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NASA NTRS1995

Thermal conductivity of zirconia thermal barrier coatings

Thermal barrier coatings (TBC's) applied to the hot gas components of turbine engines lead to enhanced fuel efficiency and component reliability. Understanding the mechanisms which control the thermal transport behavior of the TBC's is of primary importance. Physical vapor deposition (PVD) and plasma spraying (PS) are the two most commonly used coating techniques. These techniques produce coatings with unique microstructures which control their performance and stability. The PS coatings were applied with either standard powder or hollow sphere particles. The hollow sphere particles yielded a lower density and lower thermal conductivity coating. The thermal conductivity of both fully and partially stabilized zirconia, before and after thermal aging, will be compared. The thermal conductivity of the coatings permanently increases upon exposed to high temperatures. These increases are attributed to microstructural changes within the coatings. Sintering of the as-fabricated plasma sprayed lamellar structure is observed by scanning electron microscopy of coatings isothermally heat treated at temperatures greater than 1100 C. During this sintering process the planar porosity between lamella is converted to a series of small spherical pores. The change in pore morphology is the primary reason for the observed increase in thermal conductivity. This increase in thermal conductivity can be modeled using a relationship which depends on both the temperature and time of exposure. Although the PVD coatings are less susceptible to thermal aging effects, preliminary results suggest that they have a higher thermal conductivity than PS coatings, both before and after thermal aging. The increases in thermal conductivity due to thermal aging for partially stabilized plasma sprayed zirconia have been found to be less than for fully stabilized plasma sprayed zirconia coatings. The high temperature thermal diffusivity data indicate that if these coatings reach a temperature above 1100 C during operation, they will begin to lose their effectiveness as a thermal barrier.

Dinwiddie, R. B.↗

NASA NTRS2004

Health Sensing Functions in Thermal Barrier Coatings Incorporating Rare-Earth-Doped Luminescent Sublayers

Great effort has been directed towards developing techniques to monitor the health of thermal barrier coatings (TBCs) that would detect the approach of safety-threatening conditions. An unconventional approach is presented here where health sensing functionality is integrated into the TBC itself by the incorporation of rare-earth-doped luminescent sublayers to monitor erosion as well as whether the TBC is maintaining the underlying substrate at a sufficiently low temperature. Erosion indication is demonstrated in electron-beam physical vapor deposited (EB-PVD) TBCs consisting of 7wt% yttria-stabilized zirconia (7YSZ) with europium-doped and terbium-doped sublayers. Multiple ingot deposition produced sharp boundaries between the doped sublayers without interrupting the columnar growth of the TBC. The TBC-coated specimens were subjected to alumina particle jet erosion, and the erosion depth was then indicated under ultraviolet illumination that excited easily visible luminescence characteristic of sublayer that was exposed by erosion. In addition, temperature measurements from a bottom-lying europium-doped sublayer in a TBC produced by multiple ingot EB-PVD were accomplished by measuring the temperature-dependent decay time from the 606 nm wavelength emission excited in that sublayer with a 532 nm wavelength laser that was selected for its close match to one of the europium excitation wavelengths as well as being at a wavelength where the TBC is relatively transparent. It is proposed the low dopant levels and absence of interruption of the TBC columnar growth allow the addition of the erosion and temperature sensing functions with minimal effects on TBC performance.

Eldridge, J. I.↗

NASA NTRS1990

Thermal Conductivity and Temperature Limits of Electron-Beam Physical-Vapor-Deposited ZrO2-7wt%Y2O3 Thermal Barrier Coating

The electron-beam physical-vapor-deposited (EB-PVD) ZrO2-7wt%Y2O3 thermal barrier coating has been widely used to protect engine hot section components in modem aircraft engines. Thermal conductivity and the conductivity increases due to sintering and phase changes are important coating design parameters. There is a need to characterize the coating thermal conductivity behavior and temperature limits, in order to potentially take full advantage of the coating capability. In addition, since the ZrO2-7wt%Y2O3 coating is often used as a baseline coating for the development of advanced lower thermal conductivity and higher temperature capability coatings, a thorough evaluation of the coating conductivity behavior at future higher engine operating temperatures will be useful for more accurately assessing the benefit gained from the new coating systems. In this study, thermal conductivity behavior of EB-PVD ZrO2-7wt%Y2O3 coating has been systematically investigated as a function of temperature (up to 2600 F) and time under steady-state and cyclic test conditions using a laser heat-flux technique. Thermal conductivity change kinetics were determined under realistic engine high temperature thermal gradient conditions, and correlated to the coating microstructural and phase changes. The thermal conductivity prediction models have been established in terms of heat flux, time, and testing temperatures.

Zhu, Dongming↗

NASA NTRS2007

Fabrication and Characterization of Diffusion Bonds for Silicon Carbide

Diffusion bonds of silicon carbide (SiC) were fabricated using several different types of titanium (Ti) based interlayers between the SiC substrates. The interlayers were an alloyed Ti foil, a pure Ti foil, and a physically vapor deposited (PVD) Ti coating. Microscopy was conducted to evaluate the cross-sections of the resulting bonds. Microprobe analysis identified reaction formed phases in the diffusion bonded region. Uniform and well adhered bonds were formed between the SiC substrates. In the case where the alloyed Ti foil or a thick Ti coating (i.e. 20 micron) was used as the interlayer, microcracks and several phases were present in the diffusion bonds. When a thinner interlayer was used (i.e. 10 micron PVD Ti), no microcracks were observed and only two reaction formed phases were present. The two phases were preferred and fully reacted phases that did not introduce thermal stresses or microcracks during the cool-down stage after processing. Diffusion bonded samples were evaluated with the non-destructive evaluation (NDE) methods of pulsed thermography and immersion ultrasonic testing. Joined SiC substrates that were fully bonded and that had simulated bond flaws in the interlayer were also evaluated using immersion ultrasound. Pull testing was conducted on the bonds to determine the tensile strength. To demonstrate the joining approach for a complex multilayered component for a low NOx injector application, the diffusion bonding approach was used to join three 4" diameter SiC discs that contained complex fuel and air flow channels.

Halbig, Michael↗

NASA NTRS2008

Monitoring Delamination of Thermal Barrier Coatings by Near-Infrared and Upconversion Luminescence Imaging

Previous work has demonstrated that TBC delamination can be monitored by incorporating a thin luminescent sublayer that produces greatly increased luminescence intensity from delaminated regions of the TBC. Initial efforts utilized visible-wavelength luminescence from either europium or erbium doped sublayers. This approach exhibited good sensitivity to delamination of electron-beam physical-vapor-deposited (EB-PVD) TBCs, but limited sensitivity to delamination of the more highly scattering plasma-sprayed TBCs due to stronger optical scattering and to interference by luminescence from rare-earth impurities. These difficulties have now been overcome by new strategies employing near-infrared (NIR) and upconversion luminescence imaging. NIR luminescence at 1550 nm was produced in an erbium plus ytterbium co-doped yttria-stabilized zirconia (YSZ) luminescent sublayer using 980-nm excitation. Compared to visible-wavelength luminescence, these NIR emission and excitation wavelengths are much more weakly scattered by the TBC and therefore show much improved depth-probing capabilities. In addition, two-photon upconversion luminescence excitation at 980 nm wavelength produces luminescence emission at 562 nm with near-zero fluorescence background and exceptional contrast for delamination indication. The ability to detect TBC delamination produced by Rockwell indentation and by furnace cycling is demonstrated for both EB-PVD and plasma-sprayed TBCs. The relative strengths of the NIR and upconversion luminescence methods for monitoring TBC delamination are discussed.

Eldridge, J. I.↗

NASA NTRS2010

Gas Flow Detection System

This system provides a portable means to detect gas flow through a thin-walled tube without breaking into the tubing system. The flow detection system was specifically designed to detect flow through two parallel branches of a manifold with only one inlet and outlet, and is a means for verifying a space shuttle program requirement that saves time and reduces the risk of flight hardware damage compared to the current means of requirement verification. The prototype Purge Vent and Drain Window Cavity Conditioning System (PVD WCCS) Flow Detection System consists of a heater and a temperature-sensing thermistor attached to a piece of Velcro to be attached to each branch of a WCCS manifold for the duration of the requirement verification test. The heaters and thermistors are connected to a shielded cable and then to an electronics enclosure, which contains the power supplies, relays, and circuit board to provide power, signal conditioning, and control. The electronics enclosure is then connected to a commercial data acquisition box to provide analog to digital conversion as well as digital control. This data acquisition box is then connected to a commercial laptop running a custom application created using National Instruments LabVIEW. The operation of the PVD WCCS Flow Detection System consists of first attaching a heater/thermistor assembly to each of the two branches of one manifold while there is no flow through the manifold. Next, the software application running on the laptop is used to turn on the heaters and to monitor the manifold branch temperatures. When the system has reached thermal equilibrium, the software application s graphical user interface (GUI) will indicate that the branch temperatures are stable. The operator can then physically open the flow control valve to initiate the test flow of gaseous nitrogen (GN2) through the manifold. Next, the software user interface will be monitored for stable temperature indications when the system is again at thermal equilibrium with the test flow of GN2. The temperature drop of each branch from its "no flow" stable temperature peak to its stable "with flow" temperature will allow the operator to determine whether a minimum level of flow exists. An alternative operation has the operator turning on the software only long enough to record the ambient temperature of the tubing before turning on the heaters and initiating GN2 flow. The stable temperature of the heated tubing with GN2 flow is then compared with the ambient tubing temperature to determine if flow is present in each branch. To help quantify the level of flow in the manifolds, each branch will be bench calibrated to establish its thermal properties using the flow detection system and different flow rates. These calibration values can then be incorporated into the software application to provide more detailed flow rate information.

Moss, Thomas↗

NASA NTRS2012

TEM Observation of the Ti Interlayer Between SiC Substrates During Diffusion Bonding

Diffusion bonding was carried out to join SiC to SiC substrates using titanium interlayers. In this study, 10 m and 20 m thick physical vapor deposited (PVD) Ti surface coatings, and 10 and 20 m thick Ti foils were used. Diffusion bonding was performed at 1250 C for PVD Ti coatings and 1200 C for Ti foil. This study investigates the microstructures of the phases formed during diffusion bonding through TEM and selected-area diffraction analysis of a sample prepared with an FIB, which allows samples to be taken from the reacted area. In all samples, Ti3SiC2, Ti5Si3Cx and TiSi2 phases were identified. In addition, TiC and unknown phases also appeared in the samples in which Ti foils were used as interlayers. Furthermore, Ti3SiC2 phases show high concentration and Ti5Si3Cx formed less when samples were processed at a higher temperature and thinner interlayer samples were used. It appears that the formation of microcracks is caused by the presence of intermediate phase Ti5Si3Cx, which has anisotropic thermal expansion, and by the presence of an unidentified Ti-Si-C ternary phase with relatively low Si content.

Tsuda, Hiroshi↗

NASA NTRS2013

Surface Temperature Measurements from a Stator Vane Doublet in a Turbine Engine Afterburner Flame using Ultra-Bright Cr-Doped GdAlO3 Thermographic Phosphor

Luminescence-based surface temperature measurements from an ultra-bright Cr-doped GdAlO3 perovskite (GAP:Cr) coating were successfully conducted on an air-film-cooled stator vane doublet exposed to the afterburner flame of a J85 test engine at University of Tennessee Space Institute (UTSI). The objective of the testing at UTSI was to demonstrate that reliable thermal barrier coating (TBC) surface temperatures based on luminescence decay of a thermographic phosphor could be obtained from the surface of an actual engine component in an aggressive afterburner flame environment and to address the challenges of a highly radiant background and high velocity gases. A high-pressure turbine vane doublet from a Honeywell TECH7000 turbine engine was coated with a standard electron-beam physical vapor deposited (EB-PVD) 200-m-thick TBC composed of yttria-stabilized zirconia (YSZ) onto which a 25-m-thick GAP:Cr thermographic phosphor layer was deposited by EB-PVD. The ultra-bright broadband luminescence from the GAP:Cr thermographic phosphor is shown to offer the advantage of over an order-of-magnitude greater emission intensity compared to rare-earth-doped phosphors in the engine test environment. This higher emission intensity was shown to be very desirable for overcoming the necessarily restricted probe light collection solid angle and for achieving high signal-to-background levels. Luminescence-decay-based surface temperature measurements varied from 500 to over 1000C depending on engine operating conditions and level of air film cooling.

Eldridge, Jeffrey I.↗

NASA NTRS2014

High Temperature Multilayer Environmental Barrier Coatings Deposited Via Plasma Spray-Physical Vapor Deposition

Si-based ceramic matrix composites (CMCs) require environmental barrier coatings (EBCs) in combustion environments to avoid rapid material loss. Candidate EBC materials have use temperatures only marginally above current technology, but the addition of a columnar oxide topcoat can substantially increase the durability. Plasma Spray-Physical Vapor Deposition (PS-PVD) allows application of these multilayer EBCs in a single process. The PS-PVD technique is a unique method that combines conventional thermal spray and vapor phase methods, allowing for tailoring of thin, dense layers or columnar microstructures by varying deposition conditions. Multilayer coatings were deposited on CMC specimens and assessed for durability under high heat flux and load. Coated samples with surface temperatures ranging from 2400-2700F and 10 ksi loads using the high heat flux laser rigs at NASA Glenn. Coating morphology was characterized in the as-sprayed condition and after thermomechanical loading using electron microscopy and the phase structure was tracked using X-ray diffraction.

Plasma↗

NASA NTRS2015

Extreme Oxidative Durability of TBCs on Ti2AlC MAX Phases

APS and PS-PVD YSZ thermal barrier coatings, applied directly to oxidation resistant Ti2AlC substrates, were oxidized in interrupted furnace tests. Temperature was advanced in 50C intervals from 1100 to 1300C, each 500 h long with eleven cooling cycles. Damage only initiated on the APS coating at 1300C after 15 h, with complete delamination after 500 h. The PS-PVD coating survived all testing. Weight change and metallographic analyses indicate that the YSZ-Ti2AlC systems sustained alumina scale growth of 30-40 m. In comparison, widely used Pt-aluminide bondcoats on single crystal superalloy turbine blades exhibit TBC lives equivalent to alumina scale growth up to 7 m, equivalent to just 200 h at 1200C. It is demonstrated that 25x TBC life improvement (or 180C temperature increase) resulted from the close CTE match of Ti2AlC with those of alumina and YSZ.

protective coating↗

NASA NTRS2021

Solid Particle Erosion of a Plasma Spray – Physical Vapor Deposition Environmental Barrier Coating in a Combustion Environment

Environmental barrier coatings (EBCs) were developed to reduce the susceptibility of SiC-based composites to the rapid volatilization and surface recession that occurs in the presence of water vapor. Extensive research and development has been performed on EBCs, and their corresponding failure mechanisms under different environmental conditions. However, one key failure mechanism, solid particle erosion (SPE), has not been thoroughly investigated. As a result, the present work investigates the SPE behavior of a ytterbium disilicate (Yb2Si2O7) environmental barrier coating (EBC) deposited via plasma spray-physical vapor deposition (PS-PVD). Erosion testing was performed at elevated temperature (1,200 °C) in a simulated combustion environment at the NASA Glenn Research Center Erosion Burner Rig Facility. Alumina (Al2O3) particles were used as the eroding media. A range of particle kinetic energies and impingement angles were investigated along with the effect of coating surface roughness. The post-erosion damage morphology was characterized using scanning electron microscopy (SEM). The SPE behavior of the PS-PVD EBC was shown to be comparable to other EBC systems reported in the literature.

Solid particle erosion; environmental barrier coat↗

NASA NTRS2023

High Temperature Solid Particle Erosion of Environmental and Thermal Barrier Coatings

Solid particle erosion (SPE) is a common phenomenon observed in gas turbine engines. Particles entrained in the gas flow impact engine hardware resulting in micro-scale damage that leads to deleterious effects such as material removal. For protective coatings, damage due to SPE is a key concern since it can negatively affect the durability of the coating and subsequently the life of the underlying component. In this work, the high temperature SPE behavior of two state-of-the-art environmental barrier coatings (EBCs) deposited via air plasma spray (APS) is investigated using alumina erodent to understand the effect of particle kinetic energy, impingement angle and temperature. The SPE behavior of the EBCs is also compared to APS and electron beam – physical vapor deposition (EB-PVD) thermal barrier coatings (TBCs) to elucidate similarities and differences in the erosion response. The EBCs were more susceptible to SPE than the EB-PVD TBC but had greater SPE resistance compared to the APS TBC. Coating microstructure and porosity were shown to have a strong influence on the observed behavior.

Solid particle erosion↗

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↗

NASA NTRSDate not supplied

Influence of Evaporation Rate and Chamber Pressure on the FUV Reflectance and Physical Characteristics of Aluminum Films

Space telescopes for studying astrophysical phenomena from the far ultraviolet (FUV) to the near infrared (NIR) require durable mirror coatings with high and uniform reflectance over a very broad spectral region. While coatings for the optical and NIR region are well developed with proven performance, the FUV band presents significant challenges, particularly below 115 nm. Recent developments in physical vapor deposition (PVD) coating processes of aluminum mirrors that are protected with a metal-fluoride overcoat to prevent oxidation (such as LiF, MgF2, or AlF3) have improved reflectance in the FUV. While the emphasis in these studies has been placed on improving the deposition conditions of the metal-fluoride overcoats, less attention has been devoted to how deposition parameters (such as vacuum conditions or deposition rates) may affect the quality of the aluminum mirrors. This paper presents characterization of Al+MgF2 coupons made by flash evaporation of aluminum followed by resistive evaporation of MgF2. Samples were manufactured under a variety of processing conditions and the relationship between processing variables and mirror FUV reflectivity is analyzed. Performance characterization was based on the measured near-normal reflectance in the FUV (90-180 nm), and normal-incidence transmittance in the visible was done to analyze the possible presence of pinholes in the mirror. We demonstrated pinhole-free Al/MgF2 mirrors deposited at room temperature with a reflectivity of 0.91 at 122 nm wavelength. This reflectivity enhancement was achieved solely through parameter optimization.

FUV reflectance, aluminum, PVD, deposition rate, A↗

DOE OSTI2026

Ternary and Quaternary Nickel-Iron-Oxide-Based Thin Films as Oxygen Evolution Reaction Catalysts in Alkaline Media

Alkaline water electrolyzers are a promising technology for energy storage and conversion through the electrochemical production of hydrogen, however the slow kinetics of the oxygen evolution reaction (OER) pose a major challenge. The alkaline environment enables the use of non-Pt-group metals as OER catalysts, in particular NiFe-based materials. In this study, Mn and/or Cr were elementally mixed with NiFe to further improve the OER catalyst properties through a controlled, systematic synthesis process involving thin films prepared by electron beam-induced physical vapor deposition (PVD). By exploring both simultaneous co-deposition and serial deposition of the different metals, the OER performance was investigated as a function of both the location of Mn or Cr in the multi-metal NiFe-based catalysts and the difference between surface versus bulk mixing. The distinct differences in the redox dynamics, surface oxidation, and stability of the seven studied catalysts reveal metal Cr- and/or Mn-overlayers as a promising synthesis approach for fine-tuning of catalyst properties and improving the OER performance.

Alkaline Water Electrolysis↗

DOE OSTI2026

Industrial deposition of wavelength-shifting films for liquid argon photon detection systems

The Deep Underground Neutrino Experiment (DUNE) Phase-II Far Detector is considering an approximately 2000 m 2 photon detection system to achieve a target mean light yield of 180 PE/MeV. Meeting this requirement demands scalable, cost-effective, and high-quality wavelength-shifter (WLS) coatings capable of converting 127 nm liquid-argon scintillation light into visible photons with controlled and reproducible optical performance. We report on the successful realization of an industrial physical vapor deposition (PVD) process forp-terphenyl (pTP) coatings, adapted from vacuum deposition techniques developed for OLED display manufacturing, to produce uniform WLS layers on large-area inorganic substrates, a task traditionally challenged by adhesion and uniformity issues at organic-inorganic interfaces. Surface characterization by profilometry and spectroscopic measurements demonstrates edge-region thickness variation below 10% and emission spectra consistent with high-quality pTP reference samples. The industrial process demonstrates reproducibility, scalability, and significantly reduced production time compared to laboratory-based methods, while maintaining optical characteristics consistent with established pTP reference samples. These results establish a viable pathway for mass production of high-performance pTP coatings for DUNE FD3 and future neutrino experiments, from a coating manufacturing and process standpoint. Detector-level performance validation, including quantitative VUV conversion efficiency measurements at 127 nm, is identified as future work.

47 OTHER INSTRUMENTATION↗

NASA NTRS1973

Enriched aluminide coatings for dispersion strengthened nickel materials

Improved aluminide/barrier coating combinations for dispersion strengthened nickel materials were investigated. The barrier materials involved alloys with refractory metal content to limit interdiffusion between the coating and the substrate, thereby minimizing void formation. Improved aluminide coatings involved the dispersion of aluminum-rich compounds. Coatings were tested in argon at 1533 K (2300 F) for 100 hours and in cyclic oxidation at 1422 K (2100 F). Two coatings on TDNiCr completed 300 hours of oxidation testing, none on TDNi. Selected coating combinations were evaluated in Mach 1 burner rig testing using JP-4 fuel and air at 1422 K (2100 F) and 1477 K (2200 F) for 350 and 100 hours, respectively. Static oxidation in 1-hour cycles was conducted at 1533 K (2300 F) for 100 hours. For comparison purposes a physical vapor deposition (PVD) NiCrAlY coating was tested concurrently. Only the NiCrA1Y coating survived the 1477 K (2200 F)/100-hour burner rig test and 275 hours of the 350-hour 1422 K (2100 F) test. Elevated temperature exposure reduced room temperature tensile properties but had little effect on elevated temperature properties.

Levinstein, M. A.↗

NASA NTRS1977

Protection of cooled blades of complex internal structure

The problem of general protection of cooled blades of complex internal structure was solved by a method called SF technique which makes possible the protection of both external and internal surfaces, as well as those of the orifices of cooling air, whatever their diameter. The SF method is most often applied in the case of pack process, at controlled or high activity; it can be of use on previously uncoated parts, but also on pieces already coated by a thermochemical, chemical or PVD method. The respective thickness of external and internal coatings may be precisely predetermined, no parasitic particle being liable to remain inside the parts after application of the protecting treatment. Results obtained to date by application of this method are illustrated by the presentation and examination of a various selection of advanced turbo engines.

Glamiche, P.↗