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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

Interfacial solvation-structure regulation for stable Li metal anode by a desolvation coating technique

Rechargeable lithium (Li) metal batteries face challenges in achieving stable cycling due to the instability of the solid electrolyte interphase (SEI). The Li-ion solvation structure and its desolvation process are crucial for the formation of a stable SEI on Li metal anodes and improving Li plating/stripping kinetics. This research introduces an interfacial desolvation coating technique to actively modulate the Li-ion solvation structure at the Li metal interface and regulate the participation of the electrolyte solvent in SEI formation. Through experimental investigations conducted using a carbonate electrolyte with limited compatibility to Li metal, the optimized desolvation coating layer, composed of 12-crown-4 ether-modified silica materials, selectively displaces strongly coordinating solvents while simultaneously enriching weakly coordinating fluorinated solvents at the Li metal/electrolyte interface. This selective desolvation and enrichment effect reduce solvent participation to SEI and thus facilitate the formation of a LiF-dominant SEI with greatly reduced organic species on the Li metal surface, as conclusively verified through various characterization techniques including XPS, quantitative NMR, operando NMR, cryo-TEM, EELS, and EDS. The interfacial desolvation coating technique enables excellent rate cycling stability (i.e., 1C) of the Li metal anode and prolonged cycling life of the Li||LiCoO 2 pouch cell in the conventional carbonate electrolyte (E/C 2.6 g/Ah), with 80% capacity retention after 333 cycles.

42 ENGINEERING↗

Lower Temperature Annealing of Vapor Diffused Nb₃Sn for Accelerator Cavities

Nb₃Sn is a next-generation superconducting material for the accelerator cavities with higher critical temperature and superheating field, both twice compared to Nb. It promises superior performance and higher operating temperature than Nb, resulting in significant cost reduction. So far, the Sn vapor diffusion method is the most preferred and successful technique to coat niobium cavities with Nb₃Sn. Although several post-coating techniques (chemical, electrochemical, mechanical) have been explored to improve the surface quality of the coated surface, an effective process has yet to be found. Since there are only a few studies on the post-coating heat treatment at lower temperatures, we annealed Nb₃Sn-coated samples at 800 C - 1000 C to study the effect of heat treatments on surface properties, primarily aimed at removing surface Sn residues. This paper discusses the systematic surface analysis of coated samples after annealing at temperatures between 850 C and 950 C.

43 PARTICLE ACCELERATORS↗

Multi-technique characterization of spray coated and roll-to-roll coated gas diffusion fuel cell electrodes

Here this work reports the characterization of catalyst layer (CL) structure and composition for a set of gas-diffusion electrodes (GDEs) fabricated by different coating methods with the goal of developing a better understanding of CL processing-structure-property-performance relationships. The CL coating techniques used in this study were ultrasonic spray coating, and two roll-to-roll (R2R) methods - gravure and slot die. Scanning transmission electron microscopy (STEM) coupled with X-ray energy dispersive spectroscopy (EDS) analysis of GDE cross-sections provided bulk information, while scanning electron microscopy (SEM) with EDS and X-ray photoelectron spectroscopy (XPS) were used to investigate the near surface and surface composition of the CLs that will be in direct contact with the membrane once the membrane electrode assembly (MEA) is constructed. This study demonstrates that common quantification parameters, namely the F:Pt ratio extracted from cross-sectional STEM-EDS maps and top-down CL measurements with SEM and XPS, along with roughness parameters quantified from SEM micrographs are useful parameters in explaining and potentially predicting performance trends. Additionally, it highlights the importance of understanding key CL surface properties for advancing the manufacturability of high-performance components for polymer electrolyte membrane (PEM) technologies.

30 DIRECT ENERGY CONVERSION↗

Directional Crystallization of Conjugated Molecules during Coating Processes

The coating of organic molecules from the solution phase can result in directional crystal growth under certain conditions, even on a smooth isotropic surface and without the need of any kind of graphoexpitaxial preparation of the substrate. Based on reviewing the results from a variety of coating techniques and coating parameters, we identified that it is crucial for the coating speed to match the growth speed of the fastest growing crystal plane to achieve a high degree of directional crystallization.

36 MATERIALS SCIENCE↗

Co-sputter deposition of Nb₃Sn layer into SRF cavity using Nb-Sn composite target

Nb₃Sn, with its superior superconducting critical temperature (Tc ~18.3 K) and superheating field (Hsh ~400 mT), is considered a promising material for superconducting radiofrequency (SRF) cavities, offering enhanced cryogenic performance compared to bulk niobium cavities. A Nb₃Sn coating technique has been developed for Nb SRF cavities using co-sputtering of Nb-Sn composite target in a DC cylindrical magnetron sputtering system. The composite target configuration and discharge conditions for co-sputtering were optimized to deposit Nb-Sn films on flat Nb substrates, followed by annealing to form Nb₃Sn. Multiple strategies have been explored to improve the surface homogeneity of the Nb₃Sn coating, including optimizing a two-step annealing process, annealing in Sn vapor, and a light Sn recoating process. A 1.5 µm Nb-Sn co-sputtered film was deposited on the interior of a 2.6 GHz Nb SRF cavity and annealed at 600 °C for 6 h, followed by 950 °C for 1 h. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, confirming the formation of Nb₃Sn. Then, the annealed cavity underwent a light recoating treatment and attained a quality factor (Q0) of 8.5E+08 at 2.0 K.

Accelerator Physics↗

Solvent-Free Manufacturing of Lithium-Ion Battery Electrodes via Cold Plasma

Slurry casting has been used to fabricate lithium-ion battery electrodes for decades, which involves toxic and expensive organic solvents followed by high-cost vacuum drying and electrode calendering. This work presents a new manufacturing method using a nonthermal plasma to create inter-particle binding without using any polymeric binding materials, enabling solvent-free manufacturing electrodes with any electrochemistry of choice. The cold-plasma-coating technique enables fabricating electrodes with thickness (>200 μm), high mass loading (>30 mg cm -2 ), high peel strength, and the ability to print lithium-ion batteries in an arbitrary geometry. This crosscutting, chemistry agnostic, platform technology would increase energy density, eliminate the use of solvents, vacuum drying, and calendering processes during production, and reduce manufacturing cost for current and future cell designs. Here, lithium iron phosphate and lithium cobalt oxide were used as examples to demonstrate the efficacy of the cold-plasma-coating technique. It is found that the mechanical peel strength of cold-plasma-coating-manufactured lithium iron phosphate is over an order of magnitude higher than that of slurry-casted lithium iron phosphate electrodes. Full cells assembled with a graphite anode and the cold-plasma-coating-lithium iron phosphate cathode offer highly reversible cycling performance with a capacity retention of 81.6% over 500 cycles. For the highly conductive cathode material lithium cobalt oxide, an areal capacity of 4.2 mAh cm -2 at 0.2 C is attained. We anticipate that this new, highly scalable manufacturing technique will redefine global lithium-ion battery manufacturing providing significantly reduced plant footprints and material costs.

25 ENERGY STORAGE↗

Innovations in Direct Air Capture: Unveiling a Simple and Robust Synthesized Fibrous Amine-functionalized Matrix (FAM) Sorbent for Commercial Scale-up

The escalating challenge of climate change necessitates innovative solutions in the realm of carbon management, particularly in mitigating the impact of fossil fuel emissions. Direct Air Capture (DAC) technology emerged as a critical component within the spectrum of Carbon Capture and Sequestration (CCS) solutions, offering the distinct advantage of directly removing CO2 from the atmosphere irrespective of the source. This attribute grants DAC systems unparalleled flexibility in deployment locations and the potential to make substantial contributions to lowing atmospheric CO2 levels. The success of DAC technologies significantly depends on the development of an efficient, economical sorbent capable of selective and durable CO2 capture from ambient air. Recent advancements in material science have led to the exploration of amine-functionalized sorbents, hollow fiber sorbents and membranes, and other novel materials designed to meet these criteria. This study explores a novel Fibrous Amine-functionalized Matrix (FAM) sorbent. The FAM sorbent distinguished itself through its mechanical robustness, a streamlined synthesis process, and the capability for low-temperature regeneration (is 90 oC really low temperature?). FAM’s exceptional adsorption-desorption kinetics enable swift CO2 capture and release, crucial for the viability of DAC on a commercial scale. The synthesis process involves a simple dip-coating technique, allowing crosslinked amines to coat glass substrates.

Wang, Qiuming↗

Mechanical and chemical properties of PVD and cold spray Cr-coatings on Zircaloy-4

In this paper, accident-tolerant fuel (ATF) cladding materials aim to improve fuel reliability and safety during accident scenarios in water-cooled reactors. These ATF cladding should also perform comparable or better than the current zirconium alloy cladding under reactor normal operating conditions. Surface-modified Zircaloy-4 was produced by depositing a protective coating of chromium by two different coating techniques, Physical Vapor Deposition (PVD) and Cold Spray (CS). The coating thickness, structure, composition, and mechanical properties of the coated Zircaloy were assessed with advanced materials characterization techniques. Results showed a strengthening effect of the Cr-coating, along with ~83% higher hardness compared to that of the Zircaloy-4 substrate. Surface topography and surface chemistry of the Cr-coated Zircaloy-4 were assessed with contact profilometry, atomic force microscopy, contact angle goniometry, and X-ray photoelectron spectroscopy. Deposited Cr-coating significantly improved surface wettability compared to the substrate Zircaloy-4. The formation of surface oxides on the coatings by prolonged exposure to ambient air showed a further increase in the hydrophobic behavior. Surface parameters and surface chemistry after flow boiling critical heat flux tests, conducted at atmospheric pressure, evidenced a slight increase in surface roughness with notable changes in wettability associated with the formation of surface oxides.

36 MATERIALS SCIENCE↗

Nb₃Sn Coating of a 2.6 GHz SRF Cavity by Sputter Deposition Technique

Nb₃Sn is of interest as a coating for SRF cavities due to its higher transition temperature Tc ~18.3 K and superheating field Hsh ~400 mT, both are twice that of Nb. Nb₃Sn coated cavities can achieve high-quality factors at 4 K and can replace the bulk Nb cavities operated at 2 K. A cylindrical magnetron sputtering system was built, commissioned, and used to deposit Nb₃Sn on the inner surface of a 2.6 GHz single-cell Nb cavity. With two identical cylindrical magnetrons, this system can coat a cavity with high symmetry and uniform thickness. Using Nb-Sn multilayer sequential sputtering followed by annealing at 950°C for 3 hours, polycrystalline Nb₃Sn films were first deposited at the equivalent positions of the cavity’s beam tubes and equator. The film’s composition, crystal structure, and morphology were characterized by energy dispersive spectroscopy, X-ray diffraction, and atomic force microscopy. The Tc of the films was measured by the four-point probe method and was 17.61 to 17.76 K. Based on these studies, ~1.2 micron thick Nb₃Sn was deposited inside a 2.6 GHz Nb cavity. We will discuss first results from samples and cavity coatings, and the status of the coating system.

43 PARTICLE ACCELERATORS↗

Reflector coatings development (FY2020 End of Year Report)

X-ray detection instrumentation has been developed and manufactured at LANL for various DOE programs. One way to improve light collection efficiency, for a scintillator type detector, is to apply suitable reflectors. The coating capability and fabrication procedure for Al reflective coatings was established in FY19 at MST-7. Al reflective coatings with good stability, good adhesion to LSO, and reflectivity (R) up to 78% were fabricated. Materials with higher diffuse reflectivity (such as Teflon tape R=99%) are desirable. A literature search revealed a number of materials in the form of paint or free standing tape with diffuse R = 98- 99%. However, for the intended application such reflectors have to be applied in the form of a coating with strong adhesion to LSO crystals. The purpose of the FY20 project was to develop thin film coating techniques for PTFE (known as Teflon) reflectors and fabricate reflective coatings on provided LSO crystals.

36 MATERIALS SCIENCE↗

Formation and degradation mechanism of methylammonium lead iodide perovskite thin film fabricated by electrospray technique

Electrospray deposition technique has been reported previously for fabricating effective and stable perovskite thin film, leading to efficient perovskite solar cells. Here, in this work, a comprehensive investigation of the formation mechanism of methylammonium lead iodide perovskite (CH 3 NH 3 PbI 3 ) film by electrospray technique is demonstrated and compared to the formation mechanism through the conventional spin coating technique. In the electrospray process, charged MAI nanoparticles are gradually introduced onto the PbI 2 film, intercalating within the PbI 2 structure to produce the perovskite film. In contrast, the spin-coating method involves supplying the MAI solution in bulk, leading to perovskite crystal formation through the dissolution of the PbI 2 layer by the MAI solution, followed by recrystallization into perovskite oriented in the [110] direction, 30° inclined to the substrate. The impact of charge and the electric field on the formation of perovskite film using the electrospray is explored. Furthermore, the intrinsic stability of perovskite films is monitored in real-time in a highly humid environment (≥80 % relative humidity (RH)) using in-situ Grazing Incidence Wide Angle X-ray Scattering (GIWAXS), and a degradation mechanism is proposed to enhance the durability of the perovskite-based devices. The study further delves into the comparison of the stability of electrosprayed and spin-coated perovskite film, and the impact of humidity level and the presence of a hole-transporting layer on the stability of the perovskite layer. Overall, this work provides a detailed understanding of the formation and humidity-induced degradation mechanism of electrosprayed perovskite films, offering insights that can extend to various applications of perovskite materials.

14 SOLAR ENERGY↗

Universal method for the optimization of HDC coating uniformity on non-planar, non-stationary substrates for inertial confinement fusion targets

The thickness uniformity of chemical vapor deposited (CVD) diamond coatings on non-planar, non-stationary substrates depends on both the intrinsic instantaneous coating thickness distribution (ICTD) of the coating conditions used and, if applicable, on the frequency of substrate reorientation. While important for many CVD diamond applications, the relative impact of the ICTD and substrate reorientation on the coating thickness uniformity has not been studied. In this work, we systematically investigate the effect of these factors for microwave-plasma chemical vapor deposition (MPCVD) of diamond (referred to as high density carbon (HDC) in the inertial confinement fusion (ICF) community) coatings on spherical, rolling substrates. This coating technique is used to fabricate capsules for ICF experiments, which require extreme coating uniformity with <0.3 % thickness variation (so-called Mode 1 or M1) to ensure symmetric compression of imploding targets. To extract the otherwise unobservable reorientation timescale (Δt), Monte Carlo simulations were performed using experimental ICTD data as input. This combined approach confirms scaling relationships between the substrate reorientation timescale as well as coating thickness and coating uniformity, as expected from a 3D random walk. Simulations confirm that M1 is Rayleigh-distributed and scales as (Δt) 1/2 , consistent with the randomization of two angles that determine orientation of a sphere. We also demonstrate that, under the conditions studied, Δt is the dominant factor in determining thickness uniformity while the intrinsic ICTD has minimal impact. Finally, experiments show that Δt can be affected by total batch size under constant agitation conditions due to space constraints that limit the capsule reorientation kinetics. In conclusion, this study highlights the utility of a combined experiment-simulation approach as a general methodology for understanding and improving coating uniformity on non-planar, non-stationary substrates.

Capsule↗

One-Pot Coating of Ceramic Powders by Exfoliated Boron Nitride Layers with a Dense CO 2 Medium and Ultrasound-Aided Mixing

The coating or doping of substrates by two-dimensional materials to impart superior functional properties (such as improved thermal conductivity, bacterial resistance, reduced friction) is receiving increased attention. Environmentally benign, rapid and scalable coating techniques are desirable for this purpose. Here, we report a novel process for coating alumina, silicon carbide and boron carbide substrates with hexagonal boron nitride (h-BN) layers. The process consists of two sequential steps. First, h-BN layers are exfoliated from bulk h-BN in supercritical carbon dioxide (scCO 2 ) using ultrasound-aided mixing. This step is followed by self-assembly (i.e., coating) of the exfoliated h-BN on the substrates in liquid CO 2 also aided by ultrasound. The liquid CO 2 state is achieved by simply lowering the pressure and temperature of the first step below the critical point of CO 2 (P c = 72.8 atm; T c = 31.1 °C). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) micrographs clearly reveal the exfoliation of h-BN under scCO 2 conditions as well as the h-BN assembly on various substrates under liquid CO 2 conditions. X-ray diffraction patterns confirm the structural integrity of the coated h-BN layers. It was also confirmed that without a transition to the liquid CO 2 phase following exfoliation in scCO 2 , there was negligible coating of h-BN on the substrates. Researchers in the field could consider this benign process to rapidly coat or dope materials with h-BN and other 2D materials to impart improved functional properties in myriad applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tailoring Corrosion Resistance of Additively Manufactured Metals with Atomic Layer Deposition

The goal of this work is to develop a scalable post-manufacturing capability at LANL that utilizes atomic layer deposition (ALD) for corrosion-resistant coatings onto additively manufactured (AM) metals. This will provide fundamentally new and essential capabilities towards the interchangeability of AM metals with traditionally wrought or machined material. This will be accomplished by (1) formulating novel ALD precursor doses and film thicknesses onto as-printed coupons of AM metals and (2) providing electrochemical characterization of corrosion susceptibility as a function of deposited film thickness. While ALD is well-established, the unique aspect (risk) of this work is application to rough AM surfaces. This risk is mitigated by repeating ALD deposition cycles, where thicker coatings laterally branch, resulting in a uniform coating. This risk will be assessed in the phase 1 feasibility study, wherein the application of ALD coatings to small AM coupon surfaces will be demonstrated using existing hardware and characterization tools at Sigma. This study alone will provide ground-breaking insight on the compatibility of ALD coating techniques with AM metals. Going beyond the phase 1 study, a standalone deposition chamber will be built, so full AM components can be coated and tested. While this MFR investment is focused on corrosion mitigation, it is critical to highlight external benefits of this technique outside the scope of this proposed study. ALD has extraordinary universality, whereby almost any material can be given almost any coating or graded density coating with atomic precision; and, the only limiting factors to scalability is the size of the dosing chamber. The self-limiting reactions intrinsic to ALD offers high conformity to part geometry and tolerance, even for internal surfaces where electroplating or conventional chemical vapor deposition falls short due to differential diffusion. This uniquely positions ALD at the forefront of post-manufacturing strategies for AM components, especially for those with complex geometry and internal surfaces.

36 MATERIALS SCIENCE↗

Copper–Carbon Nanotube Composites Enabled by Brush Coating for Advanced Conductors

There is a growing demand for advanced conductors with enhanced electrical properties to increase the energy efficiency in various applications. A promising strategy to achieve this involves the use of ultraconductive copper (UCC) composites that incorporate highly conductive carbon materials, such as carbon nanotubes (CNTs), into the copper matrix. In this study, we present a scalable brush coating technique to incorporate CNTs onto Cu substrates to produce Cu–CNT–Cu composites. The process involves brush coating the CNT solution on Cu tape substrates, followed by vacuum-assisted thermal removal of organic moieties (e.g., surfactant/polymer). This step ensures the creation of a uniformly distributed CNT network within the Cu matrix. By addition of a thin film Cu overlayer, the fabricated Cu–CNT–Cu composite architecture demonstrates similar electrical conductivity, increased current carrying capacity, and enhanced mechanical properties compared to pure Cu reference tapes. Finally, the performance characteristics of these UCC tapes along with the scalability of the brush coating approach hold great promise for the fabrication of advanced conductors for wide-ranging energy applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Redefining precision interferometry and spectroscopy with high-performance optical interference coatings

High-performance optical interference coatings have transformed precision interferometry and spectroscopy by enabling unparalleled control over light–matter interactions. This review explores recent innovations in ion-beam sputtered amorphous dielectric, as well as substrate-transferred crystalline coatings, and their impact on systems at the forefront of precision metrology. These state-of-the-art coating techniques generate multilayers with ultralow optical losses, yielding mirrors with exceptional reflectivity. Refinements in their noise performance push the ultimate limits of sensitivity, resolution, and stability in demanding laser-based metrology applications. These technologies underpin the most advanced timekeeping and spatial measurement tools, enabling high-finesse reference cavities for the world’s most precise optical atomic clocks and low-noise reflective test masses for km-baseline gravitational-wave detectors. Emerging hybrid designs combining these techniques expand access to the mid-infrared spectral region, enabling the first ultralow-optical-loss coatings in the 3000–5000 nm wavelength range for enhanced spectroscopy and trace-gas detection. We highlight how these technologies redefine coating performance metrics and set new benchmarks in quantum science, fundamental physics, and precision optical sensing.

Cole, Garrett D. [University of Arizona, Tucson, A↗

Spray Pyrolysis-Aerosol Deposition for the Production of Thick Yttria-Stabilized Zirconia Coatings

Aerosol deposition (AD) is a coating technique wherein particles are impacted onto a target substrate at reduced pressures, and supersonic particle impact velocities lead to coating consolidation. The limiting step in AD application is often not supersonic deposition operation, but aerosolization of powder particles with the proper size distribution; the translational impact velocity is strongly size-dependent. It is demonstrated that by directly synthesizing particles in the gas phase, size-controlled ceramic particles can be injected into AD systems. This in situ formation step obviates the need for particle aerosolization. Ultrasonic spray pyrolysis (USP) is applied to produce yttria-stabilized zirconia (YSZ), and USP is directly coupled with AD to produce consolidated, thick, YSZ coatings on metal substrates. USP-AD yields YSZ coatings on stainless steel and aluminum substrates with porosities <0.20, which grow to thicknesses beyond 100 μm. Aerodynamic particle spectrometry and electron microscopy reveal that the depositing particles are 200 nm–1.2 μm in diameter, though each particle is composed of nanocrystalline YSZ. Supporting computational fluid dynamics calculations demonstrate that the YSZ particle impact speeds are above 300 m s -1 . Thermal conductivity measurements demonstrate that USP-AD coatings have conductivities consistent with those produced from high-temperature processes.

36 MATERIALS SCIENCE↗