaction for Efficient Double-Bond Assignment in Mass Spectrometry Imaging with Matrix-Assisted Laser Desorption/Ionization

Lipids make up an important class of biomolecules with diverse structures and varied chemical functions. This diversity is a major challenge in chemical analysis and limits our understanding of biological functions and regulation. A major way lipid isomers differ is by double-bond (db) position, and analyzing db-isomers is especially challenging for mass spectrometry imaging (MSI). Ozonolysis can be used to determine the dbposition and has been paired with MSI before. However, previous techniques require increased analysis time to allow for gas-phase reactions within an ion trap or ion mobility cell or additional sample preparation time to allow for offline ozonation. Here, we introduce a new ozonolysis method inside the matrix-assisted laser desorption-ionization (MALDI) source, termed OzMALDI, that simultaneously produces ozonides from all unsaturated lipids. This allows us to determine db-positions without adding additional reaction time while maintaining the high mass resolution provided by Orbitrap MS. This new technique is especially effective at determining multiple db-positions in lipids containing polyunsaturated fatty acids, which is a limitation of many previous techniques. OzMALDI-MSI was applied to the analysis of rat brain and genetically engineered Camelina and soybean seed samples, demonstrating the utility of this method and uncovering novel biological information.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Electrochemical Doping of Halide Perovskites by Noble Metal Interstitial Cations

Abstract Metal halide perovskites are an attractive class of semiconductors, but it has proven difficult to control their electronic doping by conventional strategies due to screening and compensation by mobile ions or ionic defects. Noble‐metal interstitials represent an under‐studied class of extrinsic defects that plausibly influence many perovskite‐based devices. In this work, doping of metal halide perovskites is studied by electrochemically formed Au + interstitial ions, combining experimental data on devices with a computational analysis of Au + interstitial defects based on density functional theory (DFT). Analysis suggests that Au + cations can be easily formed and migrate through the perovskite bulk via the same sites as iodine interstitials (I i + ). However, whereas I i + compensates n‐type doping by electron capture, the noble‐metal interstitials act as quasi‐stable n‐dopants. Experimentally, voltage‐dependent, dynamic doping by current density–time ( J–t ), electrochemical impedance, and photoluminescence measurements are characterized. These results provide deeper insight into the potential beneficial and detrimental impacts of metal electrode reactions on long‐term performance of perovskite photovoltaic and light‐emitting diodes, as well as offer an alternative doping explanation for the valence switching mechanism of halide‐perovskite‐based neuromorphic and memristive devices.

14 SOLAR ENERGY↗
DOE OSTI2020

The Concept of Negative Capacitance in Ionically Conductive Van der Waals Ferroelectrics

Negative capacitance (NC) provides a path to overcome the Boltzmann limit that dictates operating voltages in transistors and, therefore, may open up a path to the challenging proposition of lowering energy consumption and waste heat in nanoelectronic integrated circuits. Typically, NC effects in ferroelectric materials are based on either stabilizing a zero-polarization state or slowing down ferroelectric switching in order to access NC regimes of the free-energy distribution. Here, a fundamentally different mechanism for NC, based on CuInP 2 S 6 , a van der Waals layered ferrielectric, is demonstrated. Using density functional theory and piezo-response force microscopy, it is shown that an unusual combination of high Cu-ion mobility and its crucial role in determining polarization magnitude and orientation (P) leads to a negative slope of the polarization versus the electric field E, dP/dE < 0, which is a requirement for NC. This mechanism for NC is likely to occur in a wide class of materials, offering new possibilities for NC-based devices. Finally, the nanoscale demonstration of this mechanism can be extended to the device-level by increasing the regions of homogeneous polarization and polarization switching, for example, through strain engineering and carefully selected electric field pulses.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Incorporating Electrochemical Halide Oxidation into Drift-Diffusion Models to Explain Performance Losses in Perovskite Solar Cells under Prolonged Reverse Bias

Partial shading of a solar module can induce a set of cells within the module to operate under reverse bias. Studies have shown that metal halide perovskite solar cells with a wide variety of compositions and contacts exhibit interesting behavior in reverse bias that includes both reversible performance loss and non-reversible degradation. In this paper, an advanced drift-diffusion approach incorporating an electrochemical term to explain the short-circuit, open circuit and fill factor losses that are experimentally measured after prolonged reverse bias is used. It is shown that holes can tunnel into the perovskite due to sharp band bending near the contact, accumulate within the bulk of the perovskite absorber, and trigger the oxidation of halides to form neutral halogens. The density of neutral halogens is much higher in reverse bias because there are hardly any electrons available to reduce the iodine. The resulting halogens act as bulk recombination centers. While the interstitial halogen density does decay when the cell is operated in forward bias, permanent degradation can occur if the iodine diffuses out of the perovskite layer. Finally, the ways in which changing parameters such as the mobile ion density or the series resistance at the contact can influence device performance and stability are discussed.

degradation↗
DOE OSTI2021

Three-repeat and four-repeat tau isoforms form different oligomers

Different tauopathies are characterized by the isoform-specific composition of the aggregates found in the brain and by structurally distinct tau strains. Although tau oligomers have been implicated as important neurotoxic species, little is known about how the primary structures of the six human tau isoforms affect tau oligomerization because the oligomers are metastable and difficult to analyze. To address this knowledge gap, here, we analyzed the initial oligomers formed by the six tau isoforms in the absence of posttranslational modifications or other manipulations using dot blots probed by an oligomer-specific antibody, native-PAGE/western blots, photo-induced cross-linking of unmodified proteins, mass-spectrometry, and ion-mobility spectroscopy. We found that under these conditions, three-repeat (3R) isoforms are more prone than four-repeat (4R) isoforms to form oligomers. In this study, we also tested whether known inhibitors of tau aggregation affect its oligomerization using three small molecules representing different classes of tau aggregation inhibitors, Methylene Blue (MB), the molecular tweezer CLR01, and the all-D peptide TLKIVW, for their ability to inhibit or modulate the oligomerization of the six tau isoforms. Unlike their reported inhibitory effect on tau fibrillation, the inhibitors had little or no effect on the initial oligomerization. Our study provides novel insight into the primary–quaternary structure relationship of human tau and suggests that 3R-tau oligomers may be an important target for future development of compounds targeting pathological tau assemblies.

59 BASIC BIOLOGICAL SCIENCES↗