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DOE OSTI2021

Microstructure Investigation and Mechanical Properties of Coated Zircaloy Cladding

Accident Tolerant Fuel concepts have been developed and tested in diverse research programs presently around the world. Industry teams have developed proprietary coating compositions and geometries, but significant knowledge gaps exist in terms of the resulting properties of the coating and the cladding and how those components impact each other in reactor conditions. Furthermore, the national laboratory and university teams currently studying the industry concepts are limited in their ability to freely disseminate and discuss results obtained on commercial coatings. The Advanced Fuels Campaign is therefore working to develop an understanding of ‘generic’ coatings applied to commercial nuclear cladding alloys free of these constraints. This milestone report provides insights in the microstructure of a 7-micrometer Cr coating on Zircaloy-2 and a 5- micrometer coating on Zry-4 as reference materials. SEM and TEM methods were utilized to describe and identify the interface, while nanoindentation was used to determine hardness and E-Moduli of coating and cladding material. This milestone summarizes the acquired knowledge to build a necessary verified foundation for future simulation and qualification efforts.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Development of Standardized Property Requirements, Measurement Methods, and Reporting Guidance for Coatings

The diverse research programs presently in progress around the world have advanced a large number of coated cladding concepts to various stages of maturity. Industry teams have developed leading coating compositions and geometries, but significant disparity exists in the importance placed on different coating properties, as well as the applicability and standardization of the various methods used to measure these properties. This milestone report provides an initial assessment of the most important coating properties and the experimental methods available for their determination to lay the foundation for standardized reporting and development of comprehensive datasets for modeling efforts. This report has determined that the residual stress of the coating is the most crucial property to investigate, yet it has received minimal attention to date due to a knowledge gap about the growth and formation of the brittle Laves phase under reactor conditions. The significance of residual stress of the coating is further enhanced by its connection and interdependence with other important properties like creep and coating failure mechanisms. This milestone proposes an importance rating for residual stress properties and their associated measurement techniques to fill in knowledge. Furthermore, techniques to investigate the outlined properties are discussed, and their capabilities and limitations are illustrated to provide guidance on their use.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

High Temperature Thermal Barrier Coating Evaluation of Yttrium Aluminum Garnet for Gas Turbine Applications

The Solution Precursor Spray Process (SPPS) process has been shown to overcome the durability and property challenges of applying yttrium aluminum garnet (YAG) coating for high temperature thermal barrier coating (TBC) applications (1200°C+) but only limited testing has been performed in representative application environments. In this study, YAG coatings were developed to optimize microstructure and tailor properties for combustion components in an industrial gas turbine. Thermal conductivity, erosion resistance and furnace cycling durability were used to validate YAG properties against the standard yttria-stabilized zirconia coating (YSZ). Graded and multi-layered microstructures were applied to enhance performance while maintaining durability. Further YAG process development was required to replicate coating properties and optimize deposition on more complex fuel injector nozzle and combustion liner components. Rig testing of both components was performed and compared against the baseline YSZ coating validating the high temperature capability and lower thermal conductivity of the SPPS YAG coating. The components in both tests were cycled for a minimum of ten cycles with the fuel injector test targeting a higher operating temperature while the combustor liner operated at standard conditions. A development engine test is planned to further validate performance in a gas turbine engine of this promising material.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Enhancing Steam-Side Heat Transfer via Microdroplet Ejection using Inorganic Coatings

During condensation of water on a superhydrophobic nanostructured surfaces, droplets coalesce and jump (droplet ejection) due to the release of excess surface energy. Meticulously designed nanostructured surfaces or coatings capable of droplet ejection can enhance heat transfer performance by easy removal of droplets during condensation. In the present work, the capabilities of the Nelumbo droplet ejection coatings technology currently used in commercial heat exchangers are explored and optimized for materials and conditions relevant to steam condensers. Specifically, this includes (1) adapting and optimizing the procedures and chemistries to deposit droplet ejecting coatings on materials used in the steam condenser, (2) testing of the heat transfer, durability, and fouling of the fabricated coatings under a variety of steam condenser relevant conditions, and (3) modeling of the impact of droplet dynamics and interfacial properties on heat transfer in steam condensers. We experimentally demonstrated that at low supersaturation conditions (S~1.02), developed superhydrophobic nanostructured surface gives a 40% higher peak heat transfer flux and a 17% higher peak overall heat transfer coefficient (U) with droplet ejection mechanism compared to the dropwise condensation mechanism on the same nanostructured surface. Though the experimentally observed droplet ejection mechanism was short-lived (~3 min) due to the limitation of the chiller to maintain a constant supersaturation condition in fabricated steam condenser. And large variations in water inlet temperature (+ to - 2 degrees C) caused flooding of nanostructure (Wenzel state) at higher supersaturation (S > or = 1.12). This is an important finding because typical supersaturation levels in field operation are over 1.8 and as such, either the flooding potential for these materials should be improved or operation at lower supersaturation may be required to maximize heat transfer efficiency. If supersaturation conditions can be maintained reliably in the steam condenser in addition to droplet ejection mechanism during condensation, this could provide a potential 2% reduction in water flow rate which equates to a savings of over 3900 gallons of water per minute for a 500 MW steam turbine and over $0.3MM savings annually given a 0.02 cent marginal water withdrawal cost. It is also worth noting that these savings are based on improvement of droplet ejection coatings over coatings capable of performing consistent dropwise mechanism in in-field surface condensers. Savings due to the droplet ejections coatings when compared to bare substrates could be much higher. Additionally, the present work provides the importance of steam condenser operating conditions and insights into the challenges in modeling the condensing droplet dynamics on surfaces.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2022

Ultra-High Temperature Thermal Barrier Coating Development and Validation

The most effective method to improve industrial gas turbine power is to increase firing temperature. To maintain component durability at these higher temperatures, thermal barrier coatings (TBC’s) are playing an increasing role in protecting turbine hardware. TBC’s have been successfully used on Solar Turbines’ combustor liners and turbine airfoils, but there is a need for TBC’s that can operate at higher temperatures. Based on recent, favorable rig testing experience, Solar recognized that yttrium aluminum garnet (YAG) TBC’s made by the Solution Precursor Plasma Spray Process (SPPS) has great potential for higher turbine temperatures. This testing verified the thermal cycle durability of the SPPS YAG TBC’s, as well as demonstrated that the temperature drop through the SPPS YAG TBC was twice that measured across a companion APS YSZ TBC. The SPPS YAG TBC with the potential for a 200°C improvement in temperature capability represents a materials breakthrough. The SPPS process also produces a number of unique microstructural features that confer superior properties. SPPC TBC’s have ultra-fine splats that increase toughness and erosion resistance, and the process can be tailored to produce through-thickness cracks for strain-tolerance and control porosity for lower thermal conductivity and increase coating abradability. This proposal would include further development of SPPS YAG density-graded coatings, optimization of the application process, and validation of higher temperature capability and durability through rig and engine testing of coated combustion liners and turbine outer air seals. The technology would be advanced from a TRL 3 to a proposed TRL 6 by overcoming processing concerns on efficiency, application distance and optimization of a graded coating without impacting coating durability by demonstrating the coating performance on components in rig and development gas turbine engine testing.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Temperature-Following Thermal Barrier Coatings for High Efficiency Engines (Final Report)

HRL Laboratories and General Motors (GM), pursued this effort to increase the efficiency of internal combustion engines (ICEs) by developing and implementing temperature-following thermal barrier coatings (TBCs) to decrease heat loss from the combustion chamber. HRL developed microsphere TBCs based on hollow high-temperature alloy spheres with average diameter of 50 μm and wall thickness ~1 μm (microspheres) that achieve unprecedented low thermal conductivity and heat capacity (10X lower than the state of the art) while offering exceptional environmental and mechanical resistance.> In current ICEs, approximately 29% of the fuel’s energy is lost to the cooling system and about 22% goes into moving the car. By limiting heat losses from the combustion chamber with insulating coatings, fuel energy can be redirected into additional piston work and into the exhaust stream. The additional energy that goes into the exhaust stream can be turned into useful work through the use of an exhaust energy recovery device, such as turbocompounding and/or through driving a turbocharger to increase the power density of the engine allowing downsizing. Insulating coatings for piston crowns have been pursued in the past, but previous materials—typically ceramics—exhibited low thermal conductivity but retained high heat capacity. Such materials reduce heat losses but stabilize at a high surface temperature. The high surface temperature heats the incoming gases, which lowers volumetric efficiency and increases propensity for knock, resulting in degraded engine performance. This program developed an innovative new material that combines low thermal conductivity with low heat capacity. These unique properties allow it to follow rapid changes in gas temperature during each combustion cycle. A metallic microsphere TBC has been demonstrated that exhibits increased surface temperature during the combustion period, resulting in reduced heat transfer losses, while still returning to a low surface temperature during the gas exchange period. A 10X lower thermal conductivity and heat capacity than state-of-the-art thermal barrier coatings has been demonstrated. These unprecedented thermal properties are achieved through the coating architecture, which consists of closed pores on the microscale and exhibits a total porosity of 90% to 95%. By selecting a high-temperature nickel alloy as the coating material, the ductility and strength of metals can be harnessed to achieve much better durability and damage tolerance than brittle ceramic coatings can achieve.

33 ADVANCED PROPULSION SYSTEMS↗

DOE OSTI2021

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 OSTI2022

In-situ optical monitoring of gas turbine blade coatings under operational extreme environments

High temperature material systems consisting of thermal barrier coatings and the underlying superalloys are key to achieving higher gas temperatures which in turn control engine efficiencies and reduce emissions. With engine temperatures in excess of the limits that metallic blades and vanes can endure, advanced monitoring techniques that ensure the integrity and durability of these coatings are paramount to continuous and safe operation. Optical methods have the benefit of being non-invasive and are able to capture data under limited access available for monitoring the hot-section of turbines. Addressing Topic 5 on Advanced Instrumentation, the research and development effort for this project titled “In situ optical monitoring of gas turbine blade coatings under operational extreme environments” was completed by University of Central Florida researchers, including Raghavan (PI) and Ghosh (co-PI). In this project, the research team leveraged intrinsic properties of coatings and rare-earth dopants as active and intelligent “sensors” through their optical properties. The outcomes of this project pave the way for diagnostics of turbine blade coatings, under operating environments, through the development of the sensing thermal barrier coating configurations, calibration and associated instrumentation while ensuring coating integrity and durability goals are concurrently met.

42 ENGINEERING↗

DOE OSTI2023

Development of Hydrogen Permeation Barrier and Matrix Interaction Protection Coatings for TZM Enclosure of Hydride Moderators (Microreactor Program M3 Report)

It is important to develop a high-performance enclosure solution for hydride-based microreactor moderation components to effectively suppress hydride thermal decomposition and prevent hydrogen loss in harsh in-reactor environments. Currently, the DOE-NE Microreactor Program (MR program) is investigating the titanium-zirconium-molybdenum (TZM) canned yttrium hydride (YH 2-x ) solution, which provides acceptable hydrogen retainment performance up to ~700 °C. However, improvements in the enclosure are necessary for increasing long-term operation temperature beyond 700 °C and enhancing short-term survivability at even higher temperatures during power transients. One potential solution is the addition of a dedicated hydrogen permeation barrier, which can potentially improve the enclosure's performance. Furthermore, the hydride moderator components will be inserted into the microreactor matrix, which may consist of materials that are not chemically inert against TZM. Therefore, the TZM might need to be protected from the external environment through the application of another surface protection coating. To address these critical issues, two types of barrier coatings optimized for TZM-based moderator enclosure has been developed. A multilayer coating approach has been used to identify TZM-compatible barrier materials. Behavior of these coating designs against H 2 permeation and long-term high-temperature graphite matrix interactions has been examined in detail. Additionally, the developed coatings' behavior when exposed to both high-temperature thermal cycling and heavy-ion irradiation has also been investigated. Overall, the development of these barrier coatings is essential for achieving maturity for the metal hydride moderator technology. The results in this report will provide crucial insights into the behavior of the developed coatings and their potential for improving the long-term performance of TZM-based moderator enclosures.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Strain to failure measurements of Cr coatings with different processing

Differently processed Cr coatings on Zircaloy cladding were assessed for coating strain to failure. This report includes i) quantification of Cr coating strain to failure for several coating variants, ii) incorporation of high throughput analysis developed utilizing artificial intelligence, and iii) develop a hoop direction coating strain to failure testing approach for high temperatures that doesn’t require digital image correlation strain measurements. Room temperature strain to failure measurements indicated that heat treatment had an impact on strain to failure of the coating, with increasing heat treatment temperature increasing the average strain to failure of the Cr coating.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Influence of Ink Formulation and Drying Conditions on Ionomer Distribution in High-Performance Roll-to-Roll-Coated Gas-Diffusion Electrodes

To enable mass production of fuel cell membrane electrode assemblies (MEAs) catalyst layers production will require continuous roll-to-roll (R2R) coating processes. Gas diffusion electrodes (GDEs) are advantageous for mass production because the catalyst layer can be directely coated on the microporous layer of the gas diffusion media without the need for a decal-transfer process. It is known that the water-to-alcohol ratio in the catalyst ink influences the interactions of the ionomer with the catalyst leading to different distributions of ionomer in spray-coated catalyst layers. It is also known that during drying of colloidal mixtures, like fuel cell inks, factors such as drying rate, particle size, and agglomeration influence how the materials distribute themselves throughout the thickness of the dired film. Thus far there have only been limited studies to understand how process conditions such as ink formulation and drying temperature influence the distribution of ionomer and catalyst coated using scalable methods. This understanding is especially important for GDEs since it is known that having a sufficient amount of ionomer at the catalyst layer-membrane interface is critical for high performance. In this study we have focused on determining how the ratio of water to 1-propanol in the catalyst ink ink and drying temperature influence the distribution of ionomer throughout the thickness of the catalyst layer. Using a combination of Kelvin probe and x-ray photoelectron spectroscopy we show that an ionomer-rich surface is promoted by a higher drying rate and a water-rich catalyst ink. In contrast, a 1-propanol catalyst ink leads to a lower concentration of ionomer on the top surface. Using x-ray computed tomography, we are able to characterize the ionomer distribution throughout the thickness of the layer. We find that, in addition to promoting an ionomer-rich top surface, water-rich inks lead to a more homogenous distribution of ionomer, whereas a 1-propanol-rich ink leads to a more irregular distribution. It is found that MEA performance is improved by selecting conditions and ink formulations that promote ionomer enrichment at the top surface to facilitate a good interface with the membrane. MEAs prepared with a 75 wt% water catalyst ink with a 0.9 I/C have equivalent performance to spray-coated GDEs. Critically, these R2R-coated GDEs do not need an additional ionomer overlayer like the spray-coated GDEs do, reducing the number of processing steps in a manufacturing setting. This work shows that with the appropriate selection of materials, ink formulation, and processing conditions gas-diffusion electrodes are a viable pathway for fuel cell manufacturing.

ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATION↗

DOE OSTI2022

Oil and water resistant low adhesion surface treatment and coatings

A novel omniphobic surface coating is disclosed that provides both high oil-repellency and high-water repellency to the coated surface. The coating may contain perfluoropolyether (PFPE) or a similar fluorinated or perfluorinated polymer, as well as a hardener and a catalyst. One or more surfactants or viscosifiers may also be added. Further, the coating may contain one or more functional additives, including, but not limited to, coloring agents, anti-corrosive agents, anti-fouling agents, water-repellent agents, and/or oil-repellent agents. Methods for formulating the novel omniphobic surface coating are also described. Such methods include preparing a first part of the coating, which may contain, at minimum, a polymer such as PFPE or a similar fluorinated or perfluorinated polymer, and a suitable solvent; preparing a second part of the coating, which is a water-free system that may contain, at minimum, a hardener and a catalyst; and combining the first part and the second part together.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Infrared fluorescent coatings

A coating composition includes: (i) a film-forming resin; (ii) an infrared reflective pigment; and (iii) an infrared fluorescent pigment or dye different from the infrared reflective pigment. A multi-layer coating including the coating composition, and a substrate at least partially coated with the coating composition is also disclosed. A method of detecting an article at least partially coated with the coating composition is also disclosed.

Zalich, Michael A.↗

DOE OSTI2023

Infrared fluorescent coatings

Zalich, Michael A.↗

DOE OSTI2024

Systems and methods for thermal barrier coatings to modify engine component thermal characteristics

An engine component comprises one or more thermal barrier coatings applied to one or more areas of the engine component. The thermal barrier coatings reduce the temperature rate of change of the areas to which the thermal barrier coating is applied. Reducing the temperature rate of change can help reduce lattice structure damage caused by different temperatures in different areas of the engine component. The thermal barrier coating can be applied as a monolithic layer on a surface of the engine component or can be applied in different areas using patterns. The patterns allow for the tuning of the performance characteristics (temperature rate of change) of the areas of the engine component and can help reduce defect propagation, such as cracks, in the thermal barrier coating from one area of the thermal barrier coating to other areas of the thermal barrier coating.

Koci, Chad Palmer↗

DOE OSTI2026

Oxidation of Materials and Coatings at 1000°C and 250 bar for use in Oxy-Combustion Turbine

Combinations of materials and coatings were tested in supercritical CO2 (sCO2) to evaluate their reliability in an oxy-fuel turbine being designed to operate in the 150-300 MWe size range at inlet temperatures of 1,150 °C at 300 bar and exhaust temperatures in the 725-775 °C range. Nickel alloys and stainless steels were exposed to supercritical CO2 at 1,000 °C and 250 bar for a total of over 1,500 hours. The materials were tested bare, with a nanocrystalline MCrAlY bond coat only, or with one of two types of bond coat and a thermal barrier coating. A novel test facility using a localized heat zone generated by an induction heater inside an externally cooled autoclave was developed to perform those tests. The specimens were weighed before and after exposure to determine the oxidation rate. All specimens were inspected visually, and a smaller group of coated specimens were studied using secondary electron microscopy (SEM). The integrity of the coating, and the morphology and composition of the thermally grown oxide were especially of interest for the SEM investigation. This paper presents the up-to-date results of the testing coated and uncoated superalloys in sCO2 at up to 1150 °C and up to 300 bar performed at Southwest Research Institute.

Bocher, Florent [Southwest Research Institute, San↗

DOE OSTI2020

Artificial linear brush abrasion of coatings for photovoltaic module first-surfaces

Natural soiling and the subsequent necessary cleaning of photovoltaic (PV) modules result in abrasion damage to the cover glass. The durability of the front glass has important economic consequences, including determining the use of anti-reflective and/or anti-soiling coatings as well as the method and frequency of operational maintenance (cleaning). Artificial linear brush abrasion using Nylon 6/12 bristles was therefore examined to explore the durability of representative PV first-surfaces, i.e., the surface of a module incident to direct solar radiation. Specimens examined include silane surface functionalized-, roughened (etched)-, porous silica-coated-, fluoropolymer-coated-, and ceramic (TiO 2 or ZrO 2 /SiO 2 /ZrO 2 /SiO 2 )-coated-glass, which are compared to monolithic-poly(methyl methacrylate) and -glass coupons. Characterization methods used in this study include: optical microscopy, ultraviolet–visible–near-infrared (UV-VIS-NIR) spectroscopy, sessile drop goniometry, white-light interferometry, atomic force microscopy (AFM), and depth-profiling X-ray photoelectron spectroscopy (XPS). The corresponding characteristics examined include: surface morphology, transmittance (i.e., optical performance), surface energy (water contact angle), surface roughness, scratch width and depth, and chemical composition, respectively. The study here was performed to determine coating failure modes; identify characterization methods that can detect nascent failures; compare the durability of popular contemporary coating materials; identify their corresponding damage characteristics; and compare slurry and dry-dust abrasion. This study will also aid in developing an abrasion standard for the PV industry.

14 SOLAR ENERGY↗

DOE OSTI2022

Multilayer Chitin–Chitosan–Cellulose Barrier Coatings on Poly(ethylene terephthalate)

Currently, effective barrier properties over a wide range of humidity are achieved by layering multiple plastics, resulting in structures that are nearly impossible to recycle through current systems. There is strong interest in developing barriers that are recyclable, biodegradable, or compostable. Chitin and cellulose nanomaterials are promising alternatives because of their high crystallinity, renewable sourcing, strong electrostatic interactions, and potential for biodegradation or composting. In this paper, we explore the potential to create multilayer materials with effective oxygen and water vapor barrier properties at elevated humidity by combining recyclable poly(ethylene terephthalate) (PET) films with single-layer and bilayer coatings of chitin nanowhiskers (ChNWs), chitosan (CS), and cellulose nanocrystals (CNCs). The addition of CS to the ChNW suspension improved the gas barrier properties of ChNW coatings, likely by filling voids, and short ChNWs (SChNW, 114 nm) performed better than long ChNWs (LChNW, 230 nm). At the optimal mass ratio of 1:1 SChNW/CS, the oxygen permeability (OP) of SChNW/CS-coated PET films was 5.1 cm 3 μm m –2 day –1 kPa –1 versus 15.9 cm 3 μm m –2 day –1 kPa –1 for neat PET. To take advantage of electrostatic attraction and hydrogen bonding, CNC was first coated on the PET, followed by coating with ChNW/CS, resulting in an OP as low as 3.6 cm 3 μm m –2 day –1 kPa –1 at 50% relative humidity (RH), and 6.4 cm 3 μm m –2 day –1 kPa –1 at 80% RH. Furthermore, after thermal treatment (120 °C, 2.5 h), the OP dropped to 2.2 cm 3 μm m –2 day –1 kPa –1 (50% RH) and 4.8 cm 3 μm m –2 day –1 kPa –1 (80% RH). The ChNW/CS and CNC coating can be efficiently removed with alkali treatment enabling possible recycling of the coated PET films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗