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DOE OSTI2021

Toward Optimizing Electrospun Nanofiber Fuel Cell Catalyst Layers: Microstructure and Pt Accessibility

This work investigates how local ionomer/platinum (Pt) interactions and ionomer distribution in electrospun Pt/Vulcan nanofiber electrodes impact ionomer coverage, proton accessibility, and oxygen reduction reaction (ORR) performance in proton-exchange membrane fuel cells. Insights from various in situ electrochemical diagnostics were utilized in conjunction with ex situ microscopic characterization to understand how the electrode microstructure—both at the aggregate level and near the ionomer/platinum interface—is affected by electrospinning in comparison to ultrasonic spraying. The effect of the carrier polymer poly(acrylic acid) (PAA) concentration from 5–20 wt % (with respect to total ink solids) on the resulting nanofiber morphology is discussed. Electron microscopy observations and CO displacement measurements indicated that Pt/Vulcan nanofibers prepared with a higher PAA concentration (15 wt %) were conformally coated with a film of ionomer on the exterior of the fiber, which resulted in an overall lower ionomer coverage on both Pt and carbon throughout the fiber diameter. In contrast, 10 wt % PAA leads to a uniform intrafiber distribution of the ionomer within the fibers, increasing the overall ionomer coverage and proton accessibility under both wet and dry conditions. These differences in the local ionomer coverage on Pt between 10 and 15 wt % PAA were also attributed to differences in the adsorption/interaction affinities between PAA and the ionomer onto the catalyst surface in the ink using zeta potential measurements. Additional fuel cell electrochemical tests on the electrospun electrodes show improvements in ORR kinetics and high-current-density H 2 /air performance compared to the ultrasonically sprayed electrodes.

25 ENERGY STORAGE↗

DOE OSTI2026

Pitfalls in parameters: practical process development in chemical vapor processing of SiC

Vapor processing of high-value materials, such as silicon carbide (SiC), is of interest for many industries, including aerospace and energy production. Chemical vapor infiltration (CVI) of additively manufactured components is an especially attractive manufacturing process currently in development. Here, a novel development workflow is demonstrated with the H 2 –CH 3 SiCl 3 gas system for SiC to accelerate the process optimization of CVI SiC. A combination of calculated thermodynamics and high-throughput experimental chemical vapor deposition (CVD) coatings substantially reduced the experiments required with slow CVI processes. The computational results accurately predicted changes in the thermodynamic conditions tested, while CVD coatings – characterized by Raman spectroscopy – addressed changes in kinetic parameters. This workflow is also applicable to other vapor-processing systems, such as pyrolytic carbon, ZrC, or Si 3 N 4 .

Lamm, Benjamin W. [Oak Ridge National Laboratory (↗

DOE OSTI2023

Mitigation of ventilation air methane (VAM) using novel methanotrophic coating materials: a technical analysis

Abstract Ventilation air methane (VAM) is a potent greenhouse gas source originating from geological wells, current and extinct mineshafts and other terrestrial conduits venting methane to the atmosphere, contributing to global methane emissions and disproportionate warming potential. Herein, we introduce the concept of the methanotrophic material as an engineering solution. Such materials should be capable of converting methane at ambient temperatures and pressures to a binder product, capturing and permanently sequestering the methane while simultaneously restricting its further emission. While such materials are currently under research development, this goal is supported and facilities by the mathematical framework, introduced and used herein, to evaluate the ability to convert methane, using currently published activity data. We include a case study of the conversion of a characteristic stream of VAM (0.6% methane in air, 1.7 × 10 8 l hr −1 equivalent to 100 000 standard cubic feet per minute). We show that when appropriately designed, such systems require a surface coverage of less than 1000 m of mine tunnel length (equivalent to 20 000 m 2 areal coverage) in order to reduce the methane emission from this stream by over 99%. Finally, we highlight formaldehyde as a reactive intermediate of methane oxidation which may itself be incorporated into these coating materials. As a component of binders and polymers already used ubiquitously in commercial products, this intermediate ultimately allows these systems to sequester the carbon from methane in a stable and solid form. The results presented here are easily extended to the treatment of other methane streams—either more concentrated or dilute—and the results herein will guide the design and development of a new class of carbon-negative materials.

Environmental Sciences & Ecology↗

DOE OSTI2023

Micro- and Nanoscale Surface Analysis of Late Iron Age Glass from Broborg, a Vitrified Swedish Hillfort

Abstract Archaeological glasses with prolonged exposure to biogeochemical processes in the environment can be used to understand glass alteration, which is important for the safe disposal of vitrified nuclear waste. Samples of mafic and felsic glasses with different chemistries, formed from melting amphibolitic and granitoid rocks, were obtained from Broborg, a Swedish Iron Age hillfort. Glasses were excavated from the top of the hillfort wall and from the wall interior. A detailed microscopic, spectroscopic, and diffraction study of surficial textures and chemistries were conducted on these glasses. Felsic glass chemistry was uniform, with a smooth surface showing limited chemical alteration (<150 nm), irrespective of the position in the wall. Mafic glass was heterogeneous, with pyroxene, spinel, feldspar, and quartz crystals in the glassy matrix. Mafic glass surfaces in contact with topsoil were rougher than those within the wall and had carbon-rich material consistent with microbial colonization. Limited evidence for chemical or physical alteration of mafic glass was found; the thin melt film that coated all exposed surfaces remained intact, despite exposure to hydraulically unsaturated conditions, topsoil, and associated microbiome for over 1,500 years. This supports the assumption that aluminosilicate nuclear waste glasses will have a high chemical durability in near-surface disposal facilities.

Matthews, Bethany E. (ORCID:0000000171932583)↗

DOE OSTI2024

Using a systems biology approach to describe the role of dissimilatory phosphite oxidation in the global phosphorus cycle

We investigated the role of redox reactions in the global phosphorous (P) cycle. We identified novel microbial processes responsible for oxidation of reduced phosphorous in the form of phosphite producing bioavailable phosphate. We identified central tenets that define microbial dissimilatory phosphite oxidation (DPO) and the breadth of the taxonomy of DPO microorganisms (DPOM). We demonstrated that this metabolism is vertically evolved from 3.8 GYA contemporaneously with anoxygenic phototrophy. We further demonstrate its occurrence on extant Earth as a primary mechanism driving a phosphorous redox cycle. Finally, we showed that this metabolism is environmentally maintained by the newly described autotrophic Phosphitivorax genus which rely on the reductive glycine pathway for carbon fixation. Our results demonstrate that these species are involved in a complex nutrient-dependent symbiotic relationship with their community in which they provide the fixed carbon to support the heterotrophic community and in return receive prerequisite corrinoids to maintain their activities.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2024

Second Target Station Project: STS Cross-Directorate Workshop on Hydrogen Fuel

Hydrogen, particularly green hydrogen produced through electrolysis using renewable energy, is poised to play a critical role in decarbonizing the global economy. Its ability to address the intermittency of renewable energy sources and decarbonize hard-to-electrify sectors positions it as a vital component of a sustainable energy future. Interest in hydrogen as a clean energy carrier is in a decade of unprecedented growth, with dozens of countries having released national hydrogen strategies contributing to a global hydrogen economy. In 2021, the Department of Energy (DOE) announced the Hydrogen Shot, the first of the Energy Earthshot Initiatives, which aims to lower the cost of clean hydrogen to $\$$1/kg by 2031. This initiative was followed by a considerable increase in funding for hydrogen technologies through the Bipartisan Infrastructure Law (BIL), with $\$$18 billion recently announced for regional demonstration projects (Hydrogen Hubs) and another $\$$11.5 billion aimed at research and development of electrolyzers, fuel cells, manufacturing, and recycling. The 2023 U.S. National Clean Hydrogen Strategy and Roadmap identifies the cost of clean hydrogen as a critical challenge for achieving economic scale. This includes the cost of hydrogen production by electrolysis, delivery and dispensing, onboard storage, and end-use technologies like fuel cells. Fundamental research and development into catalysts, component architectures, and material durability are critical to lower the costs of these vital technologies aimed at achieving a net-zero carbon emission economy by 2050.

08 HYDROGEN↗

NASA NTRS1989

Radio-frequency plasma chemical vapor deposition growth of diamond

Plasma chemical vapor deposition (CVD) at 13.56 MHz has been used to produce diamond particles in two different inductively coupled systems with a mixture of methane and hydrogen. The effect of a diamondlike carbon (DLC) overcoating on silicon, niobium, and stainless-steel substrates has been investigated and in the case of silicon has been found to enhance particle formation as compared to uncoated polished silicon. In addition the use of carbon monoxide in hydrogen has been found to produce well-defined individual faceted particles as well as polycrystalline films on quartz and DLC coated silicon substrates. Plasma CVD is a competitive approach to production of diamond films. It has the advantage over microwave systems of being easily scaled to large volume and high power.

Meyer, Duane E.↗

NASA NTRS2011

NASA Tech Briefs, November 2011

The topics include: 1) Flight Test Results from the Rake Airflow Gage Experiment on the F-15B; 2) Telemetry and Science Data Software System; 3) CropEx Web-Based Agricultural Monitoring and Decision Support; 4) High-Performance Data Analysis Tools for Sun-Earth Connection Missions; 5) Experiment in Onboard Synthetic Aperture Radar Data Processing; 6) Microfabrication of a High-Throughput Nanochannel Delivery/Filtration System; 7) Improved Design and Fabrication of Hydrated-Salt Pills; 8) Monolithic Flexure Pre-Stressed Ultrasonic Horns; 9) Cryogenic Quenching Process for Electronic Part Screening; 10) Broadband Via-Less Microwave Crossover Using Microstrip-CPW Transitions; 11) Wheel-Based Ice Sensors for Road Vehicles; 12) G-DYN Multibody Dynamics Engine; 13) Multibody Simulation Software Testbed for Small-Body Exploration and Sampling; 14) Propulsive Reaction Control System Model; 15) Licklider Transmission Protocol Implementation; 16) Core Recursive Hierarchical Image Segmentation; 17) Two-Stage Centrifugal Fan; 18) Combined Structural and Trajectory Control of Variable-Geometry Planetary Entry Systems; 19) Pressure Regulator With Internal Ejector Circulation Pump, Flow and Pressure Measurement Porting, and Fuel Cell System Integration Options; 20) Temperature-Sensitive Coating Sensor Based on Hematite; 21) Standardization of a Volumetric Displacement Measurement for Two-Body Abrasion Scratch Test Data Analysis; 22) Detection of Carbon Monoxide Using Polymer-Carbon Composite Films; 23) Substituted Quaternary Ammonium Salts Improve Low-Temperature Performance of Double-Layer Capacitors; 24) Sustainably Sourced, Thermally Resistant, Radiation Hard Biopolymer; 25) Integrated Lens Antennas for Multi-Pixel Receivers; 26) 180-GHz Interferometric Imager; 27) Maturation of Structural Health Management Systems for Solid Rocket Motors; 28) Validating Phasing and Geometry of Large Focal Plane Arrays; 29) Transverse Pupil Shifts for Adaptive Optics Non-Common Path Calibration; 30) Qualification of Fiber Optic Cables for Martian Extreme Temperature Environments; 31) Solid-State Spectral Light Source System; 32) Multiple-Event, Single-Photon Counting Imaging Sensor; 33) Surface Modeling to Support Small-Body Spacecraft Exploration and Proximity Operations; and 34) Achieving Exact and Constant Turnaround Ratio in a DDS-Based Coherent Transponder.

Source record↗

DOE OSTI2021

Atomic Layer Deposition for Improved Biomass Conversion Catalysts

Heterogeneous catalysts are a key enabler of the transition towards a sustainable, bio-based economy for fuels and chemicals. However, the harsh conditions in many biomass conversion processes lead to nanoparticle sintering, support collapse, and metal leaching in conventional PGM catalysts. Next-generation catalysts must be developed to address these stability challenges. This presentation will discuss ongoing work between the Catalytic Carbon Transformation and Scale-Up Center at NREL and various industrial partners to develop scalable and cost-effective atomic layer deposition (ALD) coatings for improving the performance of biomass conversion catalysts. The substantial focus will be devoted to the benefits of TiO2 ALD coatings on supported Pd hydrogenation catalysts. Ten cycles of TiO2 ALD were found to dramatically improve the activity of a conventional Pd/Al2O3 catalyst towards aromatic hydrogenation, despite partial coverage of the Pd sites by the ALD layer. Subsequent advanced characterization and atomic-scale computational modeling revealed that the ALD coating weakened the adsorption strength of hydrogenation surface intermediates, leading to higher reaction rates. Reaction testing after exposure to sulfur impurities, high temperature oxidation, and hydrothermal treatment demonstrated the improved stability of the ALD-coated catalyst. Additionally, the ALD synthesis process was found to be scalable over two orders of magnitude with minimal deviation in synthesized catalyst properties. These results were contextualized with cost models of industrial ALD coating and aromatic hydrogenation processes to further refine the value proposition of ALD coatings. Given the demonstrated improvements in hydrogenation, TiO2 ALD coatings have also been applied to supported Pt catalysts for use in other biomass conversion reactions, such as hydrodeoxygenation for the production of sustainable aviation fuel (SAF) and the oxidation of glucose to bio-derived gluconic acid.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2021

Atomic Layer Deposition for Improved Biomass Conversion Catalysts

atomic layer deposition↗

DOE OSTI2023

High Temperature Ternary Chloride Molten Salt Pump

This work investigates the design criteria considering thermal, structural, and material selection of a ternary chloride (MgCl2-NaCl-KCl) molten salt pump that is capable of running at temperatures above 720 °C. In this work, preliminary testing of salt-wetted hydrodynamic bearings was done to investigate different material pairings including Colmonoy grades, Stellite grades, and a novel Nickel Tungsten Carbide alloy (HybrimetTM NiWC3b) used as a High Velocity Oxygen Fuel (HVOF) coating. The coating has shown to withstand the corrosive nature of the molten salt. The pump wetted components are made of Inconel 625 and features a carbon ring seal (CIRPAC Seal) flooded with a N2 gas flow on the overhead to keep salt vapors from interacting with the external ambient air. A comprehensive pump test program has been completed. Over 90 hours run time pumping hot chloride salts at temperatures up to 720 °C in which enough data was captured to produce performance curves at 3 different operating speeds. This research showcases a promising design for use in the Concentrated Solar Power (CSP) Gen 3 liquid-pathway and sets the ground for further development and use of the HybrimetTM NiWC3b as a competitive alternative to available superalloys.

14 SOLAR ENERGY↗

DOE OSTI2020

Carbon quantum dots interfacial modified graphene/silicon Schottky barrier solar cell

The two-dimensional thin film, as an effective interface modification layer to improve the power conversion efficiency (PCE) of graphene/silicon (Gr/Si) heterojunction solar cells has attracted extensive attention recently. However, the complicated manufacturing process and specialized equipment requirements impede its broad application. Herein, carbon quantum dots (CQDs) fabricated under the mild reaction condition was first time used to modify Gr/Si devices interface structure. The effects of CQDs size distributions and coating thickness on J-V characteristics and the energy band structure of Gr/CQDs/Si solar cells were systematically analyzed. The findings indicate that the PCE of resulting Gr/CQDs/Si solar cells could reach 9.97% when the thickness and sizes of CQDs interlayer are ~26 nm and 4–7 nm, without any chemical doping, which is 6.8-times PCE than that of virgin Gr/Si solar cells. The CQDs interlayer serves as both an electron blocking layer and hole transport layer to reduce the carrier recombination, leading to a lower reverse saturation current as well as a larger VOC then improved the device performance. The enhanced PCE shows that the CQDs species have the potential applications in a cost-effective photovoltaic device.

14 SOLAR ENERGY↗

NASA NTRS1976

Cleaning carbon steel

Increased etch rate using 8% citric acid actually reduces total amount of material etched away by eliminating reprocessing that was frequently required. Time required in citrosolve solution is reduced and more protective passive coating is provided.

Maynard, V.↗

NASA NTRS2003

Fracture Toughness Enhancements in Carbon Nanotube Reinforced Ceramic Matrix Composites

Determine whether benefits may be derived from the addition of nanotubes to ceramic matrix composites for the high temperature /structural applications that are of interest to NASA. These include - coating, fuel sell, "smart" engine components, sensors, piezoelectrics, etc.

Hurst, Janet↗

DOE OSTI2022

Self-Sensing Fiber Reinforced Composite (CRADA Final Report)

The project aimed to demonstrate a scalable coating process to adhere nanoparticles to the surface of fibers and fabricate composites with in-situ damage detection abilities and simultaneous mechanical performance enhancements. Carbon fiber (CF) composites have the inherent problem of hiding damage within the structure with no visual indications on the surface. Therefore, a technique to monitor for damage or excessive stress on the composite is necessary to ensure its safety and avoid catastrophic failure. This capability will be desired in future transportation vehicle designs, such as in cargo and surveillance drones developed by Dronesat, LLC, (Dronesat) who was the industrial partner on this project.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Using Fission-Track Radiography Coupled with Scanning Electron Microscopy for Efficient Identification of Solid-Phase Uranium Mineralogy at a Former Uranium Pilot Mill (Grand Junction, Colorado)

At a former uranium pilot mill in Grand Junction, Colorado, mine tailings and some subpile sediments were excavated to various depths to meet surface radiological standards, but residual solid-phase uranium below these excavation depths still occurs at concentrations above background. The combination of fission-track radiography and scanning electron microscope energy-dispersive X-ray spectroscopy (SEM-EDS) provides a uniquely efficient and quantitative way of determining mineralogic associations of uranium that can influence uranium mobility. After the creation of sample thin sections, a mica sheet is placed on those thin sections and irradiated in a nuclear research reactor. Decay of the irradiated uranium creates fission tracks that can be viewed with a microscope. The fission-track radiography images indicate thin section sample areas with elevated uranium that are focus areas for SEM-EDS work. EDS spectra provide quantitative elemental data that indicate the mineralogy of individual grains or grain coatings associated with the fission-track identification of elevated uranium. For the site in this study, the results indicated that uranium occurred (1) with coatings of aluminum–silicon (Al/Si) gel and gypsum, (2) dispersed in the unsaturated zone associated with evaporite-type salts, and (3) sorbed onto organic carbon. The Al/Si gel likely formed when low-pH waters were precipitated during calcite buffering, which in turn retained or precipitated trace amounts of Fe, As, U, V, Ca, and S. Understanding these mechanisms can help guide future laboratory and field-scale efforts in determining long-term uranium release rates to groundwater.

58 GEOSCIENCES↗

NASA NTRS1979

Preparing thin aluminum films for adhesive bonding

Carbonate pretreatment produces highly bondable surface without harming film. Treatment is useful in developing low-cost mirrors and solar concentrators fabricated from metal-coated plastic films. Treatment should cost no more than standard degreasing and rinsing procedures.

Smith, T.↗

NASA NTRS1989

The effects of atomic oxygen on the thermal emittance of high temperature radiator surfaces

Radiator surfaces on high temperature space power systems such as SP-100 space nuclear power system must maintain a high emittance level in order to reject waste heat effectively. One of the primary materials under consideration for the radiators is carbon-carbon composite. Since carbon is susceptible to attack by atomic oxygen in the low earth orbital environment, it is important to determine the durability of carbon composites in this environment as well as the effect atomic oxygen has on the thermal emittance of the surface if it is to be considered for use as a radiator. Results indicate that the thermal emittance of carbon-carbon composite (as low as 0.42) can be enhanced by exposure to a directed beam of atomic oxygen to levels above 0.85 at 800 K. This emittance enhancement is due to a change in the surface morphology as a result of oxidation. High aspect ratio cones are formed on the surface which allow more efficient trapping of incident radiation. Erosion of the surface due to oxidation is similar to that for carbon, so that at altitudes less than approximately 600 km, thickness loss of the radiator could be significant (as much as 0.1 cm/year). A protective coating or oxidation barrier forming additive may be needed to prevent atomic oxygen attack after the initial high emittance surface is formed. Textured surfaces can be formed in ground based facilities or possibly in space if emittance is not sensitive to the orientation of the atomic oxygen arrival that forms the texture.

Rutledge, Sharon K.↗