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At least 163 records · Page 9

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DOE OSTI2022

Accelerated corrosion testing of cold spray coatings on 304L in chloride environments

Cold spray is an advanced metal manufacturing technique applied across many fields for a wide range of functions. Low heat input and compressive stresses induced into the substrate by the cold spray process makes it a promising choice for protective corrosion resistant coatings. One potential application for cold spray is as a protective coating against corrosion for spent nuclear fuel (SNF) interim dry storage canisters. As these canisters are currently stored at interim storage locations longer than originally intended, chloride induced stress corrosion cracking has been identified as a high priority knowledge gap, specifically with respect to prolonging or extending canister lifetimes ( Teague et al., 2019 ). The high deployability of cold spray, for which nozzles have been developed for application in constrained spaces, in conjunction with beneficial properties inherent to cold spray makes this a good candidate for a corrosion protection coating on SNF canisters. This work explores a pathway to rapidly down-select cold spray coatings for canisters by focusing on the corrosion properties. Specifically, this study examines the corrosion protection abilities of nickel and nickel-based alloy cold spray coatings on 304 L stainless steel in chloride rich environments through electrochemical scans and ferric chloride pitting tests (ASTM G48 Method A). It was shown that the porosity of the coating, the processing gas, material selection, and deformation in the substrate all impact the corrosion behavior of cold spray coatings and are areas where optimization could reduce potential materials degradation, enabling enhanced coatings development.

Karasz, Erin K.↗

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 OSTI2026

Time of Flight Secondary Ion Mass Spectrometry for Characterization of Pt-Coated Porous Transport Layers in PEM Water Electrolyzers

Titanium-based porous transport layers (PTLs) and iridium-based catalyst layers (CLs) are two main components of proton exchange membrane water electrolyzers (PEMWEs). PTLs are typically coated with platinum to minimize interfacial losses and to support long-term operation. Optimizing coatings and the PTL-CL interface requires comprehensive characterization. This study establishes time-of-flight secondary ion mass spectrometry (ToF-SIMS) as a valuable technique for PTL characterization, addressing capabilities and limitations related to PTL morphology. A methodology was developed that uses a Cs + sputter beam for dynamic depth profiling, with data collected in both positive-ion (MCs + ) and negative-ion modes to generate depth profiles, 2D ion maps, and 3D ion reconstructions. ToF-SIMS detected relative differences in platinum-layer thickness between samples; these trends were validated by cross-sectional scanning transmission electron microscope (STEM) measurements and flat-titanium substrate controls. Interfacial oxide layers are identified in both ion modes, with enhanced oxide sensitivity in negative mode. The technique’s high sensitivity enables detection of nanometer-scale coatings and trace impurities within the bulk PTL structure. These results provide a methodological framework for analyzing Pt-coated PTLs, with the potential to extend to other components in PEMWEs and other electrolyzer systems.

36 MATERIALS SCIENCE↗

DOE OSTI2025

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↗

DOE OSTI2022

Conformal PEDOT Coating Enables Ultra-High-Voltage and High-Temperature Operation for Single-Crystal Ni-Rich Cathodes

Single-crystal Ni-rich Li[Ni x Mn y Co 1-x-y ]O 2 (SC-NMC) cathodes represent a promising approach to mitigate the cracking issue of conventional polycrystalline cathodes. However, many reported SC-NMC cathodes still suffer from unsatisfactory cycling stability, particularly under high charge cutoff voltage and/or elevated temperature. Herein, we report an ultraconformal and durable poly(3,4-ethylenedioxythiophene) (PEDOT) coating for SC-NMC cathodes using an oxidative chemical vapor deposition (oCVD) technique, which significantly improves their high-voltage (4.6 V) and high-temperature operation resiliency. The PEDOT coated SC LiNi 0.83 Mn 0.1 Co 0.07 O 2 (SC-NMC83) delivers an impressive capacity retention rate of 96.7% and 89.5% after 100 and 200 cycles, respectively. Significantly, even after calendar aging at 45 degrees C and 4.6 V, the coated cathode can still retain 85.3% (in comparison with 59.6% for the bare one) of the initial capacity after 100 cycles at a 0.5 C rate. Synchrotron X-ray experiments and interface characterization collectively reveal that the conformal PEDOT coating not only effectively stabilizes the crystallographic structure and maintains the integrity of the particles but also significantly suppresses the electrolyte's corrosion, resulting in improved electrochemical/thermal stability. Our findings highlight the promise of an oCVD PEDOT coating for single-crystal Ni-rich cathodes to meet the grand challenge of high-energy batteries under extreme conditions.

25 ENERGY STORAGE↗

DOE OSTI2022

Thermal Stability and Mechanical Properties of Cold-Sprayed Nickel-Yttria Coating

The microstructural evolution under the extreme environments imposed during cold spray deposition of cermet coatings and the microstructural recovery during post-processing annealing treatments is rather complex and not well understood. Here, Ni-Yttria cermet coatings on an SS304 substrate were produced using cold spray technique, resulting in a bimodal grain structure. The grain growth, phase stability, hardness, and wear properties are observed in as-deposited and annealed (at 400 °C) Ni-Yttria and pure Ni coatings. A multimodal microstructural characterization using electron microscopy, and atom probe tomography shows the structural and compositional stability of yttria particles and Ni grains. A fragmentation of Y-rich particles and dispersion in Ni was observed, however, no forced mixing/dissolution of Y in Ni is detected. Nano-yttria dispersed within the Ni grains slowed the grain growth during annealing. After annealing, Yttria reinforced coating was 1.5 times harder and showed better thermal and mechanical stability compared to the Ni coating.

Gwalani, Bharat↗

DOE OSTI2024

Power Dissipation on the Metallic Coating of a Ceramic Chamber in Planar Approximation

We adopt the standard field matching technique to solve the general electromagnetic problem consisting of two parallel layers with arbitrary complex relative permittivity and permeability. With parameters of the NSLS-II ceramic chambers, we calculate the power dissipated on the metallic coating and compare the result with the power lost by the beam and with the results of [4].

43 PARTICLE ACCELERATORS↗

DOE OSTI2023

Advancing radioactive material research method: the development of a novel in situ particle-attached microfluidic electrochemical cell

This study aims to develop a microgram-scale microfluidic electrochemical cell (E-cell) for investigating the redox behavior of uranium oxide (UO 2 ). The traditional bulk electrochemical methods may require shielded facilities to investigate the hazardous materials, e.g., spent nuclear fuel, due to high radiation levels. Microfluidic E-cells offer advantages such as reduced radiation exposure, control over fluid flow rates, and high-throughput capabilities. Methods: The design of the E-cell considers electrode morphology, adhesion to a thin membrane, electrode configuration, and vacuum compatibility. Three techniques, including FIB-SEM lift-out, Au coating, and polyvinylidene fluoride (PVDF) binder, are explored for fabricating and attaching microgram quantities of UO 2 as working electrodes. The PVDF binder method proves to be the most effective, enabling the creation of a vacuum-compatible microfluidic E-cell. Results and discussion: The PVDF binder method demonstrates successful electrochemical responses and allows for real-time monitoring of UO 2 electrode behavior at the microscale. It offers chemical imaging capabilities using in situ SEM/EDS analysis. The technique provides consistent redox outcomes similar to bulk electrochemical analysis. Conclusion: The development of a microgram-scale microfluidic electrochemical cell using the PVDF binder technique enables the investigation of UO 2 redox behavior. It offers a low-risk approach with reduced radiation exposure and high-throughput capabilities. The technique provides real-time monitoring and chemical imaging capabilities, making it valuable for studying spent nuclear fuel systems and material characterization.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Thermoluminescence and optically stimulated luminescence response of Al 2 O 3 coatings deposited by mist-chemical vapor deposition

Aluminum oxide (Al 2 O 3 ) is a widely used ceramic material which can be applied as a protective coating on metallic structures to improve corrosion resistance and mechanical properties. Al 2 O 3 also has great potential as a functional thin film device in optoelectronics. When it is doped with carbon (Al 2 O 3 :C), this material system can serve as a reliable radiation dosimeter. The combination of optoelectronic, dosimetric, and protective properties demonstrated by Al 2 O 3 uniquely positions it for dual use applications in nuclear forensics, nonproliferation and safeguards, emergency response, retrospective dosimetry, and nondestructive inspection. Here, in this study, an innovative ultrasonic mist-chemical vapor deposition (Mist-CVD) system was used to deposit thin (nm level) Al 2 O 3 coatings on 304 stainless steel substrates. The single aliquot regeneration (SAR) and additive dose reconstruction techniques were then used to investigate the thermoluminescence (TL) and optically stimulated luminescence (OSL) response of the coated substrates to increasing doses of β irradiation. This study demonstrates that nm-thick Al 2 O 3 coatings hold promise as novel nano-dosimeters which could be leveraged for a series of applications such as nonproliferation and safeguards, retrospective dosimetry, and nondestructive inspection.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2021

Design and Characterization of ALD-Based Overcoats for Supported Metal Nanoparticle Catalysts

Supported metal nanoparticle (SMN) catalysts are enormously crucial for many catalytic applications. However, catalyst deactivation, caused by sintering and coke formation, is a ubiquitous problem that significantly undermines catalytic processing economics. The application of material overcoating onto supported metal nanoparticles by atomic layer deposition (ALD) offers the solution to inhibit catalyst deactivation. Herein, we discuss examples in which ALD has been used to stabilize SMN catalysts in gaseous and aqueous-phase reactions. We highlight the ALD tools and methods in coating high-surface-area catalysts. Besides, various techniques are introduced to understand better how to characterize the overcoating layer and the catalyst itself. Finally, the outlook for new techniques to characterize the ALD overcoated catalytic materials is discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Young’s modulus of V 3 O 5 thin films

Vanadium oxide V 3 O 5 exhibits an insulator-to-metal transition (IMT) near 430 K, which is the highest value for all vanadium oxides exhibiting IMTs. This makes it interesting for advanced electronic applications. However, the properties of V 3 O 5 have been little studied, and, in particular, there are no reports of experimentally determined mechanical properties. In this work, Young’s modulus of sputter-deposited V 3 O 5 thin films has been determined by measuring the fundamental resonant frequency of V 3 O 5 -coated silicon microcantilevers using a laser beam deflection technique. After deposition, the films were characterized by x-ray diffraction, resistivity measurements, and atomic force microscopy. The value of Young’s modulus experimentally determined for V 3 O 5 was 198 ± 14 GPa, which is slightly lower than the computationally derived values for bulk crystal V 3 O 5 .

36 MATERIALS SCIENCE↗

DOE OSTI2024

Seeing in with X-rays: 4D Strain and Thermometry Measurements for Thermal-Mechanical Testing

Understanding temperature-dependent material decomposition and structural deformation induced by combined thermal-mechanical environments is critical for safety qualification of hardware under accident scenarios. Seeing in with X-rays elucidated the physics necessary to develop X-ray strain and thermometry diagnostics for use in optically opaque environments. Two parallel thermometry schemes were explored: X-ray fluorescence and X-ray diffraction of inorganic doped ceramics– colloquially known as thermographic phosphors. Two parallel surface strain techniques–Path-Integrated Digital Image Correlation and Frequency Multiplexed Digital Image Correlation–were demonstrated. Finally, preliminary demonstration of time-resolved digital volume correlation was performed by taking advantage of limited view reconstruction techniques. Additionally, research into blended ceramic-metal coatings was critical to generating intrinsic thermographic patterns for the future combination of X-ray strain and thermometry measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Lithium battery cathode

A novel lithium battery cathode, a lithium ion battery using the same and processes and preparation thereof are disclosed. The battery cathode is formed by force spinning. Fiber spinning allows for the formation of core-shell materials using material chemistries that would be incompatible with prior spinning techniques. A fiber spinning apparatus for forming a coated fiber and a method of forming a coated fiber are also disclosed.

25 ENERGY STORAGE↗

DOE OSTI2023

Lithium battery cathode

Bell, Nelson S.↗

DOE OSTI2024

First Results from two Nb3Sn Cavities Assembled in a CEBAF Quarter Cryomodule

Two 1.5 GHz CEBAF C75-shape 5-cell accelerator cavities were coated with Nb3Sn film using the vapor diffusion technique at Fermilab and Jefferson Labcoating facilities. Both cavities were measured at 4 K and 2 K in the vertical cavity test facility (VCTF) in each lab, then assembled into a CEBAF quartercryomodule at Jefferson Lab. The cryomodule was tested at 4 K and 2 K in the CryoModule Test Facility (CMTF) at Jefferson Lab. RF test results for bothcavities in the cryomodule are similar to those in the qualification test in VTS, with one cavity reaching Eacc =7.9 MV/m and the other - 13.3 MV/m at 4 K

Eremeev, G.↗

DOE OSTI2025

An Optothermal Raman Model Accounting for Convection, Radiation, and Substrate Effects for Evaluation of the Thermal Conductivity of Two‐Dimensional Coatings

Thermal conductivity of two‐dimensional (2D) materials is important to characterize as this will govern thermal transport physics in the various thermal and energy applications benefitting from the unique properties of these materials. Here, analytical and numerical techniques are presented to determine the thermal conductivity and interfacial conductance of a 2D material coating using confocal micro‐Raman spectroscopy as a noncontact diagnostic. While several methods have been proposed for calculating the values of thermal conductivity, interfacial conductance, and spatial temperature profile, these models often do not consider effects of radiation, convection, and substrate resistance on the temperature and heat flux profiles. We present a model to calculate the thermal conductivity and interfacial conductance which accounts for convection, radiation, and substrate effects to characterize a variety of 2D material coatings, which is demonstrated using large area graphene transferred onto copper and nickel substrates. Convection and radiation effects are found to have a negligible effect on the temperature profile of supported coatings, while the substrate effects have a considerable effect and therefore impact the quantification of thermal conductivity and interfacial conductance in addition to limiting the spatial resolution of the technique. These findings will allow for more accurate and reproducible extraction of the thermal conductivity of graphene and other 2D material coatings when employing noncontact optothermal Raman spectroscopy methods.

2D coatings↗

DOE OSTI2025

Advancing Reel-to-Reel Inspection Techniques for Long HTS Conductors: Comparison and Innovations

The continuous advancement of high-temperature superconductor (HTS) technologies has greatly accelerated the development and deployment of HTS applications. Among the critical tools supporting these advancements are reel-to-reel (R2R) critical current (I c ) measurement techniques, which are extensively used by both manufacturers and end users to characterize long-length REBCO conductors. These techniques play a vital role in quality assurance and quality control (QA/QC), ensuring the reliability and performance of HTS conductors and applications throughout the production cycle. We have developed a range of in-house devices for R2R measurements at the University of Houston and Princeton Plasma Physics Laboratory. These include one-dimensional (1D) scan using a magnetic circuit (MC) and two-dimensional (2D) magnetic field mapping systems based on scanning probe array microscope (SPAM) or scanning probe microscopy (SPM). Each technique offers distinct advantages: the MC system provides ultra-fast scanning speeds, ideal for rapid inspection in large-scale industrial production; the high-resolution SPM delivers detailed insights for conductor research and development; and the SPAM, with its simpler mechanical setup, can be upgraded for higher field and lower temperature conditions with a balanced 2D resolution. Here we compared the magnetization and detection capabilities of these techniques through experiments on rare-earth barium copper oxide (REBCO) coated conductor samples, with data analysis supported by numerical simulations. Based on our comprehensive comparative studies, we propose enhancements for each measurement system and provide guidelines for selecting the optimal technique combinations to meet specific application requirements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Laser-interference pulse number dependence of surface chemistry and sub-surface microstructure of AA2024-T3 alloy

The laser-based treatment of a metal surface is an intrinsically non-chemical technique that can alter both the topology and chemistry of surfaces. A laser-based treatment for coating and joining applications can offer alternative surface preparations to the chemically-based surface preparation techniques, which are subject to severe environmental protection and hazardous-waste management considerations. In this study, the surface chemistry and sub-surface microstructural changes are investigated for a novel surface processing method using laser interferometry produced by two beams of a pulsed Nd:YAG laser. The two-beam laser-interference allowed the structuring of the surface at length scales much less than that of the laser beam spot. Surface chemistry changes in the oxide layer of AA 2024-T3 aluminum alloy rolled sheet due to laser processing were investigated using x-ray photoelectron spectroscopy (XPS). Near surface microstructural changes have been investigated with scanning electron microscopy and energy dispersive x-ray spectroscopy (SEM/EDS), and scanning transmission electron microscopy (STEM) as a function of number of interfering laser shots. SEM microstructure pictures of the top surface shows the minimization of surface defects, as all of the sharp features from a rolled sheet surface were smoothed by laser-structuring. STEM images indicate that the laser-interference processing reduced the formation of CuMn-rich precipitates over a 500–800 nm depth from the top surface. XPS data indicated that the Al oxide layer is modified compared to that of the baseline specimen and that the oxide thickness increases with the number of shots per spot. Finally, the additional thicker oxide on Al alloys is expected to increase the corrosion resistance of the coated Al 2024.

36 MATERIALS SCIENCE↗