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DOE OSTI2023

Investigation of Nanoparticle Degradation in Hydrogen Fuel Cell Systems through Automated Electron Microscopy

Proton exchange membrane fuel cells (PEMFC) are promising devices for the deployment of hydrogen-powered heavy-duty vehicles, providing a higher efficiency for similar driving range and fueling time than the existing ones. However, PEMFCs still encounter durability challenges mainly due to catalyst degradation in the cathode. Mitigating these performance losses requires a better understanding of the degradation mechanisms under heavy-duty accelerated stress tests (ASTs) [1]. Scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDS) are key tools for the analysis of Pt and PtCo nanoparticle size, spatial distribution and composition [2]. Electron tomography is also used to determine the rate and type of degradation of catalyst nanoparticles as a function of their position on the carbon support. In this work, automated data acquisition software, paired with a custom Python code, have been used to study the effect of different accelerated stress tests (ASTs) on nanoparticle coarsening [2]. Figure 1 shows high-angle annular dark-field (HAADF)-STEM images and EDS maps comparing the cathodes of membrane electrode assemblies (MEAs) following an electrocatalyst AST performed under H2/N2 with that of the heavy-duty AST performed under H2/air. We will discuss how AST conditions affect considerably the spatial distribution of the nanoparticles across the electrode between the membrane and microporous layer. Although the median particle size increased more in the MEA aged under the heavy-duty AST, as determined using a high-throughput image analysis, the quantitative EDS measurements demonstrate that the electrocatalyst AST resulted in more Pt and Co dissolution from the cathode, which is another important indicator of electrocatalyst degradation. We will further present the impact of the relative humidity (% RH) on the degradation mechanisms demonstrated using the same approach. Electron tomography has been used to distinguish the Pt nanoparticles residing on the carbon support surface (exterior) from those within the pore structure (interior) in order to determine the relative stability of interior and exterior nanoparticles. As shown in Figure 2, we will compare the Pt catalyst particle size at the beginning of test (BOT) and end of test (EOT), and discuss the importance of automating the electron tomography workflow, i.e. acquisition, reconstruction, and visualization, to increase sampling and determine the standard deviation of these measurement. The outlook for utilizing low-dose cryo-tomography for limiting damage to the catalyst, support, and especially proton-conducting ionomer will also be discussed [3].

Amichi, Lynda↗

NASA NTRS1972

ATS-5 solar cell experiment results after one year in synchronous orbit

The results of the ATS-5 solar cell experiment after one year in synchronous orbit are reported. A partial failure in the experimental electronics package has caused a loss of data from half the 80 experimental solar cells. Procedures for extracting data due to a partial spacecraft failure are described and discussed. Data from the remaining 40 solar cells, including 15 mounted on a thin flexible structure are analyzed. Data are corrected to a solar intensity of 140 mW/sq cm and a temperature of 25 C. It was found that after one year in synchronous orbit: (1) cells with 1.52-mm-thick coverslides did not show a clear-cut advantage over those with 0.15-mm coverslides, (2) cells with solderless grid lines are degrading at the same rate as are cells with solder-dipped grid lines, (3) cells not quite completely covered with coverslides suffered a large power loss in comparison to cells fully covered, (4) no clear-cut advantage of 10-cm cells over 2-cm cells has yet been observed, (5) cells mounted on the flexible panel with relatively little backshielding did not degrade any faster than those with substantial backshielding, and (6) the flight data in large part confirms the adequacy of the ground-based techniques used in our preflight radiation test program.

Anspaugh, B. E.↗

DOE OSTI2021

Degradation mechanisms and partial shading of glass-backsheet and double-glass photovoltaic modules in three climate zones determined by remote monitoring of time-series current–voltage and power datastreams

Degradation and partial shading impact the long-term reliability and power production of photovoltaic (PV) modules and power plants. Time-series power (P mp ) and current–voltage (I-V) curve datastreams from PV modules enable a remote diagnostic approach to quantify active degradation mechanisms and identify partial shading. We study three to nine years of these datastreams, including 3.6 million P mp I-V curves and 36 million values, from eight PV modules, four each of double-glass and glass-backsheet module architectures, located in three distinctly different Köppen-Geiger climate zones, to determine the module’s performance loss rates (PLR), identify active degradation mechanisms and power loss modes, along with partial shading by local objects. Considering both module architectures, PLR results indicate that the BSh climate zone is the most aggressive for module degradation, while the Alpine ET zone is the mildest climate. PLR of double-glass modules located in BWh and BSh climate zones are different due to the significantly greater uniform current loss (ΔP Isc ) for double-glass modules in BSh, at a 5% significance level. Power loss for four out of five modules located in the BWh and BSh climates are dominated by uniform current degradation. Statistical analysis of multistep I-V curves detects partial shading experienced by three studied modules with details of the shading profile, the shading Poynting vector diagram for the obstacle’s relative position, shading scenarios, and duration. Lastly, this work demonstrates how remote monitoring and diagnosis of P mp & I-V time-series of modules can provide quantitative operations and maintenance insights into system performance, degradation mechanisms, and shading.

14 SOLAR ENERGY↗

NASA NTRS2001

Ka-Band Phased Array System Characterization

Phased Array Antennas (PAAs) using patch-radiating elements are projected to transmit data at rates several orders of magnitude higher than currently offered with reflector-based systems. However, there are a number of potential sources of degradation in the Bit Error Rate (BER) performance of the communications link that are unique to PAA-based links. Short spacing of radiating elements can induce mutual coupling between radiating elements, long spacing can induce grating lobes, modulo 2 pi phase errors can add to Inter Symbol Interference (ISI), phase shifters and power divider network introduce losses into the system. This paper describes efforts underway to test and evaluate the effects of the performance degrading features of phased-array antennas when used in a high data rate modulation link. The tests and evaluations described here uncover the interaction between the electrical characteristics of a PAA and the BER performance of a communication link.

Acosta, R.↗

DOE OSTI2020

Evolution of the Rate-Limiting step: From Thin Film to Thick Ni-rich Cathodes

Ni-rich NMC (LiNixMnyCo1-x-yO2, x = 0.6) has the attributes of high specific capacity (greater than 180 mAh g-1), high operating voltage (ca. 3.8 V) and low cost, which is therefore deemed as one of the most promising cathode candidates for next-generation high-energy Li-ion batteries (LIBs). However, challenges exist before the large-scale commercialization of Ni-rich cathode such as gas generation, capacity degradation especially at high rate or elevated temperatures. From thin film to densely pack high loading cathode, this work investigates the rate-limiting steps in Ni-rich cathodes e.g., phase structure, electronic and ionic conductivity to understand the reaction kinetics at different scales. This work provides new insights in understanding the electrochemical properties of Ni-rich cathode at different levels to inspire revolutionary ideas to address the fundamental issues of Ni-rich cathode from materials to relevant electrode levels.

Hu, Jiangtao↗

DOE OSTI2021

Editors’ Choice—Necessity to Avoid Titanium Oxide as Electrocatalyst Support in PEM Fuel Cells: A Membrane Durability Study

Pt/TiO 2 as electrocatalyst was found to significantly increase the rate of the membrane chemical degradation in a polymer electrolyte membrane (PEM) fuel cell. The increased degradation was proved to be due to TiO x (TiO 2 or Ti 4 O 7 ), which is widely recognized as a promising corrosion-resistant electrocatalyst support. The membrane degradation (thinning) appears to be preferentially in the side facing anode electrode. Migrated Ti species as a result of TiO x dissolution during fuel cell operation in an acidic environment was quantified by electron probe microanalysis (EPMA). Total fluorine inventory loss of the membrane strongly depends on the quantity of migrated Ti species (likely Ti 3+ and/or Ti 4+ ). The membrane chemical degradation induced by TiO x is proposed to be due to dissolved ionic Ti species reacting with H 2 O 2 through a Fenton reaction. TiO x is determined to be inviable as electrocatalyst support for PEM fuel cells, and future research is suggested to be directed toward alternative oxides with similar corrosion-resistance.

08 HYDROGEN↗

DOE OSTI2026

Mechanism-Informed Breakdown: Understanding Degradation by Controlling Voltage-Hold Patterns in Proton Exchange Membrane Water Electrolyzers

Low catalyst loadings pose challenges to performance stability in proton exchange membrane (PEM) water electrolysis over extended operation. To study the impact of degradation mechanisms and voltage loss rates, different stress tests are applied to membrane electrode assemblies. Potential cycling conditions were observed to induce higher degrees of iridium (Ir) oxide crystallization, ionomer degradation, and catalyst layer (CL) thinning, which likely contributed to higher kinetic loss rates. On the other hand, while Ir migrating into the PEM (Ir band) generally impairs performance, the interconnected and more uniform Ir band formed under a constant 2 V hold may allow for Ir at the catalyst/membrane interface to remain electronically connected and kinetically accessible, as well as indicate greater Ir site access during the applied stressor. The 2 V hold also demonstrates improved kinetic durability through a lower Tafel slope, faster polarization kinetics, and reduced charge transfer resistance. In contrast, potential cycling caused the migration of disconnected Ir agglomerates into the membrane bulk and created a steady increase in charge transfer resistance, a more dramatic decrease in capacitance (46.7% loss), and significant damage to the surrounding ionomer, indicating a decline in both the quality and quantity of active sites in the anode CL. This work underscores the distinct degradation pathways associated with load holds versus cycling, highlighting the role of catalyst-ionomer interactions in kinetic performance and long-term stability. These insights can inform operational strategies for PEM electrolyzers powered by intermittent energy sources, aiming to minimize efficiency losses over extended operation.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effect of X-ray free-electron laser-induced shockwaves on haemoglobin microcrystals delivered in a liquid jet

X-ray free-electron lasers (XFELs) enable obtaining novel insights in structural biology. The recently available MHz repetition rate XFELs allow full data sets to be collected in shorter time and can also decrease sample consumption. However, the microsecond spacing of MHz XFEL pulses raises new challenges, including possible sample damage induced by shock waves that are launched by preceding pulses in the sample-carrying jet. We explored this matter with an X-ray-pump/X-ray-probe experiment employing haemoglobin microcrystals transported via a liquid jet into the XFEL beam. Diffraction data were collected using a shock-wave-free single-pulse scheme as well as the dual-pulse pump-probe scheme. The latter, relative to the former, reveals significant degradation of crystal hit rate, diffraction resolution and data quality. Crystal structures extracted from the two data sets also differ. Since our pump-probe attributes were chosen to emulate EuXFEL operation at its 4.5 MHz maximum pulse rate, this prompts concern about such data collection.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Genomic Analysis Enlightens Agaricales Lifestyle Evolution and Increasing Peroxidase Diversity

Abstract As actors of global carbon cycle, Agaricomycetes (Basidiomycota) have developed complex enzymatic machineries that allow them to decompose all plant polymers, including lignin. Among them, saprotrophic Agaricales are characterized by an unparalleled diversity of habitats and lifestyles. Comparative analysis of 52 Agaricomycetes genomes (14 of them sequenced de novo) reveals that Agaricales possess a large diversity of hydrolytic and oxidative enzymes for lignocellulose decay. Based on the gene families with the predicted highest evolutionary rates—namely cellulose-binding CBM1, glycoside hydrolase GH43, lytic polysaccharide monooxygenase AA9, class-II peroxidases, glucose–methanol–choline oxidase/dehydrogenases, laccases, and unspecific peroxygenases—we reconstructed the lifestyles of the ancestors that led to the extant lignocellulose-decomposing Agaricomycetes. The changes in the enzymatic toolkit of ancestral Agaricales are correlated with the evolution of their ability to grow not only on wood but also on leaf litter and decayed wood, with grass-litter decomposers as the most recent eco-physiological group. In this context, the above families were analyzed in detail in connection with lifestyle diversity. Peroxidases appear as a central component of the enzymatic toolkit of saprotrophic Agaricomycetes, consistent with their essential role in lignin degradation and high evolutionary rates. This includes not only expansions/losses in peroxidase genes common to other basidiomycetes but also the widespread presence in Agaricales (and Russulales) of new peroxidases types not found in wood-rotting Polyporales, and other Agaricomycetes orders. Therefore, we analyzed the peroxidase evolution in Agaricomycetes by ancestral-sequence reconstruction revealing several major evolutionary pathways and mapped the appearance of the different enzyme types in a time-calibrated species tree.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS1975

Horizontal transport of the regolith, modification of features, and erosion rates on the lunar surface

Impact-ejecta systematics are developed for the smaller cratering events which, with cumulative crater populations observed in young mare regions and on Copernicus ejecta fields, yield rates and a range distribution for the horizontal transport of material by impact processes. The deposition rate for material originating more than 1 m away is found to be about 8 mm per million years. Material from 10 km away accumulates at a rate of about 0.08 mm per million years, providing a steady influx of foreign material. From the degradation of boulder tracks, a rate of 5 plus or minus 3 cm per million years is computed for the filling of shallow lunar depressions on slopes. Mass wastage and downslope movement of bedrock outcroppings on Hadley Rille seem to be proceeding at a rate of about 8 mm per million years. The Camelot profile is suggestive of a secondary impact feature.

Arvidson, R.↗

DOE OSTI2021

Competitive Exclusion and Metabolic Dependency among Microorganisms Structure the Cellulose Economy of an Agricultural Soil

Microorganisms that degrade cellulose utilize extracellular reactions that yield free by-products which can promote interactions with noncellulolytic organisms. We hypothesized that these interactions determine the ecological and physiological traits governing the fate of cellulosic carbon (C) in soil. We performed comparative genomics with genome bins from a shotgun metagenomic-stable isotope probing experiment to characterize the attributes of cellulolytic and noncellulolytic taxa accessing 13 C from cellulose. We hypothesized that cellulolytic taxa would exhibit competitive traits that limit access, while noncellulolytic taxa would display greater metabolic dependency, such as signatures of adaptive gene loss. We tested our hypotheses by evaluating genomic traits indicative of competitive exclusion or metabolic dependency, such as antibiotic production, growth rate, surface attachment, biomass degrading potential, and auxotrophy. The most 13 C-enriched taxa were cellulolytic Cellvibrio (Gammaproteobacteria) and Chaetomium (Ascomycota), which exhibited a strategy of self-sufficiency (prototrophy), rapid growth, and competitive exclusion via antibiotic production. Auxotrophy was more prevalent in cellulolytic Actinobacteria than in cellulolytic Proteobacteria, demonstrating differences in dependency among cellulose degraders. Noncellulolytic taxa that accessed 13 C from cellulose (Planctomycetales, Verrucomicrobia, and Vampirovibrionales) were also more dependent, as indicated by patterns of auxotrophy and 13 C labeling (i.e., partial labeling or labeling at later stages). Major 13 C-labeled cellulolytic microbes (e.g., Sorangium, Actinomycetales, Rhizobiales, and Caulobacteraceae) possessed adaptations for surface colonization (e.g., gliding motility, hyphae, attachment structures) signifying the importance of surface ecology in decomposing particulate organic matter. Our results demonstrated that access to cellulosic C was accompanied by ecological trade-offs characterized by differing degrees of metabolic dependency and competitive exclusion.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Microstructure Scale Lithium-Ion Battery Modeling: Part III. When and Where Lithium Plating Occurs and its Correlation with the Electrode Microstructure

Li-ion battery performance and degradation are closely related to the cell’s underlying electrode microstructure. Electrode microstructures are typically characterized with volume-averaged properties that neglect the impact of local heterogeneities. However, local heterogeneities create hot spots that can trigger degradation onset. Herein, a microstructure scale electrochemical model is used to investigate the impact of microstructure heterogeneity on lithium plating. The model predicts lithium plating is not uniform, even when considering a relatively small portion of the electrode (a cross-sectional area of 154×144 µm 2 ), preferring to plate on larger particles as compared to smaller particles. While local heterogeneities control where plating occurs, the model predicts that volume-averaged properties control when plating occurs. Additionally, the model predicts that the active material specific surface area has a linear relationship with the plating onset. However, the linear relationship between increased active material surface area and delayed plating response appears to be sensitive to the microstructure feature used to increase the active interface area. Here, a comparative case-study is explored where the specific surface area is increased by either reducing the active material particle diameter, adding open-porosity cracks, or increasing the active material surface roughness. The model predicts that increasing the specific surface area by reducing the active material particle diameter is the most effective strategy for delaying lithium plating. At 6C, reducing particle size is shown to be 3 and 20 times more effective than, respectively, adding open-porosity cracks and increasing surface roughness. A dual-layer electrode architecture combining gradations both for average properties and uniformities is eventually proposed to improve homogeneous material utilization and reduce degradation at high charge rates.

25 ENERGY STORAGE↗

NASA NTRS1988

Effects of update and refresh rates on flight simulation visual displays

An experiment was performed to study the effects of update and refresh rates on dynamic calligraphic CRT displays, particularly those used for visual displays in flight simulators. A moving horizontal line was generated on a CRT and observed at various velocities. Observations were made with both one and two refreshes per update. The data gathered from these observations are presented on plots of refresh-update rate as a function of display velocity. The display velocity where picture degradation occurs can be found by using these plots. These velocities are related to actual simulated aircraft angular and linear velocities. Results show that a visual display updated at 30 Hz and refreshed at 60 Hz degrades at very low simulated aircraft angular and linear velocities. These velocities at which degradation occurs can be significantly increased by increasing the update rate of the visual display. Only minor improvements are possible by refreshing the display twice for each uptake. To display rapidly changing flight scenery without degradation, the display update rate must be far in excess of 60 Hz, typically several hundred Hz.

Kellogg, Gary V.↗

DOE OSTI2021

Sequential Bayesian inference of transition rates in the hidden Markov model for multi-state system degradation

The more easily available system performance data and advances in data analytics have provided us with opportunities to optimize maintenance programs for engineered systems, for example nuclear power plants. One key task in maintenance optimization is to obtain an accurate model for system degradation. Here, in this research, we propose a Bayesian method to address this problem. Noting that systems usually exhibit multiple states and that the actual state of a system usually is not directly observable, in the method we first model the system degradation process and the observation process based on a hidden Markov model. Then we develop a sequential Bayesian inference algorithm based on importance sampling and the forward algorithm to infer the posterior distributions of the transition rates in the hidden Markov model based on available observations. The proposed Bayesian method allows us to take advantage of evidence from multiple sources, and also allows us to perform Bayesian inference sequentially, without the need to use the entire history of observations every time new observations are collected. We demonstrate the proposed method using both synthetic data for a nuclear power plant feedwater pump and realistic data for a nuclear power plant chemistry analytical device.

42 ENGINEERING↗

NASA NTRS2004

Ka-Band Multibeam Aperture Phased Array Being Developed

Phased-array antenna systems offer many advantages to low-Earth-orbiting satellite systems. Their large scan angles and multibeam capabilities allow for vibration-free, rapid beam scanning and graceful degradation operation for high rate downlink of data to users on the ground. Technology advancements continue to reduce the power, weight, and cost of these systems to make phased arrays a competitive alternative in comparison to the gimbled reflector system commonly used in science missions. One effort to reduce the cost of phased arrays is the development of a Ka-band multibeam aperture (MBA) phased array by Boeing Corporation under a contract jointly by the NASA Glenn Research Center and the Office of Naval Research. The objective is to develop and demonstrate a space-qualifiable dual-beam Ka-band (26.5-GHz) phased-array antenna. The goals are to advance the state of the art in Ka-band active phased-array antennas and to develop and demonstrate multibeam transmission technology compatible with spacecraft in low Earth orbit to reduce the cost of future missions by retiring certain development risks. The frequency chosen is suitable for space-to-space and space-to-ground communication links. The phased-array antenna has a radiation pattern designed by combining a set of individual radiating elements, optimized with the type of radiating elements used, their positions in space, and the amplitude and phase of the currents feeding the elements. This arrangement produces a directional radiation pattern that is proportional to the number of individual radiating elements. The arrays of interest here can scan the main beam electronically with a computerized algorithm. The antenna is constructed using electronic components with no mechanical parts, and the steering is performed electronically, without any resulting vibration. The speed of the scanning is limited primarily by the control electronics. The radiation performance degrades gracefully if a portion of the elements fail. The arrays can be constructed to conform to a mounting surface, and multibeam capability is integral to the design. However, there are challenges for mission designers using monolithic-microwave-integrated-circuit- (MMIC-) based arrays because of reduced power efficiency, higher costs, and certain system effects that result in link degradations. The multibeam aperture phased-array antenna development is attempting to address some of these issues, particularly manufacturing, costs, and system performance.

Reinhart, Richard C.↗

DOE OSTI2024

Color‐Stable, All‐Phosphorescent White Organic Light Emitting Diodes Using the Polariton‐Enhanced Purcell Effect

Abstract The short operational lifetimes of high efficiency phosphorescent organic blue light emitting devices (PHOLEDs) has limited their use in displays and lighting. Previously, this problem has been avoided by using less efficient fluorescent blue devices in separately biased red, green, and blue emissive elements to achieve stable full color emission. However, the operational lifetime of blue phosphorescent OLEDs has been significantly improved through the utilization of the plasmon‐exciton‐polariton‐enhanced (PEP) Purcell effect. Here, a white emitting PHOLED comprising stacked red, green, and blue elements is demonstrated that exploits PEPs to extend the operational lifetime of the blue element such that all emissive layers degrade at the same rate. The device features white light emission with an external quantum efficiency of 19.1 ± 0.4%, luminous power efficiency of 13.3 ± 0.3 lm W −1 at a luminance of 1000 cd m −2 when measured over 4π solid angle, with a color rendering index of 76 unchanged throughout the device aging to 70% of its initial luminance, T 70 . A 2.9 times enhancement in the operational lifetime of the Purcell‐enhanced device is achieved to yield T 70 = 2900 ± 100 h for an initial luminance of 1000 cd m −2 , compared to devices lacking this enhancement with T 70 = 1000 ± 100 h.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Understanding Operando Water Management in Hydroxide‐Exchange‐Membrane Fuel Cells

The water balance in hydroxide-exchange-membrane fuel cells (HEMFCs) is a key challenge for improved performance and durability, intimately linked with the various interfaces and coupled phenomena. For every 4 electrons produced, 4 water molecules are generated in the anode and 2 consumed in the cathode, while electroosmosis transports water across the HEM from the cathode to the anode. Consequently, a concentration gradient drives water back, from anode to cathode. Ineffective water management could lead to cathode dry-out, limiting reaction rate and causing ionomer degradation, or to anode flooding. To address these concerns, it is critical to measure the water transport operando . Herein, a home-built water-flux station is used to measure total water flux during cell operation with different inlet relative humidities and back pressures. Increasing the HEM thickness fourfold decreases the water flux at high current density, and utilizing microporous layers on both the anode and cathode decreases the water flux from the anode to the cathode. However, the most significant variable in changing the water flux was found by increasing the anode back pressure. Furthermore, humidity cycling significantly changed electrochemical performance without affecting the overall water fluxes. These findings can be translated to other devices utilizing an HEM.

AEMFC↗

DOE OSTI2025

Contrasting Chemical Kinetic Parameters for Near In‐Service‐Temperature Aging and High‐Temperature Thermal Decomposition of Triaminotrinitrobenzene Formulations

Triaminotrinitrobenzene-based high explosives such as LX-17 offer high energy density and exceptional safety, yet their long-term aging behavior at low temperatures remains poorly understood. In this study, several legacy and new production lots of LX-17 were subjected to accelerated aging experiments below 100°C, during which the formation rate of the initial degradation product, monofurazan (F1), was monitored. Kinetic analysis was performed using a sample-age-aware computational approach, yielding activation energy estimates of 82–91 kJ mol −1 for the low-temperature initiation step—markedly lower than the ∼200 kJ mol −1 associated with high-temperature thermal decomposition. Extrapolation from established cookoff models supports the conclusion that the dominant degradation mechanism at low temperatures differs from that at high temperatures. In conclusion, our results provide a unified kinetic framework that bridges the gap between in-service conditions and high-temperature damage.

Chemistry - Chemical explosives↗