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DOE OSTI2017

Achieving Leak Tightness in New Savannah River Site Saltstone Disposal Units - 17454

Saltstone Disposal Unit (SDU) 6 is a new disposal unit at the Department of Energy's Savannah River Site Saltstone Disposal Facility. The Saltstone Facility is part of the site's overarching waste management and disposal system. It receives the low-level waste stream and will immobilize in grout more than 90 percent of the liquid volume generated during treatment of the site's liquid high level waste. SDU-6 is the first in a series of large disposal units to be constructed on site. Its internal diameter and height are 114 m (375 ft) and 13.1 m (43 ft), respectively. It uses a cylindrical wire-wrapped concrete water tank design (AWWA D110, Type I), and at 121 ML (32 Mgal), it is one of the largest structures of its kind in the country. Because of its size, SDU-6's base slab was placed in ten sections. Earlier placed sections restrained newer adjacent sections, resulting in shrinkage cracking. Visible cracks were repaired with epoxy. However, the SDU basemat leaked at less than an estimated 4 L/min rate during its first full-height hydrostatic test (2015). The project baseline was to install a coating system to chemically protect the concrete from the high-pH, high-sulfate Saltstone solutions. The coating was not installed during the first hydrostatic test, and subsequently, an adhered elastomeric liner system was chosen to provide higher assurance of bridging floor cracks and preventing leakage. A robust process was used to select and install a liner that will not only provide chemical protection but also achieve leak tightness, which was successfully demonstrated in a second hydrostatic test late in 2016. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

A statistical representation of bond coating oxidation under environmental barrier coatings

Environmental barrier coatings (EBCs) protect SiC-based ceramic matrix composites (CMCs) in turbine hot sections from high-temperature volatilization in combustion gases. The formation of a SiO 2 thermally grown oxide (TGO) is expected under the EBC after long-term operation. The oxidation resistance of the EBC is understood as a life-limiting factor for the CMC, and this work predicts long-term oxidation behavior under EBCs through a simple statistical approach. Specimens were exposed to 1350°C isothermal conditions for 100-h thermal cycles in flowing steam for up to 1000 h. The EBC morphology, SiO 2 thickness, and SiO 2 cracking behavior were assessed. Using thousands of SiO 2 thickness measurements across many millimeters of the interface, a realistic representation of the entire TGO was captured via a lognormal distribution. The lognormal fit parameters were extrapolated out to 25 000 h to assess the degree of SiO 2 growth, the spread of SiO 2 thicknesses related to the rough oxidizing interface, and percentages of the intermediate bond coating consumed. In conclusion, local interfacial defects from the coating deposition process are identified as local failure points for EBC—CMC systems.

SiO 2↗

DOE OSTI2015

Irradiation performance of AGR-1 high temperature reactor fuel

The AGR-1 experiment contained 72 low-enriched uranium oxide/uranium carbide TRISO coated particle fuel compacts in six capsules irradiated to burnups of 11.2 to 19.6% FIMA, with zero TRISO coating failures detected during the irradiation. The irradiation performance of the fuel including the extent of fission product release and the evolution of kernel and coating microstructures was evaluated based on detailed examination of the irradiation capsules, the fuel compacts, and individual particles. Fractional release of 110m Ag from the fuel compacts was often significant, with capsule-average values ranging from 0.01 to 0.38. Analysis of silver release from individual compacts indicated that it was primarily dependent on fuel temperature history. Europium and strontium were released in small amounts through intact coatings, but were found to be significantly retained in the outer pyrocarbon and compact matrix. The capsule-average fractional release from the compacts was 1 × 10 –4 to 5 × 10 –4 for 154 Eu and 8 × 10 –7 to 3 × 10 –5 for 90 Sr. The average 134 Cs fractional release from compacts was <3 × 10 –6 when all particles maintained intact SiC. An estimated four particles out of 2.98 × 10 5 in the experiment experienced partial cesium release due to SiC failure during the irradiation, driving 134 Cs fractional release in two capsules to approximately 10 –5 . Identification and characterization of these particles has provided unprecedented insight into the nature and causes of SiC coating failure in high-quality TRISO fuel. In general, changes in coating morphology were found to be dominated by the behavior of the buffer and inner pyrolytic carbon (IPyC), and infrequently observed SiC layer damage was usually related to cracks in the IPyC. Palladium attack of the SiC layer was relatively minor, except for the particles that released cesium during irradiation, where SiC corrosion was found adjacent to IPyC cracks. In conclusion, palladium, silver, and uranium were found in the SiC layer of irradiated particles, and characterization of these elements within the SiC microstructure is the subject of ongoing focused study.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

High-temperature all-fiber non-destructive multi-parameter sensing system with consistent performance

A high-temperature all-fiber non-destructive multi-parameter sensing system is developed. The system can operate consistently in a wide range of temperature changes by specially designed active signal generation and detection units. It is capable of monitoring temperature up to 600°C and cracks on metal pipes with an acoustic wave generation unit and an acoustic detection unit. A gold-coated multi-mode fiber is used to deliver a laser pulse for acoustic excitation while minimizing parasitic acoustic signals at high temperature. An in-fiber Fabry–Perot fiber Bragg grating (FP-FBG) is fabricated in another single-mode fiber and bonded to the test object for acoustic detection. The FP-FBG avoids strain redistribution inside the bonder at high temperature to ensure consistent operation. The feasibility of the system for temperature monitoring and crack detection in real-world applications is also demonstrated on an industry-standard P91 pipe.

He, Jiaji (ORCID:0000000165661887)↗

NASA NTRS1998

Creep of Uncoated and Cu-Cr Coated NARloy-Z

Stress rupture creep tests were performed on uncoated and Cu-30vol%Cr coated NARloy-Z copper alloy specimens exposed to air at 482 C to 704 C. The results showed that creep failure in air of unprotected NARloy-Z was precipitated by brittle intergranular surface cracking produced by strain assisted grain boundary oxidation (SAGBO) which in turn caused early onset of tertiary creep. For the protected specimens, the Cu-Cr coating remained adherent throughout the tests and was effective in slowing down the rate of oxygen absorption, particularly at the higher temperatures, by formation of a continuous chromium oxide scale. As the result of reducing oxygen ingress, the coating prevented SAGBO initiated early creep failure, extended creep deformation and increased the creep rupture life of NARloy-Z over the entire 482 C to 704 C test temperature range.

Walter, R. J.↗

DOE OSTI2019

High Moisture Barrier with Synergistic Combination of SiO x and Polyelectrolyte Nanolayers

Abstract The lifespan of most organic electronics, and many types of food, depend on the oxygen and moisture barrier of the packaging materials. Despite exhibiting excellent oxygen barrier and being relatively easy to produce, polyelectrolyte multilayer nanocoatings (PEM) show limited moisture barrier. SiO x thin films can exhibit good moisture barrier, but rigidity that leads to cracking is a challenge for flexible packaging. In this work, layer‐by‐layer assembled PEM coatings are paired with inorganic SiO x to form a three‐layer sandwich‐type moisture barrier. The barrier property of this organic/inorganic/organic structure is an order of magnitude better than any individual component or other combination thereof. This behavior is attributed to the underlying PEM layer smoothing the substrate surface and the top PEM layer eliminating defects in the underlying SiO x . This study provides a new twist in the development of flexible films with exceptional moisture barrier.

Qin, Shuang↗

DOE OSTI2024

Shelf-life of ball-milled catalyst inks for the fabrication of fuel cell electrodes

A major factor driving fuel cell costs is the quantity of precious metal required. Therefore, it is important to understand a timeframe where inks can be reused. Here, in this work, we explore differences between a freshly prepared catalyst ink and one that has been stored for over a year – comparing ink properties, cathode catalyst layer microstructure, and their respective fuel cell performance. Ink studies revealed smaller agglomerate sizes and a decrease in shear viscosity for the aged ink. Longer storage time also results in fewer cracks and a more uniform ionomer distribution, as evidenced by microscopy characterization of rod-coated electrodes. Lastly, polarization curves show improved performance at higher current densities for the electrode prepared from the aged ink. We rationalize such effect in terms of enhanced ionomer adsorption onto the catalyst over time.

08 HYDROGEN↗

DOE OSTI2024

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

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

36 MATERIALS SCIENCE↗

NASA NTRS1990

Micromechanical thermal analysis of interphase region in a titanium aluminide MMC

The high reactivity between the fiber and matrix in silicon carbide/titanium aluminide MMCs leads to the formation of brittle reaction products at the fiber/matrix (F/M) interface. Also, the high thermal expansion coefficient mismatch between the fiber and matrix leads to high tensile residual stresses at the F/M interface, and this can lead to premature cracking during cooldown. One solution to these problems is the use of a metallic fiber coating like Ta which acts as an F/M diffusion barrier and reacts with the matrix to form a beta stabilized compliant layer. A finite element micromechanics analysis was performed to study the effects of Ta and beta interphase layers on the thermal residual stresses during consolidation. A 5-micron-thick beta layer reduced cool-down stresses by 8 percent compared to a 2 percent reduction computed for a Ta layer of the same thickness. Plastic yielding in the Ta was not effective in reducing cool-down stresses. Compliant alpha-2 particles next to the stiffer gamma particles reduced stresses in the gamma particles by less than 2 percent. A simple closed form analysis was developed to calculate thermal residual stresses in a fiber/interphase/matrix system. A 2-micron-thick Ag interphase layer was found to reduce residual stresses by about 11 percent.

Naik, R. A.↗

NASA NTRS1995

Eddy-Current Detection Of Cracks In Reinforced Carbon/Carbon

Investigations of failures of components made of reinforced carbon/carbon show eddy-current flaw-detection techniques applicable to these components. Investigation focused on space shuttle parts, but applicable to other parts made of carbon/carbon materials. Techniques reveal cracks, too small to be detected visually, in carbon/carbon matrix substrates and in silicon carbide coates on substrates. Also reveals delaminations in carbon/carbon matrices. Used to characterize extents and locations of discontinuities in substrates in situations in which ultrasonic techniques and destructive techniques not practical.

Christensen, Scott V.↗

NASA NTRS2005

Application of Eddy Current Techniques for Orbiter Reinforced Carbon-Carbon Structural Health Monitoring

The development and application of advanced nondestructive evaluation techniques for the Reinforced Carbon-Carbon (RCC) components of the Space Shuttle Orbiter Leading Edge Structural Subsystem (LESS) was identified as a crucial step toward returning the shuttle fleet to service. In order to help meet this requirement, eddy current techniques have been developed for application to RCC components. Eddy current technology has been found to be particularly useful for measuring the protective coating thickness over the reinforced carbon-carbon and for the identification of near surface cracking and voids in the RCC matrix. Testing has been performed on as manufactured and flown RCC components with both actual and fabricated defects representing impact and oxidation damage. Encouraging initial results have led to the development of two separate eddy current systems for in-situ RCC inspections in the orbiter processing facility. Each of these systems has undergone blind validation testing on a full scale leading edge panel, and recently transitioned to Kennedy Space Center to be applied as a part of a comprehensive RCC inspection strategy to be performed in the orbiter processing facility after each shuttle flight.

Wincheski, Buzz↗

NASA NTRS2007

High Temperature Materials for Chemical Propulsion Applications

Radiation or passively cooled thrust chambers are used for a variety of chemical propulsion functions including apogee insertion, reaction control for launch vehicles, and primary propulsion for planetary spacecraft. The performance of these thrust chambers is limited by the operating temperature of available materials. Improved oxidation resistance and increased operating temperatures can be achieved with the use of thermal barrier coatings such as zirconium oxide (ZrO2) and hafnium oxide (HfO2). However, previous attempts to include these materials showed cracking and spalling of the oxide layer due to poor bonding. Current research at NASA's Marshall Space Flight Center (MSFC) has generated unique, high temperature material options for in-space thruster designs that are capable of up to 2500 C operating temperatures. The research is focused on fabrication technologies to form low cost Iridium,qF_.henium (Ir/Re) components with a ceramic hot wall created as an integral, functionally graded material (FGM). The goal of this effort is to further de?celop proven technologies for embedding a protective ceramic coating within the Ir/Re liner to form a robust functional gradient material. Current work includes the fabrication and testing of subscale samples to evaluate tensile, creep, thermal cyclic/oxidation, and thermophysical material properties. Larger test articles have also being fabricated and hot-fire tested to demonstrate the materials in prototype thrusters at 1O0 lbf thrust levels.

Elam, Sandra↗

DOE OSTI2019

Comparative In Vitro Evaluation Between Zirconia and Veneer Ceramic Materials Using Different Techniques

Zirconia surface treatment using different techniques could be employed to overcome the delamination issue reported between veneering ceramic materials and the corresponding zirconia core. The study subjected yttria partially stabilized zirconia core material to grinding and sandblasting as a first surface treatment. An airbrush gun spraying technique was used to coat a uniform thin layer of veneering ceramic (IPS e.max Ceram and Noritake Cerabien ZR) on the core materials followed by performing laser scanning as a second surface treatment. The specimens were investigated for surface topography, interface analysis, elemental compositions, phase transformation, and fracture mode patterns using profilometer, SEM, EDS, XRD, and stereomicroscope. The impact of laser scanning on the shear bond strength before and after storage of specimens in artificial saliva was also studied. Transformable tetragonal phase to monoclinic was predominant in sandblasted specimens followed by laser scanning with observation of micro-cracks at interface. The grinding followed by laser scanning yielded satisfactory outcomes in terms of the presence of coating property. The phase transformation was not detected through the latter technique. The technique greatly enhanced the roughness property and bond strength values which might be considered as a reliable application to improve the longevity of fixed dental crowns in load bearing areas.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Surface coating by mechanofusion modulates bulk charging pathways and battery performance of Ni-rich layered cathodes

Ni-rich layered oxides as high-capacity battery cathodes suffer from degradation at high voltages. Here, we utilize a dry surface modification method, mechanofusion (MF), to achieve enhanced battery stability. The simplicity, high yield, and flexibility make it cost-effective and highly attractive for processing at the industrial scale. The underlying mechanisms responsible for performance improvement are unveiled by a systematic study combining multiple probes, e.g., 3D nano-tomography, spectroscopic imaging, in situ synchrotron diffraction, and finite element analysis (FEA). MF affects the bulk crystallography by introducing partially disordered structure, microstrain, and local lattice variation. Furthermore, the crack initiation and propagation pattern during delithiation are regulated and the overall mechanical fracture is reduced after such surface coating. We validate that MF can alter the bulk charging pathways. Such a synergic effect between surface modification and bulk charge distribution is fundamentally important for designing next-generation battery cathode materials.

25 ENERGY STORAGE↗

DOE OSTI2019

Tritium Retention in Hexavalent Chromate-Conversion–Coated Aluminum Alloy

In this work, 6061-T6 aluminum samples were subjected to MIL-DTL-5541F type I, class-3 anodic coatings, where a yellow irradiate finish was achieved. Both chromate-conversion coatings (CCC) and unmodified samples were exposed to DT (PT = 0.51 atm) gas for 24 h at room temperature. Following loading, the samples were subjected to one of two desorption techniques: temperature-programmed desorption, or a surface stripping technique. The results show that chromic-acid anodizing of aluminum dramatically increases the total quantity of tritium retained by the treated surface as compared to unmodified aluminum. X-ray photoelectron spectroscopy and scanning electron microscopy studies of both treated aluminum and unmodified samples indicate that the CCC coating contain significant quantities of hydrated chromium. Using transmission electron microscopy, the surface is shown to have significant cracking and fracturing of the film and leads to a highly grained and porous surface. Such surface defects coupled with the vast quantity of hydration sites are likely reasons for the increased retained tritium inventory observed for CCC samples. Finally, due to the physical and chemical properties of unmodified CCC samples, they are not suitable for use in tritium environments.

36 MATERIALS SCIENCE↗

NASA NTRS1972

Detection of lack of fusion using opaque additives, phase 1

Two major problems in welded aluminum spacecraft structure, reliable nondestructive inspection for incomplete weldment penetration and the rapid oxidation of aluminum surfaces left exposed to the atmosphere are investigated. The approach employed to solve both problems was to employ copper as a coating to prevent oxidation of the aluminum and as an opaque additive in the weldment to enhance X-ray detection in the event of incomplete penetration. Both plasma spray and vacuum vapor deposition techniques were evaluated for depositing the copper. A series of welded panels was made using three thicknesses of vacuum-vapor-deposited copper. All weldments were nondestructively inspected by X-ray, then excised into tensile and bend specimens. Mechanical tests were conducted and all data evaluated. It was determined that the vacuum-vapor-deposited coating was superior to a plasma sprayed coating of the same thickness. The vacuum-vapor-deposited coating was more uniform in thickness, provided complete coverage of the aluminum, and was free of cracks and porosity.

Cook, J. L.↗

NASA NTRS1991

Near-Earth asteroids: Metals occurrence, extraction, and fabrication

Near-earth asteroids occur in three principle types of orbits: Amor, Apollo, and Aten. Amor asteroids make relatively close (within 0.3 AU) approaches to the earth's orbit, but do not actually overlap it. Apollo asteroids spend most of their time outside the earth's orbital path, but at some point of close approach to the sun, they cross the orbit of the earth. Aten asteroids are those whose orbits remain inside the earth's path for the majority of their time, with semi-major axes less than 0.1 AU. Near-earth orbit asteroids include: stones, stony-irons, irons, carbonaceous, and super-carbonaceous. Metals within these asteroids include: iron, nickel, cobalt, the platinum group, aluminum, titanium, and others. Focus is on the extraction of ferrous and platinum group metals from the stony-iron asteroids, and the iron asteroids. Extraction of the metal fraction can be accomplished through the use of tunnel-boring-machines (TBM) in the case of the stony-irons. The metals within the story-iron asteroids occur as dispersed granules, which can be separated from the stony fraction through magnetic and gaseous digestion separation techniques. The metal asteroids are processes by drilling and gaseous digestion or by gaseous digestion alone. Manufacturing of structures, housings, framing networks, pressure vessels, mirrors, and other products is accomplished through the chemical vapor deposition (CVD) of metal coating on advanced composites and on the inside of contour-defining inflatables (CDI). Metal coatings on advanced composites provide: resistance to degradation in the hostile environments of space; superior optical properties; superior heat dissipation; service as wear coatings; and service as evidential coatings. Metal coatings on the inside of CDI produce metal load-bearing products. Fibers such as graphite, kevlar, glass, ceramic, metal, etc., can be incorporated in the metal coatings on the inside of CDI producing metal matrix products which exhibit high strength and resist crack propagation.

Westfall, Richard↗

NASA NTRS1991

Sprayable lightweight ablative coating

An improved lightweight, ablative coating is disclosed that may be spray applied and cured without the development of appreciable shrinkage cracks. The ablative mixture consists essentially of phenolic microballoons, hollow glass spheres, glass fibers, ground cork, a flexibilized resin binder, and an activated colloidal clay.

Simpson, William G.↗