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DOE OSTI2021

Interfacial Characterization of Positive Bias Voltage Degradation in PV Modules

Degradation from high system voltage is a prevailing failure mode in fielded photovoltaic modules, and the degradation mechanism is inherently dependent on the bias polarity. Here we report the effects of positive bias. Modules under positive bias demonstrated a significant photocurrent loss caused by two routes. First, delamination and discoloration of the silicon nitride layer, leading to optical loss determined by reflectance measurements. Second, chemical discoloration of the cell gridlines and encapsulant (EVA), which is linked to an electrochemical reaction at the silver electrodes. Chemical compositional analysis using X-ray photoemission spectroscopy demonstrated that the discoloration is attributed to Ag 2 S and/or Ag 2 O. Evidence of Ag ion migration from the cell grid into the encapsulant is observed after shallow depth profiling on the EVA surface. However, Ag was not detected at the EVA/glass interface, inferring limited Ag ion transport through the EVA. The source of sulfur is believed to be ambient air, which diffused into the module through the breathable backsheet.

characterization↗

DOE OSTI2020

Safe, Low-Cost, High Energy-Density, Solid-State Li-Ion Batteries

We developed intrinsically safe, robust, low-cost, high-energy-density solid-state Li-ion batteries, by integrating high conductivity garnet-type solid Li ion electrolytes and several different cathodes in tailored microstructures, fabricated by low-cost supported thin-film ceramic techniques, to overcome the primary technological barriers to next generation battery technology. In this ARPA-E project we employed Li-garnet solid-state electrolytes pioneered by one of the co-investigators (Thangadurai) which has room temperature (RT) conductivity of ~10 -3 S cm -1 . The highly stable garnet SSE allowed the use of S, NMC, and other cathodes with Li metal anodes without stability or flammability concerns. We studied the garnet’s stability when exposed to CO 2 and humidity (with or without an ALD coating) and showed that the material can be processed in ambient air for most steps prior to battery assembly, significantly reducing production costs. We extensively studied and scaled up the synthesis of the powder and explored external suppliers of garnet to determine the best pathway for commercial success. We used low-cost and scalable tapecasting fabrication methods to create porous-dense-porous “trilayer” solid electrolyte microstructures with a ~20 μm separating dense layer, and >70% porosity porous layers to host the electrodes. These scalable multilayer ceramic fabrication techniques, without need for dry rooms or vacuum equipment, also provide for dramatically reduced manufacturing costs. The tailored microstructured electrode supports (scaffold) increased interfacial area ~50x, overcoming the high impedance typical of planar geometry SSLiBs, resulting in record-setting 10 mA/cm 2 lithium cycling in a symmetric cell. We expanded our tapecasting ability and showed tapes >25m in length by the end of the project. We demonstrated the ability to sinter garnet without the use of a garnet powderbed, which could have been a major obstacle and waste of material at scale. At the same time, we expanded the size of our trilayers from coin cells (0.7 cm 2 ) to the full format design (30 cm 2 ). To develop full cells, we demonstrated 250 Wh/kg at room temperature with commercial NMC electrode films in a bilayer configuration. Similarly, we demonstrated 280 Wh/kg trilayer Li-S cells at room temperature with >90% capacity retention over 300 cycles. At 90°C we demonstrated 350 Wh/kg with a Li-S trilayer. The high thermal stability of the garnet electrolyte also enabled extended cycling (400 cycles) of a Li-TiS 2 cell at 150 °C, showcasing the exceptional safety and nonflammability of the solid-state trilayer batteries. Ion Storage Systems has taken this technology and knowledge to produce trilayer garnet electrolytes and is building out facilities to commercialize high performance solid state batteries. ISS has hired a strong staff, identified and communicated with a large number of potential partners, and successfully secured follow-on funding.

25 ENERGY STORAGE↗

DOE OSTI2024

Upcycling Polyethylene Waste to Advanced Carbon Materials for Energy Storage Applications

Polyethylene is notoriously difficult to upcycle because it decomposes into light gases at approximately 350-400 °C which prevents processing it at higher temperatures to convert it into high-value carbon materials, such as graphene or graphite. We address this challenge by using an air-based, thermo-oxidation process, which heats polyethylene (PE) just below the decomposition point to initiate oxidation and cross-linking of PE alkyl chains. These molecular transformations allow PE to be further graphenized or graphitized at higher temperatures without decomposing. The PE-derived graphene has a specific surface area up to 1,800 m 2/g and Raman ID/IG ratio of 0.85, which enables it to be used as an electrode material for a symmetric supercapacitor with the 1 M H2SO4 electrolyte. The PE-derived graphene material has a comparable electrochemical capacitive performance, such as power density, specific capacitance, and long cycle stability, to the commercial state of art porous carbon electrode. The stabilized PE could also be converted into highly crystalline flake graphite via low-temperature catalytic graphitization. The PE-derived graphite is used for the lithium-ion battery anode, which showed comparable electrochemical battery performance, such as reversible rate performance and long-term cyclic stability, to the current use battery-grade graphite, thus providing a scalable method to upcycle PE plastic waste into high-value carbon material.

Gao, Yuan↗

DOE OSTI2024

A thermal evaporation–trapping strategy to synthesize flexible and robust oxygen electrocatalysts for rechargeable zinc–air batteries

Great efforts have been devoted to the development of bifunctional electrocatalysts to accelerate the sluggish kinetics of cathodic oxygen reduction/evolution reactions (ORR/OER) in zinc–air batteries (ZABs). Here we report a thermal evaporation–trapping synergistic strategy to fabricate a bifunctional electrocatalyst of flexible N-doped carbon fiber cloth loaded with both CoFe-oxide nanoparticles and single-atom Co/Fe–Nx sites, in which the thermal evaporation process functions in both downsizing CoFe-oxide nanoparticles and trapping the evaporated Co/Fe species to generate Co/Fe–Nx sites. The obtained flexible electrocatalyst, directly serving as an oxygen electrode, displays a small potential gap of 0.542 V for the OER/ORR, large peak power densities (liquid-state ZAB: 237.4 mW cm2 ; solid-state ZAB: 141.1 mW cm2 ), and excellent charge–discharge cycling stability without decay after working more than 770 hours. Furthermore, in situ Raman spectroscopy characterization and theoretical calculations reveal that CoFe2O4 species is responsible for the OER while atomic Fe/Co sites play a key role in the ORR

Zhang, Hong-Bo↗

NASA NTRS2002

Experimental Visualization of Bubble Formation from an Orifice In Microgravity in the Presence of Electric Fields

The formation of air bubbles injected into a stagnant, isothermal liquid in microgravity through an orifice was studied. The bubbles grew very large in microgravity. They attained a nearly spherical shape and showed pronounced affinity towards coalescence in the absence of electric fields and other perturbations. Under the influence of electric fields, periodic detachment was observed, with bubble sizes larger than in terrestrial conditions. The bubble shape was elongated. After detachment, the bubbles moved away from the electrode at which they formed without coalescing with other bubbles. Experimental data on bubble shape and size at detachment showed good agreement with models.

Herman, C.↗

NASA NTRS2017

Experimental Setup for the Laboratory Investigation of Micrometeoroid Ablation Using a Dust Accelerator

A facility has been developed to simulate the ablation of micrometeoroids in laboratory conditions. An electrostatic dust accelerator is used to generate iron particles with velocities of 10-70 kilometers. The particles are then introduced into a chamber pressurized with a target gas, where the pressure is adjustable between 0.01 and 0.5 Torr, and the particle partially or completely ablates over a short distance. An array of biased electrodes above and below the ablation path is used to collect the generated ions/electrons with a spatial resolution of 2.6 centimeters along the ablating particles path, thus allowing the study of the spatiotemporal evolution of the process. For completely ablated particles, the total collected charge directly yields the ionization coefficient of a given dust material-target gas combination. The first results of this facility measured the ionization coefficient of iron atoms with N2, air, CO2, and He target gases for impact velocities greater than 20 kilometers per second, and are reported by Thomas et al. The ablation chamber is also equipped with four optical ports that allow for the detection of the light emitted by the ablating particle. A multichannel photomultiplier tube system is used to observe the ablation process with a spatial and temporal resolution of 0.64 centimeters and 90 nanoseconds. The preliminary results indicate that it is possible to calculate the velocity of the ablating particle from the optical observations, and in conjunction with the spatially resolved charge measurements allow for experimental validation of ablation models in future studies.

Thomas, Evan↗

DOE OSTI2020

In situ , in vivo , and in operando imaging and spectroscopy of liquids using microfluidics in vacuum

This review offers a succinct overview of the development of a vacuum-compatible microfluidic reactor system for analysis at the liquid vacuum interface (SALVI), and its diverse applications in in situ, in vivo, and in operando imaging of liquid surfaces as well as the air-liquid (a-l), liquid-liquid (l-l), and solid-liquid (s-l) interfaces in the past decade. SALVI is one of the first microfluidics-based reactors that has enabled direct analysis of volatile liquids in vacuum surface tools such as scanning electron microscopy (SEM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). Its integration into ambient and vacuum spectroscopy and microscopy is illustrated. Several applications are highlighted including (1) imaging nanoparticles in liquid using in situ SEM; (2) mapping the evolving l-l interface using in situ x-ray absorption spectroscopy and ToF-SIMS; (3) following complex a-l interfacial oxidation reaction products using in situ ToF-SIMS; (4) capturing biological interfaces of cells and microbes via in vivo multimodal and correlative imaging; and (5) monitoring the dynamic solid electrode and liquid electrolyte interface using in operando molecular imaging. Finally, outlook and recommendations are presented. Besides showing the holistic information volume obtained by real-time multiplexed imaging, this review intends to convey the importance of tool development in revolutionizing surface and interface analysis using vacuum platforms previously limited to solid surfaces. Microfluidics is manifested to be not limited to ambient conditions in many examples in this review. Moreover, fundamental interfacial phenomena underpinning mass and charge transfer can now be pursued in real time via innovated chemical imaging and spectroscopy.

42 ENGINEERING↗

NASA NTRS1992

Pressure dependence of the oxygen reduction reaction at the platinum microelectrode/nafion interface - Electrode kinetics and mass transport

The investigation of oxygen reduction kinetics at the platinum/Nafion interface is of great importance in the advancement of proton-exchange-membrane (PEM) fuel-cell technology. This study focuses on the dependence of the oxygen reduction kinetics on oxygen pressure. Conventional Tafel analysis of the data shows that the reaction order with respect to oxygen is unity at both high and low current densities. Chronoamperometric measurements of the transport parameters for oxygen in Nafion show that oxygen dissolution follows Henry's isotherm. The diffusion coefficient of oxygen is invariant with pressure; however, the diffusion coefficient for oxygen is lower when air is used as the equilibrating gas as compared to when oxygen is used for equilibration. These results are of value in understanding the influence of O2 partial pressure on the performance of PEM fuel cells and also in elucidating the mechanism of oxygen reduction at the platinum/Nafion interface.

Parthasarathy, Arvind↗

DOE OSTI2022

Facile Dual-Protection Layer and Advanced Electrolyte Enhancing Performances of Cobalt-free/Nickel-rich Cathodes in Lithium-Ion Batteries

Despite cobalt (Co)-free/nickel (Ni)-rich layered oxides being considered as one of the promising cathode materials due to their high specific capacity, their highly reactive surface is one of the shortcomings that still hinder their practical usages in high-energy-density batteries. Herein, a polyimide/polyvinylpyrrolidone (PI/PVP, denoted as PP) coating layer is demonstrated as dual-protection for LiNi 0.96 Mg 0.02 Ti 0.02 O 2 (NMT) cathode material to suppress surface contamination against moisty air and to prevent unwanted side reactions between cathode and electrolyte during electrochemical cycling. The optimal PP-coated NMT (PP@NMT) preserves a clean surface without generation of lithium (Li) residues, structural degradation, and gas evolution after exposure to air with ~30% humidity for 2 weeks. Contrarily, the exposed bare NMT shows severe contamination, structural shrinkage due to Li loss, and increased gas release during charging. In addition, the exposed PP@NMT significantly enhances the electrochemical performance of graphite (Gr)||NMT cells by decreasing byproducts and maintaining structural stability. Moreover, the exposed PP@NMT achieves a high capacity retention of 86.7% after 500 cycles in Gr||NMT cells using an advanced localized high-concentration electrolyte. Furthermore, this work demonstrates a promising facile approach to the protection of Co-free/Ni-rich layered cathodes for their practical applications even after exposure to moisty air.

25 ENERGY STORAGE↗

NASA NTRS2009

Small CO2 Sensors Operate at Lower Temperature

Solid-electrolyte-based amperometric sensors for measuring concentrations of CO2 in air are being developed for use in detection of fires, environmental monitoring, and other applications where liquid-based electrochemical cells are problematic. These sensors are small (sizes of the order of a millimeter), are robust, are amenable to batch fabrication at relatively low cost, and exhibit short response times (seconds) and wide detection ranges. A sensor of this type at a previous stage of development included a solid electrolyte of Na3Zr2Si2PO12 deposited mainly between interdigitated Pt electrodes on an alumina substrate, all overcoated with an auxiliary solid electrolyte of (Na2CO3:BaCO3 in a molar ratio of 1:1.7). It was necessary to heat this device to a temperature as high as 600 C to obtain the desired sensitivity and rapid response. Heating sensors increases the power consumption of the sensor system and complicates the use of the sensor in some applications. Thus, decreasing a sensor s power consumption while maintaining its performance is a technical goal of ongoing development.

Hunter, Gary W.↗

DOE OSTI2025

Pick-and-Place Transfer of Arbitrary-Metal Electrodes for van der Waals Device Fabrication

Van der Waals electrode integration is a promising strategy to create nearly perfect interfaces between metals and 2D materials, with advantages such as eliminating Fermi-level pinning and reducing contact resistance. However, the lack of a simple, generalizable pick-and-place transfer technology has greatly hampered the wide use of this technique. Here, we demonstrate the pick-and-place transfer of prefabricated electrodes from reusable polished hydrogenated diamond substrates without the use of any sacrificial layers due to the inherent low-energy and dangling-bond-free nature of the hydrogenated diamond surface. The technique enables transfer of arbitrary-metal electrodes and an electrode array, as demonstrated by successful transfer of eight different elemental metals with work functions ranging from 4.22 to 5.65 eV. We also demonstrate the electrode array transfer for large-scale device fabrication. The mechanical transfer of metal electrodes from diamond to van der Waals materials creates atomically smooth interfaces with no interstitial impurities or disorder, as observed with cross-section high-resolution transmission electron microscopy and energy-dispersive X-ray spectroscopy. As a demonstration of its device application, we use the diamond transfer technique to create metal contacts to monolayer transition metal dichalcogenide semiconductors with high-work-function Pd, low-work-function Ti, and semimetal Bi to create n- and p-type field-effect transistors with low Schottky barrier heights. We also extend this technology to air-sensitive materials (trilayer 1T’ WTe 2 ) and other applications such as ambipolar transistors, Schottky diodes, and optoelectronics. This highly reliable and reproducible technology paves the way for new device architectures and high-performance devices.

2D materials↗

NASA NTRS1990

Hybrid air revitalization system for a closed ecosystem

An air-revitalization concept is presented with experimental results to assess the practicality and applicability of the proposed system to extended-duration manned missions. The Hybrid Air Revitalization System (HARS) uses plants in a habitat to remove metabolic CO2 and moisture and produce oxygen and food. CO2 and O2 partial pressures, temperature, and humidity are regulated by means of electrochemical CO2 and O2 chemical separators and a moisture condenser separator. A cell-test facility is described in which the electrochemical CO2 removal processes are investigated with and without using H2. Performance is optimized by using 25-30 percent Teflon in the gas-diffusion-type electrode, employing a thin electrolyte matrix, operating at higher temperatures and lower dew points. The HARS concept is found to be a feasible approach to the electrochemical separation of CO2 and O2.

Lee, M. G.↗

DOE OSTI2025

Long-Range Resonant Charge Transport through Open-Shell Donor–Acceptor Macromolecules

A grand challenge in molecular electronics is the development of molecular materials that can facilitate efficient longrange charge transport. Research spanning more than two decades has been fueled by the prospects of creating a new generation of miniaturized electronic technologies based on molecules whose synthetic tunability offers tailored electronic properties and functions unattainable with conventional electronic materials. However, current design paradigms produce molecules that exhibit off-resonant transport under low bias, which limits the conductance of molecular materials to unsatisfactorily low levels several orders of magnitude below the conductance quantum 1 G 0 and often results in an exponential decay in conductance with length. Here, we demonstrate a chemically robust, air-stable, and highly tunable molecular wire platform comprised of open-shell donor−acceptor macromolecules that exhibit remarkably high conductance close to 1 G 0 over a length surpassing 20 nm under low bias, with no discernible decay with length. Single-molecule transport measurements and ab initio calculations show that the ultralong-range resonant transport arises from extended π-conjugation, a narrow bandgap, and diradical character, which synergistically enables excellent alignment of frontier molecular orbitals with the electrode Fermi energy. The implementation of this long-sought-after transport regime within molecular materials offers new opportunities for the integration of manifold properties within emerging nanoelectronic technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2020

The Effect of Membrane Casting Irregularities on Initial Fuel Cell Performance

Membrane electrode assemblies (MEA) for polymer electrolyte membrane fuel cells (PEMFC) may possess as-manufactured non-uniformities in any of its constituent components. This article studies casting irregularities located within the PEM to understand their potential impact on MEA initial performance. Membrane material was cast on a lab-scale polymer casting line operating either within or at the boundaries of the process window. The resulting membrane material was either pristine in the former case, or, in the latter case, contained air bubbles, cracks, and other irregularities, ranging in size from about 0.6 to 3 mm. Spatial polarization experiments were conducted using a 121-channel segmented fuel cell system, and thermal imaging was performed subsequently to map hydrogen crossover to spatial performance. While total-cell polarization data was minimally impacted by the irregularities, the spatial diagnostics showed local performance impacts that, in operation over time, could cause degradation in performance or earlier failure of the MEA. Such impacts could lead to these irregularities being classified as defects, i.e., manufacturing variations that should be identified and not included in a fuel cell stack. Classification of irregularities as defects will ultimately assist the industry by contributing to the development of threshold detection limits for in-line quality control diagnostics.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2022

Investigations into Plasma-Mediated Decomposition of Organoiodide Species as a Pretreatment for Mitigation of Radioiodine Emissions

A plasma-mediated pretreatment step is proposed to decompose methyl iodide (CH 3 I) for facilitating the capture of the iodine radioisotopes present in off-gas streams from used nuclear fuel reprocessing operations. Simulated CH 3 I gas streams were exposed to dielectric barrier discharge (DBD) plasma in a quartz glass continuous-flow reactor using copper electrodes. The kinetics of decomposition of CH 3 I in nitrogen was investigated by varying the applied voltage, inlet concentration, and residence time. The rate of decomposition was proportional to CH 3 I concentration and increased as the applied potential was increased. This effect was incorporated in the kinetics through the dependence of the rate constant on the applied electric field. Decomposition of CH 3 I was not affected by moisture, and the DBD pretreatment is likely to be similarly effective in an air environment as well; however, the results were confounded by a plasma-mediated reaction between nitrogen and oxygen.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2020

A low temperature unitized regenerative fuel cell realizing 60% round trip efficiency and 10 000 cycles of durability for energy storage applications

Unitized regenerative fuel cells (URFC) convert electrical energy to and from chemical bonds in hydrogen. URFCs have the potential to provide economical means for efficient long-term, seasonal, energy storage and on-demand conversion back to electrical energy. We first optimize the catalyst layer for discrete electrolyzer and fuel cell and then configure the URFC. The goal is to identify a cost competitive configuration for URFCs, and demonstrate it in terms of upper limit of round trip efficiencies (RTEs). Two possible configurations of URFCs are compared via experiments and techno-economic analysis (TEA), which emphasize the advantages of the unconventional constant-electrode (CE) URFC over the traditional constant-gas (CG) configuration. We also study the stability via accelerated stress tests (ASTs) and demonstrate steady state operation in a daily cycle for day to night energy shifting. From the investigations, the optimum composition of the URFC anode catalyst layer is 90 at% Ir-black balanced by Pt-black for both CE and CG configurations. At 80 °C and 1 A cm -2 , the optimized CE URFC achieves 57% and 60% RTE with air and O 2 as the reductant gases, respectively. We then evaluated the differences in durability using an AST over 10k charge–discharge cycles; the results reveal that the wider potential window at the anode in CE (0.05–1.55 V) has minimal effect on catalyst layer stability compared to CG (0.55–1.55 V). Furthermore, there was no degradation up to the range of 2k–5k cycles; beyond that the fuel cell (discharge) performance degraded while the electrolyzer (charge) performance was still stable. Finally, the observations here indicate substantial potential to employ URFCs as efficient and cost-effective bidirectional energy-conversion devices within energy storage and utilization systems after appropriate technological and operational optimizations.

25 ENERGY STORAGE↗

DOE OSTI2024

“Green” Fabrication of High-performance Transparent Conducting Electrodes by Blade Coating and Photonic Curing on PET for Perovskite Solar Cells

This study presents an innovative material processing approach to fabricate transparent conducting electrodes (TCEs) on polyethylene terephthalate (PET) substrates using blade coating and photonic curing. The hybrid TCEs consist of a multiscale Ag network, combining silver metal bus lines and nanowires, overcoated by an indium zinc oxide layer, and then photonically cured. Blade coating ensures film uniformity and thickness control over large areas. Photonic curing, a non-thermal processing method with significantly lower carbon emissions, enhances the conductivity and transparency of the coated layers. Our hybrid TCEs achieve an average transmittance of (81 ± 0.4)% referenced to air ((90 ± 0.4)% referenced to the PET substrate) in the visible range, an average sheet resistance of (11 ± 0.5) Ω sq−1, and an average surface roughness of (4.3 ± 0.4) nm. We benchmark these values against commercial PET/TCE substrates. Mechanical durability tests demonstrate <3% change in resistance after 2000 bending cycles at a 1 in radius. The scalable potential of the hybrid TCE fabrication method is demonstrated by high uniformity and excellent properties in 7 in × 8 in large-area samples and by performing the photonic curing process at 11 m min−1. Furthermore, halide perovskite solar cells fabricated on these hybrid TCEs achieve average and champion power conversion efficiencies of (10.5 ± 1.0) % and 12.2%, respectively, and significantly outperform devices made on commercial PET/TCEs. This work showcases our approach as a viable pathway for high-speed “green” manufacturing of high-performance TCEs on PET substrates for flexible optoelectronic devices.

Bonner, Justin C↗

NASA NTRS2013

Electrical Capacitance Volume Tomography for the Packed Bed Reactor ISS Flight Experiment

Fixed packed bed reactors are compact, require minimum power and maintenance to operate, and are highly reliable. These features make this technology a highly desirable unit operation for long duration life support systems in space. NASA is developing an ISS experiment to address this technology with particular focus on water reclamation and air revitalization. Earlier research and development efforts funded by NASA have resulted in two hydrodynamic models which require validation with appropriate instrumentation in an extended microgravity environment. To validate these models, the instantaneous distribution of the gas and liquid phases must be measured.Electrical Capacitance Volume Tomography (ECVT) is a non-invasive imaging technology recently developed for multi-phase flow applications. It is based on distributing flexible capacitance plates on the peripheral of a flow column and collecting real-time measurements of inter-electrode capacitances. Capacitance measurements here are directly related to dielectric constant distribution, a physical property that is also related to material distribution in the imaging domain. Reconstruction algorithms are employed to map volume images of dielectric distribution in the imaging domain, which is in turn related to phase distribution. ECVT is suitable for imaging interacting materials of different dielectric constants, typical in multi-phase flow systems. ECVT is being used extensively for measuring flow variables in various gas-liquid and gas-solid flow systems. Recent application of ECVT include flows in risers and exit regions of circulating fluidized beds, gas-liquid and gas-solid bubble columns, trickle beds, and slurry bubble columns. ECVT is also used to validate flow models and CFD simulations. The technology is uniquely qualified for imaging phase concentrations in packed bed reactors for the ISS flight experiments as it exhibits favorable features of compact size, low profile sensors, high imaging speed, and flexibility to fit around columns of various shapes and sizes. ECVT is also safer than other commonly used imaging modalities as it operates in the range of low frequencies (1 MHz) and does not radiate radioactive energy. In this effort, ECVT is being used to image flow parameters in a packed bed reactor for an ISS flight experiment.

Tomography↗