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NASA NTRS1988

Molten-salt corrosion of silicon nitride. I - Sodium carbonate. II - Sodium sulfate

An experimental study of the corrosion of Si3N4 under thin films of Na2CO3 at 1000 C has been conducted using both pure Si3N4 and Si3N4 with various additives. The reaction mechanism is shown to consist of: (1) the decomposition of Na2CO3 and the formation of Na2SiO3; (2) rapid oxidation; and (3) the formation of a protective silica layer below the silicate. In the second part, the corrosion mechanism of Si3N4 + Na2SO4/O2 at 1000 C was studied for both pure and additive-containing Si3N4. The reaction of Si3N4 + Na2SO4 was found to involve an initial period of slow weight loss (due to Na2SO4 vaporization and oxidation-dissolution) followed by further oxidation or the near termination of the reaction, depending on the Si3N4 additive.

Fox, Dennis S.↗

NASA NTRS2017

Water Vapor Corrosion in EBC Constituent Materials

Environmental Barrier Coating (EBC) materials are sought after to protect ceramic matrix composites (CMC) in high temperature turbine engines. CMCs are particularly susceptible to degradation from oxidation, Ca-Al-Mg-Silicate (CMAS), and water vapor during high temperature operation which necessitates the use of EBCs. However, the work presented here focuses on water vapor induced recession in EBC constituent materials. For example, in the presence of water vapor, silica will react to form Si(OH)4 (g) which will eventually corrode the material away. To investigate the recession rate in EBC constituent materials under high temperature water vapor conditions, thermal gravimetric analysis (TGA) is employed. The degradation process can then be modeled through a simple boundary layer expression. Ultimately, comparisons are made between various single- and poly-crystalline materials (e.g. TiO2, SiO2) against those found in literature.

coating↗

DOE OSTI2026

Cathodic Protection Modeling for Hanford Underground Double-Shell Tank Farms

Hanford stores millions of gallons of radioactive and chemically hazardous waste from the production of weapon materials in tank farms consisting of underground carbon-steel storage tanks surrounded by reinforced concrete. Six of these Hanford tank farms use double-shell storage tanks (DSTs). The DST farms were constructed from 1968 to 1986 with a planned 40–50 year design life, so some are already operating beyond their initial life expectancy. Ultrasonic testing (UT) has indicated significant thinning on the bottom of the secondary (outer) liner of these tanks, believed to arise from groundwater intrusion driving concrete side corrosion. There is no direct access to the steel/concrete interface between the tank and the concrete pad, making it difficult to apply a chemical-based mitigation strategy or to conduct repairs, but cathodic protection (CP) is a possible method to inhibit further concrete-side corrosion. Hanford already uses CP to protect below grade steel piping within the tank farms and connected to the tanks, but this system was not designed to protect the tank bottoms. CP design must account for the structures surrounding the DSTs, including the steel reinforcing bars (rebar) within the concrete pad and vault, various process lines, and the existing CP system. In this study, finite element analysis (FEA) modeling was carried out to simulate CP protection of 1) a single tank and CP anode to develop options for modeling the rebar and to compare to a simpler circuit model and 2) the entire Hanford AN tank farm as a representative example consisting of seven tanks, associated piping, and both existing and new CP anodes. Both circuit and FEA models predict that significant protective current could be delivered to the bottoms of the tanks with the addition of tank-protection anodes below the depth of the tanks. Simulations with only the existing pipe-protection anodes active confirmed that only a very small current to the tank bottoms is predicted under present conditions. Multiple simplified representations of the dome and wall rebar were tested to reduce the computational complexity of the tank-farm simulations, resulting in modeling the rebar as edge elements with a prescribed effective circumference that matches the real rebar surface area. The geometry of the rebar is also simplified into horizontal hoops around the tank walls and radial rebar over the dome with increased effective circumference to retain the target surface area. This simplification was found to greatly reduce the complexity and solution time of the models without large changes in current distributions, especially to the tank bottom. A range of values were tested for model parameters such as soil and concrete resistivities and polarization resistance to investigate their impact on the current and electric potential distributions. Depending on the parameters used, FEA simulations predict some risk of overprotection, particularly on the piping system; since overprotection can also lead to surface damage associated with hydrogen gas generation at the interface (e.g. hydrogen embrittlement or damage to coatings), this needs to be considered when refining the design of the new CP system. Comparison between the FEA models and the circuit model representation demonstrated that the circuit model could not match the predicted FEA current distribution, even when using the exact same surface areas. This discrepancy appeared to be at least partly attributable to the impact of the relative positions of the tank components and anodes to each other and to the ground surface. The FEA model accounts for the relative positions since it solves the governing equations in three dimensions, but the circuit model cannot account for the positioning. In particular, the circuit model underpredicts the current to the tank bottom and overpredicts the current to the dome compared to FEA for the baseline geometry. The FEA models omitted the electrically isolated rebar in the bottom concrete slab. However, a circuit based stray current model estimated that only 2.1% of the total current through the slab would stray into the rebar, corresponding to ~0.21 A for a target current density of 2 mA/ft2 to the tank bottom. The estimated corrosion driven by this amount of stray current is predicted to yield a lifetime of >400 years for the minimum rebar diameter, assuming an acceptable cross-section area loss of 10%.

d'Entremont, Anna [Savannah River National Laborat↗

DOE OSTI2021

Galvanic Transformation Dynamics in Heterostructured Nanoparticles

Corrosion is a significant problem for the stability of structural metals and potentially for functional nanomaterials in operating environments. When two metals with different electrochemical potentials form a junction, galvanic corrosion occurs, resulting in the sacrificial dissolution of the metal with a higher oxidation potential (lower electrode potential). In this report it is shown that bimetallic hetero-nanostructures composed of phase-segregated metals undergo galvanic corrosion in aqueous environments. Such selective etching of the sacrificial metal in heterojunction particles leads to the formation of unusual and kinetically stabilized half-spheroid particles. By using a fluid cell and in situ scanning transmission electron microscopy, a two-stage corrosion process can be observed where the Cu experiences a fractal breakdown before the Ag corrodes due to the lack of a protective oxide layer. However, when treated with a mild Ar plasma, the stability of these structures against corrosion is enhanced due to the conversion of the amorphous native oxide to a denser, thin layer of CuO on the Cu surface. Taken together, this work highlights the importance of considering the effects of galvanic corrosion on the stability of multicomponent nanoparticles, and it shows how mass transport in a nanoscale system is influenced by redox processes.

36 MATERIALS SCIENCE↗

NASA NTRS2021

Astro-biological Exploration of Ocean Worlds, Enabled by an RPS Inside a Pressure Vessel

Exploring Ocean and Ice Worlds could help us to understand the origin and evolution of life in the universe. In our solar system we have identified six Ocean and Ice Worlds, namely Earth, Europa, Ganymede, Callisto, Enceladus, and Titan. Other potential targets include Dione, Triton, and Pluto. As documented in the Planetary Decadal Survey [1] and the NASA Roadmap to Ocean Worlds [2], these worlds are compelling science destinations, with oceans situated below their tens of kilometers thick ice shells. To reach them we need a new exploration paradigm with novel technological solutions. Key technological challenges revolve around the power for the probe and for melting, as well as protecting the payload against the extreme environments, including high pressure, low temperature, corrosion, and radiation. Far away from the Sun, and melted into the ice, we may only rely on long-lived internal power generation. Radioisotope Power Systems (RPS) with either static or dynamic conversion, utilizing the heat of decaying Plutonium-238, could be good candidates. We need suitable payloads that are protected and could survive the extreme environments, as well as enabling power and thermal systems for melting through the ice shield and to swim in the ocean below the ice. RPS could support the probe’s instruments and sub-systems, as well as provide a heat source for melting the ice while keeping the components at operating temperatures. Mitigating the external pressure while immersing inside the ice shell, and in the ocean, would require a new RPS design that operates inside a Pressure Vessel. In our paper, we will discuss general mission architecture trades and the sizing of a next generation RPS housed in a pressure vessel, broadly applicable to any of the Ocean Worlds satellites of interest. Through a technology focused approach, we address interconnected design and mission architecture aspects, including considerations for: the RPS and the Pressure Vessel; extreme environmental constraints; g-load tolerance; power and thermal systems sizing for science measurements; spacecraft operations through all mission phases; subsurface mobility; and planetary protection. The findings will inform the science community on instrument accommodation possibilities; the mission planning community on possible mission concepts; and the RPS development community on the science driven technology considerations.

Donitz, Benjamin P.↗

NASA NTRS1981

Oxidation and hot corrosion of coated and bare oxide dispersion strengthened superalloy MA-755E

Cyclic hot corrosion and oxidation of an experimental oxide dispersion strengthened (ODS) superalloy MA-755E were conducted in a hot gas stream at Mach 0.3. The response of the ODS alloy, bare or with protective coatings, was similar to that of a conventional cast alloy, IN-792, in hot corrosion at 900 C. However, during oxidation at 1100 and 1150 C the ODS alloy differed from the cast alloy by developing a greater amount of subsurface porosity. Compared with a diffused aluminide coating, an electron beam vapor deposited NiCrAlY coating offered superior oxidation protection and decreased porosity formation. In additional testing, the tendency to form porosity was associated with the large grains of recrystallized powder metallurgy alloys but was independent of the presence of an oxide dispersion.

Glasgow, T. K.↗

DOE OSTI2021

High-temperature corrosion of a nickel-based alloy in a molten chloride environment – The effect of thermal and chemical purifications

There is currently an ever-increasing demand for higher process efficiencies in next generation (Gen3) concentrating solar power (CSP). Higher process efficiencies may be procured by increasing the operating temperature, and simultaneously, minimizing the degradation of materials used for construction of CSP plants (e.g., piping, thermal storage tanks, solar receivers and heat exchangers). Thus, understanding materials corrosion in the presence of molten salt mixtures used as thermal energy storage media and heat transfer fluids is indispensable for CSP development. The present paper provides insights into the effects of salt purification on the corrosion of a nickel-based alloy (Haynes 230) isothermally exposed to a stagnant chloride-based salt mixture at 800 °C. The MgCl 2 -based salt mixture was thermally dehydrated and chemically treated with (0.1 and 0.5 wt %) elemental magnesium. Results reveal the electrochemical nature of the corrosion process, and the formation of corrosion products such as oxides (MgO, MgCr 2 O 4 , and MgAl 2 O 4 ) and nitrides (CrN) on the alloy surface and in sub-surface regions. Magnesium additions enhanced the ability to resist corrosion by reducing the concentration of impurities (H 2 O, MgOH + , OH - species) and polarizing the alloy surface. The formation of nitrides in all cases studied indicates the impact of using nitrogen as a protective gas in the system. Results also reveal that a single step treatment of the salt using metallic Mg could be considered as a measure to control the salt's impurity level, e.g., if required for system control.

14 SOLAR ENERGY↗

NASA NTRS2019

Pre-Demonstration Development of Controlled-Release Corrosion Inhibitors and Healing Agents as Alternatives to Hexavalent Chromium

This Limited Scope Study was directed to achieve the following objectives: (1) Scale-up of materials that can meet MIL-PRF-23377 (solvent-based primer). (2) Provide evidence of resistance to aircraft alkaline cleaners and de-icing fluids. (3) Provide formulation for initial ecological and toxicity screening. (4) Submit an interim report that will provide the basis for a future ESTCP (the Dept. of Defense's (DoD's) Environmental Security Technology Certification Program) demonstration effort.The encapsulation procedure for two corrosion inhibitors was scaled up from lab scale to 2.0 kilograms. This scale will accommodate high volume production of coatings with encapsulated corrosion inhibitors for large surface areas during a follow-on ESTCP demonstration effort. Test results provided evidence of resistance to alkaline cleaners and aircraft de-icing fluids and compliance with MIL-PRF-23377. All the MIL-PRF-23377 requirements were met with the exception of the adhesion requirement, in top coated panels, and the flexibility requirement. Work on solving these two problems will be done prior to validation and demonstration of the technology. An initial ecological and toxicity screening identified several factors that were not critical to the acceptance of the encapsulated corrosion inhibitor. This new technology will lead to environmentally friendly alternatives to hexavalent chromium that will enable DoD to protect its assets. Field demonstration, licensing, qualification, and commercialization will allow its real world utilization. Abstract for Appendix A. Toxicology Report: Corrosion controls a significant problem for military equipment. Many surface treatment materials currently in use on items of military or aerospace materiel contain chromium (VI) as a component, a source of significant human health and environmental hazard. The formulation under evaluation contains no chromium. Most of the proposed components are low to moderate toxicity and are not a significant concern. Two of the formulation components are associated with some cancer hazard - 2-mercaptobenzothiazole and formaldehyde, but both find widespread use in industry and additional investigation is not required for this project.

Calle, Luz Marina↗

DOE OSTI2025

Ab Initio Insights to Metal Passivation: Diffusion and Defect Formation in Amorphous Zirconia and Alumina

Metal passivation refers to the formation of protective oxide films on metals, which shield them from further corrosion and oxidation, playing a crucial role in maintaining their stability. The mesoscopic Point Defect Model has successfully predicted passivity as a steady state process where oxide growth from oxygen vacancies at the metal/film interface competes with oxide dissolution at the film/environment interface. In this work, informed by the Point Defect Model parameters, we use first-principles calculations to calculate defect formation and atomic diffusion in amorphous materials and correlate these descriptors with the behavior and growth of the oxide film. Focusing on amorphous zirconia and alumina, we demonstrate that defect formation energies exhibit significant variability in amorphous systems. In alumina, vacancies dominate, with cation and anion vacancies occurring at comparable concentrations. Diffusion calculations for stoichiometric amorphous alumina and zirconia, as well as oxygen-deficient zirconia, reveal faster diffusion in the oxygen-deficient case, highlighting the impact of defects on transport. Comparison of calculated self-diffusion coefficients for the dominant defect species with experimentally measured oxide thicknesses shows a clear correlation, suggesting that first-principles-derived diffusivity information can serve as a key descriptor for surface passivation film growth.

Farnell, Mackinzie S. [University of California, B↗

NASA NTRS1995

Bondable Stainless Surface Coats Protect Against Rust

Report describes tests conducted to assess use of bondable stainless surface (BOSS) coating materials to protect steel cases of solid-fuel rocket motors against corrosion and to provide surface microstructure and chemistry suitable for bonding to insulating material. Eliminates need to cover cases with grease to prevent corrosion and degreasing immediately prior to use.

Davis, G. D.↗

NASA NTRS2018

The Effectiveness of a NiCrY-Coating on a Powder Metallurgy Disk Superalloy

Protective ductile coatings could be necessary to mitigate oxidation and corrosion attack on superalloy disks in some turbine engine applications. However, the effects of coatings on fatigue life of the disk during service are an important concern. The objective of this study was to investigate how such a coating could perform after varied post-coating processing. Cylindrical gage fatigue specimens of powder metallurgy-processed disk superalloy LSHR were coated with a NiCrY coating, shot peened, preparation treated, exposed, and then subjected to fatigue at high temperature. The effects of varied shot peening, preparation treatment, and exposures on fatigue life with and without the coating were compared. Each of these variables and several of their interactions significantly influenced fatigue life.

ductile coatings↗

DOE OSTI2022

High Temperature Ternary Chloride Molten Salt Pump

This work investigates the design criteria considering thermal, structural, and mate-rial selection of a ternary chloride (MgCl2-NaCl-KCl) molten salt pump that is capable of running at temperatures above 720 °C. In this work, preliminary testing of salt-wetted hydrodynamic bearings was done to investigate different material pairings including colmonoy grades, stellite grades, and a novel NiWC-based alloy (i.e. HybrimetTM NiWC3b) used as a High Velocity Ox-ygen Fuel (HVOF) coating. The coating has shown to withstand the corrosive nature of the salt, and is additionally used to protect a 316L stainless steel pump reservoir. The pump wetted components are made of Inconel 625, and it features a carbon ring seal developed by Flows-erve flooded with a N2 gas flow on the overhead to keep salt vapors from interacting with the external ambient air. This research showcases a promising design for use in the CSP Gen 3 liquid-pathway and sets the ground for further development and use of the HybrimetTM NiWC3b as a competitive alternative to available superalloys. Further work will further characterize the pump by performance & cycle testing in molten salt at higher temperatures.

14 SOLAR ENERGY↗

NASA NTRS1974

Coatings for directional eutectics

Eleven coating systems based on MCrAlY overlay and diffusion aluminide prototypes were evaluated to determine their capability for protecting the gamma/gamma prime-delta directionally solidified eutectic alloy (Ni-20Cb-6Cr-2.5Al) in gas turbine engine applications. Furnace oxidation and hot corrosion, Mach 0.37 burner-rig, tensile ductility, stress-rupture and thermomechanical fatigue tests were used to evaluate the coated gamma/gamma prime-delta alloy. The diffusion aluminide coatings provided adequate oxidation resistance at 1144 K (1600 F) but offered very limited protection in 114 K (1600 F) hot corrosion and 1366 K (2000 F) oxidation tests. A platinum modified NiCrAlY overlay coating exhibited excellent performance in oxidation testing and had no adverse effects upon the eutectic alloy.

Felten, E. J.↗

DOE OSTI2021

A percolation theory for designing corrosion-resistant alloys

Iron-chromium and nickel-chromium binary alloys containing sufficient quantities of chromium serve as the prototypical corrosion-resistant metals owing to the presence of a nanometre-thick protective passive oxide film. Should this film be compromised by a scratch or abrasive wear, it reforms with little accompanying metal dissolution, a key criterion for good passive behaviour. This is a principal reason that stainless steels and other chromium-containing alloys are used in critical applications ranging from biomedical implants to nuclear reactor components. Unravelling the compositional dependence of this electrochemical behaviour is a long-standing unanswered question in corrosion science. Herein, we develop a percolation theory of alloy passivation based on two-dimensional to three-dimensional crossover effects that accounts for selective dissolution and the quantity of metal dissolved during the initial stage of passive film formation. We validate this theory both experimentally and by kinetic Monte Carlo simulation. Our results reveal a path forward for the design of corrosion-resistant metallic alloys.

36 MATERIALS SCIENCE↗

NASA NTRS2000

Characterization of Molybdate Conversion Coatings for Aluminum Alloys by Electrochemical Impedance Spectroscopy

Electrochemical impedance spectroscopy (EIS) was used to investigate the corrosion inhibiting properties of newly developed proprietary molybdate conversion coatings on aluminum alloy 2024-T3 under immersion in aerated 5% (w/w) NaCl. Corrosion potential and EIS measurements were gathered for six formulations of the coating at several immersion times for two weeks. Nyquist as well as Bode plots of the data were obtained. The conversion-coated alloy panels showed an increase in the corrosion potential during the first 24 hours of immersion that later subsided and approached a steady value. Corrosion potential measurements indicated that formulations A, D, and F exhibit a protective effect on aluminum 2024-T3. The EIS spectra of the conversion-coated alloy were characterized by an impedance that is higher than the impedance of the bare alloy at all the immersion times. The low frequency impedance, Z(sub lf) (determined from the value at 0.05 Hz) for the conversion-coated alloy was higher at all the immersion times than that of the bare panel. This indicates improvement of corrosion resistance with addition of the molybdate conversion coating. Scanning electron microscopy (SEM) revealed the presence of cracks in the coating and the presence of cubic crystals believed to be calcium carbonate. Energy dispersive spectroscopy (EDS) of the test panels revealed the presence of high levels of aluminum, oxygen, and calcium but did not detect the presence of molybdenum on the test panels. X-ray photoelectron spectroscopy (XPS) indicated the presence of less than 0.01 atomic percent molybdenum on the surface of the coating.

Calle, Luz Marina↗

DOE OSTI2020

Progress in Understanding the Origins of Excellent Corrosion Resistance in Metallic Alloys: From Binary Polycrystalline Alloys to Metallic Glasses and High Entropy Alloys

Some of the factors responsible for good corrosion resistance of select polycrystalline and emerging alloys in chloride solutions are discussed with a goal of providing some perspectives on the current status and future directions. Traditional metallic glass alloys, single phase high entropy alloys (HEAs), early metallic glasses, and high entropy metallic glasses are all emerging corrosion-resistant alloys (CRAs) that utilize traditional strategies for improved corrosion resistance as well as take advantage of some other novel beneficial attributes. These materials enjoy many degrees of freedom as far as choice of both composition and structure, providing great flexibility in the pursuit of superior corrosion resistance. The new materials depart from classical solvent-solute type polycrystalline binary or ternary alloys. Thus, such emerging materials provide significant opportunities to achieve even greater improvements in corrosion resistance in harsh environments. Several examples of the unique corrosion properties of selected materials in the context of modern theories of corrosion are discussed herein. Discussion is restricted to solid-solution binary or ternary polycrystalline alloys, several metallic glass alloys, and single phase HEAs. A common feature of many CRAs is that composition and microstructure often affect both passivity and resistance to localized corrosion that can be divided into initiation, stabilization, and propagation stages. Enormous complexities in protective oxide structures and chemistries and the large number of combinatorial possibilities in newer materials such as HEAs preclude trial-and-error approaches and perhaps even combinatorial experimental design. Computational materials methodologies will be required in the search for new corrosion-resistant alloys in these material classes. The search must consider the best scientific insights available regarding how major and minor alloy additions, as well as various microstructural attributes, contribute to corrosion mitigation. Additional scientific insights, as they emerge, will enable choices beyond the reliance on high concentrations of alloying elements that are known to affect passivity breakdown and pit stabilization. A challenge is to connect the “basic attributes” of an alloy with its properties. The strength of this connection will likely require new scientific principles enabling deep multiphysics insights in order to link feature(s) such as composition and metallurgical phases to the desired corrosion properties. Application of data informatics will likely also play a role given the plethora of variables that are important in corrosion and the difficulty in assessing all relationships. Here, the opportunity exists to accelerate the design of emerging materials for high corrosion resistance.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Constructing Highly Durable Fuel Cell Catalysts Through Integrating Graphitic Shell‐Protected Composite Carbon Support with Gaseous Co Deposition‐Driven PtCo Intermetallics

Metal dissolution, nanoparticle agglomeration, and carbon support corrosion cause significant performance degradation of current PtCo catalysts under acidic and oxidative oxygen reduction reaction. Here, in this study, an integrated strategy is presented to design high-performance Pt 3 Co intermetallic catalysts by regulating gaseous Co deposition-driven diffusion into Pt nanoparticles supported on a composite carbon. The composite carbon is derived from ZIF-8/polyaniline, consisting of a high-surface-area (HSC) core and a protective graphitic shell (GS), which is employed to design 40 wt.% Pt/HSC@GS catalyst. The corresponding membrane electrode assemblies (MEAs) can maintain 1.09 A cm −2 at 0.7 V (20. 7% loss) after 10 000 cycles (1.0–1.5 V for carbon stability) and 1.15 A cm −2 (16.1% loss) after 150 000 cycles (0.60–0.95 V for catalyst stability). A ordered Pt 3 Co intermetallic is synthesized via a gaseous Co-deposition process, which yields a homogeneous Co-rich layer onto the Pt nanoparticles on the composite support, thereby facilitating Co diffusion into Pt crystal during subsequent ordering annealing to form the ordered intermetallic structure. This gaseous deposition leads to a thin carbon layer on PtCo nanoparticles, inhibiting particle growth during the annealing and mitigating Co dissolution under dynamic electrochemical conditions. The PtCo catalyst achieves impressive MEA performance and long-term durability (1.45 A cm −2 at 0.7 V after 120 000 cycles) under heavy-duty conditions.

30 DIRECT ENERGY CONVERSION↗

NASA NTRS1996

Corrosion of Mullite by Molten Salts

The interaction of molten salts of different Na2O activities and mullite is examined with furnace and burner tests. The more-acidic molten salts form small amounts of Al2O3; the more-basic molten salts form various Na2O-Al2O3-SiO2 compounds. The results are interpreted using the Na2O-Al203-SiO2 ternary phase diagram, and some possible diffusion paths are discussed. The generally higher melting points of Na2O-Al2O3-SiO2 compounds lead to better behavior of mullite in molten salts, as compared to SiO2-protected ceramics such as SiC. Mullite-coated SiC is discussed, and the corrosion behavior is evaluated.

Jacobson, Nathan S.↗