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DOE OSTI2019

Advanced Materials for High–Temperature Thermal Transport

High temperature processes are widely used in a variety of existing and emerging industrial and aerospace applications. Thermal properties of high-temperature materials thus play an important role in controlling the thermal energy, as highlighted by successful applications of thermal barrier coating and aerogels. While thermal transport processes at room and low temperature have witnessed tremendous progresses in the past two decades, particularly on the fronts of understanding basic heat transfer properties at micro- and nano- scale, the understanding at high temperature is still at the nascent stage, owing to several unique features at high temperature, such as the dominant Umklapp scattering effect that could render a crystalline material amorphous-like thermal properties, and the important radiation contribution at high temperature. Furthermore, this lack of systematic understating, coupled with the challenges in maintaining high temperature stability in a large number of materials, has limited the development of materials to meet the thermal transport properties pertaining to several current and emerging high-temperature applications. In this Review, we aim to provide an overview of basic mechanisms governing thermal transport processes at high temperature, to identify their unique features and challenges, and to explore opportunities in material research for high temperature thermal materials.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Electrochemically reduced graphene oxide nanosheet coatings as solid lubricants in humid air

Highlights: • A facile, low cost and green approach to fabricate ERGO coatings is reported. • The feasibility of using ERGO coatings as solid lubricants is demonstrated. • ERGO coatings reduce copper’s COF to 1/6 and wear rate to more than 1/260. - Abstract: A facile, low cost and green approach to fabricating graphene nanosheet coatings is reported. It is composed of spraying graphene oxide (GO) suspension to form GO nanosheet coatings followed by a low voltage electrochemical reduction process. The tribological performance of the as-prepared electrochemically reduced graphene oxide (ERGO) nanosheet coatings on copper disk are evaluated by sliding against steel ball in humid air. The friction coefficient of copper is reduced to 1/6 its value, and its specific wear rate is reduced more than two orders of magnitude when copper disk is coated with ERGO nanosheet coatings. These improved tribological performance are attributed to the presence of ERGO nanosheets in the sliding interface of steel vs. copper friction pair. They not only provide easy shearing, reducing the friction coefficient, but also effectively suppress abrasive wear and adhesive wear, decreasing the wear rate of copper disk.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2022

Thermal Stability and Mechanical Properties of Cold-Sprayed Nickel-Yttria Coating

The microstructural evolution under the extreme environments imposed during cold spray deposition of cermet coatings and the microstructural recovery during post-processing annealing treatments is rather complex and not well understood. Here, Ni-Yttria cermet coatings on an SS304 substrate were produced using cold spray technique, resulting in a bimodal grain structure. The grain growth, phase stability, hardness, and wear properties are observed in as-deposited and annealed (at 400 °C) Ni-Yttria and pure Ni coatings. A multimodal microstructural characterization using electron microscopy, and atom probe tomography shows the structural and compositional stability of yttria particles and Ni grains. A fragmentation of Y-rich particles and dispersion in Ni was observed, however, no forced mixing/dissolution of Y in Ni is detected. Nano-yttria dispersed within the Ni grains slowed the grain growth during annealing. After annealing, Yttria reinforced coating was 1.5 times harder and showed better thermal and mechanical stability compared to the Ni coating.

Gwalani, Bharat↗

NASA NTRS1978

Investigation of the effect of ceramic coatings on rocket thrust chamber life

Two cylindrical rocket thrust chamber cylinders were coated with a 0.203 mm layer of zirconium oxide using a process that employed electrodeposition of metal to a spray-coated mandrel. The cylinders were cyclically tested using hydrogen-oxygen propellants at a nominal chamber pressure of 4.14 MN/sq m to show the effect of the coating on life. Both cylinders failed prematurely due to causes unrelated to the coatings. Post destructive analysis showed no cooling passage wall deformation. Where erosion of the coating occurred, the coating thickness stabilized at 0.061 mm within 80 cycles and remained well adhered throughout the tests. The hot-gas-side metal wall temperature and the theoretical maximum effective strain were reduced by 80 and 92%, respectively, where the coating was 0.203 mm thick and by 40 and 50%, respectively, where the coating was 0.061 mm thick compared to an uncoated cylinder. The 50 and 92% reductions in maximum effective strain resulted in theoretical lives of 1900 cycles and greater than 10,000 cycles, respectively, compared to 300 cycles for the uncoated cylinder.

Quentmeyer, R. J.↗

NASA NTRS1979

An investigation of the adhesive bonding of Teflon solar cell covers

The concept of introducing organic agents into silicone resins to stabilize these materials against the ravages of ultraviolet radiation is presented. A screening of coating materials, cover materials and ultraviolet screening agents is described. Fabrication processes were developed for the application of thin 25 micrometer coatings to Teflon. Temperature shock and temperature-humidity tests were conducted.

Rayl, G. J.↗

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 NTRS1992

Mach 6 electroformed nickel nozzle refurbishment: FNAS investigation of ultra-smooth surfaces

The task objective has been to apply a coating of nickel-phosphorous alloy to a laminar flow wind tunnel nozzle by catalytic deposition and then polish and inspect the inside surface using optical device processes. The surface of the nozzle was coated with a nickel-phosphorous alloy of sufficient hardness and corrosion resistance to improve the durability. Due to plating defects that were clearly process related and not inherent, the final polished part was less than the desired quality. Surface finishing processes and lapping media were identified which produced a submicron surface finish on the interior plated surface. Defects apparently manifested by the first plating attempt were repaired using a small brush plating process demonstrating that individual small defects can be repaired. Measurement and analysis by profilometry demonstrated that quantitative control of the surface can be achieved.

Rood, Robert↗

DOE OSTI2018

Scalable slot-die coating of high performance perovskite solar cells

Perovskite based photovoltaic devices hold the promise to greatly reduce the cost of solar energy production; however, this potential depends greatly on the ability to deposit perovskite active layers using large scale deposition methods such as slot-die coating without sacrificing efficiency. Using a perovskite precursor ink with long wet-film processing window, we demonstrate efficient perovskite solar cells based on slot-die coated perovskite layer. We found almost no difference in the photophysical and structural details of perovskite films that were deposited by spin coating to films deposited by slot-die coating. Furthermore, we explored various slot-die coating parameters to determine their effect on the performance of the device metrics. In addition to slot-die coating, we demonstrate the versatility of this wide wet-film processing window by fabricating perovskite solar cells with active layers deposited by spin coating, blade coating, and spray coating that all exhibited similar performance.

14 SOLAR ENERGY↗

NASA NTRS1978

Investigation of the effect of ceramic coatings on rocket thrust chamber life

Cylindrical rocket thrust chamber cylinders were coated with a 0.203 mm (0.008 in.) layer of zirconium oxide using a process that employed electrodeposition of metal to a spray coated mandrel. The cylinders were cyclically tested using hydrogen oxygen propellants at a nominal chamber pressure of 4.14 MN/sq m (600 psia) to show the effect of the coating on life. Both cylinders failed prematurely due to causes unrelated to the coatings. Post destructive analysis showed no cooling passage wall deformation. Where erosion of the coating occurred, the coating thickness stabilized at 0.061 mm (0.0024 in.) within 80 cycles and remained well adhered throughout the tests.

Quentmeyer, R. J.↗

NASA NTRS2001

Effectiveness of Diffusion Barrier Coatings for Mo-Re Embedded in C/SiC and C/C

Advanced high-temperature cooling applications may often require the elevated-temperature capability of carbon/silicon carbide or carbon/carbon composites in combination with the hermetic capability of metallic tubes. In this paper, the effects of C/SiC and C/C on tubes fabricated from several different refractory metals were evaluated. Though Mo, Nb, and Re were evaluated in the present study, the primary effort was directed toward two alloys of Mo-Re, namely, arc cast Mo-41Re and powder metallurgy Mo-47.5Re. Samples of these refractory metals were subjected to either the PyC/SiC deposition or embedding in C/C. MoSi2(Ge), R512E, and TiB2 coatings were included on several of the samples as potential diffusion barriers. The effects of the processing and thermal exposure on the samples were evaluated by conducting burst tests, microhardness surveys, and scanning electron microscopic examination (using either secondary electron or back scattered electron imaging and energy dispersive spectroscopy). The results showed that a layer of brittle Mo-carbide formed on the substrates of both the uncoated Mo-41Re and the uncoated Mo-47.5Re, subsequent to the C/C or the PyC/SiC processing. Both the R512E and the MoSi2(Ge) coatings were effective in preventing not only the diffusion of C into the Mo-Re substrate, but also the formation of the Mo-carbides. However, none of the coatings were effective at preventing both C and Si diffusion without some degradation of the substrate.

Glass, David E.↗

DOE OSTI2022

Managing Sn-Supply to Tune Surface Characteristics of Vapor-Diffusion Coating of Nb₃Sn

Nb₃Sn promises better RF performance (Q and E_{acc}) than niobium at any given temperature because of superior superconducting properties. Nb₃Sn-coated SRF cavities are now produced routinely by growing a few microns thick Nb₃Sn films inside Nb cavities via the tin vapor diffusion technique. Sn evaporation and consumption during the growth process notably affect the quality of the coating. Aiming at favorable surface characteristics that could enhance the RF performance, many coatings were produced by varying Sn sources and temperature profiles. Coupon samples were examined using different material characterization techniques, and a selected few sets of coating parameters were used to coat 1.3 GHz single-cell cavities for RF testing. The Sn supply’s careful tuning is essential to manage the microstructure, roughness, and overall surface characteristics of the coating. We summarize the material analysis of witness samples and discuss the performance of several Nb₃Sn-coated single-cell cavities linked to Sn-source characteristics and observed Sn consumption during the film growth process.

Pudasaini, U.↗

DOE OSTI2021

Managing Sn-supply to tune surface characteristics of vapor-diffusion coating of Nb3Sn

Pudasaini, U.↗

NASA NTRS2017

Anisotropic Copoly(Imide Oxetane) Coatings and Articles of Manufacture, Copoly(Imide Oxetane)s Containing Pendant Fluorocarbon Moieties, Oligomers and Processes Therefor

Copoly(imide oxetane) materials are disclosed that can exhibit a low surface energy while possessing the mechanical, thermal, chemical and optical properties associated with polyimides. The copoly(imide oxetane)s are prepared using a minor amount of fluorinated oxetane-derived oligomer with sufficient fluorine-containing segments of the copoly(imide oxetane)s that migrate to the exterior surface of the polymeric material to yield low surface energies. Thus the coatings and articles of manufacture made with the copoly(imide oxetane)s of this invention are characterized as having an anisotropic fluorine composition. The low surface energies can be achieved with very low content of fluorinated oxetane-derived oligomer. The copolymers of this invention can enhance the viability of polyimides for many applications and may be acceptable where homopolyimide materials have been unacceptable.

Wohl, Christopher J.↗

DOE OSTI2020

Spatial Atomic Layer Deposition to Scale Manufacturing of Robust Catalysts for Biomass Conversion Applications: Cooperative Research and Development Final Report, CRADA Number CRD-17-715

This CRADA will facilitate technology maturation for NREL-developed ALD-coated catalyst materials that are tailored for durability during harsh biomass conversion chemistries. This project will address optimizing process parameters for scale-up of Al2O3 ALD-coated catalysts, demonstrating ALD-coated catalyst performance for muconic acid hydrogenation, and validating economic models that project significant cost benefits for ALD-enhanced catalytic processes. This work will strengthen private-public partnerships in the area of advanced catalyst manufacturing for energy-related technology. Critical information will be collected to elevate the Technology Readiness Level and increase our competitiveness for cooperative R&D agreements and licensing. Success of this work will be crosscutting as it can facilitate advanced catalyst development for both renewable and conventional processes.

09 BIOMASS FUELS↗

NASA NTRS1995

Ultra-high pressure water jetting for coating removal and surface preparation

This paper shall examine the basics of water technology with particular attention paid to systems currently in use and some select new applications. By providing an overview of commercially available water jet systems in the context of recent case histories, potential users may evaluate the process for future applications. With the on going introduction of regulations prohibiting the use of chemical paint strippers, manual scrapping and dry abrasive media blasting, the need for an environmentally compliant coating removal process has been mandated. Water jet cleaning has been a traditional part of many industrial processed for year, although it has only been in the last few years that reliable pumping equipment capable of ultra-high pressure operation have become available. With the advent of water jet pumping equipment capable of sustaining pressures in excess of 36,000 psi. there has been shift away from lower pressure, high water volume systems. One of the major factors in driving industry to seek higher pressures is the ability to offer higher productivity rates while lowering the quantity of water used and subsequently reprocessed. Among benefits of the trend toward higher pressure/lower volume systems is the corresponding reduction in water jet reaction forces making hand held water jetting practical and safe. Other unique applications made possible by these new generation pumping systems include the use of alternative fluids including liquid ammonia for specialized and hazardous material removal applications. A review of the equipment used and the required modifications will be presented along with the conclusions reached reached during this test program.

Johnson, Spencer T.↗

DOE OSTI2022

Synthesis of high-density olivine LiFePO 4 from paleozoic siderite FeCO 3 and its electrochemical performance in lithium batteries

The lithium-ion cathode material olivine LiFePO 4 (LFP) has been synthesized for the first time from natural paleozoic iron carbonate (FeCO 3 ). The ferrous carbonate starting material consists of the mineral siderite at about 92 wt. % purity. Because FeCO 3 has divalent iron, the reaction with lithium dihydrogen phosphate (LiH 2 PO 4 ) provides a unique method to develop iron-(II) containing LFP in an inert atmosphere. Since siderite FeCO 3 is a common mineral that can be directly mined, it may, therefore, provide an inexpensive route for the production of LFP. After carbon-coating, the LFP yields a capacity in the range of 80–110 mAh g -1 LFP (in one chosen specimen sample), which is lower than commercially available LiFePO 4 (150–160 mAh g -1 LFP ). However, the tap density of LFP derived from siderite is noticeably high at 1.65 g cm -3 . The material is likely to be improved with powder purification, nanosized processing, and more complete carbon-coating coverage with increased optimization.

36 MATERIALS SCIENCE↗

NASA NTRS2019

Materials and Processes for New Propulsion Systems with Reduced Environmental Impact

Aeronautics research at NASA Glenn Research Center includes development, characterization and modeling of high temperature, lightweight materials and fabrication processes for aircraft propulsion systems with increased efficiency and reduced emissions, fuel burn and noise. Current propulsion materials research includes Ceramic Matrix Composites and Environmental Barrier Coatings, Polymer Matrix Composites and Additive Manufacturing processes. This presentation will summarize recent progress and plans in these areas. Ceramic Matrix Composites for Turbine Components: As part of NASA's Aeronautics research, Glenn Research Center has developed Ceramic Matrix Composites for 2700 degrees Fahrenheit turbine engine applications in the next generation of ultra-efficient aircraft. In this presentation, the development of advanced fiber and matrix constituents that enabled this advancement will be reviewed, and characterization of the resulting improvements in mechanical properties and durability will be summarized. Progress toward the development and validation of models predicting the effects of the engine environment on durability of Ceramic Matrix Composites and Environmental Barrier Coatings will be summarized. Progress and plans for collaborative research with industry and other government agencies will be reviewed. Polymer Matrix Composites for Powertrain and Impact Protection: A lightweight, hybrid polymer matrix composite/steel gear concept for rotorcraft power transmission applications was evaluated at realistic speed, torque, and power conditions. Dynamic testing was performed at 5000 horsepower and 5400 revolutions per minute with no performance degradation. Test results demonstrated the potential of hybrid composite / metal gears to reduce gear weight by approximately 15 percent, enabling the implementation of multi-speed drive systems, which would otherwise have a weight penalty, for increased speed and efficiency. Results of post-test inspection and endurance tests will be presented. Separately, ballistic impact tests demonstrated improved damage tolerance in polymer matrix composites by incorporating lightweight, thermoplastic veil materials between selected composite plies during the composite fabrication process. Results of impact tests and post-test inspection will be presented. Additive Manufacturing for Electric Propulsion: Additive Manufacturing processes offer the potential to fabricate new, high power density electric motor designs with complex geometries, multi-material components and optimally designed components that would not be feasible with traditional manufacturing processes. High performance stator components using advanced 3-phase conductive coils were fabricated using direct printing with optimized silver pastes. Additional additive manufacturing methods are being used to fabricate rotors and motor housing components. Systems studies show that the higher performance and lower weight motors offer improved energy efficiency and reduced emissions. Improvements to motor performance resulting from optimized materials and component designs will be presented.

Additive Manufacturing↗

DOE OSTI2025

Harnessing Machine Learning to Predict MoS 2 Solid Lubricant Performance

Physical vapor deposited (PVD) molybdenum disulfide (MoS 2 ) solid lubricant coatings are an exemplar material system for machine learning methods due to small changes in process variables often causing large variations in microstructure and mechanical/tribological properties. Here, in this work, a gradient boosted regression tree machine learning method is applied to an existing experimental data set containing process, microstructure, and property information to create deeper insights into the process-structure–property relationships for molybdenum disulfide (MoS 2 ) solid lubricant coatings. The optimized and cross-validated models show good predictive capabilities for density, reduced modulus, hardness, wear rate, and initial coefficients of friction. The contribution of individual deposition variables (i.e., argon pressure, deposition power, target conditioning) on coating properties is highlighted through feature importance. The process-property relationships established herein show linear and non-linear relationships and highlight the influence of uncontrolled deposition variables (i.e., target conditioning) on the tribological performance.

MoS2↗