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All sourcesNASA NTRSDOE OSTI
NASA NTRS2016

NASA and ESA Collaboration on Alternative to Nitric Acid Passivation: Parameter Optimization of Citric Acid Passivation for Stainless Steel Alloys

National Aeronautics and Space Administration (NASA) Headquarters chartered the Technology Evaluation for Environmental Risk Mitigation Principal Center (TEERM) to coordinate agency activities affecting pollution prevention issues identified during system and component acquisition and sustainment processes. The primary objectives of NASA TEERM are to: Reduce or eliminate the use of hazardous materials or hazardous processes at manufacturing, remanufacturing, and sustainment locations. Avoid duplication of effort in actions required to reduce or eliminate hazardous materials through joint center cooperation and technology sharing. Corrosion is an extensive problem that affects the National Aeronautics and Space Administration (NASA) and the European Space Agency (ESA). The damaging effects of corrosion result in steep costs, asset downtime affecting mission readiness, and safety risks to personnel. Consequently, it is vital to reduce corrosion costs and risks in a sustainable manner. NASA and ESA have numerous structures and equipment that are fabricated from stainless steel. The standard practice for protection of stainless steel is a process called passivation. Passivation is defined by The American Heritage Dictionary of the English Language as to treat or coat (a metal) in order to reduce the chemical reactivity of its surface. Passivation works by forming a shielding outer (metal oxide) layer that reduces the impact of destructive environmental factors such as air or water. Consequently, this process necessitates a final product that is very clean and free of iron and other contaminants. Typical passivation procedures call for the use of nitric acid; however, there are a number of environmental, worker safety, and operational issues associated with its use. Citric acid is an alternative to nitric acid for the passivation of stainless steels. Citric acid offers a variety of benefits including increased safety for personnel, reduced environmental impact, and reduced operational cost. The primary objective of this effort is to qualify citric acid as an environmentally-preferable alternative to nitric acid for the passivation of stainless steel alloys. While citric acid use has become more prominent in industry, there is little evidence that citric acid is a technically sound passivation agent, especially for the unique and critical applications encountered by NASA and ESA.

citric acid passivation↗
NASA NTRS2003

Carbon-Based Wear Coatings: Properties and Applications

The technical function of numerous engineering systems - such as vehicles, machines, and instruments - depends on the processes of motion and on the surface systems. Many processes in nature and technology depend on the motion and dynamic behavior of solids, liquids, and gases. Smart surface systems are essential because of the recent technological push toward higher speeds, loads, and operating temperatures; longer life; lighter weight and smaller size (including nanotechnology); and harsh environments in mechanical, mechatronic, and biomechanical systems. If proper attention is not given to surface systems, then vehicles, machines, instruments, and other technical systems could have short lives, consume excessive energy, experience breakdowns, result in liabilities, and fail to accomplish their missions. Surface systems strongly affect our national economy and our lifestyles. At the NASA Glenn Research Center, we believe that proper attention to surface systems, especially in education, research, and application, could lead to economic savings of between 1.3 and 1.6 percent of the gross domestic product. Wear coatings and surface systems continue to experience rapid growth as new coating and surface engineering technologies are discovered, more cost-effective coating and surface engineering solutions are developed, and marketers aggressively pursue, uncover, and exploit new applications for engineered surface systems in cutting tools and wear components. Wear coatings and smart surface systems have been used widely in industrial, consumer, automotive, aerospace, and biomedical applications. This presentation expresses the author's views of and insights into smart surface systems in wear coatings. A revolution is taking place in carbon science and technology. Diamond, an allotrope of carbon, joins graphite, fullerenes, and nanotubes as its major pure carbon structures. It has a unique combination of extreme properties: hardness and abrasion resistance; adhesion and friction; thermal conductivity; chemical and thermal inertness; corrosion and wear resistance; radiation resistance and biocompatibility; electronic, acoustic, and electrochemical characteristics; and environmental compatibility. These properties make diamond attractive for a wide range of diverse applications. In particular, chemical-vapor-deposited (CVD) diamond coatings offer a broad potential, since size and cost are not as limiting. The production of large, superhard diamond films or sheets at low cost make designer materials possible. This presentation is divided into two sections: properties and applications of hard coatings. The first section is concerned with the fundamental properties of the surfaces of CVD diamonds and related materials. The surface properties of hard coatings with favorable coefficients of friction (less than or equal to 0.1) and dimensional wear coefficients (less than or equal to 10(exp -6) cubic millimeters/N.m) in specific environments are discussed. The second section is devoted to applications. Examples of actual, successful applications and of potential challenging applications of the coatings.such as CVD diamond, diamondlike carbon, and cubic boron nitride-are described. Cutting tools coated with CVD diamond are of immediate commercial interest. Other applications, such as microelectromechanical systems (MEMS), valves, and bearings of CVD diamond, are being developed, but at a slow pace. There is a continually growing interest in commercializing diamondlike carbon for wear parts applications, such as biomedical parts and implants, forming dies, transport guides, magnetic tapes and disks, valves, and gears. Cubic boron nitride films are receiving attention because they can be used on tools to machine ferrous materials or on wear parts in sliding contact with ferrous materials.

Miyoshi, Kazuhisa↗
DOE OSTI2016

o-Vanillin functionalized mesoporous silica – coated magnetite nanoparticles for efficient removal of Pb(II) from water

o-Vanillin functionalized mesoporous silica – coated magnetite (Fe{sub 3}O{sub 4}@MCM-41-N-oVan) was synthesized and fully characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy, N{sub 2} adsorption–desorption technique and magnetic measurements. The capacity of Fe{sub 3}O{sub 4}@MCM-41-N-oVan to adsorb Pb(II) from aqueous solutions was evaluated in comparison with raw mesoporous silica – coated magnetite (Fe{sub 3}O{sub 4}@MCM-41) and amino – modified mesoporous silica coated magnetite (Fe{sub 3}O{sub 4}@MCM-41-NH{sub 2}). The effect of adsorption process parameters such us pH, contact time, initial Pb(II) concentration was also investigated. The adsorption data were successfully fitted with the Langmuir model, exhibiting a maximum adsorption capacity of 155.71 mg/g at pH=4.4 and T=298 K. The results revealed that the adsorption rate was very high at the beginning of the adsorption process, 80–90% of the total amount of Pb(II) being removed within the first 60 min, depending on the initial concentration. The results of the present work suggest that Fe{sub 3}O{sub 4}@MCM-41-N-oVan is a suitable candidate for the separation of Pb(II) from contaminated water. - Graphical abstract: A novel magnetic adsorbent based on o-vanillin functionalized mesoporous silica – coated magnetite was synthesized and fully characterized and its adsorption capacity for Pb(II) ions in aqueous solutions was evaluated. The maximum adsorption capacity for Pb(II) ions was determined to be 155.71 mg g{sup −1}. The adsorption rate was very high at the beginning of the adsorption process, 90% of the total amount of Pb(II) being removed within the first 60 min. Display Omitted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Control of Ionomer Distribution in Roll-to-Roll Coated Fuel Cell Catalyst Layers

Fuel cell catalyst layers are a complex mixture of catalyst particles and ion-conducting polymers. The performance of catalyst layers is highly dependent on microstructure, which must balance proton and electron conduction with gas transport. As fuel cells transition from the laboratory to industrial production for vehicles and other applications, there is a need to understand how manufacturing processes impact the microstructure and, ultimately, the performance of catalyst layers. In this work, we have focused on the roll-to-roll coating of catalyst layers for proton exchange membrane fuel cells. The catalyst layers are responsible for the electrochemical reactions that enable power production. In these devices the catalyst is commonly a Pt nanoparticle supported on porous carbon blacks. The ion conducting polymer, or ionomer, is typically a perfluorosulfonic acid. The most common being Nafion. To fabricate the catalyst layer, the catalyst particles are dispersed in an ink with the ionomer and cast to form the catalyst layer. Commonly, laboratory samples are prepared using spray coating or hand painting, which effectively coat many thin layers to achieve the desired catalyst layer thickness. This creates catalyst layers with uniform distributions of materials throughout the thickness of the full catalyst layer. In contrast, roll-to-roll methods, like slot die, gravure or screen printing, coat the catalyst layer as a single wet film. As the film dries, ink constituents are able to segregate, leading to a heterogeneous distribution of materials through the thickness of the layer. It is also known that the choice of solvent and drying rate can affect the morphology of the catalyst layer. Thus, there is a need to understand how ink formulation and the drying process influence the distribution of materials and catalyst layer morphology. Here, we have explored the influence of solvent and drying rate on morphology of roll-to-roll coated catalyst layers. We show the development of the Kelvin probe method as a rapid screening technique for qualitative analysis of ionomer distribution. We also utilize nano X-ray computed tomography to visualize electrode structure and to quantify particle-size and pore-size distributions, thickness-dependent ionomer distribution, tortuosity, and effective transport properties. We find that solvent has a strong influence on ionomer distribution, with less of an effect on porosity. Conversely, drying temperature has a strong influence on porosity, but less influence on ionomer distribution. Finally, we utilize in situ fuel cell performance testing and other advanced diagnostics to quantify the impact of catalyst layer properties on fuel cell performance and demonstrate that roll-to-roll coating is capable of coating high performance catalyst layers in multi-meter lengths.

14 SOLAR ENERGY↗
DOE OSTI2020

Experimental Investigation of Low Cost, Low Thermal Conductivity Thermal Barrier Coating on HCCI Combustion, Efficiency, and Emissions

In-cylinder surface temperature is of heightened importance for Homogeneous Charge Compression Ignition (HCCI) combustion since the combustion mechanism is thermo-kinetically driven. Thermal Barrier Coatings (TBCs) selectively manipulate the in-cylinder surface temperature, providing an avenue for improving thermal and combustion efficiency. A surface temperature swing during combustion/expansion reduces heat transfer losses, leading to more complete combustion and reduced emissions. At the same time, achieving a highly dynamic response sidesteps preheating of charge during intake and eliminates the volumetric efficiency penalty. The magnitude and temporal profile of the dynamic surface temperature swing is affected by the TBC material properties, thickness, morphology, engine speed, and heat flux from the combustion process. This study follows prior work of authors with Yttria Stabilized Zirconia, which systematically engineered coatings for HCCI combustion. Herein, a modeling study was used to assess the impacts of various TBC material properties, e.g. density, thickness, and thermal conductivity on the temperature swing effect. Reducing conductivity emerged as a most promising avenue, rather than reducing both the density and effective conductivity by increasing porosity, the current work emphasizes a material with natively low conductivity. A novel TBC formulation was developed, leverages a class of materials that, to the author’s best knowledge, have not been used as a thermal barrier coating previously. Here, a systematic experimental investigation was carried out using single-cylinder research engine. Experimental engine studies utilizing the novel ‘glassy’ low-K coating exhibit advanced ignition phasing and reduced combustion duration relative to the baseline engine. Heat transfer measurements indicate a net reduction in heat flux over the entire cycle, although main effect is felt during expansion, and the reduced heat transfer losses manifest in higher gross indicated thermal efficiency by approximately 5-6% on a relative basis.

42 ENGINEERING↗
NASA NTRS2011

A Multifunctional Coating for Autonomous Corrosion Control

This slide presentation reviews the effects of corrosion on various structures at the Kennedy Space Center, and the work to discover a corrosion control coating that will be autonomous and will indicate corrosion at an early point in the process. Kennedy Space Center has many environmental conditions that are corrosive: ocean salt spray, heat, humidity, sunlight and acidic exhaust from the Solid Rocket Boosters (SRBs). Presented is a chart which shows the corrosion rates of carbon steel at various locations. KSC has the highest corrosion rates with 42.0 mils/yr, leading the next highest Galeta Point Beach, in the Panama Canal Zone with 27 mils/yr corrosion. A chart shows the changes in corrosion rate with the distance from the ocean. The three types of corrosion protective coatings are described: barrier (passive), Barrier plus active corrosion inhibiting components, and smart. A smart coating will detect and respond actively to changes in its environment in a functional and predictable manner and is capable of adapting its properties dynamically. The smart coating uses microcapsules, particles or liquid drops coated in polymers, that can detect and control the corrosion caused by the environment. The mechanism for a pH sensitive microcapsule and the hydrophobic core microcapsule are demonstrated and the chemistry is reviewed. When corrosion begins, the microcapsule will release the contents of the core (indicator, inhibitor, and self healing agent) in close proximity to the corrosion. The response to a pH increase is demonstrated by a series of pictures that show the breakdown of the microcapsule and the contents release. An example of bolt corrosion is used, as an example of corrosion in places that are difficult to ascertain. A comparison of various coating systems is shown.

Calle, L. M.↗
DOE OSTI2017

Enhanced Cycling Stability of Sulfur Electrodes through Effective Binding of Pyridine-Functionalized Polymer

Porous carbons have previously been widely used as host materials for sulfur (S) electrodes because of their high conductivity and high surface area. However, they generally lack strong chemical affinity to stabilize polysulfide species. Therefore, conducting polymers have been employed to stabilize S electrodes. Integrating conducting polymers with high-surface-area carbons can create a new materials platform and synergize their functions. However, the previously used conducting polymers were often insoluble, and coating them uniformly from solution onto a nonpolar carbon substrate is a challenge. Here, we report that solution-processable isoindigo-based polymers incorporating polar substituents provide critical features: the conjugated backbone provides good conductivity; functional pyridine groups provide high affinity to polysulfide species; and they possess high solubility in organic solvents. Here, these lead to effective coating on various carbonaceous substrates to provide highly stable sulfur electrodes. Importantly, the electrodes exhibit good capacity retention (80% over 300 cycles) at sulfur mass loading of 3.2 mg/cm 2 , which significantly surpasses the performance of others reported in polymer-enabled sulfur cathodes.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Mechanisms of alumina growth via atomic layer deposition on nickel oxide and metallic nickel surfaces

We aim at elucidating the mechanism of the trimethyl aluminum (TMA) decomposition on oxidized nickel (NiO) and metallic nickel (Ni) facets in the absence of a source of hydroxyl groups. This TMA decomposition mechanism constitutes the earliest stage of growth of Al 2 O 3 coatings with the atomic layer decomposition (ALD) method, which stabilizes nickel catalysts in energy-intensive processes such as the dry reforming of methane. Our first-principles calculations suggest thermodynamic favorability for the TMA decomposition on metallic nickel compared to oxidized nickel. Moreover, the decomposition of TMA on metallic nickel showed almost no differences in terms of energy barriers between flat and stepped surfaces. Regarding the impact of the CH 3 radicals formed after TMA decomposition, we calculated stronger adsorption on metallic nickel facets than on oxidized nickel, and these adsorption energies are comparable to the adsorption energies calculated in earlier works on Al 2 O 3 ALD growth on palladium surfaces. These results lead us to believe in the growth of porous Al 2 O 3 coatings triggered by CH 3 contamination rather than due to preferential TMA decomposition on stepped and/or defective facets. The CH 3 radicals are likely to be thermally stable at temperatures used during Al 2 O 3 ALD processes, partially passivating the surface towards further TMA decomposition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1978

Laser-zone growth in a Ribbon-To-Ribbon (RTR) process. Silicon sheet growth development for the large area sheet task of the low-cost solar array project

A new calculation of the effects of thermal stresses during growth on silicon ribbon quality is reported. Thermal stress distributions are computed for ribbon growth under a variety of temperature profiles. A growth rate of 55 cu cm/min with a single ribbon was achieved. The growth of RTR ribbon with a fairly uniform parallel dendritic structure was demonstrated. Results with two approaches were obtained for reducing the Mo impurity level in polycrystalline feedstock. Coating the Mo substrate with Si3N4 does not effect thermal shear separation of the polyribbon; this process shows promise of improving cell efficiency and also increasing the useful life of the molybdenum substrate. A number of solar cells were fabricated on RTR silicon grown from CVD feedstock.

Baghdadi, A.↗
DOE OSTI2022

Asymmetric side-chain engineering in semiconducting polymers: a platform for greener processing and post-functionalization of organic electronics

Organic semiconducting polymers are a powerful platform for the design of next-generation technologies due to their excellent optoelectronic properties and solution processability, allowing access to low-cost and scalable manufacturing techniques such as spin-coating, slot-die coating and roll-to-roll printing. However, their extended π-conjugation results in low solubility, requiring the use of toxic halogenated solvents to generate thin films and devices. Furthermore, accessible post-functionalization of semiconductors toward the development of multifunctional devices and sensors remains a challenge due to limited solid-state chemistry for alkyl side chains. In this work, an asymmetric side-chain engineering approach was used to introduce terminal hydroxyl moieties alongside traditional solubilizing branched alkyl chains into an isoindigo-based polymer. The hydroxyl moieties led to significantly improved processability in alcohol-based solvents without sacrificing electronic performance in thin film organic field-effect transistors. Solid state morphologies of the thin films processed from both alcohol-based and traditional halogenated solvents were further characterized using atomic force microscopy and grazing incidence wide angle X-ray scattering. Additionally, Cryo-EM was utilized in order to characterize the role of asymmetric side-chain functionality in solution state aggregation. The versatility of this design was further probed using fluorescein isothiocyanate to directly functionalize the asymmetric polymer in thin film. Furthermore, this facile solid-state post-functionalization further demonstrates asymmetric side-chain engineering to be a viable approach toward the development of sustainably manufactured multifunctional electronics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Roll-to-Roll Advanced Materials Manufacturing DOE Laboratory Collaboration - FY2018 Final Report

High-value R2R processing is used to support a wide range of products in applications which span many industrial business sectors. The overall R2R process technology can be considered as “mature” as the process methodology and has been in use for decades. This continuous processing technique traditionally involves deposition of material(s) onto moving webs or carriers or other continuous R2R, belt-fed, or conveyor-based processes that enable successive steps to build a final version which serves to support the deposited materials. Current process technologies, which typify “roll to roll”, include tape casting, silk-screen printing, reel-to-reel vacuum deposition/coating and R2R lithography. Products supported by R2R manufacturing include micro-electronics, electro-chromic window films, PVs, fuel cells for energy conversion, battery electrodes for energy storage, and barrier materials. Due to innovation in materials and process equipment, high-quality yet very low-cost multi-layer technologies can be manufactured on a very cost-competitive basis. To move energy-related products from high-cost niche applications to the commercial sector, a means must be available to enable manufacture of these products in a cost-competitive manner that is affordable by the general consumer. Fortunately, products such as fuel cells, thin- and mid-film PVs, batteries, electrochromic and piezoelectric films, water separation membranes, and other energy saving technologies readily lend themselves to manufacture using R2R approaches.Within the DOE EERE AMO, it was recognized that establishment of a program supported at the DOE National Laboratories, along with their immense design of materials and equipment modelling capabilities enabled with use of high-performance computing, could take advantage of available R2R infrastructure to manufacture new technologies. In FY 2016, a R2R Consortium was established and provided with initial “seed” funding to take an approach that was envisioned to be supportable by advanced manufacturing R2R processes. This collaborative approach was designed to foster identification and development of materials and processes related to R2R for clean-energy product development. Using computational and experimental capabilities by acknowledged subject matter experts within the supported National Laboratory system, this collaborative project would leverage the capabilities and expertise at each of four laboratories to further the development of an enabling high-volume cost-competitive platform technology. The collaboration team that is comprised of ORNL, ANL, NREL and LBNL, coordinating with EPB and other selected industry partners, was formed in April 2016 to initially address enhancing battery electrode performance and R2R manufacturing challenges. The research efforts were to predict and measure changes and results in electrode morphology and performance based on process condition changes; to evaluate mixed, active, particle size deposition and drying for novel electrode materials; to model various process condition changes and the resulting morphology and electrode performance; and to develop and validate NDE techniques for in-line measurement of battery electrode material properties. These efforts carried through FY 2017 and completed at the end of FY 2018.The approach was to look at compositions of materials with different particle sizes to make electrode samples using a R2R manufacturing process. The shape, size, and morphology of the materials, the chemistry of the formulation, the nature of slurries, their coating rate, the rate of drying all play a role in determining the final coating architecture, quality, and performance. A commercial cathode material was selected to make a series of cathodes and anodes by single pass, dual pass and slot die methods. Analysis of all the compiled results for this battery electrode development were that the best performing cathodes included: dual-pass electrode with large particles near the foil, mixed small and large particles, and small particles only. Whereas, the best performing anodes were with a mix of small and large graphite particles. An additional core project was added in FY 2017 to conduct studies of fuel cell materials that can be produced using R2R processes. The goal of this project is to explore, understand and optimize material and process parameters to support increased throughput, increased quality, and reduced cost for high volume production of gas-diffusion electrodes (GDEs) for PEMFCs. Project work in FY 2018 were to use a R2R process to fabricate electrodes without ionomer overlayer that can produce the equivalent mass activity as spray-coated electrodes with an ionomer overlayer. Oxygen-limiting current measurements were utilized to optimize oxygen mass transport. Alcohol-rich solvents were investigated, and results were that the alcohol and water ratio can be tuned to control ionomer distribution. Water-rich solvents produce a more dispersed ink which results in better high-current density performance.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Adhesion measurement of highly-ordered TiO 2 nanotubes on Ti-6Al-4V alloy

Self-assembled nanotubular arrays on Ti alloys could be used for more effective implantable devices in various medical approaches. In the present work, the adhesion of TiO 2 nanotubes (TiO 2 NTs) on Ti-6Al-4V (Ti64) was investigated by laser spallation and scratch test techniques. At first, electrochemical anodization was performed in an ammonium fluoride solution dissolved in a 90:10 ethane-1,2-diol (ethylene glycol) and water solvent mixture. This process was performed at room temperature (23 °C) at a steady potential of 60 V for 1 h. Next, the TiO 2 nanotubes layer was heat-treated to improve the adhesion of the coating. The formation of self-organized TiO 2 nanotubes as well as the microstructural evolution, are strongly dependent on the processing parameters and subsequent annealing. From microscopic analysis, highly oriented arrays of TiO 2 nanotubes were grown by thermal treatment for 90 min at 500 °C. Further heat treatment above 500 °C led to the detachment of the nanotubes and the complete destruction of the nanotubes occurred at temperature above 700 °C. Scratch test analysis over a constant scratch length (1000 μm) indicated that the failure point was shifted from 247.4 to 557.9 μm while the adhesion strength was increased from ~862 to ~1814 mN after annealing at 500 °C. Finally, the adhesion measurement determined by laser spallation technique provided an intrinsic adhesion strength of 51.4 MPa for the TiO 2 nanotubes on the Ti64 substrate.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Electrical properties of undoped zinc oxide nanostructures at different annealing temperature

This project has been focused on the electrical and optical properties respectively on the effect of Undoped zinc oxide (ZnO) thin films at different annealing temperature which is varied 400 °C, 450 °C, 500 °C, and 550 °C.Undoped ZnO solutions were deposited onto the glass substrates using sol-gel spin coating method. This project was involved with three phases, which are thin films preparation, deposition and characterization. The thin films were characterized using Current Voltage (I-V) measurement and UV-vis-NIR spectrophotometer for electrical properties and optical properties. The electrical properties show that the resistivity is the lowest at 500 °C which its resistivity is 5.36 × 10{sup 4} Ωcm{sup −1}. The absorption coefficient spectrum obtained from UV-Vis-NIR spectrophotometer measurement shows all films exhibit very low absorption in the visible (400-800 nm) and near infrared (NIR) (>800 nm) range but exhibit high absorption in the UV range.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Effect of water on critical and subcritical fracture properties of Woodford shale

Subcritical fracture behavior of shales under aqueous conditions is poorly characterized despite increased relevance to oil and gas resource development and seal integrity in waste disposal and subsurface carbon sequestration. In this paper, we measured subcritical fracture properties of Woodford shale in ambient air, dry CO 2 gas, and deionized water by using the double-torsion method. Compared to tests in ambient air, the presence of water reduces fracture toughness by 50%, subcritical index by 77%, and shear modulus by 27% and increases inelastic deformation. Comparison between test specimens coated with a hydrophobic agent and uncoated specimens demonstrates that the interaction of water with the bulk rock results in the reduction of fracture toughness and enhanced plastic effects, while water-rock interaction limited to the vicinity of the propagating fracture tip by a hydrophobic specimen coating lowers subcritical index and increases fracture velocity. Finally, the observed deviation of a rate-dependent subcritical index from the power law K-V relations for coated specimens tested in water is attributed to a time-dependent weakening process resulting from the interaction between water and clays in the vicinity of the fracture tip.

58 GEOSCIENCES↗
DOE OSTI2022

Designer Metasurfaces for Antireflective Applications Enabled by Advanced Nanoparticle Technology

Optic processing advances have shifted system limitations, with current constraints consisting of antireflective (AR) coatings applied to optics and the inability to reduce size, weight, and price. Metasurfaces, and more broadly metaoptics, provide an avenue to overcome these limitations. The ability to generate substrate-engraved metasurfaces that can be tailored is demonstrated within a broad design space to satisfy large-area AR applications for bandpass or broadband needs, demonstrating an optically equivalent surface roughness standard deviation of only 5 Å. Using an advanced nanoparticle masking approach, two metasurfaces are fabricated: 1) vertical sidewall nanofeature metasurface (MS) for AR applications at 351 nm, and 2) sloped sidewall MS designed for broadband AR applications. For the 351 nm MS, the reflectance is measured to be 0.127%. In the case of the sloped sidewall MS, the reflectance is measured to be <0.25% over 400–700 nm and <1% over 400–1100 nm. To the best of the authors’ knowledge, this is the first demonstration of a broadband AR capable of this performance. The tunability of these structures, with a parameter space spanning even more remarkable designs such as broader bands and acceptance angles, coupled with high laser-induced damage durability and mechanical robustness, displays the strength of metasurfaces for AR applications.

36 MATERIALS SCIENCE↗
DOE OSTI2019

A Study on the Surface Composition and Migration of Materials and Their Effect on Surface Microhardness during Micro-EDM of Ti-6Al-4V

This study aims to investigate the effect of machining parameters on the surface topography and composition of Ti-6Al-4V after micro-EDM as well as the effect of elemental composition on the surface microhardness. The surface topography has been studied in terms of quality of machined surface, crater sizes, and the presence of surface defects. Statistical analysis was carried out to study the influence of micro-EDM process parameters, i.e., voltage, capacitance, discharge energy, electrode rotational speed, and the electrode coating, on the elemental composition of the machined surface. It was found that the crater size, and hence the surface finish, was dependent on the electrical parameters only, with more pronounced effect of capacitance over voltage. The 60 V and 30 pF combination resulted in crater size as small as 1 µm, whereas crater size of 12 µm was obtained using a combination of 4700 pF and 112 V. Although smaller capacitance resulted in smaller crater sizes, it also increased the chances of defects or deposition of debris on the machined surface. There was migration of material from the tool electrode, dielectric oil, and atmosphere to the workpiece surface, which influenced the surface topography, crater sizes, and surface microhardness. The effects of non-electrical parameters on the relative percentage of various elements were found to be statistically insignificant. The surface microhardness was found to increase slightly due to the surface modification after EDM. The reason for increase in surface microhardness was identified as the migration of tungsten from the tool electrode and carbon from the dielectric. The maximum surface microhardness of 455 HV was obtained at a surface composition after micro-EDM containing 7.96% C and 9.69% W, where non-machined Ti-6Al-4V surface does not have any carbon or tungsten on the surface.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Aligned carbon fibers-carbon nanotube-polymer-based composite as lithium-ion battery current collector

High energy density demand is pushing the development of high-voltage cathode materials, which necessitates improved electrochemical stability of other battery components such as binders, electrolytes, and current collectors. Current collectors are considered to be an inactive component but still play an essential role. In this study, a metal-free composite film containing directionally aligned carbon fiber (CF), carbon nanotube (CNT), and polymer (P) was developed to replace aluminum foil as a cathode current collector, which relies on forming an Al 2 O 3 layer to ensure electrochemical stability at high voltage. Here, each component in the new cathode current collector played a functional role. The CNTs provided uniform current densities, and CFs improved the electronic conductivity and mechanical strength of the composite material. The polymer enhanced the adhesion of the cathode coating with the current collector and provided an impervious support to the cathode materials. The CF-CNT-P composite demonstrated excellent electrochemical and thermal stability. Cathodes coated on the CF-CNT-P composite exhibited lower charge transfer resistance, improved rate capability, and improved cyclic stability compared with the cathodes deposited on conventional aluminum foil. Additionally, the composite current collector was lighter (1.81 mg/cm 2 and 15 µm thick) than the commonly used aluminum foil (4.35 mg/cm2 and 15 µm thick), which can increase the cell energy density. Additionally, the CF-CNT-P did not need to be separated from the cathode coating during recycling and can be burnt out with binder, simplifying the recycling process.

25 ENERGY STORAGE↗
DOE OSTI2025

A critical review of the history of fabricating monolithic U-Mo fuel plates

The fabrication of monolithic uranium-molybdenum alloy fuels, specifically those developed for high-performance research and test reactors, began in the early 2000s. The primary fuel form consists of uranium alloyed with 10-wt% molybdenum in a thin foil coated with zirconium and encapsulated in aluminum-6061 cladding. Over the years, the process has evolved with different types of casting, heat treatments, rolling schedules, and cladding applications. This review examines the history of these fabrication processes and their impact on microstructure and fuel-swelling performance. Even though various fabrication methods were used, we found little correlation between fabrication variation and fuel swelling. This insensitive relationship between fabrication variation and fuel swelling is primarily due to inhomogeneous microstructures that formed during casting and grain refinement that occurred during rolling. We conclude that the fabrication processes we examined produced similar microstructures, indicating that the fuel microstructure is somewhat insensitive to the fabrication parameters evaluated. However, the relatively small amount of historic data, such as those for grain sizes, limited this analysis. More recently fabricated materials, such as those from ongoing irradiation experiment, Mini-Plate-1 and Mini-Plate-2, were also excluded from this analysis and are intended to be reviewed separately. The findings, that fuel microstructure is somewhat insensitive to the fabrication parameters, do not imply that any fabrication method is acceptable, given the uncertainties in data and fuel-swelling observations. For example, only arc melting and vacuum induction melting casting processes were previously explored in the historic fabrication efforts. In conclusion, the findings should not be extrapolated to other casting processes.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗