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NASA NTRS2004

Improved BN Coatings on SiC Fibers in SiC Matrices

Modifications of BN-based coatings that are used as interfacial layers between the fibers and matrices of SiCfiber/SiC-matrix composite materials have been investigated to improve the thermomechanical properties of these materials. Such interfacial coating layers, which are also known as interphases (not to be confused with interphase in the biological sense), contribute to strength and fracture toughness of a fiber/matrix composite material by providing for limited amounts of fiber/matrix debonding and sliding to absorb some of the energy that would otherwise contribute to the propagation of cracks. Heretofore, the debonding and sliding have been of a type called inside debonding because they have taken place predominantly on the inside surfaces of the BN layers that is, at the interfaces between the SiC fibers and the interphases. The modifications cause the debonding and sliding to include more of a type, called outside debonding, that takes place at the outside surfaces of the BN layers that is, at the interfaces between the interphases and the matrix (see figure). One of the expected advantages of outside debonding is that unlike in inside debonding, the interphases would remain on the crack-bridging fibers. The interphases thus remaining should afford additional protection against oxidation at high temperature and should delay undesired fiber/fiber fusion and embrittlement of the composite material. A secondary benefit of outside debonding is that the interphase/matrix interfaces could be made more compliant than are the fiber/interphase interfaces, which necessarily incorporate the roughness of the SiC fibers. By properly engineering BN interphase layers to favor outside debonding, it should be possible, not only to delay embrittlement at intermediate temperatures, but also to reduce the effective interfacial shear strength and increase the failure strain and toughness of the composite material. Two techniques have been proposed and partially experimentally verified as candidate means to promote outside debonding in state-of-the-art SiC/SiC composites.

Morscher, Gregory N.↗

DOE OSTI2019

Test Plan for the Third Reirradiation Heating Test of Fuel Particles from AGR 2 Compact 5-4-2

Post irradiation examination (PIE) and high-temperature heating tests of tristructural isotropic (TRISO)-coated fuel particles and compacts from the second Advanced Gas Reactor (AGR) irradiation experiment, AGR 2, are in progress. This test plan describes the reirradiation and subsequent high-temperature testing of loose fuel particles obtained from AGR 2 Compact 5-4-2. To simulate exposed kernels, four of these particles have been cracked at Oak Ridge National Laboratory (ORNL) to produce localized defects that extend through the TRISO layers (outer pyrolytic carbon, silicon carbide [SiC], and inner pyrolytic carbon) while keeping these layers in place and maintaining the shape and integrity of the kernel. To generate short-lived fission products, these particles will be reirradiated in the Neutron Radiography Reactor (NRAD) at the Hot Fuel Examination Facility (HFEF) at the Idaho National Laboratory (INL) Materials and Fuels Complex prior to heating testing in the Fuel Accident Condition Simulator (FACS) furnace at HFEF. FACS testing will be at 1200°C, and fission products released from the reirradiated particles will be measured. The intention of the test is to assess the retention of short-lived fission products I-131 (t1/2 = 8.02 days) and Xe-133 (t1/2 = 5.2 days) in the fuel kernels at high temperatures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Test Plan for the Reirradiation Heating Test of Fuel Particles from AGR 2 Compact 5-4-2

Post irradiation examination (PIE) and high-temperature heating tests of tristructural isotropic (TRISO)-coated fuel particles and compacts from the second Advanced Gas Reactor (AGR) irradiation experiment, AGR 2, are in progress. This test plan describes the reirradiation and subsequent high-temperature testing of loose fuel particles obtained from AGR 2 Compact 5-4-2. To simulate exposed kernels, four of these particles have been cracked at Oak Ridge National Laboratory (ORNL) to produce localized defects that extend through the TRISO layers (outer-pyrolytic carbon [OPyC], silicon carbide [SiC], and inner-pyrolytic carbon [IPyC]) while keeping these layers in-place and maintaining the shape and integrity of the kernel. To generate short-lived fission products, these particles will be reirradiated in the Neutron Radiography (NRAD) reactor prior to heating testing in the Fuel Accident Condition Simulator (FACS) furnace. FACS testing will be at 1600°C, and fission products released from the reirradiated particles will be measured. The intention of the test is to assess the retention of short-lived fission products I-131 (t1/2 = 8.02 days) and Xe-133 (t1/2 = 5.2 days) in the fuel kernels at accident temperatures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

Corrosion resistance of ZrO{sub 2}–TiO{sub 2} nanocomposite multilayer thin films coated on carbon steel in hydrochloric acid solution

This work reports the achievement of preparing of x% zirconia (ZrO{sub 2})–titania (TiO{sub 2}) composite coatings with different ZrO{sub 2} percent on the carbon steel by dipping substrates in sol–gel solutions. The prepared coated samples were investigated by various surface techniques including X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDAX). Open-circuit potential (OCP), potentiodynamic polarization, and electrochemical impedance spectroscopy (EIS) methods were employed to investigate the corrosion resistance of the coated carbon steel substrates in 1.0 M HCl solution at 50 °C. The data showed that, the corrosion protection property is not always proportional to the percent of ZrO{sub 2}. It can be inferred that there is an optimum percent (10%ZrO{sub 2}) for beneficial effects of loading ZrO{sub 2} on the protection efficiency (98.70%), while higher loading percent of ZrO{sub 2} in the sol–gel coating leads to the formation of a fragile film with poor barrier properties. EDAX/SEM suggests that the metal surface was protected through coating with ZrO{sub 2}–TiO{sub 2} composite films. - Highlights: • Sol–gel TiO{sub 2} doped with ZrO{sub 2} films deposited on carbon steel substrate • XRD measurements of x wt.% ZrO{sub 2}–TiO{sub 2} showed the (101) peaks broader than that of TiO{sub 2}. • SEM results proved that, the cracking decreases with the number of layers. • The prepared films can improve the corrosion resistance of the carbon steel substrate. • 10%ZrO{sub 2} loading is the optimal percent for useful effects on the corrosion resistance.

36 MATERIALS SCIENCE↗

NASA NTRS2017

Tutorial on Atomic Oxygen Effects and Contamination

Atomic oxygen is the most predominant specie in low Earth orbit (LEO) and is contained in the upper atmosphere of many other planetary bodies. Formed by photo-dissociation of molecular oxygen, it is highly reactive and energetic enough to break chemical bonds on the surface of many materials and react with them to form either stable or volatile oxides. The extent of the damage for spacecraft depends a lot on how much atomic oxygen arrives at the surface, the energy of the atoms, and the reactivity of the material that is exposed to it. Oxide formation can result in shrinkage, cracking, or erosion which can also result in changes in optical, thermal, or mechanical properties of the materials exposed. The extent of the reaction can be affected by mechanical loading, temperature, and other environmental components such as ultraviolet radiation or charged particles. Atomic oxygen generally causes a surface reaction, but it can scatter under coatings and into crevices causing oxidation much farther into a spacecraft surface or structure than would be expected. Contamination can also affect system performance. Contamination is generally caused by arrival of volatile species that condense on spacecraft surfaces. The volatiles are typically a result of outgassing of materials that are on the spacecraft. Once the volatiles are condensed on a surface, they can then be fixed on the surface by ultraviolet radiation andor atomic oxygen reaction to form stable surface contaminants that can change optical and thermal properties of materials in power systems, thermal systems, and sensors. This tutorial discusses atomic oxygen erosion and contaminate formation, and the effect they have on typical spacecraft materials. Scattering of atomic oxygen, some effects of combined environments and examples of effects of atomic oxygen and contamination on spacecraft systems and components will also be presented.

Earth orbital environments↗

NASA NTRS2018

Atomic Oxygen Environments, Effects, and Mitigation

Oxygen atoms↗

NASA NTRS2021

Micromechanics-based Modeling of Laminated SiC/SiC Ceramic Matrix Composites

The behavior and response of ceramic matrix composites (CMCs), in particular silicon carbide fiber reinforced silicon carbide matrix (SiC/SiC), is affected by many factors such as variation of fiber volume fraction, residual stresses resulting from processing of the composites at high temperature, random microstructures, and the presence of matrix flaws (e.g., voids, pores, cracks etc.) as well as general material nonlinearity and heterogeneity that occurs randomly in a composite. Residual stresses arising from the phase change of constituents are evaluated in this paper and it is shown that they do influence composite strength and need to be properly accounted for. Additionally, the microstructures (location of fiber centers, coating thickness etc.) of advanced CMCs are usually disordered (or random) and fiber diameter and strength typically have a distribution. They rarely resemble the ordered fiber packing (square, rectangular, or hexagonal) that is generally assumed in micromechanics-based models with periodic boundary conditions for computational expediency. These issues raise the question of how should one model such systems effectively? Can an ordered hexagonal packed repeating unit cell (RUC) accurately represent the random microstructure behavior? How many fibers need to be included to enable accurate representation? Clearly, the number of fibers within an RUC must be limited to insure a balance between accuracy and efficiency. NASA’s in-house micromechanics-based code MAC/GMC provides a framework to analyze such RUCs for the overall composite behavior and the FEAMAC computer code provides linkage of MAC/GMC to the commercial FEA code, ABAQUS. The appropriate level of discretization of the RUC as well as the analysis method employed, i.e., Generalized Method of Cells (GMC) or High Fidelity Generalized Method of Cells (HFGMC), is investigated in this paper in the context of a unidirectional as well as a cross-ply laminated CMC. Results including effective composite properties, proportional limit stress (an important design parameter) and fatigue are shown utilizing both GMC as well as HFGMC. Finally, a few multiscale analyses are performed on smooth bar test coupons as well as test coupons with features such as open-hole and double notches using FEAMAC. Best practices and guidance are provided to take these phenomena into account and keep a proper balance between fidelity (accuracy) and efficiency. Following these guidelines can account for important physics of the problem and provide significant advantages when performing large multiscale composite structural analyses.

Ceramic Matrix Composites↗

DOE OSTI2026

Overview of advanced plasma-facing materials testing for Fusion Pilot Plants at DIII-D

Characterization and testing of advanced plasma-facing materials (PFMs) for Fusion Pilot Plants (FPP) is being conducted at the DIII-D National Fusion Facility through the ongoing two-year FPP Candidate Materials Thrust. Year one tested 17 novel materials utilizing the Divertor Materials Evaluation System (DiMES), with samples analyzed pre- and post-experiment via SEM, EDS, and confocal microscopy. Repeatable reference discharges were developed to ensure uniformity between experiments, including a new strike-point rastering scenario to provide more uniform heat/particle flux across DiMES during ELMing H-mode discharges. Various sample geometries and temperatures were used to achieve FPP-relevant conditions, including samples angled 10° towards the incident plasma flux and pre-heating up to 500 °C. The first exposure of liquid lithium (Li) capillary porous structures in a tokamak demonstrated uniform emission of Li vapor and suppression of Li droplets in H-mode when preheated to 350 °C. Dispersoid-strengthened W with 1 wt% TaC, TiC, and ZrC exposed to H-mode showed cracking and dispersoid ejection for all varieties except TiC, providing a clear down-selection. Ultra-high temperature ceramic materials TiB 2 and ZrB 2 showed minimal degradation under L-mode exposure. Silicon carbide (SiC) fiber composites showed arcing along edges, while CVD SiC remained pristine. Atmospheric plasma-sprayed W and SiC coatings endured H-mode exposure without macroscopic delamination; SiC exhibited granular ejection, while W showed increased outgassing. Additional W-based alloys were stress tested in H-mode, including Ni-based W heavy alloys, W f SiC f /W composites, W multi-principle element alloys, and functionally-graded W/SiC, to varying degrees of success.

DIII-D↗

DOE OSTI2021

Directly Probing the Fracture Behavior of Ultrathin Polymeric Films

Understanding fracture mechanics of ultrathin polymeric films is crucial for modern technologies, including semiconductor and coating industries. However, up to now, the fracture behavior of sub-100 nm polymeric thin films is rarely explored due to challenges in handling samples and limited testing methods available. In this work, we report a new testing methodology that can not only visualize the evolution of the local stress distribution through wrinkling patterns and crack propagation during the deformation of ultrathin films but also directly measure their fracture energies. Using ultrathin polystyrene films as a model system, we both experimentally and computationally investigate the effect of the film thickness and molecular weight on their fracture behavior, both of which show a ductile-to-brittle transition. Furthermore, we demonstrate the broad applicability of this testing method in semicrystalline semiconducting polymers. We anticipate our methodology described here could provide new ways of studying the fracture behavior of ultrathin films under confinement.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1982

Mechanisms of deformation and fracture in high temperature low cycle fatigue of Rene 80 and IN 100

Specimens tested for the AGARD strain range partitioning program were investigated. Rene 80 and IN 100 were tested in air and in vacuum; at 871 C, 925 C, and 1000 C; and in the coated and uncoated condition. The specimens exhibited a multiplicity of high-temperature low-cycle fatigue damage. Observations of the various forms of damage were consistent with material and testing conditions and were generally in agreement with previous studies. In every case observations support a contention that failure occurs at a particular combination of crack length and maximum stress. A failure criterion which is applicable in the regime of testing studied is presented. The predictive capabilities of this criterion are straight forward.

Romanoski, G. R., Jr.↗

NASA NTRS1981

A sputtered zirconia primer for improved thermal shock resistance of plasma-sprayed ceramic turbine seals

It is shown that the application of sputtered Y2O3-stabilized ZrO2 (YSZ) primer in plasma-sprayed YSZ ceramic-coated turbine blades results in an improvement, by a factor of 5-6, in the thermal shock life of specimens with a sprayed, porous, Ni-Cr-Al-Y intermediate layer. Species with and without the primer were found to be able to survive 1000 cycles when the intermediate layer was used, but reduced laminar cracking was observed in the specimen with the primer. It is suggested that the sputtered YZS primer-induced properties are due to (1) more effective wetting and adherence of the plasma-sprayed YZS particles to the primer, and (2) the primer's retardation of impinging, molten plasma sprayed particles solidification rates, which result in a less detrimental residual stress distribution.

Bill, R. C.↗

DOE OSTI2018

Exploring the feasibility of crack detection in plate weldments through an interposed layer of viscoelastic material.

Development of new approaches in the nondestructive evaluation of welded steel plates for large naval structures continues to be an area of interest for the DoD and the military complex. In this report we will evaluate an elastic-microwave based detection and imaging method using both numerical finite element (3D FEM) and experimental methods. The evaluation was performed on two test articles that were designed to represent critical structural components with flaws of interest. Details of the materials and the mechanical drawings were provided with the test articles. Flaws, cracks and weld defects have been included in the test articles to determine detection sensitivity and accuracy of the proposed method. Our approach uses a microwave interferometer (MI) to record the scattered response of flaws in the steel plated as it is driven by an incident elastic field. The MI can “see” (penetrate) through the viscoelastic coating to the upper surface of the plate. Out-of-plane displacement amplitudes of 10nm in the frequency range (1kHz to 25kHz) are readily observable, with the key feature being, that the surface bond between the coating and the steel plate are undisturbed. The non-contact aspect of the interferometer allows for large surface regions to be accurately and efficiently scanned in space and time. Spatiotemporal data sets of this kind and specialized wavefield processing provide powerful detection and imaging modalities. From these wavefield data sets, a plate thickness mapping capability has been demonstrated that can detect thickness changes on the order of 0.79 mm (1/32”) with spatial resolution on the order of the spatial sampling rate, 15mm (~5/8”). We have also shown that a topological energy analysis of the wavefield data can detect and locate small flaws, on the order of 5-10 mm (0.025-0.40”) in the welded joint of a 1.5” thick T-plate. As before, these results are obtained through a 2” thick viscoelastic coating without altering the integrity of coating or the coating bond. These results show that we are detecting and locating damage (flaws) in the plate that are much smaller than the wavelength of the propagating guided modes. Classical scattering theory places a (λ/2) resolution limit on the detectability of flaws in terms of the incident field [22], however, since the spatial resolution of the scanned region is much smaller, (Δx=Δy=15mm) and the inherent natural focusing of the time reversal operation, we are able to detect smaller flaws on the order of (λ/10). It is important to realize that we are not imaging the flaw but detecting and localizing a difference between a reference (pristine) sample and the measured (damaged) sample, relative to a spatial grid on the surface. The current scan resolution is 15mm x 15mm. At present we cannot expect to resolve individual flaws within a grid space only their cumulative effect. Even with the current limitations, this imaging approach appears to be a promising alternative to current methods where the coating layer is removed.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Novel Accident-Tolerant Fuel Meat and Cladding

A novel accident-tolerant fuel meat and cladding are here proposed. The fuel meat design incorporates annular fuel with inserts and discs that are fabricated from a material having high thermal conductivity, for example niobium. The inserts are rods or tubes. Discs separate the fuel pellets. Using the BISON fuel performance code it was found that the peak fuel temperature can be lowered by more than 600 degrees C for one set of conditions with niobium metal as the thermal conductor. In addition to improved safety margin, several advantages are expected from the lower temperature such as decreased fission gas release and fuel cracking. Advantages and disadvantages are discussed. An enrichment of only 7.5% fully compensates the lost reactivity of the displaced UO2. Slightly higher enrichments, such as 9%, allow uprates and increased burnups to offset the initial costs for retooling. The design has applications for fast reactors and transuranic burning, which may accelerate its development. A zirconium silicide coating is also described for accident tolerant applications. A self-limiting degradation behavior for this coating is expected to produce a glassy, self-healing layer that becomes more protective at elevated temperature, with some similarities to MoSi2 and other silicides. Both the fuel and coating may benefit from the existing technology infrastructure and the associated wide expertise for a more rapid development in comparison to other, more novel fuels and cladding.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2007

Triboluminescent Materials for Smart Optical Damage Sensors for Space Applications

Triboluminescence is light that is produced by pressure, friction or mechanical shock. New composite materials are constantly being reengi neered in an effort to make lightweight spacecrafts for various NASA missions. For these materials there is interest in monitoring the con dition of the composite in real time to detect any delamination or cr acking due to damage, fatigue or external forces. Methods of periodic inspection of composite structures for mechanical damage such as ult rasonic testing are rather mature. However, there is a need to develop a new technique of damage detection for composites, which could dete ct cracking or delamination from any desired location within a materi al structure in real time. This could provide a valuable tool in the confident use of composite materials for various space applications. Recently, triboluminnescent materials have been proposed as smart sen sors of structural damage. To sense the damage, these materials can b e epoxy bonded or coated in a polymer matrix or embedded in a composi te host structure. When the damage or fracture takes place in the hos t structure, it will lead to the fracture of triboluminescent crystal s resulting in a light emission. This will warn, in real time, that a structural damage has occurred. The triboluminescent emission of the candidate phosphor has to be sufficiently bright, so that the light signal reaching from the point of fracture to the detector through a fiber optic cable is sufficiently strong to be detected. There are a large number of triboluminescent materials, but few satisfy the above criterion. Authors have synthesized a Eu based organic material know n as Europium tetrakis (dibenzoylmethide) triethylammonium .(EuD(sub 4)TEA), one of the bright triboluminescent materials, which is a pote ntial candidate for application as a damage sensor and could be made into a wireless sensor with the addition of microchip, antenna and el ectronics. Preliminary results on the synthesis and characterization of this material shall be presented.

Aggarwal, Mohan D.↗

NASA NTRS1983

Fracture behavior of unidirectional boron/aluminum composite laminates

An experiment was conducted to verify the results of mathematical models which predict the stresses and displacements of fibers and the amount of damage growth in a center-notched lamina as a function of the applied remote stress and the matrix and fiber material properties. A brittle lacquer coating was used to detect the yielding in the matrix while X-ray techniques were used to determine the number of broken fibers in the laminate. The notched strengths and the amounts of damage found in the specimens agree well with those predicted by the mathematical model. It is shown that the amount of damage and the crack opening displacement does not depend strongly on the number of plies in the laminate for a given notch width. By heat-treating certain laminates to increase the yield stress of the alumina matrix, the effect of different matrix properties on the fracture behavior was investigated. The stronger matrix is shown to weaken the notched laminate by decreasing the amount of matrix damage, thereby making the laminate more notch sensitive.

Goree, J. G.↗

NASA NTRS1982

Creep of plasma-sprayed-ZrO2 thermal-barrier coatings

Specimens of plasma-sprayed-zirconia thermal-barrier coatings with three different porosities and different initial particle sizes were deformed in compression at initial loads of 6900, 13,800, and 24,100 kPa (1000, 2000, and 3500 psi) and temperatures of 1100, 1250, and 1400 C. The coatings were stabilized with lime, MgO, and two different concentrations of Y2O3. Creep began as soon as the load was applied and continued at a constantly decreasing rate until the load was removed. Temperature and stabilization had a pronounced effect on creep rate while the stress, particle size, and porosity had a lesser effect. Creep deformation was due to cracking and particle sliding.

Firestone, R. F.↗

DOE OSTI2015

Micro-wrinkling and delamination-induced buckling of stretchable electronic structures

This paper presents the results of experimental and theoretical/computational micro-wrinkles and buckling on the surfaces of stretchable poly-dimethylsiloxane (PDMS) coated with nano-scale Gold (Au) layers. The wrinkles and buckles are formed by the unloading of pre-stretched PDMS/Au structure after the evaporation of nano-scale Au layers. They are then characterized using atomic force microscopy and scanning electron microscopy. The critical stresses required for wrinkling and buckling are analyzed using analytical models. The possible interfacial cracking that can occur along with film buckling is also studied using finite element simulations of the interfacial crack growth. The implications of the results are discussed for potential applications of micro-wrinkles and micro-buckles in stretchable electronic structures and biomedical devices.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2021

Multiscale operando X-ray investigations provide insights into electro-chemo-mechanical behavior of lithium intercalation cathodes

The electrochemical performance and cycle life of lithium-ion batteries (LIBs) depend on the electrochemical, chemical, and mechanical behavior of electrodes and electrolytes. Despite extensive studies conducted previously, challenges exist to decouple these behaviors, capture the evolution of electro-chemo-mechanical behavior in realistic conditions, and correlate atomic-scale stress evolution to micro-scale bulk mechanical degradation. Here, we report multiscale operando techniques to investigate polydisperse battery electrodes by integrating volume-averaged quantitative synchrotron X-ray scattering with high-resolution transmission X-ray microscopy (TXM). The former provides us information spanning a wide spatial range, from Angstrom-level atomic structures to micrometer-level particle scales, while the latter provides time-resolved 2D images of the particles during cycling. The complementarity of the two operando techniques is demonstrated by an over-lithiation test of LiCoO 2 electrodes, where particles crack and eventually pulverize. Additionally, the techniques are applied to study LiCoO 2 cycling stability from 3.0 V to 4.5 V. Operando X-ray scattering result shows nanometer-scale features keep forming in LiCoO 2 electrodes during cycling, resulting in an increased projected area observed by the TXM experiment. The formation of such features is inhibited by a polymer coating on the electrode, leading to vastly improved cycling stability. The polymer coating alleviates LiCoO 2 surface deterioration, reduces side product generation, and inhibits LiCoO 2 particles volume expansion during the cycling test. These operando multimodal X-ray techniques presented herein thus offer a novel, multiscale diagnostic modality for studying existing and emerging battery materials, aiding the development of next-generation LIBs.

25 ENERGY STORAGE↗