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At least 55 records · Page 3

Improved damage tolerance of SiC-based nuclear fuel cladding with novel multi-layered SiC coating design at 1200 °C

Continuous SiC fibre reinforced SiC matrix composites (SiC f -SiC m ) with monolithic SiC outer coatings are considered as a damage-tolerant cladding design for loss of coolant accident (LOCA) conditions in light water reactors. However, monolithic SiC coatings are brittle and prone to catastrophic failure. In this study, a SiC f -SiC m cladding with a novel multi-layer SiC outer coating (11 sub-layers, ∼260 µm in total thickness) was investigated under C-ring compression at room temperature and 1200 °C in argon environment. Real-time synchrotron X-ray computed tomography (XCT) was employed to capture crack initiation and propagation processes. Compared to conventional monolithic SiC outer coatings, the multi-layer coating structure facilitated crack deflection and bifurcation enhancing its damage tolerance at both temperatures. Despite pre-existing surface cracks, claddings exhibited stable mechanical-performance at both temperatures. These initial cracks did not critically affect the failure processes as they were not aligned with the maximum stress direction. Furthermore, the microstructure, distribution of residual stresses, and local properties of individual components in the material were thoroughly characterized, and compared with open literature on conventional claddings with monolithic outer coatings. These results provide new insights into the failure mechanisms of multi-layer SiC coatings and offer guidance for the future design of accident-tolerant nuclear fuel claddings.

36 - MATERIALS SCIENCE↗

One-Pot Coating of Ceramic Powders by Exfoliated Boron Nitride Layers with a Dense CO 2 Medium and Ultrasound-Aided Mixing

The coating or doping of substrates by two-dimensional materials to impart superior functional properties (such as improved thermal conductivity, bacterial resistance, reduced friction) is receiving increased attention. Environmentally benign, rapid and scalable coating techniques are desirable for this purpose. Here, we report a novel process for coating alumina, silicon carbide and boron carbide substrates with hexagonal boron nitride (h-BN) layers. The process consists of two sequential steps. First, h-BN layers are exfoliated from bulk h-BN in supercritical carbon dioxide (scCO 2 ) using ultrasound-aided mixing. This step is followed by self-assembly (i.e., coating) of the exfoliated h-BN on the substrates in liquid CO 2 also aided by ultrasound. The liquid CO 2 state is achieved by simply lowering the pressure and temperature of the first step below the critical point of CO 2 (P c = 72.8 atm; T c = 31.1 °C). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) micrographs clearly reveal the exfoliation of h-BN under scCO 2 conditions as well as the h-BN assembly on various substrates under liquid CO 2 conditions. X-ray diffraction patterns confirm the structural integrity of the coated h-BN layers. It was also confirmed that without a transition to the liquid CO 2 phase following exfoliation in scCO 2 , there was negligible coating of h-BN on the substrates. Researchers in the field could consider this benign process to rapidly coat or dope materials with h-BN and other 2D materials to impart improved functional properties in myriad applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Validation of the VUV-reflective coating for next-generation liquid xenon detectors

Abstract Coating detector materials with films highly reflective in the vacuum ultraviolet region improves sensitivity of the next-generation rare-event detectors that use liquid xenon. In this work, we investigate the MgF 2 -Al-MgF 2 coating designed to achieve high reflectance at 175 nm, the mean wavelength of liquid xenon (LXe) scintillation. The coating was applied to an unpolished, passivated copper substrate mimicking a realistic detector component of the proposed nEXO experiment, as well as to two unpassivated substrates with “high” and “average” levels of polishing. After confirming the composition and morphology of the thin-film coating using TEM and EDS, the samples underwent reflectance measurements in LXe and gaseous nitrogen (GN2). Measurements in LXe exposed the coated samples to -100°C for several hours. No peeling of the coatings was observed after several thermal cycles. Polishing is found to strongly correlate with the measured specular reflectance (R spec ). In particular, 5.8(5)% specular spike reflectance in LXe was measured for the realistic sample at 20° of incidence, while the values for similar angles of incidence on the high and average polish samples are 62.3(1.3)% and 27.4(7)%, respectively. At large angles (66°–75°), theR spec in LXe for the three samples increases to 23(5)%, 80(8)%, and 84(18)%, respectively. The R spec at around 45° was measured in both GN2 and LXe for average polish sample and shows a reasonable agreement. Importantly, the total reflectance of the samples is comparable and estimated to be 92(8)%, 85(8)%, and 83(8)% in GN2 for the realistic, average, and high polish samples, respectively. This is considered satisfactory for the next-generation LXe experiments that could benefit from using reflective films, such as nEXO and DARWIN, thus validating the design of the coating.

Instruments & Instrumentation↗

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↗

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↗

The effect of copper additives on hybrid Zr-based chemical conversion coating morphology and chemical compositions

In the realm of corrosion protection, Zr-based conversion coatings offer an environmentally friendly, chromate-free alternative to conventional coating. This study uses advanced X-ray, electron microscopy and electrochemical testing techniques to better understand the impact of varying Cu²⁺ ion concentrations on the characteristics of Zr-based coatings on Fe substrates. Our findings demonstrate that within the tested conditions, higher Cu²⁺ additive concentrations at 40 ppm enhance surface characteristics, increasing stability towards anti-corrosion capability, particularly under NaCl treatment. Conversely, at a lower Cu²⁺ concentration of 20 ppm, coatings exhibited more significant dissolution of Cu clusters and increased vulnerability to chloride-induced degradation. X-ray photoelectron spectroscopy and synchrotron X-ray fluorescence (XRF) and X-ray absorption near edge structure (XANES) spectroscopy analyses revealed Cu²⁺ formation in Cu20, while Cu40 retained its metallic state (Cu⁰) with a slower reaction rate. Cu20 offers some protection but lacks durability, whereas in Cu40, lower I corr , and enhance corrosion resistance, making it ideal for protective coatings in salt-water environments. This study underscores the importance of balancing Cu²⁺ ions concentration in the coating solution to optimize performance, highlighting the role of Cu in enhancing both surface properties and long-term stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Development of a coupled experimental–computational approach for engineering optimization of spout-fluidized bed particle coating systems

The design of spout-fluidized bed (SFB) coating systems for nuclear particle fuels typically relies on trial-and-error processes, comprising iterative and time-consuming coating deposition experiments and post-deposition characterization. At an engineering scale, this approach to guided SFB system design is inefficient, highlighting the need for streamlined experimental methodologies which can correlate fluidization conditions to downstream coating outcomes. In this study, we combine time-resolved particle image velocimetry (PIV) with CFD–DEM simulations to benchmark hydrodynamic behavior in a 3D spout-fluidized bed. By exploiting easily accessible optical measurements of particle motion at the bed wall and within the spouting region, we obtain quantitative velocity fields that can be directly compared with model predictions of the occluded bed region, without resorting to complex imaging and characterization techniques such as X-ray or magnetic resonance tomography. Experimental benchmarking reveals strong agreement between CFD–DEM and PIV in the spout and annulus regions, while discrepancies near the wall highlight areas for future model development. Here, the proposed integrated experimental–numerical framework will enable a direct connection between measured variables and numerically predicted fluidization performance of dense, surrogate nuclear particle fuel feedstock such that experimental SFB component design can be rapidly evaluated, informing design decisions for nozzle geometry and operating conditions. Future work will extend this framework by correlating quantified fluidization metrics across nozzle geometries and operating conditions with the resulting coating morphology, microstructure, and uniformity. Establishing these correlations will enable predictive links between hydrodynamic performance and coating quality, providing a rational, scalable basis for optimizing SFB design prior to coating deposition.

CFD/DEM↗

Investigation of the Mechanical Degradation of Zinc-Based Cold Spray Coatings for Steel Pipelines

Internal corrosion in wet natural gas is a big challenge in the oil and gas industry due to corrosive constituents such as carbon dioxide (CO2), hydrogen sulfide (H2S), other forms of sulfur, and water in the gas stream. To mitigate internal corrosion, zinc-based cold spray coatings were designed for use in natural gas pipelines to increase the lifespan of the pipeline network. However, one of the requirements in designing internal coatings is the resistance of the coatings to mechanical forces applied on the pipeline's internal wall during pigging operations. These forces are primarily compressive and shear/friction forces. This study examines material properties that must be considered when evaluating mechanical considerations. To determine the viability of the developed coatings with respect to the shear/friction forces, the shear adhesion and wear resistance of the materials have been evaluated. Shear adhesion testing was performed with modified clevises to determine the shear stress required to cause adhesion failure at the coating/substrate interface. Scanning electron microscopy was utilized to characterize the interfaces after failure. Wear testing was performed on coatings and pipeline materials utilizing pin-on-drum testing. These tests display the stress limitations and wear that the coatings can tolerate from pigging.

mechanical degradation↗

Distributed strain sensing using Bi-metallic coated fiber optic sensors embedded in stainless steel

Silica fiber optic sensors are resistant to corrosive environments and high temperatures, making them attractive candidates for harsh conditions found in nuclear and aerospace industries. Moreover, fibers can be deployed remotely for continuous measuring of spatially distributed temperatures and strains. Here, this study investigated embedding a Ni/Cu bi-metallic coated fiber in a stainless-steel 316 (SS316) matrix using laser powder bed fusion towards functionalizing metal components for site-specific health monitoring. The embedded fiber was continuously interrogated during controlled heating to 1000°C. The measured fiber strains were similar to the expected differential thermal strains between the fiber and the SS316 matrix, until divergent behavior was observed at temperatures >500°C. No debonding at the matrix–coating–fiber interfaces was observed during microscopy, but significant interactions between the coatings and matrix resulted in diffusion-driven chemistry variations and Kirkendall void formation. Applying the strain-lag theory revealed plastic behavior in the Ni coating at temperatures >500°C, limiting the strain transfer to the fiber at higher temperatures. It was estimated that the elastic modulus in the Ni coating had decreased from ~200 GPa at room temperature to below 40 GPa, starting at 600°C. The low elastic modulus above 600°C is within the margin of what the tangent modulus would be in the case of bilinear isotropic hardening. Regardless of the divergent strain transfer at higher temperatures, the fiber was exposed to the equivalent of 1.9 % engineering strain at 1000°C, but measured only a 0.7 % engineering strain due to the poor strain transfer. Although compensating for the plastic behavior of Ni proved challenging, the bonding of a brittle silica fiber to a metal matrix surviving to 1000°C invites potential iterations on coating material for future application. For example, the embedded fiber is sufficient for acoustic energy transfer, realizing high temperature distributed acoustic sensing.

36 MATERIALS SCIENCE↗

All-alumina quarter-wave plate coatings fabricated by glancing angle deposition using serial bideposition

Anisotropic phase retarders, used in high power laser facilities to perform polarization smoothing, can be obtained by the glancing angle deposition (GLAD) coating process. Due to its high laser resistance, the coatings are mainly made of silica. Therefore, limited attention has been given to other dielectric materials. Here we present a study on alumina GLAD anisotropic coatings; a material with high laser resistance, higher birefringence and lower environmental sensitivity than silica. Since the anisotropy is related to the coatings microstructure through the deposition angle, samples were coated at angles varying from ± 68° to ± 82° using the serial bideposition technique. They were characterized by ellipsometry, polarimetry, spectrophotometry and electron microscopy. We showed that the highest birefringence is obtained at a deposition angle of ± 76° with an in-plane value of 0.053. Based on these results, a quarter-wave plate at 351 nm was designed as a multilayer with seven pairs of anisotropic layers deposited at ± 76° and isotropic layers deposited at 0°. The fabricated coating exhibited a uniform retardance of 88.51 ± 0.45 nm. The alumina GLAD wave plates presented here, open the door to new possibilities in the laser field and especially in the field of fusion energy.

36 MATERIALS SCIENCE↗

Investigation of the temperature-dependent failure processes in PVD Cr-coated ZIRLO nuclear fuel cladding using in situ X-ray micro-tomography imaging

In this work, an accident tolerant fuel cladding system with Cr coating deposited using physical vapour deposition (PVD) method onto commercial Optimized ZIRLO™ was studied. The cladding tubes were machined into C-rings and loaded to failure under compression with real-time synchrotron micro-X-ray computed tomography (XCT) imaging at room temperature (RT), 345 °C, 650 °C and 950 °C in argon (Ar) atmosphere. The mechanical behaviour and failure processes were found strongly temperature-dependent where the Cr coating showed brittle fracture at RT and 345 °C, ductile fracture at 650 °C and a reversion to brittle fracture at 950 °C. Nanoindentation measurements and scanning electron microscopy (SEM) imaging were conducted on the materials after high temperature testing. It was found that recrystallisation of the Cr coating occurred at elevated temperatures, which significantly affected its local properties hence the failure behaviour at different temperatures. This work represents the first in situ 3D XCT observation of progressive failure processes in PVD Cr-coated ZIRLO claddings up to 950 °C providing critical insights into its brittle-to-ductile transition (BDTT) behaviour and subsequent ductile-to-brittle reversion with the increase in temperature. Moreover, results are compared with other PVD Cr-coated Zircaloy materials from open literature; the influences of the coating microstructure and local properties on the failure stress/strain and fracture processes are discussed.

Yuan, Guanjie↗

Erosion of high-Z refractory coatings for helicon plasma source window

Proto-MPEX (Materials Plasma Exposure eXperiment), a linear plasma device (LPD), using a high power radio frequency (RF) (⩾100 kW, 13.56 MHz) helicon plasma source, has suffered RF sheath-induced window erosion. The sputtered impurities from the window surface transport toward the downstream target affecting plasma-material interaction studies. The rectified sheath voltage formed was high enough to cause window erosion by light ions due to its low-Z components (e.g. Si 3 N 4 and AlN). Hence, we are proposing impurity mitigation strategies, which involve the application of a Faraday screen to lower the rectified sheath voltage and the application of high-Z refractory coatings on the existing window plasma-facing surface. In this work, we report the erosion of two different coatings, i.e., tantalum oxide (Ta 2 O 5 ) and hafnium oxide (HfO 2 ) on a silicon nitride (Si 3 N 4 ) window material under conditions of low-energy deuterium (D) ion impact, well below the Ta 2 O 5 sputtering energy threshold (i.e. 250 eV). The test samples were RF-biased and exposed to a high D-ion fluence (∼10 26 m −2 ) in Plasma Interaction with Surface Component Experimental Station (PISCES-A) LPD. The experimentally measured sputtering yields of the high-Z refractory coatings below the sputtering energy threshold of Ta 2 O 5 indicate an increased erosion due to the plasma impurities, especially due to oxygen. Improving the vacuum level could reduce the oxygen impurities and increase the lifespan of the coated helicon window for plasma operation. Post-surface analysis indicates no preferential erosion of oxygen or enrichment of the high-Z surface component. This is likely due to an effective energy transfer from the impurity ion for sputtering of the high-Z component in the coating. With the reduced rectified sheath voltage at the window surface and improved vacuum conditions, the proposed high-Z refractory coatings offer a promising solution for reducing window erosion in future MPEX plasma operations at ORNL.

RF bias↗

Impact of high-temperature annealing on hafnia-silica composite coatings deposited via ion beam sputtering for high-peak power 1064 nm lasers

The maximum power handling fluence of high-peak and average power laser systems is often limited by the laser damage of the coatings on optical components. Furthermore, these multilayer dielectric coatings are limited in their maximum power handling due to laser-damage-prone defects in the lower optical bandgap, higher optical index material. Some of these defects can be mitigated by thermal annealing to high temperatures, which can greatly reduce the linear absorbative precursors. Typically, hafnia and silica are the materials of choice for high-peak and average power laser systems in the ultraviolet through infrared spectral range; however, hafnia crystalizes readily when annealed at high temperatures. In this study, we prepare composite HfO 2 -SiO 2 coatings by co-sputtering hafnia and silica in an ion beam sputtering system and compare them to pure hafnia-based coatings. We demonstrate that crystallinity in hafnia can be completely suppressed when it is mixed with silica, such as the composite coatings in this study. High reflectors were fabricated and annealed, demonstrating that the multilayer dielectric stacks can survive high-temperature annealing and exhibit an excellent linear absorption of 0.2 +/- 1 ppm at 1064 nm. Short- and long-pulse laser damage was explored, demonstrating the complex relationship between linear absorption and the non-linear absorption which drives pulsed laser damage. These results provide an excellent route to the creation of very low linear absorption optical coatings, which also utilize low scattering materials that are best suited for high-peak and average power applications.

Harthcock, Colin [Lawrence Livermore National Labo↗

Effect of X-ray Irradiation and Carnauba Wax Coating on Quality of Lime (Citrus latifolia Tan.) Fruit

The quality of Persian (Tahiti) lime (Citrus latifoliaTan.) fruit was determined following coating with carnauba wax and X-ray irradiation at doses suitable for disinfestation of quarantine pests. Fruit with or without carnauba wax coating were treated with irradiation doses of 0, 150, 300, or 450 Gy, and stored for 14 days at 13 °C and 6 days at 20 °C to simulate commercial transportation and marketing conditions from Hawaii to the continental United States. The fruit color, weight loss, total soluble solids (TSS) content, and titratable acidity (TA) were analyzed at 7, 14, and 14 + 6 days post irradiation. Wax coating significantly delayed fruit peel discoloration, and reduced fruit weight loss by more than 7% compared with the unwaxed controls. Irradiation did not affectΔEof the peel for coated fruit at day 14 + 6. Irradiation with or without coating did not affectΔEof flesh color, weight loss, TSS content, or TA. Wax coating combined with irradiation treatment of limes at doses ≤450 Gy ensured marketable visual quality and chemical composition while providing quarantine security.

Agriculture↗

Tuning Molecular Interactions between Peptoids and Substrates to Achieve Surface-Agnostic Coating

Achieving programmable and robust coatings that maintain functionality while adhering to various surface types with molecular-level tunability and programmable features remains challenging. In this study, we develop adaptable and stable surface-agnostic coatings (SACs) based on crystalline peptoid membranes by tuning interpeptoid and peptoid-substrate interactions. We utilize two complementary methods: (1) surfaceinduced assembly, where peptoid membranes form directly on substrates, and (2) depositing preformed peptoid crystalline membranes via an aqueous layer-by-layer (LbL) assembly technique. These strategies are applied to substrates with diverse surface chemistries and topographies, including mica, highly ordered pyrolytic graphite (HOPG), MoS 2 , sapphire, and porous membranes like porous alumina and polysulfide. Atomic force microscopy confirms the formation of peptoid coatings and reveals differences in assembly behavior across surfaces. Moisture vapor transport measurements serve as a proof-of-concept test for membrane continuity and tunable permeance. Together, these findings demonstrate the adaptability and programmability of peptoid-based SACs, enabling rational coating design on surfaces with diverse chemical and topographical features. Furthermore, this work opens pathways for using peptoid membranes as programmable surface modifiers in functional interfaces, protective coatings, and membrane platforms.

biomimetic polymers↗

"Soiling, Cleaning, and Abrasion: The Results of the Five-Year Photovoltaic Glass Coating Field Study" [Slides]

External contamination ("soiling") of the incident surface is a major limiting factor for solar technologies. A 5-year field glass coupon study was conducted to better understand external contamination and its effects; compare cleaning methods and the use of preventative coatings; and explore the abrasion resulting from cleaning to advise on accelerated abrasion testing. Test sites included the cities of Dubai (UAE), Kuwait City (Kuwait), Mesa (AZ), Mumbai (India), and Sacramento (CA). Through the 5-year cumulative study, dry brush, water spray, and wet sponge and squeegee cleaning methods were compared to no cleaning. Optical microscopy was used to obtain images, including representative color images, grayscale images for object analysis, and oblique images for coating integrity assessment. A thresholding protocol was developed to analyze and distinguish specimens using the ImageJ software. Optical performance was quantified using a spectrophotometer, including comprehensive optical characterization (transmittance, reflectance, and absorptance in addition to forward- and back-scattering). Atomic force microscopy was used to verify the abrasion damage morphology, including the width and depth of surface scratches. Analysis of the results included correlation of optical performance and particle area coverage, rank order (by coating or location), and the acceleration factor for abrasion damage. The efficacy of external cleaning was more readily distinguished from the effectiveness of antisoiling coatings. The acceleration factor for dry brush cleaning of a porous silica coating was found to be on the order of unity.

14 SOLAR ENERGY↗

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↗

Spray-Coated Silver as Backside Metal for III–V Photovoltaic Devices on GaAs and Ge Substrates

The accelerated increase in demand for III-V space photovoltaics on GaAs and Ge substrates, as well as growing interests in terrestrial applications, motivate the development of cost-effective, high-throughput processing routes of these materials. Here, in this study, we assess spray-coated silver (Ag) back contact metallization as a substitute for electron-beam-evaporated metals currently used in industry. We find that the spray-coated Ag films are dense and continuous. By means of quantum efficiency, dark current-voltage, and illuminated current-voltage characterizations, we show that spray-coated GaAs and Ge solar cells perform similarly to baseline devices with electroplated Au, including under high current densities. We estimate that the thresholds for specific contact resistance below which back contacts do not significantly contribute to resistive loss are 2.1 x 10 -1 Ω•cm 2 for GaAs and 4.7 x 10 -2 Ω•cm 2 for Ge. We experimentally confirm that our spray-coated samples meet these requirements. Peel tests show that the adhesion of plain spray-coated Ag films to the back of p-type Ge substrates used in III-V solar cells is currently insufficient, whereas adhesion to p-type GaAs substrates is outstanding and requires no further optimization.

14 SOLAR ENERGY↗