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At least 55 records · Page 3

The role of Li doping in layered/layered Na x Li y Ni 0.4 Fe 0.2 Mn 0.4 O 2 intergrowth electrodes for sodium ion batteries

Here, the layered NaTMO 2 (TM = Ni, Fe, Mn) materials with the O3-type structure are attractive as positive electrodes for sodium ion batteries because of their high theoretical capacity. Additionally, Li doping in these materials has been shown to offer substantial enhancements to their electrochemical properties by promoting the formation of intergrowth structures, which are combinations of specific phases. However, the mechanism by which the intergrowth modifies the electrochemical properties is often unclear. Systematic variation of Li content in Na x Li y Ni 0.4 Fe 0.2 Mn 0.4 O 2 (NFM-Li y ) was conducted to identify its role in structural modification and electrochemical performance. Li contents of 0.15 and greater generate a layered/layered Na-O3/Li-O’3 intergrowth structure. 7 Li and 23 Na nuclear magnetic resonance and x-ray absorption spectroscopy identify that when the total solubility for alkali ions in the layered structure is exceeded, Li continues to form the Li-O’3 phase while the excess Na forms residual sodium compounds such as Na 2 O. Higher Li content is associated with improved capacity retention in the initial cycles from the superior stability of the mechanically linked NaO3/Li-O’3 structure that suppresses the P3 to OP2 phase transition during charge. However, high Li contents are associated with increased rates of parasitic side reactions that reduce long-term cycling stability. These side reactions are associated with the instability of the cathode-electrolyte interphase, which can be partially mitigated by atomic layer deposition (ALD) coating with alumina, which significantly enhances the capacity retention and Coulombic efficiency over many cycles. Overall, we find that the layered/layered Na-O3/Li-O’3 intergrowth structure is able to provide structural stability and suppress undesired phase transformations but is overwhelmed by the increased reactivity of the surface if not protected by surface coating.

25 ENERGY STORAGE↗

Comparative Study of Zinc Cold-Spray Coating and Pre-treatments for Magnesium Alloys

Magnesium (Mg) alloys are appealing for automotive lightweighting owing to their high specific strength. However, their susceptibility to corrosion in harsh environments remains a major challenge. Conventional industrial pre-treatment coatings, including zinc phosphate, chromate conversion, and non-chromate conversion, often exhibit discontinuities and microcracks, leading to localized corrosion near fasteners and parting lines. Here, this study investigates cold-sprayed zinc (Zn) coatings as a novel pre-treatment alternative for high-pressure die cast (HPDC) AZ91 Mg alloys, demonstrating significant improvements in wear and corrosion performance. Cold spray produces uniform and robust coatings, reducing wear rate by over 50% and reducing corrosion rate by over 99.3%, as measured by evolved hydrogen release, compared to traditional pre-treatments. Multimodal corrosion testing reveals that Zn cold-spray coatings form a protective layer during exposure, minimizing general and filiform corrosion, and exhibiting corrosion potential (E corr ) that is nobler by ~ 400 mV than the surfaces of both pre-treated and uncoated AZ91. Scalability of cold spray for selective application around multimaterial joints further strengthens their industrial viability. This work establishes Zn cold-spray coatings as highly effective pre-treatment solutions for the advancement of corrosion resistant Mg alloy components in automotive applications.

multimodal corrosion↗

Applied Research and Development to Support Open Water Testing at PacWave – Task 5: Development of additively manufactured, functionally graded, corrosion resistant clads for wave energy applications

In this task, we focused on developing corrosion-resistant claddings for wave energy applications. Wave energy systems are exposed to saline conditions, which are corrosive to many metallic structural materials (e.g., carbon steel). Corrosion-resistant (stainless) steels are typically alloyed with >18% chromium (Cr) and >8% nickel (Ni), which dramatically raises material costs and can hinder the development of wave energy systems; thus, coatings are a necessary corrosion protection method for most. Non-metallic coatings (paint, epoxy) have shorter service lives, limited resistance to mechanical stress and wear, plus additional costs of inspection and eventual replacement. Therefore, overlay stainless steel (SS) claddings have a cost-effective use case for protecting components from corrosion, particularly for those that may be subject to mechanical stress / wear and with long service lives.

16 TIDAL AND WAVE POWER↗

Monitoring pipeline integrity of underground gas storage facilities using membrane-based electrochemical sensors

Effective monitoring of internal corrosion risk is crucial to ensuring the safety and longevity of natural gas pipeline infrastructure. While electrochemical sensors are commonly used to assess corrosion rates and corrosion indicators in aqueous fluids, they are rarely used in gas pipelines as these fluids lack the ionic conductivity needed for electrochemical measurements. The inclusion of ion-conductive membranes into electrochemical sensors can extend their functionality into humidified gas streams, providing critical information about emerging corrosion events that are common during withdrawal season in pipeline systems downstream from underground storage facilities. In parallel, new protective films, like those obtained through cold spray coating, are being developed to protect oil and gas pipelines and recover losses in structural integrity due to corrosion damage. Herein, we demonstrate how membrane-based electrochemical sensors (MBES) can be used to monitor fluid corrosivity by examining their response to changes in water content for a wide range of fluid compositions. It was found that MBES readings were highly sensitive to water content changes with membrane conductivity measurements varying from 10 –6 to 10 –1 S cm -1 , and corrosion rate measurements which varied from 10 –7 to 1 mm y -1 . Electron microscopy confirmed that the self-healing characteristics of metal coating films were still active despite their inclusion into an MBES probe. In conclusion, these findings indicate that membrane-based corrosion monitoring can be expanded to monitor coated-pipeline materials and provide early detection of emerging corrosion upsets relevant to underground gas storage facilities.

Electrochemical sensor↗

Impact of Irradiation on Corrosion Performance of Hybrid Organic/Inorganic Coatings on Austenitic Stainless Steel

The effects of gamma radiation on the performance of two corrosion-resistant coatings applied to stainless-steel 304L (SS304L) surfaces are presented. Specifically, the ability of the coatings to mitigate corrosion of SS304L surfaces as a function of the dose received (0–1300 Mrad) and dose rate (176 compared to 1054 rad/s) is evaluated using electrochemical methods, spectroscopy, and microscopy. Coating A, an organic/inorganic hybrid coating consisting of a two-part silica ceramic component and a polymer linker was evaluated in comparison to Coating B, which utilized Coating A as a topcoat for a commercial, off-the-shelf, Zn-rich primer. Post irradiation, Coating A demonstrated some corrosion protection following exposure to low levels of gamma radiation, but coating degradation occurred with an increased exposure dose and resulted in isolated regions of corrosion initiation. For Coating B, greater corrosion resistance was observed compared to Coating A due to the sacrificial nature of the Zn at elevated doses of gamma radiation. No effect of the dose rate (for the single dose examined) was observed for either coating. It is proposed for Coating B that as the polymer coating thermally degrades above 250 °C (bond scission of the polymer occurs), the remaining Zinc layer adhered to the SS304L post-irradiation enables enhanced corrosion resistance as compared to Coating A, which displays solely polymer degradation. The results presented herein establish an understanding of coating behavior with radiation exposure, specifically the relationship between corrosion coating performance and radiation dose, and can inform ageing and lifetime management for various applications.

degradation↗

The Effect of Flow on CO2 Corrosion of Self-Healing Metallic Coatings

Internal corrosion is an issue that affects natural gas pipelines, a significant part of the United States’ energy infrastructure. Over time, this corrosion has worn away longstanding pipelines due to the original construction materials used for the lines and impurities in the gas and liquid streams flowing through them. The main impurities in natural gas are H2O, CO2, H2S, and O2. One of the leading causes of corrosion is the CO2 dissolved in water, giving rise to carbonic acid formation, which can further dissolve the steel pipe. The National Energy Technology Laboratory (NETL) has been studying different solutions to this problem. One potential answer is a self-healing sacrificial metallic coating applied by a novel cold spray technique. This study explored the impact of flow on corrosion with this coating and carbon steel when exposed to a saturated CO2 environment by simulating the pipeline flow profile in a small-scale lab setting. The samples were evaluated using multiple electrochemical techniques that found corrosion rates and were backed up with surface analysis to conclude the behavior of the corrosion mechanisms. The cold spray coating exhibited steel corrosion protection under flow conditions. This study has significantly advanced our understanding of CO2 corrosion, particularly in the context of natural gas pipelines and coating design.

carbon steel↗

High Entropy Rare-earth Oxide (HERO) Coatings for Refractory Alloys

The HERO coating was developed to protect refractory alloys for application in the harsh hot section of the turbine engine environment addressing ARPA-E ULTIMATE Project Topic 2: Coating Development. The effort was both innovative in its utilization of high entropy rare earth oxides as well as transformational in our approach: holistic design of a single layer thermal/environmental barrier coating (T/EBC) for refractory alloys, with an excellent coefficient of thermal expansion (CTE) match to the alloy substrate, chemical compatibility with the underlying alloy, low oxidant permeability, stability in combustion environments, low thermal conductivity, thermal shock resistance, and resistance to degradation by siliceous debris (calcium magnesium alumino-silicates-CMAS). The high entropy rare earth oxide approach enables two critical coating properties: tailoring CTE match to the substrate and, most significantly, substantially reduced thermal conductivity. The summation of these proposed coating capabilities goes well beyond the technical requirements specified in the ULTIMATE program objectives, and additionally is essential for a successful first stage turbine blade application.

36 MATERIALS SCIENCE↗

Composite coatings from polycarbosilane derived SiC and Al/SiC cermet active fillers as protective barriers against steel corrosion

Stainless steel is used throughout the world as a structural material. However, it undergoes corrosion damage when exposed to extremely corrosive media, such as the marine environment. An alternative to solve this problem lies in the development of coatings that can withstand extreme conditions but also be easily deposited with inherently corrosion-resistant materials such as silicon carbide (SiC). The present study shows a simple method to produce Al/SiC cermet powders by attrition milling. The resulting cermet powders with a metallic matrix and hemispherical morphology, were employed as fillers in polycarbosilane (PCS) solutions that were sprayed on A304 stainless steel substrates. Al/SiC composite coatings were produced after heating the sprayed suspensions at 700 °C for 1 h in Ar atmosphere. The resulting composite coatings exhibited low surface energies (< 35 mN/m), water contact angles of 53°, and adhesion strength of up to 30 MPa. Finally, corrosion tests were performed in a cyclic corrosion test chamber, showing that these coatings effectively reduced the corrosion rate of stainless steel by 87%, reaching corrosion rate values of 0.007 g/cm 2 year.

36 MATERIALS SCIENCE↗

Integrated process-structure–property–performance optimization of cold-sprayed zinc coatings on AZ91 magnesium alloy

High-pressure die cast (HPDC) AZ91 magnesium alloy is widely used in automotive components such as transmission housings and brackets for its excellent strength-to-weight ratio. Zinc-based cold spray coatings can be applied selectively to vulnerable areas to enhance corrosion resistance, minimize galvanic coupling with dissimilar metals, and eliminate the need for full-surface oxide coatings, making the process more efficient and targeted. A comprehensive evaluation of 16 combinations of nitrogen carrier gas temperatures and pressures led to the identification of an optimal range of process parameters, yielding Zn coatings with porosity <0.5 % by area, wear rates reduced by a factor of two compared to uncoated AZ91, and adhesion strengths up to 35 MPa. The enhanced mechanical performance of the coating is attributed to the low porosity and the formation of a metallurgical bond at the coating-substrate interface. Corrosion studies using macroscale potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) revealed a significant decrease in corrosion rate and a shift to more noble corrosion potentials (ZCP) for coated substrates. Furthermore, the Zn cold-sprayed samples exhibited significantly lower corrosion-induced evolved hydrogen content compared to the base AZ91 substrate and AZ91 coated with industrial coatings, demonstrating that the Zn layer effectively protects the substrate from the corrosive environment. Overall, cold spray Zn coatings significantly improve the mechanical and corrosion performance of AZ91 Mg alloys, addressing key material challenges and enabling their broader use in automotive applications.

Corrosion performance↗

High pressure effects on EBC systems in high temperature environments

Environmental barrier coatings (EBCs) are designed to protect SiCfiber/SiCmatrix ceramic matrix composites (CMCs) in turbine engines by mitigating wear in high-temperature water vapor environments. The failure of EBCs is frequently attributed to the accelerated oxidation of the silicon bond coating layer when exposed to high-temperature steam, leading to the formation of a thickened thermally grown oxide (TGO). TGO growth increases interfacial stress, weakens adhesion, and results in coating spallation. Understanding the impact of high-temperature oxidation of EBC systems is essential for developing accurate lifespan models for turbine components, although pressurized oxidation testing is extremely sparse in the open literature. In this work, oxidation tests were performed on rare earth silicate EBCs coated onto SiC substrates under increased pressure conditions. The coated specimens were tested at 1100°C, 1200°C, and 1300°C at both 1 atm and 10 atm total pressure in steam environments. Subsequent characterization focused on the microstructural evolution of the EBC/Si/SiC system. The experimental findings indicated that TGO behavior is dependent on high-pressure conditions, with elevated pressure leading to an increase in oxide scale thickness and modifications in its morphology.

Ardrey, Kristyn [ORNL] (ORCID:0000000184407796)↗

Design of an alumina forming coating for Nb-base refractory alloys

Refractory multi-principal element alloys (RMPEAs) promise to significantly enhance gas turbine engine efficiency, but their poor oxidation performance inhibits their implementation. Alumina-forming bond coat alloys can provide oxidation protection, but discovering suitable chemistries remains a challenge. We employed a design methodology that screens for alumina-formation capability using Al activity and phase constitution predictions from CalPhaD (Thermo-Calc). Alloy down-selection from approximately 7,800 alloys in the Nb-Si-Ti-Al-Hf system was conducted via analysis of calculated thermodynamic properties with number-density topology style maps. This approach is validated by creating and testing the composition Nb 12 Si 23 Ti 24 Al 36 Hf 5 , which forms protective alumina scales up to 1400 °C and resists pesting at 800 °C. Further, the alloy has an average coefficient of thermal expansion of ~10.1 ppm/K, making it well matched to Nb-based refractory alloys. The methodology will be useful for the design of coatings for RMPEAs, enabling their implementation and significant efficiency benefits sooner.

36 MATERIALS SCIENCE↗

Inverse Consequences of the SnO 2 Protection Layers on Pt/C Catalysts in Proton-Exchange Membrane Fuel Cells

Proton-exchange membrane fuel cells (PEMFCs) are promising energy-conversion systems, offering an appealing blend of high energy efficiency and low environmental impact. However, carbon corrosion of PEMFCs is known to significantly degrade their performance, remaining a critical challenge to overcome. In this study, we applied a Nb-doped SnO 2 (Nb-SnO 2 ) nanoparticle coating on Pt/C catalysts as a protective layer, with the Sn/C ratio in the precursors varying from 0.25:1 to 2.0:1. Contradictory behaviors of the coated Pt/C catalysts were observed at different Sn/C ratios. The Sn/C = 1.0 sample exhibited improved electrochemically active surface area retention after 500 cycles of accelerated stress testing (AST) but with more significant polarization and resistance increase observed in the polarization curves. In addition, agglomeration of Nb-SnO 2 particles was observed at a higher Sn/C ratio in the AST of a membrane electrode assembly, with less shrinkage of the total thickness of the Nb-SnO 2 -coated Pt/C electrode. We speculate that formation of Nb-SnO 2 agglomerates occurs once the protective layer is broken down or the unprotected carbon surface is corroded and that these Nb-SnO 2 agglomerates increase the tortuosity of the electron pathways and significantly increase the cell polarization.

30 DIRECT ENERGY CONVERSION↗

Photoelectron Spectroscopic Determination of the Interfacial Energetics of Metal Oxide Protection Layers on p-InP Photocathodes

The interfacial energetics between p-type InP and a series of metal oxides, including TiO 2 , Nb 2 O 5 , Ta 2 O 5 , and HfO 2 , were evaluated using X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), and optical absorption spectroscopy. The energy of the conduction-band minimum ( E cb ) of TiO 2 and Nb 2 O 5 was more negative (i.e., further from the vacuum level) than the conduction-band minimum at the surface of InP ( E cb,s ), whereas E cb for Ta 2 O 5 and HfO 2 was more positive than E cb,s for InP. The data are consistent with the electrochemical behavior of p-InP coated with various metal oxide candidate protection layers, with TiO 2 and Nb 2 O 5 facilitating interfacial transfer of photogenerated minority-carrier electrons in p-InP photocathodes, and Ta 2 O 5 and HfO 2 blocking photogenerated electrons in p-InP from readily transferring across the oxide-coated photocathodes. The energy of the valence-band maximum ( E vb ) for all of the oxides was much more negative than E vb,s for InP, consistent with observations that these protection layers effectively block hole transport and consequently suppress oxidative degradation of the underlying p-InP photocathodes.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗

ULTIMATE Phase I project: Development of Niobium-based alloys for Turbine Applications

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer. The first class of alloys developed in this project was a Nb-alloy designed to serve as the turbine blade core with excellent room temperature strength, ductility, and high temperature strength and creep resistance required for 1300°C operation. These alloys were designed to contain sufficient solute solution strengthening elements (W, Mo) but constrained by the density of alloy, along with the addition of elements such as Zr, Hf, Ta, C, and N to achieve a combination of primary and secondary carbide precipitation. A total of 38 “creep-resistant” alloys were designed and cast during the duration of the project. Processing techniques were developed to keep the oxygen contents as low as possible with typical oxygen contents less than 250 ppm. One alloy with a density of < 9.5 g/cc was successful in meeting the Phase 2 intermediate project mechanical property milestone requirements of room temperature ductility greater than 1.0%, 1200°C creep strain of less than 3% at 150 MPa and 100 hours in vacuum, and with solidus temperature greater than 1500ᵒC. The second class of alloys was designed to be a Nb-rich alloy with improved oxidation resistance when compared to the core layer and was designed specifically to be compatible with the core layer and the outer environmental barrier coating. This Nb- alloy will be specifically designed to be microstructurally stable at these temperatures when in contact with the core alloy and provide protection against catastrophic failure of the barrier coating. Two alloys were cast and processed but further development was discontinued to focus on the development of the creep resistant alloy.

36 MATERIALS SCIENCE↗

Predicted Fracture Tendency of Naturally Occurring Aluminum Surface Coatings under Tensile Loading

Naturally occurring coatings on aluminum metal, such as its oxide or hydroxide, serve to protect the material from corrosion. Understanding the conditions under which these coatings mechanically fail is therefore expected to be an important aspect of predictive models for aluminum component lifetimes. To this end, we develop and apply a molecular dynamics (MD) modeling framework for conducting tension tests that is capable of isolating factors governing the mechanical strength as a function of coating chemistry, defect morphology, and variables associated with the loading path. We consider two representative materials, including γ-Al 2 O 3 and γ-Al(OH) 3 (i.e., oxide and hydroxide), both of which form readily as aluminum surface coatings. Our results indicate that defects have a significant bearing on the strength of aluminum oxide, with grain boundaries serving to reduce the strain at failure from ε zz = 0.300 to 0.219, relative to perfect single crystal. Our simulations also predict that porosity lowers the elastic stiffness and yield strength of the oxide. Relative to perfect crystal, we find porosity factors of 5%, 10% and 20% decrease the yield stress by 26%, 36% and 53%, respectively. MD predicts that perfect hydroxide and oxide single crystal have respective strains at failure of 0.08 and 0.31 under tensile uniaxial strain loading, and that the corresponding yield stresses are respectively 1.6 and 11.1 GPa. These data indicate that the hydroxide is substantially more susceptible to mechanical failure than the oxide. Our results, coupled with literature findings that indicate hot and humid conditions favor formation of hydroxide and defective oxide coatings, indicate the potential for a complicated dependence of aluminum corrosion susceptibility and stress corrosion cracking on aging history.

36 MATERIALS SCIENCE↗

Nb 2 O 5 Protection Layers for Hydrogen Evolution by p-InP Photocathodes in Acidic Electrolytes

Coatings of HfO 2 , Ta 2 O 5 , TiO 2 , and Nb 2 O 5 were evaluated as protection layers for p-InP photocathodes in aqueous acidic electrolytes. Each candidate protection layer was characterized based on interfacial conduction of photogenerated electrons, the thermodynamic and kinetic stability of the overlayer over the relevant potential and pH range for cathodic fuel-forming half-reactions, and inhibition of the primary anodic and/or chemical dissolution processes that limit electrode stability. The conduction of photogenerated electrons and inhibition of anodic oxidation was evaluated using V 3+ / 2+ in 5.0 M HCl(aq) as a one-electron redox couple with a potential close to that of hydrogen evolution in acidic media. Failure modes due to cathodic plating of metal, as well as anodic dissolution and chemical dissolution processes, were evaluated for photocathodes made from etched p-InP, platinized p-InP, and p-InP photoelectrodes that had been coated with the various oxide films and then platinized for use in photoelectrochemical hydrogen evolution in acidic aqueous electrolytes. Nb 2 O 5 best met all of the criteria, contrasting with TiO 2 , which is thermodynamically and kinetically unstable in acid over the potential range relevant for the hydrogen evolution and/or CO 2 reduction electrochemical half-reactions. Furthermore, these protocols should be useful for other materials and semiconductors to determine the effectiveness of protection layers for photocathodes.

Electrodes↗

An Oxygen‐Scavenger Sulfide Coating Enabling Long‐Term Stable Nickel‐Rich Cathodes

Oxygen release is a major issue associated with layer-structured metal oxide cathodes in lithium batteries, which can further cause a series of problems, such as irreversible phase transition, microcracking, and electrolyte decomposition. Eventually, these issues jointly result in cell performance degradation and safety hazards. Thus, it is very significant to tackle oxygen release for achieving long-term stable cyclability, but very challenging. Although intensive efforts have been invested to date, there still lacks a feasible solution. In this study, nanoscale ZrS 2 coatings are applied on prefabricated LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) cathodes directly via atomic layer deposition (ALD). Very encouragingly, we reveal that this ALD-deposited conformal ZrS 2 nanocoating can serve as an exceptional oxygen scavenger and then convert into a stable sulfate (Zr(SO 4 ) 2 ) coating. Such an in situ conversion is very beneficial and effective for protecting the electrolyte from decomposition. In addition, the resultant Zr(SO 4 ) 2 coating further inhibits undesirable reactions, stabilizes the interface between NMC811 and the electrolyte, suppresses microcracking, mitigates transition metal dissolution, and maintains the structural stability of the NMC811 cathode. Consequently, the ZrS 2 -coated NMC811 cathode has demonstrated extraordinary performance. Thus, this study advances the understanding of interface engineering while paving a new technical pathway for commercializing NMC811 cathodes.

Nickel-rich cathodes↗

Stoichiometric effects on grain growth in zirconium carbide coatings for high-temperature nuclear fuel

Interest in coated particle fuel for space nuclear propulsion (SNP) has expanded in recent years due to successful demonstrations of the resiliency of the coatings to extreme environments. For SNP applications, the coating layer for the particle design needs to be able to withstand exposure to high temperature hydrogen during operating conditions. ZrC has been proposed as a protective layer, however, it is important to understand the high temperature behavior to ensure adequate protection to this fuel. In this study, surrogate ZrC coated particles were heat treated at 1900 °C up to 300 min, to examine how the microstructure evolves when exposed to high temperature. Scanning electron microscopy and electron backscatter diffraction (EBSD) were conducted to determine grain size and grain boundary character and orientation to determine the degree of change in the ZrC layer post heat treatment. Raman spectroscopy provided insight to understand how the as-fabricated stoichiometry of each sample contributed to the differences in grain growth behavior. Despite the as-fabricated samples showing a similar initial grain size and grain boundary character, the samples with a higher amount of excess carbon exhibited smaller grain areas and slower growth rates when exposed to 1900 °C. In conclusion, this investigation details the as-fabricated microstructure of the ZrC layer, specifically grain size, evolved under high temperature as this can impact the performance of the fuel under operating conditions.

EBSD↗