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All sources NASA NTRS DOE OSTI

DOE OSTI2020

Strongly adhesive dry transfer technique for van der Waals heterostructure

That one can stack van der Waals materials with atomically sharp interfaces has provided a new material platform of constructing heterostructures. The technical challenge of mechanical stacking is picking up the exfoliated atomically thin materials after mechanical exfoliation without chemical and mechanical degradation. Chemically inert hexagonal boron nitride (hBN) has been widely used for encapsulating and picking up vdW materials. However, due to the relatively weak adhesion of hBN, assembling vdW heterostructures based on hBN has been limited. Here, we report a new dry transfer technique. We used two vdW semiconductors (ZnPS 3 and CrPS 4 ) to pick up and encapsulate layers for vdW heterostructures, which otherwise are known to be hard to fabricate. By combining with optimized polycaprolactone (PCL) providing strong adhesion, we demonstrated various vertical heterostructure devices, including quasi-2D superconducting NbSe 2 Josephson junctions with atomically clean interface. The versatility of the PCL-based vdW stacking method provides a new route for assembling complex 2D vdW materials without interfacial degradation.

36 MATERIALS SCIENCE↗

NASA NTRS2017

The MISSE 7 Flexural Stress Effects Experiment After 1.5 Years of Wake Space Exposure

Low Earth orbit space environment conditions, including ultraviolet radiation, thermal cycling, and atomic oxygen exposure, can cause degradation of exterior spacecraft materials over time. Radiation and thermal exposure often results in bond- breaking and embrittlement of polymers, reducing mechanical strength and structural integrity. An experiment called the Flexural Stress Effects Experiment (FSEE) was flown with the objective of determining the role of space environmental exposure on the degradation of polymers under flexural stress. The FSEE samples were flown in the wake orientation on the exterior of International Space Station for 1.5 years. Twenty-four samples were flown: 12 bent over a 0.375 in. mandrel and 12 were over a 0.25 in. mandrel. This was designed to simulate flight configurations of insulation blankets on spacecraft. The samples consisted of assorted polyimide and fluorinated polymers with various coatings. Half the samples were designated for bend testing and the other half will be tensile tested. A non-standard bend-test procedure was designed to determine the surface strain at which embrittled polymers crack. All ten samples designated for bend testing have been tested. None of the control samples' polymers cracked, even under surface strains up to 19.7%, although one coating cracked. Of the ten flight samples tested, seven show increased embrittlement through bend-test induced cracking at surface strains from 0.70%to 11.73%. These results show that most of the tested polymers are embrittled due to space exposure, when compared to their control samples. Determination of the extent of space induced embrittlement of polymers is important for designing durable spacecraft.

Snow, Kate E.↗

NASA NTRS1994

Lamb Wave Response of Fatigued Composite Samples

Composite materials are being more widely used today by aerospace, automotive, sports equipment, and a number of other commercial industries because of their advantages over conventional metals. Composites have a high strength-to-weight ratio and can be constructed to meet specific design needs. Composite structures are already in use in secondary parts of the Douglas MD-11 and are planned to be used in the new MD-12X. Plans also exist for their use in primary and secondary structures on the Boeing 777. Douglas proposed MD-XX may also incorporate composite materials into primary structures such as the wings and tail. Use of composites in these structures offers weight savings, corrosion resistance, and improved aerodynamics. Additionally, composites have been used to repair cracks in many B-1Bs where traditional repair techniques were not very effective. Plans have also been made to reinforce all of the remaining B-1s with composite materials. Verification of the structural integrity of composite components is needed to insure safe operation of these aerospace vehicles. One aspect of the use of these composites is their response to fatigue. To track this progression of fatigue in aerospace structures, a convenient method to nondestructively monitor this damage needs to be developed. Traditional NDE techniques used on metals are not easily adaptable to composites due to the inhomogeneous and anisotropic nature of these materials. Finding an effective means of nondestructively monitoring fatigue damage is extremely important to the safety and reliability of such structures. Lamb waves offer one method of evaluating these composite materials. As a material is fatigued, the modulus degrades. Since the Lamb wave velocity can be related to the modulus of the material, an effective tool can be developed to monitor fatigue damage in composites by measuring the velocity of these waves. In this work, preliminary studies have been conducted which monitor fatigue damage in composite samples using strain gage measurements as well as Lamb wave velocity measurements. A description of the test samples is followed by the results of two different measurements of Lamb wave velocity. The first technique is a contact measurement done at a single frequency, while the second involves an immersion study of Lamb waves in which dispersion curves are obtained. The results of the Lamb wave monitoring of fatigue damage is compared to the damage progression measured by strain gages. The final section discusses the results and conclusions.

Seale, Michael↗

DOE OSTI2026

Oxide nucleation via threshold-driven volume instability in Ni oxidation

Oxide nucleation dictates the onset of metal oxidation, yet the atomistic pathways bridging initial oxygen adsorption to bulk phase transformation remain elusive. Here, we utilize in-situ atomic-resolution imaging to directly capture the nucleation of nickel oxide, revealing a threshold-driven, cooperative transformation of Ni into NiO. Our observations identify a distinct incubation period during which oxygen progressively accumulates in subsurface layers. Once a critical concentration and penetration depth are reached, a collective lattice reconfiguration is triggered, abruptly converting multiple Ni layers into NiO. Atomistic simulations corroborate this mechanism, identifying a cooperative lattice instability induced by subsurface oxygen saturation. These results establish subsurface oxygen incorporation as the missing mechanistic link between surface adsorption and three-dimensional oxide formation, providing an atomistic framework to understand and control reactive phase transformations in materials synthesis, catalysis, and degradation.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Kinetically Dormant Ni‐Rich Layered Cathode During High‐Voltage Operation

Abstract The degradation of Ni‐rich cathodes during long‐term operation at high voltage has garnered significant attention from both academia and industry. Despite many post‐mortem qualitative structural analyses, precise quantification of their individual and coupling contributions to the overall capacity degradation remains challenging. Here, by leveraging multiscale synchrotron X‐ray probes, electron microscopy, and post‐galvanostatic intermittent titration technique, the thermodynamically irreversible and kinetically reversible capacity loss is successfully deconvoluted in a polycrystalline LiNi 0.83 Mn 0.1 Co 0.07 O 2 cathode during long‐term charge/discharge cycling in full cell configuration. Contradicting the dramatic capacity loss, the layered structure remains highly alive even after 1000 cycles at 4.6 V while undergoing a three‐order of magnitude reduction in the mass transfer kinetics, leading to almost fully recoverable capacity under kinetic‐free conditions. Such kinetic dormant behavior after cycling is not simply ascribed to poor chemical diffusion by reconstructed cathode surface but highly synchronizes with the lattice strain evolution stemming from the structural heterogeneity between deeply delithiated layered and degraded rock‐salt phases at high voltage. These findings deepen the degradation mechanism of high‐voltage cathodes to achieve long‐cycling and fast‐charging performance.

36 MATERIALS SCIENCE↗

NASA NTRS2010

Formula for the Removal and Remediation of Polychlorinated Biphenyls in Painted Structures

An activated metal treatment system (AMTS) removes and destroys polychlorinated biphenyls (PCBs) found in painted structures or within the binding or caulking material on structures. It may be applied using a "paint-on and wipe-off" process that leaves the structure PCB-free and virtually unaltered in physical form. AMTS is used in conjunction with a solvent solution capable of donating hydrogen atoms. AMTS as a treatment technology has two functions: first, to extract PCBs from the material, and second, to degrade the extracted PCBs. The process for removing PCBs from structures is accomplished as an independent step to the degradation process. The goal is to extract the PCBs out of the paint, without destroying the paint, and to partition the PCBs into an environmentally friendly solvent. The research to date indicates this can be accomplished within the first 24 hours of AMTS contact with the paint. PCBs are extremely hydrophobic and prefer to be in the AMTS over the hardened paint or binder material. The solvent selected must be used to open, but not to destroy, the paint s polymeric lattice structure, allowing pathways for PCB movement out of the paint and into the solvent. A number of solvent systems were tested and are available for use within the AMTS. The second process of the AMTS is the degradation or dehalogenation of the PCBs. The solvent selection for this process is limited to solvents that are capable of donating a hydrogen atom to the PCB structure. Additional AMTS formulation properties that must be addressed for each site-specific application include viscosity and stability. The AMTS must be thick enough to remain where it is applied. Several thickening agents have been tested. Adding a stabilizing agent ensures that the AMTS will not evaporate and leave unprotected, activated metal exposed. During AMTS formulation testing, a number of reagents were evaluated to ensure the rate of dehalogenation was not inhibited by its addition to the system.

Quinn, Jacqueline↗

NASA NTRS1984

Nonlinear analysis for high-temperature multilayered fiber composite structures

A unique upward-integrated top-down-structured approach is presented for nonlinear analysis of high-temperature multilayered fiber composite structures. Based on this approach, a special purpose computer code was developed (nonlinear COBSTRAN) which is specifically tailored for the nonlinear analysis of tungsten-fiber-reinforced superalloy (TFRS) composite turbine blade/vane components of gas turbine engines. Special features of this computational capability include accounting of; micro- and macro-heterogeneity, nonlinear (stess-temperature-time dependent) and anisotropic material behavior, and fiber degradation. A demonstration problem is presented to mainfest the utility of the upward-integrated top-down-structured approach, in general, and to illustrate the present capability represented by the nonlinear COBSTRAN code. Preliminary results indicate that nonlinear COBSTRAN provides the means for relating the local nonlinear and anisotropic material behavior of the composite constituents to the global response of the turbine blade/vane structure.

Hopkins, D. A.↗

DOE OSTI2022

Multi-Modal Characterization of Nuclear Fuels and Materials at the Idaho National Laboratory Materials & Fuels Complex

The Idaho National Laboratory (INL) leads cutting-edge research pertaining to the advancement of nuclear reactor technologies, including nuclear fuels and materials. The INL Irradiated Materials Characterization Laboratory (IMCL), Electron Microscopy Laboratory (EML), and future Sample Preparation Laboratory (SPL) are available to the nuclear research community to assess the behavior of nuclear fuels and materials, efficiently and comprehensively characterizing from the engineering to atomistic scale. The IMCL is a unique, 12,000-square-foot facility located at the INL Materials and Fuels Complex designed for analysis of irradiated materials. The facility operates advanced characterization instruments that are sensitive to vibration, temperature, and electromagnetic interference in modular radiological shielding and confinement systems, granting researchers the ability to assess the microstructural, chemical, mechanical and thermophysical properties of nuclear materials, especially irradiated fuels. The EML is dedicated to advanced characterization of materials with optical and electron microscopy tools, including scanning electron microscopy/focused-ion beam (SEM/FIB) and transmission electron microscopy (TEM). Upon construction, the SPL will be a 3 story, 49,000 sq. ft facility, that is the most modern reactor structural materials testing and analysis facility in the world, designed to investigate reactor structural materials in support of life-extension programs and development of advanced reactor concepts, including mechanical testing and advanced characterization capabilities. This presentation will showcase some of the main capabilities available at both IMCL, EML, and SPL, specifically illustrating how these characterization techniques are incorporated into multi-modal characterization work scopes to elucidate the degradation of nuclear structural materials and irradiated fuels.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Thermal stability of filler‐based ethylene/vinyl acetate/vinyl alcohol terpolymer in nitroplasticizer oxidative environment

Abstract To study the thermal stability of ethylene/vinyl acetate/vinyl alcohol (EVA‐OH) composite with filler particles, systematic thermogravimetric analysis (TGA) investigation was conducted in both nonisothermal and isothermal modes. The effect of polymer concentration on the aging behavior of EVA‐OH was investigated in the nitroplasticizer (NP) environment. Fourier transform infrared spectroscopy was used to probe chemical structural changes in the EVA‐OH polymer before and after thermal aging. The results suggest that filler addition accelerates the rate of NP exudation out of the EVA‐OH composites and deteriorates the thermal stability of NP at moderate temperatures (up to 70°C). The degradation of NP, in turn, accelerates the degradation of EVA‐OH polymer in its composite form through oxidation and hydrolysis indicating the importance of antioxidants in such phase blends.

36 MATERIALS SCIENCE↗

DOE OSTI2025

THE DESIGN OF RADIAL HONEYCOMB LATTICES FOR IMPACT ENERGY ABSORPTION IN RADIOACTIVE MATERIALS PACKAGES

In this research we present a variation on the corrugation technique of honeycomb lattices, for cylindrical honeycombs, making them much easier to design for impact energy absorption in radioactive materials packages. This variation, termed radial honeycomb lattices, eliminates the residual strain and saddle effect. The use of honeycomb lattices provides advantages over the typically used foams. While foams are effective at absorbing impact energy, they can burn, their material properties are difficult to control, they can degrade over time, and procurement of raw materials can be dependent on timing of manufacturer batch runs. While the weaknesses of foam are strengths for honeycomb lattices, lattices have a different set of problems. Typically, when cylindrical honeycomb lattices are manufactured, they are manufactured flat, wrapped around a mandrel of the desired radius, and then brazed. This approach introduces residual strains, resulting in the saddle effect, which limits both the radial thickness and cylinder length. The radial honeycomb lattice approach presented here makes the design of thicker and longer cylinder honeycombs possible. To address these issues, we propose a honeycomb lattice which changes in cross-section from the inner to the outer radius of the cylinder. This causes the lattice to automatically wrap into a cylinder as it exits the corrugating gears. The theoretically bounding case, of a square cross-section at the inner radius, transitioning through a hexagon, to a diamond cross-section at the outer radius, results in a maximum thickness of approximately 41% of the inner radius. Full mathematical derivations, implemented in computer code, allow for the design of an entire radial honeycomb lattice, including the corrugating gears. To accomplish this only the radial thickness, inner cross-section shape, cell size, and nominal gear radius need to be specified, making the design of these lattices very efficient. Radial honeycomb lattice prototypes have demonstrated that the honeycomb does indeed wrap into a cylinder as intended, without the saddle effect, and can therefore be used to create thick-walled cylinders of any length. These design improvements make cylindrical honeycomb lattices much more accessible as a design element for radioactive materials packages

Johnson, William R. [Savannah River National Labor↗

DOE OSTI2020

Effect of ATF Cr-coated-Zircaloy on BWR In-vessel Accident Progression during a Station Blackout

The deposition of protective coatings on nuclear fuel cladding has been considered as a near-term Accident Tolerant Fuel (ATF) concept that will reduce the high-temperature oxidation rate and enhance accident tolerance of the cladding while providing additional benefits during normal and transient. In this study, the performance of the proposed ATF concept of Cr-coated-Zircaloy is assessed using a generic Boiling Water Reactor MELCOR plant model considering a Short-term Station Blackout (STSBO) scenario. Simulation results indicate that the use of Cr-coated-Zircaloy as cladding and canister material mitigates the core degradation process as compared to the traditional Zircaloy cladding and canister design. The onset of fuel degradation and collapse is delayed by over thirty minutes, and the extent of fuel degradation is reduced. Specifically, the gross in-vessel hydrogen generation decreased by almost a factor of three. Although the eutectic reaction between Cr-coating and Zircaloy could cause an early failure of the coating, the improvement in the delay of fuel degradation is still notable. In addition, a thicker coating is found helpful to obtain additional coping time and to decrease hydrogen generation. In addition to the eutectic formation that may compromise Cr-coated Zr, a different failure mode is identified for the Cr-coated-Zr when compared to Zircaloy; i.e., a complete melt of base material leads to component collapse before the coating is oxidized and consumed. These findings can help the industry focus on productive areas of research and development for accident-tolerant fuel concepts and enhancement of core safety margins.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

NASA NTRS1978

Performance degradation mechanisms and modes in terrestrial photovoltaic arrays and technology for their diagnosis

Accelerated life-prediction test methodologies have been developed for the validation of a 20-year service life for low-cost photovoltaic arrays. Array failure modes, relevant materials property changes, and primary degradation mechanisms are discussed as a prerequisite to identifying suitable measurement techniques and instruments. Measurements must provide sufficient confidence to permit selection among alternative designs and materials and to stimulate widespread deployment of such arrays. Furthermore, the diversity of candidate materials and designs, and the variety of potential environmental stress combinations, degradation mechanisms and failure modes require that combinations of measurement techniques be identified which are suitable for the characterization of various encapsulation system-cell structure-environment combinations.

Noel, G. T.↗

NASA NTRS2014

X-Ray Absorption near Edge Structure Spectroscopic Study of Hayabusa Category 3 Carbonaceous Particles

Analyses with a scanning transmission x-ray microscope (STXM) using x-ray absorption near edge structure (XANES) spectroscopy were applied for the molecular characterization of two kinds of carbonaceous particles of unknown origin, termed category 3, which were collected from the Hayabusa spacecraft sample catcher. Carbon-XANES spectra of the category 3 particles displayed typical spectral patterns of heterogeneous organic macromolecules; peaks corresponding to aromatic/olefinic carbon, heterocyclic nitrogen and/or nitrile, and carboxyl carbon were all detected. Nitrogen-XANES spectra of the particles showed the presence of N-functional groups such as imine, nitrile, aromatic nitrogen, amide, pyrrole, and amine. An oxygen-XANES spectrum of one of the particles showed a ketone group. Differences in carbon- and nitrogen-XANES spectra of the category 3 particles before and after transmission electron microscopic (TEM) observations were observed, which demonstrates that the carbonaceous materials are electron beam sensitive. Calcium-XANES spectroscopy and elemental contrast mapping identified a calcium carbonate grain from one of the category 3 particles. No fluorine-containing molecular species were detected in fluorine-XANES spectra of the particles. The organic macromolecular features of the category 3 particles were distinct from commercial and/or biological ‘fresh (non-degraded)’ polymers, but the category 3 molecular features could possibly reflect degradation of contaminant polymer materials or polymer materials used on the Hayabusa spacecraft. However, an extraterrestrial origin for these materials cannot currently be ruled out.

Asteroides↗

DOE OSTI2025

Evaluating Autoxidation Radical Scavengers and Additives to Enhance Aminopolymer Sorbent Stability

Solid amine sorbents have shown promise in the removal of ultradilute CO 2 from the atmosphere. Despite being a promising candidate material type for this application, these sorbents are prone to degradation during long-term exposure to environmental components such as CO 2 , O 2 , and H 2 O, with amine oxidation being a particularly challenging problem. In this study, we investigate the potency of different radical scavengers and additives in mitigating the degradation of a model poly- (ethylenimine) (PEI)/Al 2 O 3 sorbent under direct air capture (DAC)-relevant conditions. The results reveal that a 4,4′-bis(α,α- dimethylbenzyl)diphenylamine (BDDPA)-incorporated PEI/Al 2 O 3 sorbent showed the most resistance toward oxidative degradation at varying exposure times and BDDPA loadings under CO 2 -free air (21% O 2 /balance N 2 ) at 120 °C. Interestingly, under humid (∼43% relative humidity (RH) at 26 °C) and dry 0.04% CO 2 -air, the BDDPA/PEI/Al 2 O 3 sorbent showed enhanced sorbent stability both at 70 and 120 °C after 4.5 h of exposure. Under humid CO 2 -free air, at 120 °C, the antioxidant performance slightly declined (in comparison to the dry CO 2 -free air condition) but displayed a much higher stability than the pristine sorbent. Overall, the ability of BDDPA to inhibit sorbent degradation under dry and humid, CO 2 -free and CO 2 -containing (0.04%) air at intermediate (70 °C) and elevated (120 °C) temperatures is promising in prolonging sorbent stability and underscores the importance of performing accelerated oxidation studies in the presence of all species that are expected to be present in DAC processes to identify suitable stabilization treatments for sorbent materials.

36 MATERIALS SCIENCE↗

DOE OSTI2021

BACKFLIP: Identification of Materials and Changes Upon Aging of Emerging Fluoropolymer-Free and Industry-Benchmark PV Backsheets

Extending lifetimes of photovoltaic (PV) modules and decreasing manufacturing and decommissioning costs are motivating research of novel PV module backsheet materials. Backsheet integrity is critical to the safety and performance of a PV module, however, the polymeric materials are often vulnerable to environmental degradation. The long-term durability of emerging polyolefin (PO) materials is being examined to inform regarding the possible replacement of laminated backsheets containing polyethylene terephthalate (PET) cores and fluoropolymer protective inner/outer layers. This study compares traditional PET-based backsheets with novel, co-extruded, and recyclable PO-based backsheets after being subjected to hygrometric and UV photolytic accelerated weathering. A large set of characterization methods will compare physical, chemical, structural, mechanical, and insulating properties of these backsheets and the resulting mini-module (MiMo) PV performances. The study of chemical composition, glass- and phase-transition temperatures, degree of crystallinity, and crystalline structure are described here.

mini-module↗

DOE OSTI2022

Bonded Interfaces for High-Temperature Power Electronics

Wide-bandgap devices have pushed the operational limit of semiconductor devices in automotive power electronics packages to higher temperatures (>200 degrees C). While a higher efficiency can be achieved through the use of wide-bandgap devices, the entire package must be re-designed with components that can withstand the higher temperature limits. Sintered silver and transient liquid phase bonds are potential candidates as bonded materials for use in higher temperatures however, the underlying mechanics of deformation under thermal loads and the resulting failure mechanisms in these materials are not well understood. Furthermore, thermomechanical modeling plays a key role in understanding the degradation behavior of bonded interface materials and for design optimization of power electronics packages.

ADVANCED PROPULSION SYSTEMS,DIRECT ENERGY CONVERSI↗

NASA NTRS1983

Metallurgical studies of NITRONIC 40 with reference to its use for cryogenic wind tunnel models

The characterstics of NITRONIC 40 were investigated in connection with its use in cryogenic wind tunnel models. In particular, the effects of carbide and sigma-phase precipitation resulting from heat treatment and the presence of delta ferrite were evaluated in relation to their effects on mechanical properties and the potential consequences of such degradation. Methods were examined for desensitizing the material and for possible removal of delta ferrite as a means of restoring the material to its advertised properties. It was found that heat treatment followed by cryogenic quenching is a technique capable of desensitizing NITRONIC 40. However, it was concluded that it is extremely difficult, if not impossible, to remove the delta ferrite from the existing stock of material. Furthermore, heat treatments for removing delta ferrite have to take place at temperatures that cause very large grain growth. The implications of using the degraded NITRONIC 40 material for cryogenic model testing were reviewed, and recommendations were submitted with regard to the acceptability of the material. The experience gained from the study of NITRONIC 40 clearly identifies the need to implement a policy for purchasing top-quality materials for cryogenic wind tunnel model applications.

Wigley, D. A.↗

NASA NTRS2018

Application of PoF Based Virtual Qualification Methods for Reliability Assessment of Mission Critical PCBs

Reliability is the ability of a product to perform the function for which it was intended for a specified period of time (or cycles) for a given set of life cycle conditions. In today's compressed mission development cycles where designing, building and testing the physical models has to occur in a matter of months not years, Projects don't have the luxury of iteratively building and testing those models. Physics of failure (PoF) is an engineering-based approach to reliability that begins with an understanding of materials, processes, physical interactions, degradation and failure mechanisms, as well as identifying failure models. The PoF approach uses modeling and simulation to qualify a design and manufacturing process, with the ultimate intent of eliminating failures early in the design process by addressing the root cause. The physics-of-failure analysis proactively incorporates reliability into the design process by establishing a scientific basis for evaluating new materials, structures and technologies. Virtual physics-of-failure modeling allows engineers to determine if new technological node can be added to an existing system. This presentation will illustrate an application of a PoF based tool during the initial phases of a printed circuit board assembly development and how the NASA GSFC team was able to dynamically study the effects of electronics parts and printed circuit board material configuration changes under simulated thermal and vibrational stresses

Electronics packaging↗